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3,400 | 14,269,582 | 1,741 | Certain example embodiments relate to frit materials that have an improved IR absorption property. Certain examples relate to frit materials that substantially melt in about 3 minutes at a temperature of about 525° C. Certain examples relate to a method of making an edge seal by using IR energy. Certain examples relate to adjusting the IR energy applied to a frit material to form an edge seal. Certain examples also relate to making a VIG unit by applying IR energy and adjusting the amount of IR energy over multiple periods of time, e.g., in an oscillating manner. | 1-24. (canceled) 25. A method of making an edge seal for a VIG window unit, the method comprising:
applying a first IR energy to a frit material for a first predetermined period of time, wherein the fit material along with a plurality of spacers are located between first and second substrates, wherein the frit material comprises metal oxides in amounts sufficient to absorb at least 80% of infrared (IR) energy having a wavelength of 1100-2100 nm; after applying the first IR energy, applying a second IR energy from at least one IR emitter to the frit material for a second predetermined period of time; after applying the second IR energy, applying another IR energy to the frit material for a third predetermined period of time so as increase the temperature of the frit material compared to the temperature of the frit material resulting from the second IR energy; and after applying the another IR energy, cooling and/or allowing the frit material to cool over a fourth period of time in making the VIG window unit. | Certain example embodiments relate to frit materials that have an improved IR absorption property. Certain examples relate to frit materials that substantially melt in about 3 minutes at a temperature of about 525° C. Certain examples relate to a method of making an edge seal by using IR energy. Certain examples relate to adjusting the IR energy applied to a frit material to form an edge seal. Certain examples also relate to making a VIG unit by applying IR energy and adjusting the amount of IR energy over multiple periods of time, e.g., in an oscillating manner.1-24. (canceled) 25. A method of making an edge seal for a VIG window unit, the method comprising:
applying a first IR energy to a frit material for a first predetermined period of time, wherein the fit material along with a plurality of spacers are located between first and second substrates, wherein the frit material comprises metal oxides in amounts sufficient to absorb at least 80% of infrared (IR) energy having a wavelength of 1100-2100 nm; after applying the first IR energy, applying a second IR energy from at least one IR emitter to the frit material for a second predetermined period of time; after applying the second IR energy, applying another IR energy to the frit material for a third predetermined period of time so as increase the temperature of the frit material compared to the temperature of the frit material resulting from the second IR energy; and after applying the another IR energy, cooling and/or allowing the frit material to cool over a fourth period of time in making the VIG window unit. | 1,700 |
3,401 | 15,222,254 | 1,764 | A polyamide resin composition and a molded article manufactured using the same. The polyamide resin composition includes: a base resin comprising an aliphatic polyamide resin having a terminal amine group concentration of about 0.1 μeq/g to about 45 μeq/g and including a repeat unit represented by the following Formula 1 wherein a is an integer from 4 to 10, and b is an integer from 6 to 12 and an aromatic polyamide resin including a repeat unit represented by the following Formula 2 wherein c is an integer from 6 to 12; and inorganic fillers. The polyamide resin composition can exhibit excellent properties in terms of impact resistance, stiffness, processability, appearance, and balance therebetween. | 1. A polyamide resin composition comprising:
a base resin comprising an aliphatic polyamide resin having a concentration of a terminal amine group of about 0.1 μeq/g to about 45 μeq/g and including a repeat unit represented by the following Formula 1 and an aromatic polyamide resin including a repeat unit represented by the following Formula 2; and inorganic fillers:
wherein a is an integer from 4 to 10, and b is an integer from 6 to 12;
wherein c is an integer from 6 to 12. 2. The polyamide resin composition according to claim 1, wherein the aliphatic polyamide resin is present in an amount of about 50 wt % to about 90 wt % based on the total weight of the base resin; the aromatic polyamide resin is present in an amount of about 10 wt % to about 50 wt % based on the total weight of the base resin; and the inorganic fillers are present in an amount of about 50 parts by weight to about 500 parts by weight based on about 100 parts by weight of the base resin. 3. The polyamide resin composition according to claim 1, wherein the aliphatic polyamide resin has the terminal amine group and a terminal carboxyl group, a concentration of the terminal amine group ranges from about 10 μeq/g to about 40 μeq/g, and the concentration of the terminal amine group is about 0.1 times to about 0.3 times the concentration of the terminal carboxyl group. 4. The polyamide resin composition according to claim 1, wherein the aliphatic polyamide resin has an intrinsic viscosity of about 0.9 dL/g to about 1.2 dL/g; the aromatic polyamide resin has an intrinsic viscosity of about 0.6 dL/g to about 1.0 dL/g; and
the base resin has an intrinsic viscosity of about 1.0 dL/g to about 1.1 dL/g. 5. The polyamide resin composition according to claim 1, wherein the aliphatic polyamide resin is polyamide 66 and the aromatic polyamide resin is polyamide 61. 6. The polyamide resin composition according to claim 1, wherein the inorganic fillers are glass fibers, and the glass fibers take a fibrous form and have a sectional diameter of about 5 μm to about 20 μm and a ratio of minor axis to major axis of about 1:about 1 to about 1:about 6 in a cross-sectional view thereof. 7. The polyamide resin composition according to claim 6, wherein the glass fibers are surface-treated with a coupling agent comprising at least one of a urethane coupling agent, a silane coupling agent, and an epoxy coupling agent. 8. The polyamide resin composition according to claim 1, wherein the polyamide resin composition has an intrinsic viscosity of about 1.0 dL/g to about 1.1 dL/g, and a difference in intrinsic viscosity between the base resin and the polyamide resin composition is about 0.05 dL/g or less. 9. The polyamide resin composition according to claim 1, wherein the polyamide resin composition has a notched Izod impact strength of about 10 kgf·cm/cm to about 30 kgf·cm/cm, as measured on an about ⅛″ thick specimen in accordance with ASTM D256. 10. The polyamide resin composition according to claim 1, wherein the polyamide resin composition has a spiral flow length of about 95 mm to about 160 mm, as measured on a specimen prepared by injection molding under conditions of a molding temperature of about 300° C., a mold temperature of about 80° C., an injection pressure of about 1,500 kgf/cm2, and an injection rate of about 120 mm/s in a spiral mold having a thickness of about 0.5 mm. 11. The polyamide resin composition according to claim 1, wherein the polyamide resin composition has a falling dart impact strength of about 40 cm to about 80 cm, as measured on an about 0.8 mm thick specimen (about 10 cm×about 10 cm×about 0.8 mm) using an about 500 g dart in accordance with the DuPont drop test method by measuring a height of the dart at which the specimen is cracked. 12. A molded article formed of the polyamide resin composition according to claim 1. | A polyamide resin composition and a molded article manufactured using the same. The polyamide resin composition includes: a base resin comprising an aliphatic polyamide resin having a terminal amine group concentration of about 0.1 μeq/g to about 45 μeq/g and including a repeat unit represented by the following Formula 1 wherein a is an integer from 4 to 10, and b is an integer from 6 to 12 and an aromatic polyamide resin including a repeat unit represented by the following Formula 2 wherein c is an integer from 6 to 12; and inorganic fillers. The polyamide resin composition can exhibit excellent properties in terms of impact resistance, stiffness, processability, appearance, and balance therebetween.1. A polyamide resin composition comprising:
a base resin comprising an aliphatic polyamide resin having a concentration of a terminal amine group of about 0.1 μeq/g to about 45 μeq/g and including a repeat unit represented by the following Formula 1 and an aromatic polyamide resin including a repeat unit represented by the following Formula 2; and inorganic fillers:
wherein a is an integer from 4 to 10, and b is an integer from 6 to 12;
wherein c is an integer from 6 to 12. 2. The polyamide resin composition according to claim 1, wherein the aliphatic polyamide resin is present in an amount of about 50 wt % to about 90 wt % based on the total weight of the base resin; the aromatic polyamide resin is present in an amount of about 10 wt % to about 50 wt % based on the total weight of the base resin; and the inorganic fillers are present in an amount of about 50 parts by weight to about 500 parts by weight based on about 100 parts by weight of the base resin. 3. The polyamide resin composition according to claim 1, wherein the aliphatic polyamide resin has the terminal amine group and a terminal carboxyl group, a concentration of the terminal amine group ranges from about 10 μeq/g to about 40 μeq/g, and the concentration of the terminal amine group is about 0.1 times to about 0.3 times the concentration of the terminal carboxyl group. 4. The polyamide resin composition according to claim 1, wherein the aliphatic polyamide resin has an intrinsic viscosity of about 0.9 dL/g to about 1.2 dL/g; the aromatic polyamide resin has an intrinsic viscosity of about 0.6 dL/g to about 1.0 dL/g; and
the base resin has an intrinsic viscosity of about 1.0 dL/g to about 1.1 dL/g. 5. The polyamide resin composition according to claim 1, wherein the aliphatic polyamide resin is polyamide 66 and the aromatic polyamide resin is polyamide 61. 6. The polyamide resin composition according to claim 1, wherein the inorganic fillers are glass fibers, and the glass fibers take a fibrous form and have a sectional diameter of about 5 μm to about 20 μm and a ratio of minor axis to major axis of about 1:about 1 to about 1:about 6 in a cross-sectional view thereof. 7. The polyamide resin composition according to claim 6, wherein the glass fibers are surface-treated with a coupling agent comprising at least one of a urethane coupling agent, a silane coupling agent, and an epoxy coupling agent. 8. The polyamide resin composition according to claim 1, wherein the polyamide resin composition has an intrinsic viscosity of about 1.0 dL/g to about 1.1 dL/g, and a difference in intrinsic viscosity between the base resin and the polyamide resin composition is about 0.05 dL/g or less. 9. The polyamide resin composition according to claim 1, wherein the polyamide resin composition has a notched Izod impact strength of about 10 kgf·cm/cm to about 30 kgf·cm/cm, as measured on an about ⅛″ thick specimen in accordance with ASTM D256. 10. The polyamide resin composition according to claim 1, wherein the polyamide resin composition has a spiral flow length of about 95 mm to about 160 mm, as measured on a specimen prepared by injection molding under conditions of a molding temperature of about 300° C., a mold temperature of about 80° C., an injection pressure of about 1,500 kgf/cm2, and an injection rate of about 120 mm/s in a spiral mold having a thickness of about 0.5 mm. 11. The polyamide resin composition according to claim 1, wherein the polyamide resin composition has a falling dart impact strength of about 40 cm to about 80 cm, as measured on an about 0.8 mm thick specimen (about 10 cm×about 10 cm×about 0.8 mm) using an about 500 g dart in accordance with the DuPont drop test method by measuring a height of the dart at which the specimen is cracked. 12. A molded article formed of the polyamide resin composition according to claim 1. | 1,700 |
3,402 | 15,076,825 | 1,717 | A stacked up structure can include a first environmental barrier coating (EBC) layer and a second EBC layer. A first process can be used to form the first layer and a second process can be used to form the second layer. In one embodiment interfacial material can be formed for improved bonding of the second layer to the first layer. The interfacial material can define a continuous or discontinuous layer of nonuniform thickness. | 1. A stacked up structure comprising:
a first rare earth disilicate layer; a second rare earth disilicate layer; and interfacial material defining a bond surface on which the second rare earth disilicate layer is bonded, said interfacial material formed between the first rare earth disilicate layer and the second rare earth disilicate layer, wherein a roughness of the bond surface is greater than a roughness of a surface for bonding the second rare earth disilicate layer in an absence of the interfacial material. 2. The stacked up structure of claim 1, wherein the interfacial material is formed on the first rare earth disilicate layer. 3. The stacked up structure of claim 1, wherein the interfacial material comprises particles at least partially embedded in the first rare earth disilicate layer. 4. The stacked up structure of claim 1, further having a bond coat layer below the first rare earth disilicate layer. 5. The stacked up structure of claim 1, wherein the interfacial material defines a continuous layer formed on the first rare earth disilicate layer. 6. The stacked up structure of claim 1, wherein the interfacial material defines a discontinuous layer formed on the first rare earth disilicate layer. 7. The stacked up structure of claim 1, wherein the first rare earth disilicate layer includes a sintered microstructure, and wherein the second rare earth disilicate layer includes a splat microstructure. 8. The stacked up structure of claim 1, wherein a length of a bond line defined at the bond surface in a cross section projection of the stacked up structure is more than 20 percent longer than a bond line defined at the surface for bonding in the cross sectional projection of the stacked up structure. 9. The stacked up structure of claim 1, wherein the interfacial material has an average thickness of less than 50 percent of an average thickness of the first rare earth disilicate layer. 10. The stacked up structure of claim 1, wherein the bond surface is defined by the interfacial material. 11. The stacked up structure of claim 1, wherein the bond surface is defined by the interfacial material and the first rare earth disilicate layer. 12. The stacked up structure of claim 1, wherein the stacked up structure includes a CMC substrate, wherein the first rare earth disilicate layer is formed over the CMC substrate. 13. A method comprising:
forming a first rare earth disilicate layer on a surface; forming interfacial material on the first rare earth disilicate layer to define a bond surface; and forming a second rare earth disilicate layer on the bond surface, wherein the forming interfacial material results in the bond surface having a roughness greater than a roughness of a surface for bonding of the second rare earth disilicate layer in an absence of the interfacial material. 14. The method of claim 13, wherein the forming a first rare earth disilicate layer includes using a first process and wherein the forming a second rare earth disilicate layer includes using a second process. 15. The method of claim 13, wherein the bond surface is defined by the interfacial material. 16. The method of claim 13, wherein the bond surface is defined by the interfacial material and the first rare earth disilicate layer. 17. The method of claim 13, wherein the forming interfacial material includes using an additive process. 18. The method of claim 13, wherein the forming interfacial material is performed so that the interfacial material defines a continuous layer. 19. The method of claim 13, wherein the forming interfacial material is performed so that the interfacial material defines a discontinuous layer. 20. The method of claim 13, wherein the forming interfacial material includes using spray evaporating. 21. The method of claim 13, wherein the forming interfacial material includes sprinkling particles onto the first rare earth disilicate layer with the rare earth disilicate layer in a wet state. 22. The method of claim 13, wherein the forming interfacial material includes sprinkling particles onto the first rare earth disilicate layer, wherein the particles include agglomerates of particles. 23. The method of claim 13, wherein the forming a first rare earth disilicate layer includes forming a slurry, and wherein the forming a second rare earth disilicate layer includes using an air plasma spray (APS) process. 24. The method of claim 13, wherein the first rare earth disilicate layer includes a sintered microstructure, and wherein the second rare earth disilicate layer includes a splat microstructure. 25. The method of claim 13, wherein the forming a first rare earth disilicate layer on a surface includes forming the first rare earth disilicate layer over a CMC substrate. 26. A stacked up structure comprising:
a plurality of rare earth material layers defining an environmental barrier coating (EBC); a first vertical cross section extending through one or more layers of the plurality of rare earth material layers, the first vertical cross section having a first layer profile; and a second vertical cross section extending through one or more layers of the plurality of rare earth material layers, the second vertical cross section having a second layer profile. 27. The stacked up structure of claim 26, wherein the second layer profile is absent a layer included in the first layer profile. 28. The stacked up structure of claim 26, wherein the second layer profile is absent a plurality of layers included in the first layer profile. 29. The stacked up structure of claim 26, wherein the second layer profile is absent a layer included in the first layer profile, and wherein the first layer profile and the second layer profile include a common top layer. 30. The stacked up structure of claim 26, wherein the stacked up structure defines an article selected from the group consisting of an airfoil, a shroud, a blade, a vane, a nozzle, a turbine center frame, a cowl, an exhaust mixer. 31. The method of claim 13 wherein the forming the first rare earth disilicate layer comprises depositing an aerosol slurry of the first rare earth disilicate, and wherein the forming interfacial material comprises spraying a slurry of the interfacial material onto the first rare earth disilicate or depositing particles of the interfacial material onto the first rare earth disilicate layer, and wherein the forming the second rare earth disilicate layer comprises air plasma spraying the second rare earth disilicate. | A stacked up structure can include a first environmental barrier coating (EBC) layer and a second EBC layer. A first process can be used to form the first layer and a second process can be used to form the second layer. In one embodiment interfacial material can be formed for improved bonding of the second layer to the first layer. The interfacial material can define a continuous or discontinuous layer of nonuniform thickness.1. A stacked up structure comprising:
a first rare earth disilicate layer; a second rare earth disilicate layer; and interfacial material defining a bond surface on which the second rare earth disilicate layer is bonded, said interfacial material formed between the first rare earth disilicate layer and the second rare earth disilicate layer, wherein a roughness of the bond surface is greater than a roughness of a surface for bonding the second rare earth disilicate layer in an absence of the interfacial material. 2. The stacked up structure of claim 1, wherein the interfacial material is formed on the first rare earth disilicate layer. 3. The stacked up structure of claim 1, wherein the interfacial material comprises particles at least partially embedded in the first rare earth disilicate layer. 4. The stacked up structure of claim 1, further having a bond coat layer below the first rare earth disilicate layer. 5. The stacked up structure of claim 1, wherein the interfacial material defines a continuous layer formed on the first rare earth disilicate layer. 6. The stacked up structure of claim 1, wherein the interfacial material defines a discontinuous layer formed on the first rare earth disilicate layer. 7. The stacked up structure of claim 1, wherein the first rare earth disilicate layer includes a sintered microstructure, and wherein the second rare earth disilicate layer includes a splat microstructure. 8. The stacked up structure of claim 1, wherein a length of a bond line defined at the bond surface in a cross section projection of the stacked up structure is more than 20 percent longer than a bond line defined at the surface for bonding in the cross sectional projection of the stacked up structure. 9. The stacked up structure of claim 1, wherein the interfacial material has an average thickness of less than 50 percent of an average thickness of the first rare earth disilicate layer. 10. The stacked up structure of claim 1, wherein the bond surface is defined by the interfacial material. 11. The stacked up structure of claim 1, wherein the bond surface is defined by the interfacial material and the first rare earth disilicate layer. 12. The stacked up structure of claim 1, wherein the stacked up structure includes a CMC substrate, wherein the first rare earth disilicate layer is formed over the CMC substrate. 13. A method comprising:
forming a first rare earth disilicate layer on a surface; forming interfacial material on the first rare earth disilicate layer to define a bond surface; and forming a second rare earth disilicate layer on the bond surface, wherein the forming interfacial material results in the bond surface having a roughness greater than a roughness of a surface for bonding of the second rare earth disilicate layer in an absence of the interfacial material. 14. The method of claim 13, wherein the forming a first rare earth disilicate layer includes using a first process and wherein the forming a second rare earth disilicate layer includes using a second process. 15. The method of claim 13, wherein the bond surface is defined by the interfacial material. 16. The method of claim 13, wherein the bond surface is defined by the interfacial material and the first rare earth disilicate layer. 17. The method of claim 13, wherein the forming interfacial material includes using an additive process. 18. The method of claim 13, wherein the forming interfacial material is performed so that the interfacial material defines a continuous layer. 19. The method of claim 13, wherein the forming interfacial material is performed so that the interfacial material defines a discontinuous layer. 20. The method of claim 13, wherein the forming interfacial material includes using spray evaporating. 21. The method of claim 13, wherein the forming interfacial material includes sprinkling particles onto the first rare earth disilicate layer with the rare earth disilicate layer in a wet state. 22. The method of claim 13, wherein the forming interfacial material includes sprinkling particles onto the first rare earth disilicate layer, wherein the particles include agglomerates of particles. 23. The method of claim 13, wherein the forming a first rare earth disilicate layer includes forming a slurry, and wherein the forming a second rare earth disilicate layer includes using an air plasma spray (APS) process. 24. The method of claim 13, wherein the first rare earth disilicate layer includes a sintered microstructure, and wherein the second rare earth disilicate layer includes a splat microstructure. 25. The method of claim 13, wherein the forming a first rare earth disilicate layer on a surface includes forming the first rare earth disilicate layer over a CMC substrate. 26. A stacked up structure comprising:
a plurality of rare earth material layers defining an environmental barrier coating (EBC); a first vertical cross section extending through one or more layers of the plurality of rare earth material layers, the first vertical cross section having a first layer profile; and a second vertical cross section extending through one or more layers of the plurality of rare earth material layers, the second vertical cross section having a second layer profile. 27. The stacked up structure of claim 26, wherein the second layer profile is absent a layer included in the first layer profile. 28. The stacked up structure of claim 26, wherein the second layer profile is absent a plurality of layers included in the first layer profile. 29. The stacked up structure of claim 26, wherein the second layer profile is absent a layer included in the first layer profile, and wherein the first layer profile and the second layer profile include a common top layer. 30. The stacked up structure of claim 26, wherein the stacked up structure defines an article selected from the group consisting of an airfoil, a shroud, a blade, a vane, a nozzle, a turbine center frame, a cowl, an exhaust mixer. 31. The method of claim 13 wherein the forming the first rare earth disilicate layer comprises depositing an aerosol slurry of the first rare earth disilicate, and wherein the forming interfacial material comprises spraying a slurry of the interfacial material onto the first rare earth disilicate or depositing particles of the interfacial material onto the first rare earth disilicate layer, and wherein the forming the second rare earth disilicate layer comprises air plasma spraying the second rare earth disilicate. | 1,700 |
3,403 | 15,115,766 | 1,771 | A lubricating oil composition which can reduce the occurrence frequency of LSPI and which can ensure detergency. The lubricating oil composition which includes a lubricant base oil, a compound having calcium and/or magnesium, a compound having molybdenum and/or phosphorus, and an ashless dispersant having nitrogen and which satisfies X≦−0.85 and Y≧0.18 (wherein X is calculated according to formula (1): X=([Ca]+0.5[Mg])×8−[Mo]×8−[P]×30 and Y is calculated according to formula (2): Y=[Ca]+1.65[Mg]+[N]). The lubricating oil composition for use in an internal combustion engine, more particularly, a lubricating oil composition for use in a supercharged gasoline engine. | 1. A lubricating oil composition, comprising: a lubricating oil base oil, a compound having at least one element selected from calcium and magnesium, a compound having at least one element selected from molybdenum and phosphorous, and an ashless dispersant having nitrogen; wherein,
X as determined from following equation (1):
X=([Ca]+0.5[Mg])×8−[Mo]×8−[P]×30 (1)
wherein [Ca], [Mg], [Mo] and [P] in equation (1) respectively represent the concentrations (wt %) of calcium, magnesium, molybdenum and phosphorous in the lubricating oil composition, satisfies the expression X≦−0.85; and, Y as determined from following equation (2):
Y=[Ca]+1.65[Mg]+[N] (2)
wherein [Ca], [Mg] and [N] in equation (2) respectively represent the concentrations (wt %) of calcium, magnesium and nitrogen derived from ashless dispersant in the lubricating oil composition, satisfies the expression Y≧0.18. 2. The lubricating oil composition according to claim 1, wherein Z as determined from following equation (3):
Z=[N]/([Ca]+[Mg]) (3)
wherein [Ca], [Mg] and [N] respectively represent the concentrations (wt %) of calcium, magnesium and nitrogen derived from an ashless dispersant in the lubricating oil composition, further satisfies the expression 0.3≦Z≦1.5. 3. The lubricating oil composition according to claim 1, wherein the concentration of phosphorous [P] contained in the lubricating oil composition satisfies the expression [P]≦0.12% by weight. 4. The lubricating oil composition according to claim 1, wherein the concentration of molybdenum [Mo] contained in the lubricating oil composition satisfies the expression [Mo]≦0.1% by weight. 5. The lubricating oil composition according to claim 1, wherein the concentration of calcium [Ca] and the concentration of magnesium [Mg] contained in the lubricating oil composition satisfy the expression [Ca]+1.65[Mg]≧0.08% by weight. 6. The lubricating oil composition according to claim 1, wherein the lubricating base oil has a kinetic viscosity at 100° C. of 2 mm2/s to 15 mm2/s. 7. The lubricating oil composition according to claim 1, containing at least one metal cleaner [A] having calcium or magnesium. 8. The lubricating oil composition according to claim 1, containing at least one wear inhibitor [B] having phosphorous. 9. The lubricating oil composition according to claim 1, containing at least one friction modifier [C] having molybdenum. 10. The lubricating oil composition according to claim 1, containing at least one viscosity index improver [E]. 11. The lubricating oil composition according to claim 1, which is for an internal combustion engine. 12. The lubricating oil composition according to claim 11, wherein the internal combustion engine is a supercharged gasoline engine. | A lubricating oil composition which can reduce the occurrence frequency of LSPI and which can ensure detergency. The lubricating oil composition which includes a lubricant base oil, a compound having calcium and/or magnesium, a compound having molybdenum and/or phosphorus, and an ashless dispersant having nitrogen and which satisfies X≦−0.85 and Y≧0.18 (wherein X is calculated according to formula (1): X=([Ca]+0.5[Mg])×8−[Mo]×8−[P]×30 and Y is calculated according to formula (2): Y=[Ca]+1.65[Mg]+[N]). The lubricating oil composition for use in an internal combustion engine, more particularly, a lubricating oil composition for use in a supercharged gasoline engine.1. A lubricating oil composition, comprising: a lubricating oil base oil, a compound having at least one element selected from calcium and magnesium, a compound having at least one element selected from molybdenum and phosphorous, and an ashless dispersant having nitrogen; wherein,
X as determined from following equation (1):
X=([Ca]+0.5[Mg])×8−[Mo]×8−[P]×30 (1)
wherein [Ca], [Mg], [Mo] and [P] in equation (1) respectively represent the concentrations (wt %) of calcium, magnesium, molybdenum and phosphorous in the lubricating oil composition, satisfies the expression X≦−0.85; and, Y as determined from following equation (2):
Y=[Ca]+1.65[Mg]+[N] (2)
wherein [Ca], [Mg] and [N] in equation (2) respectively represent the concentrations (wt %) of calcium, magnesium and nitrogen derived from ashless dispersant in the lubricating oil composition, satisfies the expression Y≧0.18. 2. The lubricating oil composition according to claim 1, wherein Z as determined from following equation (3):
Z=[N]/([Ca]+[Mg]) (3)
wherein [Ca], [Mg] and [N] respectively represent the concentrations (wt %) of calcium, magnesium and nitrogen derived from an ashless dispersant in the lubricating oil composition, further satisfies the expression 0.3≦Z≦1.5. 3. The lubricating oil composition according to claim 1, wherein the concentration of phosphorous [P] contained in the lubricating oil composition satisfies the expression [P]≦0.12% by weight. 4. The lubricating oil composition according to claim 1, wherein the concentration of molybdenum [Mo] contained in the lubricating oil composition satisfies the expression [Mo]≦0.1% by weight. 5. The lubricating oil composition according to claim 1, wherein the concentration of calcium [Ca] and the concentration of magnesium [Mg] contained in the lubricating oil composition satisfy the expression [Ca]+1.65[Mg]≧0.08% by weight. 6. The lubricating oil composition according to claim 1, wherein the lubricating base oil has a kinetic viscosity at 100° C. of 2 mm2/s to 15 mm2/s. 7. The lubricating oil composition according to claim 1, containing at least one metal cleaner [A] having calcium or magnesium. 8. The lubricating oil composition according to claim 1, containing at least one wear inhibitor [B] having phosphorous. 9. The lubricating oil composition according to claim 1, containing at least one friction modifier [C] having molybdenum. 10. The lubricating oil composition according to claim 1, containing at least one viscosity index improver [E]. 11. The lubricating oil composition according to claim 1, which is for an internal combustion engine. 12. The lubricating oil composition according to claim 11, wherein the internal combustion engine is a supercharged gasoline engine. | 1,700 |
3,404 | 13,324,296 | 1,761 | The thermoplastic molding composition comprises, based on the thermoplastic molding composition,
a) as component A, at least one polyamide or copolyamide, or one polymer blend comprising polyamide, b) as component B, from 3 to 20% by weight of carbon black or graphite, or a mixture thereof, c) as component C, from 0.1 to 3% by weight of ionic liquids. | 1-11. (canceled) 12. A thermoplastic molding composition comprising, based on the thermoplastic molding composition,
a) as component A, at least one polyamide or copolyamide, or one polymer blend comprising polyamide, b) as component B, from 3 to 20% by weight of carbon black or graphite, or a mixture thereof, c) as component C, from 0.1 to 3% by weight of ionic liquids. 13. The thermoplastic molding composition according to claim 12, wherein the amount of component B comprised in the thermoplastic molding composition is from 3.5 to 10% by weight, based on the thermoplastic molding composition. 14. The thermoplastic molding composition according to claim 12, wherein the amount of component C comprised in the thermoplastic molding composition is from 0.1 to 1.5% by weight, based on the thermoplastic molding composition. 15. The thermoplastic molding composition according to claim 13, wherein the amount of component C comprised in the thermoplastic molding composition is from 0.1 to 1.5% by weight, based on the thermoplastic molding composition. 16. The thermoplastic molding composition according to claim 12, wherein the polyamides in component A have been selected from the following list, the starting monomers being stated between parentheses:
PA 26 (ethylenediamine, adipic acid) PA 210 (ethylenediamine, sebacic acid) PA 46 (tetramethylenediamine, adipic acid) PA 66 (hexamethylenediamine, adipic acid) PA 69 (hexamethylenediamine, azelaic acid) PA 610 (hexamethylenediamine, sebacic acid) PA 612 (hexamethylenediamine, decanedicarboxylic acid) PA 613 (hexamethylenediamine, undecanedicarboxylic acid) PA 1212 (1,12-dodecanediamine, decanedicarboxylic acid) PA 1313 (1,13-diaminotridecane, undecanedicarboxylic acid) PA MXD6 (m-xylylenediamine, adipic acid) PA TMDT (trimethylhexamethylenediamine, terephthalic acid) PA 4 (pyrrolidone) PA 6 (ε-caprolactam) PA 7 (ethanolactam) PA 8 (capryllactam) PA 9 (9-aminononanoic acid) poly-p-phenylenediamineterephthalamide (phenylenediamine, terephthalic acid) PA11 (11-aminoundecanoic acid) PA12 (laurolactam) or a mixture or copolymer thereof. 17. The thermoplastic molding composition according to claim 12, wherein component A comprises, as blend polymer, natural or synthetic rubbers, acrylate rubbers, polyesters, polyolefins, polyurethanes, or a mixture thereof, optionally in combination with a compatibilizer. 18. The thermoplastic molding composition according to claim 12, which also comprises a metal salt mixed with or dissolved in component C. 19. The thermoplastic molding composition according to claim 12, wherein the cation of the ionic liquid in component C has been selected from the group consisting of quaternary ammonium cations, phosphonium cations, imidazolium cations, H-pyrazolium cations, pyridazinium ions, pyrimidinium ions, pyrazinium ions, pyrrolidinium cations, guanidinium cations, 5- to at least 6-membered cations which comprise at least one phosphorus or sulfur atom, the 1,8-diazabicyclo[5.4.0]undec-7-enium cation and the 1,8-diazabicyclo[4.3.0]non-5-inium cation or else from oligo- and polymers which comprise these cations. 20. The thermoplastic molding composition according to claim 12, wherein the anion in the ionic liquid in component C has been selected from halide, optionally substituted C1-4-carboxylate, phosphate, C1-4-alkyl phosphate, Di-C1-4-alkyl phosphate, C1-4-alkyl sulfate, C1-4-alkylsulfonate, hydrogensulfate, triflimide, tetrafluoroborate, triflate, or a mixture thereof. 21. The thermoplastic molding composition according to claim 19, wherein the anion in the ionic liquid in component C has been selected from halide, optionally substituted C1-4-carboxylate, phosphate, C1-4-alkyl phosphate, Di-C1-4-alkyl phosphate, C1-4-alkyl sulfate, C1-4-alkylsulfonate, hydrogensulfate, triflimide, tetrafluoroborate, triflate, or a mixture thereof. 22. A process for producing the thermoplastic molding compositions according to claim 12, which comprises introducing components B and C into component A in a corotating twin-screw extruder. 23. The process according to claim 22, wherein the extrusion process is carried out at a temperature in the range from 170 to 350° C. 24. A molding made of the thermoplastic molding composition according to claim 12. | The thermoplastic molding composition comprises, based on the thermoplastic molding composition,
a) as component A, at least one polyamide or copolyamide, or one polymer blend comprising polyamide, b) as component B, from 3 to 20% by weight of carbon black or graphite, or a mixture thereof, c) as component C, from 0.1 to 3% by weight of ionic liquids.1-11. (canceled) 12. A thermoplastic molding composition comprising, based on the thermoplastic molding composition,
a) as component A, at least one polyamide or copolyamide, or one polymer blend comprising polyamide, b) as component B, from 3 to 20% by weight of carbon black or graphite, or a mixture thereof, c) as component C, from 0.1 to 3% by weight of ionic liquids. 13. The thermoplastic molding composition according to claim 12, wherein the amount of component B comprised in the thermoplastic molding composition is from 3.5 to 10% by weight, based on the thermoplastic molding composition. 14. The thermoplastic molding composition according to claim 12, wherein the amount of component C comprised in the thermoplastic molding composition is from 0.1 to 1.5% by weight, based on the thermoplastic molding composition. 15. The thermoplastic molding composition according to claim 13, wherein the amount of component C comprised in the thermoplastic molding composition is from 0.1 to 1.5% by weight, based on the thermoplastic molding composition. 16. The thermoplastic molding composition according to claim 12, wherein the polyamides in component A have been selected from the following list, the starting monomers being stated between parentheses:
PA 26 (ethylenediamine, adipic acid) PA 210 (ethylenediamine, sebacic acid) PA 46 (tetramethylenediamine, adipic acid) PA 66 (hexamethylenediamine, adipic acid) PA 69 (hexamethylenediamine, azelaic acid) PA 610 (hexamethylenediamine, sebacic acid) PA 612 (hexamethylenediamine, decanedicarboxylic acid) PA 613 (hexamethylenediamine, undecanedicarboxylic acid) PA 1212 (1,12-dodecanediamine, decanedicarboxylic acid) PA 1313 (1,13-diaminotridecane, undecanedicarboxylic acid) PA MXD6 (m-xylylenediamine, adipic acid) PA TMDT (trimethylhexamethylenediamine, terephthalic acid) PA 4 (pyrrolidone) PA 6 (ε-caprolactam) PA 7 (ethanolactam) PA 8 (capryllactam) PA 9 (9-aminononanoic acid) poly-p-phenylenediamineterephthalamide (phenylenediamine, terephthalic acid) PA11 (11-aminoundecanoic acid) PA12 (laurolactam) or a mixture or copolymer thereof. 17. The thermoplastic molding composition according to claim 12, wherein component A comprises, as blend polymer, natural or synthetic rubbers, acrylate rubbers, polyesters, polyolefins, polyurethanes, or a mixture thereof, optionally in combination with a compatibilizer. 18. The thermoplastic molding composition according to claim 12, which also comprises a metal salt mixed with or dissolved in component C. 19. The thermoplastic molding composition according to claim 12, wherein the cation of the ionic liquid in component C has been selected from the group consisting of quaternary ammonium cations, phosphonium cations, imidazolium cations, H-pyrazolium cations, pyridazinium ions, pyrimidinium ions, pyrazinium ions, pyrrolidinium cations, guanidinium cations, 5- to at least 6-membered cations which comprise at least one phosphorus or sulfur atom, the 1,8-diazabicyclo[5.4.0]undec-7-enium cation and the 1,8-diazabicyclo[4.3.0]non-5-inium cation or else from oligo- and polymers which comprise these cations. 20. The thermoplastic molding composition according to claim 12, wherein the anion in the ionic liquid in component C has been selected from halide, optionally substituted C1-4-carboxylate, phosphate, C1-4-alkyl phosphate, Di-C1-4-alkyl phosphate, C1-4-alkyl sulfate, C1-4-alkylsulfonate, hydrogensulfate, triflimide, tetrafluoroborate, triflate, or a mixture thereof. 21. The thermoplastic molding composition according to claim 19, wherein the anion in the ionic liquid in component C has been selected from halide, optionally substituted C1-4-carboxylate, phosphate, C1-4-alkyl phosphate, Di-C1-4-alkyl phosphate, C1-4-alkyl sulfate, C1-4-alkylsulfonate, hydrogensulfate, triflimide, tetrafluoroborate, triflate, or a mixture thereof. 22. A process for producing the thermoplastic molding compositions according to claim 12, which comprises introducing components B and C into component A in a corotating twin-screw extruder. 23. The process according to claim 22, wherein the extrusion process is carried out at a temperature in the range from 170 to 350° C. 24. A molding made of the thermoplastic molding composition according to claim 12. | 1,700 |
3,405 | 15,448,727 | 1,764 | A thermoplastic resin composition containing 25 to 50 parts by mass of a rubber-containing graft copolymer (A) obtained by copolymerizing a monomer mixture containing an aromatic vinyl compound and a vinyl cyanide compound in the presence of a diene-based rubber-like polymer, and 50 to 75 parts by mass of a hard copolymer mixture (B) containing a hard copolymer (B-I) and a hard copolymer (B-II). | 1. A thermoplastic resin composition comprising:
25 to 50 parts by mass of a rubber-containing graft copolymer (A) obtained by copolymerizing a monomer mixture comprising an aromatic vinyl compound and a vinyl cyanide compound in presence of a diene-based rubber-like polymer, and 50 to 75 parts by mass of a hard copolymer mixture (B) comprising a hard copolymer (B-I) and a hard copolymer (B-II), wherein the rubber-containing graft copolymer (A) comprises a hard copolymer component (A′) in which the aromatic vinyl compound and the vinyl cyanide compound are grafted to the diene-based rubber-like polymer, a weight-average molecular weight of the hard copolymer component (A′) is from 50,000 to 200,000, an amount of the hard copolymer (B-II) in the hard copolymer mixture (B) is at least 5% by mass but less than 20% by mass, the hard copolymer (B-I) is a polymer comprising monomer units derived from the aromatic vinyl compound and monomer units derived from the vinyl cyanide compound, and has a weight-average molecular weight of 50,000 to 150,000, wherein 25 to 32% by mass of a total mass of the hard copolymer (B-I) is composed of monomer units derived from the vinyl cyanide compound, and the hard copolymer (B-II) is a polymer comprising monomer units derived from the aromatic vinyl compound and monomer units derived from the vinyl cyanide compound, and has a weight-average molecular weight of 50,000 to 150,000, wherein 35 to 50% by mass of a total mass of the hard copolymer (B-II) is composed of monomer units derived from the vinyl cyanide compound. 2. The thermoplastic resin composition according to claim 1, wherein an amount of components derived from the diene-based rubber-like polymer in the rubber-containing graft copolymer (A) is from 35 to 70% by mass. 3. A resin molded article formed from the thermoplastic resin composition according to claim 1. 4. A resin molded article formed from the thermoplastic resin composition according to claim 2. 5. A coated article formed from the resin molded article according to claim 3. 6. A coated article formed from the resin molded article according to claim 4. | A thermoplastic resin composition containing 25 to 50 parts by mass of a rubber-containing graft copolymer (A) obtained by copolymerizing a monomer mixture containing an aromatic vinyl compound and a vinyl cyanide compound in the presence of a diene-based rubber-like polymer, and 50 to 75 parts by mass of a hard copolymer mixture (B) containing a hard copolymer (B-I) and a hard copolymer (B-II).1. A thermoplastic resin composition comprising:
25 to 50 parts by mass of a rubber-containing graft copolymer (A) obtained by copolymerizing a monomer mixture comprising an aromatic vinyl compound and a vinyl cyanide compound in presence of a diene-based rubber-like polymer, and 50 to 75 parts by mass of a hard copolymer mixture (B) comprising a hard copolymer (B-I) and a hard copolymer (B-II), wherein the rubber-containing graft copolymer (A) comprises a hard copolymer component (A′) in which the aromatic vinyl compound and the vinyl cyanide compound are grafted to the diene-based rubber-like polymer, a weight-average molecular weight of the hard copolymer component (A′) is from 50,000 to 200,000, an amount of the hard copolymer (B-II) in the hard copolymer mixture (B) is at least 5% by mass but less than 20% by mass, the hard copolymer (B-I) is a polymer comprising monomer units derived from the aromatic vinyl compound and monomer units derived from the vinyl cyanide compound, and has a weight-average molecular weight of 50,000 to 150,000, wherein 25 to 32% by mass of a total mass of the hard copolymer (B-I) is composed of monomer units derived from the vinyl cyanide compound, and the hard copolymer (B-II) is a polymer comprising monomer units derived from the aromatic vinyl compound and monomer units derived from the vinyl cyanide compound, and has a weight-average molecular weight of 50,000 to 150,000, wherein 35 to 50% by mass of a total mass of the hard copolymer (B-II) is composed of monomer units derived from the vinyl cyanide compound. 2. The thermoplastic resin composition according to claim 1, wherein an amount of components derived from the diene-based rubber-like polymer in the rubber-containing graft copolymer (A) is from 35 to 70% by mass. 3. A resin molded article formed from the thermoplastic resin composition according to claim 1. 4. A resin molded article formed from the thermoplastic resin composition according to claim 2. 5. A coated article formed from the resin molded article according to claim 3. 6. A coated article formed from the resin molded article according to claim 4. | 1,700 |
3,406 | 12,076,101 | 1,712 | Certain example embodiments relate to the deposition of metal oxide coatings via combustion deposition. In certain example embodiments, the metal oxide coating may be a silicon oxide coating (e.g., SiO 2 , or other suitable stoichiometry) and, in certain example embodiments, the silicon oxide coating may serve as an anti-reflective (AR) coating. In certain example embodiments, a percent visible transmission gain of at least about 2.0%, and more preferably between about 3.0-3.25%, may be realized through the growth of films on a first surface of the substrate. The coatings produced in accordance with certain example embodiments possess an enhanced transmission increase over previously combustion deposition produced single-layer anti-reflective coatings. This may be accomplished in certain example embodiments by provided mixed or graded microstructure metal oxide coatings (e.g., silicon oxide growths that alternate between using process conditions that produce small nucleation particle size distributions and process conditions that produce large agglomerate nano-particle size distributions) and/or by in situ nano-particle matrix loading of metal oxide coatings via combustion deposition. | 1. A method of forming a coating on a glass substrate using combustion deposition, the method comprising:
providing a glass substrate having at least one surface to be coated; selecting a reagent, the reagent being selected such that at least a portion of the reagent is used in forming the coating; introducing a first precursor to be combusted by a first flame; combusting at least a portion of the reagent and the first precursor to form a first combusted material, the first combusted material comprising non-vaporized material; providing the glass substrate in a first area so that the glass substrate is heated sufficiently to allow the first combusted material to form a first growth directly or indirectly, on the glass substrate; introducing a second precursor to be combusted by a second flame; combusting at least a portion of the reagent and the second precursor to form a second combusted material, the second combusted material comprising non-vaporized material; and providing the glass substrate in a second area so that the glass substrate is heated sufficiently to allow the second combusted material to form a second growth directly or indirectly, in or on the first growth, wherein the coating comprises at least the first and second growths, the first growth being made with process conditions that produce small nucleation particle size distributions and the second growth being made with process conditions that produce large agglomerate nano-particle size distributions. 2. The method of claim 1, wherein the coating comprises an oxide of silicon. 3. The method of claim 2, wherein the first growth has a particle size distribution mean less than about 30 nm and would produce a film having an index of refraction of between about 1.43-1.46 if coated independently. 4. The method of claim 2, wherein the second growth has a particle size distribution mean of between about 100-1500 angstroms and would produce a film having an index of refraction of between about 1.25-1.43 if coated independently. 5. The method of claim 1, wherein the coating increases visible transmission of the glass substrate by at least about 2.0%. 6. The method of claim 1, wherein the coating increases visible transmission of the glass substrate by between about 3.0-3.25%. 7. The method of claim 1, further providing first and second burners for respectively providing the first and second flames. 8. The method of claim 1, further comprising depositing one or more additional growths, the additional growths being made with process conditions that produce small nucleation particle size distributions and process conditions that produce large agglomerate nano-particle size distributions. 9. The method of claim 1, further comprising passing the substrate under the first and/or second flames at least two times to form a coating comprising multiple growths, and
wherein the multiple growths alternate between process conditions that produce small nucleation particle size distributions and process conditions that produce large agglomerate nano-particle size distributions. 10. The method of claim 1, further comprising respectively providing the first and second precursors at low and high concentrations thereof. 11. The method of claim 2, wherein the coating comprises a silicon oxide matrix including nano-particles, the nano-particles being embedded therein in situ via the combustion deposition. 12. The method of claim 12, wherein the nano-particles are distributed in a range of between about 100-1500 angstroms. 13. The method of claim 12, wherein the nano-particles are deposited by the second flame. 14. The method of claim 1, further comprising depositing at least one additional coating via combustion deposition on a second surface of the glass substrate. 15. The method of claim 1, wherein the coating increases visible transmission of the glass substrate by at least about 2.0%. 16. A method of applying a coating to a substrate using combustion deposition, the method comprising:
providing a glass substrate having at least one surface to be coated; selecting a reagent, the reagent being selected such that at least a portion of the reagent is used in forming the coating; introducing a first silicon based precursor to be combusted by a first flame; combusting at least a portion of the reagent and the first precursor to form a first combusted material, the first combusted material comprising non-vaporized material; providing the glass substrate in a first area so that the glass substrate is heated sufficiently to allow the first combusted material to form a first growth directly or indirectly, on the glass substrate; introducing a second silicon based precursor to be combusted by a second flame; combusting at least a portion of the reagent and the second precursor to form a second combusted material, the second combusted material comprising non-vaporized material; and providing the glass substrate in a second area so that the glass substrate is heated sufficiently to allow the second combusted material to form a second growth directly or indirectly, in or on the first growth, wherein the first growth is made with process conditions that produce small nucleation particle size distributions and the second growth is made with process conditions that produce large agglomerate nano-particle size distributions, or the first growth is made with process conditions that produce large agglomerate nano-particle size distributions and the second growth is made with process conditions that produce small nucleation particle size distributions, wherein the coating comprises silicon oxide having a matrix including nano-particles, the nano-particles being embedded therein in situ via the combustion deposition, and wherein the coating increases visible transmission of the glass substrate by at least about 2.0%. 17. The method of claim 16, the first growth has a particle size distribution mean less than about 30 nm and would produce a film having an index of refraction of between about 1.43-1.46 if coated independently. 18. The method of claim 16, wherein the second growth has a particle size distribution mean of between about 100-1500 angstroms and would produce a film having an index of refraction of between about 1.25-1.43 if coated. 19. The method of claim 16, wherein the coating increases visible transmission of the glass substrate by between about 3.0-3.25%. 20. The method of claim 16, further providing first and second burners for respectively providing the first and second flames. 21. The method of claim 16, further comprising depositing one or more additional growths, the additional growths alternating between process conditions that produce small nucleation particle size distributions and process conditions that produce large agglomerate nano-particle size distributions. 22. A coated article including a coating supported by a glass substrate, the coating comprising:
at least two combustion deposition deposited growths being arranged such that the growths collectively comprise generally alternating process conditions that produce small nucleation particle size distributions and process conditions that produce large agglomerate nano-particle size distributions, wherein the at least two combustion deposition deposited growths collectively form a metal oxide matrix including nano-particles, the nano-particles being embedded therein in situ, and wherein the coating increases visible transmission of the glass substrate by at least about 2.0%. 23. The coated article of claim 22, wherein the coating comprises an oxide of silicon. 24. The coated article of claim 22, wherein the first growth has a particle size distribution mean less than about 30 nm and would produce a film having an index of refraction of between about 1.43-1.46 if coated independently, and wherein the second growth has a particle size distribution mean of between about 100-1500 angstroms and would produce a film having an index of refraction of between about 1.25-1.43 if coated independently. 25. The coated article of claim 22, wherein the nano-particles are distributed in a range of between about 100-1500 angstroms. 26. A method of making a coated article including a coating supported by a glass substrate, the method comprising:
forming a metal oxide matrix including in situ embedded nano-particles, wherein the metal oxide matrix is formed by growing a film using process conditions that produce small nucleation particle size distributions via combustion deposition directly or indirectly in or on the glass substrate and growing film using process conditions that produce large agglomerate nano-particle size distributions via combustion deposition directly or indirectly in or on the film using process conditions that produce small nucleation particle size distributions. | Certain example embodiments relate to the deposition of metal oxide coatings via combustion deposition. In certain example embodiments, the metal oxide coating may be a silicon oxide coating (e.g., SiO 2 , or other suitable stoichiometry) and, in certain example embodiments, the silicon oxide coating may serve as an anti-reflective (AR) coating. In certain example embodiments, a percent visible transmission gain of at least about 2.0%, and more preferably between about 3.0-3.25%, may be realized through the growth of films on a first surface of the substrate. The coatings produced in accordance with certain example embodiments possess an enhanced transmission increase over previously combustion deposition produced single-layer anti-reflective coatings. This may be accomplished in certain example embodiments by provided mixed or graded microstructure metal oxide coatings (e.g., silicon oxide growths that alternate between using process conditions that produce small nucleation particle size distributions and process conditions that produce large agglomerate nano-particle size distributions) and/or by in situ nano-particle matrix loading of metal oxide coatings via combustion deposition.1. A method of forming a coating on a glass substrate using combustion deposition, the method comprising:
providing a glass substrate having at least one surface to be coated; selecting a reagent, the reagent being selected such that at least a portion of the reagent is used in forming the coating; introducing a first precursor to be combusted by a first flame; combusting at least a portion of the reagent and the first precursor to form a first combusted material, the first combusted material comprising non-vaporized material; providing the glass substrate in a first area so that the glass substrate is heated sufficiently to allow the first combusted material to form a first growth directly or indirectly, on the glass substrate; introducing a second precursor to be combusted by a second flame; combusting at least a portion of the reagent and the second precursor to form a second combusted material, the second combusted material comprising non-vaporized material; and providing the glass substrate in a second area so that the glass substrate is heated sufficiently to allow the second combusted material to form a second growth directly or indirectly, in or on the first growth, wherein the coating comprises at least the first and second growths, the first growth being made with process conditions that produce small nucleation particle size distributions and the second growth being made with process conditions that produce large agglomerate nano-particle size distributions. 2. The method of claim 1, wherein the coating comprises an oxide of silicon. 3. The method of claim 2, wherein the first growth has a particle size distribution mean less than about 30 nm and would produce a film having an index of refraction of between about 1.43-1.46 if coated independently. 4. The method of claim 2, wherein the second growth has a particle size distribution mean of between about 100-1500 angstroms and would produce a film having an index of refraction of between about 1.25-1.43 if coated independently. 5. The method of claim 1, wherein the coating increases visible transmission of the glass substrate by at least about 2.0%. 6. The method of claim 1, wherein the coating increases visible transmission of the glass substrate by between about 3.0-3.25%. 7. The method of claim 1, further providing first and second burners for respectively providing the first and second flames. 8. The method of claim 1, further comprising depositing one or more additional growths, the additional growths being made with process conditions that produce small nucleation particle size distributions and process conditions that produce large agglomerate nano-particle size distributions. 9. The method of claim 1, further comprising passing the substrate under the first and/or second flames at least two times to form a coating comprising multiple growths, and
wherein the multiple growths alternate between process conditions that produce small nucleation particle size distributions and process conditions that produce large agglomerate nano-particle size distributions. 10. The method of claim 1, further comprising respectively providing the first and second precursors at low and high concentrations thereof. 11. The method of claim 2, wherein the coating comprises a silicon oxide matrix including nano-particles, the nano-particles being embedded therein in situ via the combustion deposition. 12. The method of claim 12, wherein the nano-particles are distributed in a range of between about 100-1500 angstroms. 13. The method of claim 12, wherein the nano-particles are deposited by the second flame. 14. The method of claim 1, further comprising depositing at least one additional coating via combustion deposition on a second surface of the glass substrate. 15. The method of claim 1, wherein the coating increases visible transmission of the glass substrate by at least about 2.0%. 16. A method of applying a coating to a substrate using combustion deposition, the method comprising:
providing a glass substrate having at least one surface to be coated; selecting a reagent, the reagent being selected such that at least a portion of the reagent is used in forming the coating; introducing a first silicon based precursor to be combusted by a first flame; combusting at least a portion of the reagent and the first precursor to form a first combusted material, the first combusted material comprising non-vaporized material; providing the glass substrate in a first area so that the glass substrate is heated sufficiently to allow the first combusted material to form a first growth directly or indirectly, on the glass substrate; introducing a second silicon based precursor to be combusted by a second flame; combusting at least a portion of the reagent and the second precursor to form a second combusted material, the second combusted material comprising non-vaporized material; and providing the glass substrate in a second area so that the glass substrate is heated sufficiently to allow the second combusted material to form a second growth directly or indirectly, in or on the first growth, wherein the first growth is made with process conditions that produce small nucleation particle size distributions and the second growth is made with process conditions that produce large agglomerate nano-particle size distributions, or the first growth is made with process conditions that produce large agglomerate nano-particle size distributions and the second growth is made with process conditions that produce small nucleation particle size distributions, wherein the coating comprises silicon oxide having a matrix including nano-particles, the nano-particles being embedded therein in situ via the combustion deposition, and wherein the coating increases visible transmission of the glass substrate by at least about 2.0%. 17. The method of claim 16, the first growth has a particle size distribution mean less than about 30 nm and would produce a film having an index of refraction of between about 1.43-1.46 if coated independently. 18. The method of claim 16, wherein the second growth has a particle size distribution mean of between about 100-1500 angstroms and would produce a film having an index of refraction of between about 1.25-1.43 if coated. 19. The method of claim 16, wherein the coating increases visible transmission of the glass substrate by between about 3.0-3.25%. 20. The method of claim 16, further providing first and second burners for respectively providing the first and second flames. 21. The method of claim 16, further comprising depositing one or more additional growths, the additional growths alternating between process conditions that produce small nucleation particle size distributions and process conditions that produce large agglomerate nano-particle size distributions. 22. A coated article including a coating supported by a glass substrate, the coating comprising:
at least two combustion deposition deposited growths being arranged such that the growths collectively comprise generally alternating process conditions that produce small nucleation particle size distributions and process conditions that produce large agglomerate nano-particle size distributions, wherein the at least two combustion deposition deposited growths collectively form a metal oxide matrix including nano-particles, the nano-particles being embedded therein in situ, and wherein the coating increases visible transmission of the glass substrate by at least about 2.0%. 23. The coated article of claim 22, wherein the coating comprises an oxide of silicon. 24. The coated article of claim 22, wherein the first growth has a particle size distribution mean less than about 30 nm and would produce a film having an index of refraction of between about 1.43-1.46 if coated independently, and wherein the second growth has a particle size distribution mean of between about 100-1500 angstroms and would produce a film having an index of refraction of between about 1.25-1.43 if coated independently. 25. The coated article of claim 22, wherein the nano-particles are distributed in a range of between about 100-1500 angstroms. 26. A method of making a coated article including a coating supported by a glass substrate, the method comprising:
forming a metal oxide matrix including in situ embedded nano-particles, wherein the metal oxide matrix is formed by growing a film using process conditions that produce small nucleation particle size distributions via combustion deposition directly or indirectly in or on the glass substrate and growing film using process conditions that produce large agglomerate nano-particle size distributions via combustion deposition directly or indirectly in or on the film using process conditions that produce small nucleation particle size distributions. | 1,700 |
3,407 | 14,933,024 | 1,744 | A method of producing a patterned apertured web is provided. The method comprises providing a web having a central longitudinal axis. The web comprises a plurality of overbonds extending substantially parallel to the central longitudinal axis. The method comprises conveying the web in a machine direction that is substantially parallel to a direction of extension of the central longitudinal axis of the web. The method comprises stretching the web in a cross-machine direction to cause at least some of the overbonds to at least partially rupture and at least partially form patterned apertures in the web. At least some of the patterned apertures have Absolute Feret Angles, according to the Aperture Test herein, of at least about 20 degrees. At least some of the patterned apertures have an Aspect Ratio, according to the Aperture Test herein, in the range of about 2:1 to about 6:1. | 1. A method of producing a patterned apertured web, the method comprising:
providing a web having a central longitudinal axis, wherein the web comprises a plurality of overbonds extending substantially parallel to the central longitudinal axis; conveying the web in a machine direction, wherein the machine direction is substantially parallel to a direction of extension of the central longitudinal axis of the web; and stretching the web in a cross-machine direction that is substantially perpendicular to the machine direction to cause at least some of the overbonds to at least partially rupture and at least partially form patterned apertures in the web; wherein at least some of the patterned apertures have Absolute Feret Angles, according to the Aperture Test herein, of at least about 20 degrees; and wherein at least some of the patterned apertures have an Aspect Ratio, according to the Aperture Test herein, in the range of about 2:1 to about 6:1. 2. The method of claim 1, wherein at least some of the patterned apertures have Absolute Feret Angles, according to the Aperture Test herein, in the range of 0 degrees to five degrees. 3. The method of claim 1, wherein the patterned apertures comprise a first plurality of patterned apertures and a second plurality of patterned apertures, wherein central longitudinal axes of the first plurality of patterned apertures extend in a first direction relative to the machine direction, and wherein central longitudinal axes of the second plurality of apertures extend in a second, different direction relative to the machine direction. 4. The method of claim 3, wherein the second, different direction is at least about 10 degrees different than the first direction. 5. The method of claim 3, wherein the second, different direction is at least about 25 degrees different than the first direction. 6. The method of claim 3, wherein the first direction has a negative slope relative to the machine direction, and wherein the second direction has a positive slope relative to the machine direction. 7. The method of claim 1, wherein at least some of the plurality of the overbonds form a diamond-shaped pattern in the web. 8. The method of claim 1, wherein land areas are formed around at least some of the plurality of the overbonds. 9. The method of claim 1, wherein at least some of the patterned apertures have an Absolute Feret Angle of at least about 25 degrees. 10. The method of claim 1, wherein at least some of the patterned apertures have an Absolute Feret Angle of at least about 30 degrees. 11. The method of claim 1, wherein the patterned apertures have an Average Absolute Feret Angle of at least about 35 degrees. 12. The method of claim 1, wherein at least some of the patterned apertures have an Aspect Ratio, according to the Aperture Test herein, in the range of about 2:1 to about 4:1. 13. The method of claim 1, wherein at least three of the patterned apertures are nonhomogeneous. 14. The method of claim 1, wherein at least three of the patterned apertures have a different Effective Aperture Area, according to the Aperture Test herein, shape, or Absolute Feret Angle, according to the Aperture Test herein. 15. The method of claim 1, wherein at least three of the patterned apertures have a different Aspect Ratio, according to the Aperture Test herein. 16. A method of forming patterned apertures in a web, the method comprising:
providing a web having a central longitudinal axis; conveying the web in a machine direction that is substantially parallel to the central longitudinal axis; creating a plurality of overbonds in the web, wherein the overbonds have central longitudinal axes that are substantially parallel to the central longitudinal axis of the web; and stretching the web in a cross-machine direction that is substantially perpendicular to the machine direction to at least partially form patterned apertures in the web at, at least some of the overbonds; wherein at least some of the patterned apertures have Absolute Feret Angles, according to the Aperture Test herein, of at least about 20 degrees; and wherein the at least some of the patterned apertures have an Aspect Ratio, according to the Aperture Test herein, of greater than about 2:1. 17. The method of claim 16, wherein at least some of the patterned apertures have Absolute Feret Angles, according to the Aperture Test herein, of at least about 30 degrees. 18. The method of claim 17, wherein the patterned apertures comprise a first plurality of patterned apertures and a second plurality of patterned apertures, wherein central longitudinal axes of the first plurality of patterned apertures extend in a first direction, and wherein central longitudinal axes of the second plurality of patterned apertures extend in a second, different direction, and wherein the second different direction is at least about 10 degrees different than the first direction. 19. The method of claim 16, wherein the second different direction is at least 30 degrees different than the first direction. 20. A method of producing a patterned apertured web, the method comprising:
providing a web having a central longitudinal axis, wherein the web comprises a plurality of overbonds extending substantially parallel to the central longitudinal axis; conveying the web in a machine direction, wherein the machine direction is substantially parallel to a direction of extension of the central longitudinal axis of the web; and stretching the web in a cross-machine direction that is substantially perpendicular to the machine direction to cause at least some of the overbonds to at least partially rupture and at least partially form apertures in the web; wherein at least some of the patterned apertures have Absolute Feret Angles, according to the Aperture Test herein, that are at least about 25 degrees; wherein at least some of the patterned apertures have an Aspect Ratio, according to the Aperture Test herein, in the range of about 2:1 to about 6:1; and wherein at least three of the patterned apertures are nonhomogeneous. | A method of producing a patterned apertured web is provided. The method comprises providing a web having a central longitudinal axis. The web comprises a plurality of overbonds extending substantially parallel to the central longitudinal axis. The method comprises conveying the web in a machine direction that is substantially parallel to a direction of extension of the central longitudinal axis of the web. The method comprises stretching the web in a cross-machine direction to cause at least some of the overbonds to at least partially rupture and at least partially form patterned apertures in the web. At least some of the patterned apertures have Absolute Feret Angles, according to the Aperture Test herein, of at least about 20 degrees. At least some of the patterned apertures have an Aspect Ratio, according to the Aperture Test herein, in the range of about 2:1 to about 6:1.1. A method of producing a patterned apertured web, the method comprising:
providing a web having a central longitudinal axis, wherein the web comprises a plurality of overbonds extending substantially parallel to the central longitudinal axis; conveying the web in a machine direction, wherein the machine direction is substantially parallel to a direction of extension of the central longitudinal axis of the web; and stretching the web in a cross-machine direction that is substantially perpendicular to the machine direction to cause at least some of the overbonds to at least partially rupture and at least partially form patterned apertures in the web; wherein at least some of the patterned apertures have Absolute Feret Angles, according to the Aperture Test herein, of at least about 20 degrees; and wherein at least some of the patterned apertures have an Aspect Ratio, according to the Aperture Test herein, in the range of about 2:1 to about 6:1. 2. The method of claim 1, wherein at least some of the patterned apertures have Absolute Feret Angles, according to the Aperture Test herein, in the range of 0 degrees to five degrees. 3. The method of claim 1, wherein the patterned apertures comprise a first plurality of patterned apertures and a second plurality of patterned apertures, wherein central longitudinal axes of the first plurality of patterned apertures extend in a first direction relative to the machine direction, and wherein central longitudinal axes of the second plurality of apertures extend in a second, different direction relative to the machine direction. 4. The method of claim 3, wherein the second, different direction is at least about 10 degrees different than the first direction. 5. The method of claim 3, wherein the second, different direction is at least about 25 degrees different than the first direction. 6. The method of claim 3, wherein the first direction has a negative slope relative to the machine direction, and wherein the second direction has a positive slope relative to the machine direction. 7. The method of claim 1, wherein at least some of the plurality of the overbonds form a diamond-shaped pattern in the web. 8. The method of claim 1, wherein land areas are formed around at least some of the plurality of the overbonds. 9. The method of claim 1, wherein at least some of the patterned apertures have an Absolute Feret Angle of at least about 25 degrees. 10. The method of claim 1, wherein at least some of the patterned apertures have an Absolute Feret Angle of at least about 30 degrees. 11. The method of claim 1, wherein the patterned apertures have an Average Absolute Feret Angle of at least about 35 degrees. 12. The method of claim 1, wherein at least some of the patterned apertures have an Aspect Ratio, according to the Aperture Test herein, in the range of about 2:1 to about 4:1. 13. The method of claim 1, wherein at least three of the patterned apertures are nonhomogeneous. 14. The method of claim 1, wherein at least three of the patterned apertures have a different Effective Aperture Area, according to the Aperture Test herein, shape, or Absolute Feret Angle, according to the Aperture Test herein. 15. The method of claim 1, wherein at least three of the patterned apertures have a different Aspect Ratio, according to the Aperture Test herein. 16. A method of forming patterned apertures in a web, the method comprising:
providing a web having a central longitudinal axis; conveying the web in a machine direction that is substantially parallel to the central longitudinal axis; creating a plurality of overbonds in the web, wherein the overbonds have central longitudinal axes that are substantially parallel to the central longitudinal axis of the web; and stretching the web in a cross-machine direction that is substantially perpendicular to the machine direction to at least partially form patterned apertures in the web at, at least some of the overbonds; wherein at least some of the patterned apertures have Absolute Feret Angles, according to the Aperture Test herein, of at least about 20 degrees; and wherein the at least some of the patterned apertures have an Aspect Ratio, according to the Aperture Test herein, of greater than about 2:1. 17. The method of claim 16, wherein at least some of the patterned apertures have Absolute Feret Angles, according to the Aperture Test herein, of at least about 30 degrees. 18. The method of claim 17, wherein the patterned apertures comprise a first plurality of patterned apertures and a second plurality of patterned apertures, wherein central longitudinal axes of the first plurality of patterned apertures extend in a first direction, and wherein central longitudinal axes of the second plurality of patterned apertures extend in a second, different direction, and wherein the second different direction is at least about 10 degrees different than the first direction. 19. The method of claim 16, wherein the second different direction is at least 30 degrees different than the first direction. 20. A method of producing a patterned apertured web, the method comprising:
providing a web having a central longitudinal axis, wherein the web comprises a plurality of overbonds extending substantially parallel to the central longitudinal axis; conveying the web in a machine direction, wherein the machine direction is substantially parallel to a direction of extension of the central longitudinal axis of the web; and stretching the web in a cross-machine direction that is substantially perpendicular to the machine direction to cause at least some of the overbonds to at least partially rupture and at least partially form apertures in the web; wherein at least some of the patterned apertures have Absolute Feret Angles, according to the Aperture Test herein, that are at least about 25 degrees; wherein at least some of the patterned apertures have an Aspect Ratio, according to the Aperture Test herein, in the range of about 2:1 to about 6:1; and wherein at least three of the patterned apertures are nonhomogeneous. | 1,700 |
3,408 | 15,558,815 | 1,722 | The present invention relates to liquid-crystalline media (LC media), characterised in that they comprise one or more compounds of the formula I,
and one or more compounds of the formula II,
where the parameters have the meaning indicated in claim 1, to the use thereof in electro-optical displays, and to LC displays which contain these LC media. | 1. LC medium, characterised in that it comprises one or more compounds of the formula I,
in which the individual radicals have the following meanings:
R1 and R2 denote H, F, Cl, Br, —CN, —SCN, —NCS, SF5 or straight-chain or branched alkyl having 1 to 12 C atoms, in which, in addition, one or more non-adjacent CH2 groups may each be replaced, independently of one another, by—CH═CH—, —C≡C—, —O—, —CO—, —CO—O—, —O—CO—, —O—CO—O— in such a way that O atoms are not linked directly to one another, and in which, in addition, one or more H atoms may be replaced by F, Cl or Br,
A0, A1 and A2 each, independently of one another, denote phenylene-1,4-diyl, in which, in addition, one or two CH groups may be replaced by N and one or more H atoms may be replaced by halogen, CN, CH3, CHF2, CH2F, CF3, OCH3, OCHF2 or OCF3, cyclohexane-1,4-diyl, in which, in addition, one or two non-adjacent CH2 groups may be replaced, independently of one another, by O and/or S and one or more H atoms may be replaced by F, cyclohexene-1,4-diyl, bicyclo-[1.1.1]pentane-1,3-diyl, bicyclo[2.2.2]octane-1,4-diyl, spiro[3.3]-heptane-2,6-diyl, tetrahydropyran-2,5-diyl or 1,3-dioxane-2,5-diyl,
Z1 and Z2 each, independently of one another, denote —CF2O—, —OCF2—, —CH2O—, —OCH2—, —CO—O—, —O—CO—, —C2H4—, —C2F4—, —CF2CH2—, —CH2CF2—, —CFHCFH—, —CFHCH2—, —CH2CFH—, —CF2CFH—, —CFHCF2—, —CH═CH—, —CF═CH—, —CH═CF—, —CF═CF—, —C≡C— or a single bond, m and n each, independently of one another, denote 0, 1, 2 or 3,
and
one or more compounds selected from the group of the compounds of the formula II,
in which
q denotes 1 or 2,
p denotes (2-q),
Z11 and Z12, independently of one another, denote —O—, —(C═O)— or a single bond, but do not both simultaneously denote —O—,
r and s, independently of one another, denote 0 or 1,
Y11 to Y14 each, independently of one another, denote alkyl having 1 to 4 C atoms and alternatively also, independently of one another, one or both of the pairs (Y11 and Y12) and (Y13 and Y14) together denote a divalent group having 3 to 6 C atoms,
R11 on each occurrence, independently of one another, denotes H, alkyl, O-alkyl, O-cycloalkyl, O⋅ or OH,
Sp11 denotes a straight-chain or branched alkyl chain having 2-20 C atoms, in which one or more —CH2— groups may be replaced by —O—, but two adjacent —CH2— groups cannot be replaced by —O—, or denotes a hydrocarbon radical which contains a cycloalkyl or alkylcycloalkyl unit and in which one or more —CH2— groups may be replaced by —O—, but two adjacent —CH2— groups cannot be replaced by —O—. 2. LC medium according to claim 1, characterised in that it comprises one or more compounds of the formula I selected from the group of the compounds I1 to I16,
in which R1, R2 and L1 to L6 have the meanings indicated in claim 1. 3. LC medium according to claim 1, characterised in that, in formula I, m denotes 1, n denotes 0 and A0 denotes 4. LC medium according to claim 1, characterised in that it additionally comprises one or more compounds of the formula III and/or IV:
in which
A denotes 1,4-phenylene or trans-1,4-cyclohexylene,
a is 0 or 1,
R3 denotes alkyl or alkenyl having up to 9 C atoms, and
R4 denotes alkyl having 1 to 12 C atoms, where, in addition, one or two non-adjacent CH2 groups may be replaced by —O—, —CH═CH—, —CO—, —OCO— or —COO— in such a way that O atoms are not linked directly to one another. 5. LC medium according to claim 1, characterised in that it additionally comprises one or more compounds selected from the group consisting of the following formulae:
in which
R0 denotes an alkyl or alkoxy radical having 1 to 15 C atoms, where, in addition, one or more CH2 groups in these radicals may each be replaced, independently of one another, by —C≡C—, —CF2O—, —CH═CH—,
—O—, —CO—O— or —O—CO— in such a way that O atoms are not linked directly to one another, and in which, in addition, one or more H atoms may be replaced by halogen,
X0 denotes F, Cl, CN, SF5, SCN, NCS, a halogenated alkyl radical, halogenated alkenyl radical, halogenated alkoxy radical or halogenated alkenyloxy radical, each having up to 6 C atoms,
Y1-6 each, independently of one another, denote H or F,
Z0 denotes —C2H4—, —(CH2)4—, —CH═CH—, —CF═CF—, —C2F4—, —CH2CF2—, —CF2CH2—, —CH2O—, —OCH2—, —COO—, —CF2O— or —OCF2—, in the formulae V and VI also a single bond, and
b and c each, independently of one another, denote 0 or 1. 6. LC medium according to claim 1, characterised in that it additionally comprises one or more compounds selected from the group consisting of the following formulae:
in which R0 , X0 and Y1-4 have the meanings indicated above, and
each, independently of one another, denote 7. LC medium according to claim 1, characterised in that the total concentration of the compounds of the formula II in the LC medium is in the range from 10 ppm to 10,000 ppm. 8. LC medium according to claim 1, characterised in that the compounds of the formula II are selected from the group of the compounds of the formulae I11 to I15, 9. LC medium according to claim 1, characterised in that the total concentration of the compounds of the formula I in the medium as a whole is 1% to 25%. 10. An electro-optical device comprising an LC medium according to claim 1. 11. LC display containing an LC medium according to claim 1. 12. Display according to claim 11, characterised in that it is based on the IPS or FFS effect. 13. Display according to claim 11, characterised in that it has an active-matrix addressing device. 14. Process for the preparation of an LC medium according to claim 1, characterised in that one or more compounds of the formula I are mixed with one or more compounds of the formula II and with one or more further mesogenic compounds. | The present invention relates to liquid-crystalline media (LC media), characterised in that they comprise one or more compounds of the formula I,
and one or more compounds of the formula II,
where the parameters have the meaning indicated in claim 1, to the use thereof in electro-optical displays, and to LC displays which contain these LC media.1. LC medium, characterised in that it comprises one or more compounds of the formula I,
in which the individual radicals have the following meanings:
R1 and R2 denote H, F, Cl, Br, —CN, —SCN, —NCS, SF5 or straight-chain or branched alkyl having 1 to 12 C atoms, in which, in addition, one or more non-adjacent CH2 groups may each be replaced, independently of one another, by—CH═CH—, —C≡C—, —O—, —CO—, —CO—O—, —O—CO—, —O—CO—O— in such a way that O atoms are not linked directly to one another, and in which, in addition, one or more H atoms may be replaced by F, Cl or Br,
A0, A1 and A2 each, independently of one another, denote phenylene-1,4-diyl, in which, in addition, one or two CH groups may be replaced by N and one or more H atoms may be replaced by halogen, CN, CH3, CHF2, CH2F, CF3, OCH3, OCHF2 or OCF3, cyclohexane-1,4-diyl, in which, in addition, one or two non-adjacent CH2 groups may be replaced, independently of one another, by O and/or S and one or more H atoms may be replaced by F, cyclohexene-1,4-diyl, bicyclo-[1.1.1]pentane-1,3-diyl, bicyclo[2.2.2]octane-1,4-diyl, spiro[3.3]-heptane-2,6-diyl, tetrahydropyran-2,5-diyl or 1,3-dioxane-2,5-diyl,
Z1 and Z2 each, independently of one another, denote —CF2O—, —OCF2—, —CH2O—, —OCH2—, —CO—O—, —O—CO—, —C2H4—, —C2F4—, —CF2CH2—, —CH2CF2—, —CFHCFH—, —CFHCH2—, —CH2CFH—, —CF2CFH—, —CFHCF2—, —CH═CH—, —CF═CH—, —CH═CF—, —CF═CF—, —C≡C— or a single bond, m and n each, independently of one another, denote 0, 1, 2 or 3,
and
one or more compounds selected from the group of the compounds of the formula II,
in which
q denotes 1 or 2,
p denotes (2-q),
Z11 and Z12, independently of one another, denote —O—, —(C═O)— or a single bond, but do not both simultaneously denote —O—,
r and s, independently of one another, denote 0 or 1,
Y11 to Y14 each, independently of one another, denote alkyl having 1 to 4 C atoms and alternatively also, independently of one another, one or both of the pairs (Y11 and Y12) and (Y13 and Y14) together denote a divalent group having 3 to 6 C atoms,
R11 on each occurrence, independently of one another, denotes H, alkyl, O-alkyl, O-cycloalkyl, O⋅ or OH,
Sp11 denotes a straight-chain or branched alkyl chain having 2-20 C atoms, in which one or more —CH2— groups may be replaced by —O—, but two adjacent —CH2— groups cannot be replaced by —O—, or denotes a hydrocarbon radical which contains a cycloalkyl or alkylcycloalkyl unit and in which one or more —CH2— groups may be replaced by —O—, but two adjacent —CH2— groups cannot be replaced by —O—. 2. LC medium according to claim 1, characterised in that it comprises one or more compounds of the formula I selected from the group of the compounds I1 to I16,
in which R1, R2 and L1 to L6 have the meanings indicated in claim 1. 3. LC medium according to claim 1, characterised in that, in formula I, m denotes 1, n denotes 0 and A0 denotes 4. LC medium according to claim 1, characterised in that it additionally comprises one or more compounds of the formula III and/or IV:
in which
A denotes 1,4-phenylene or trans-1,4-cyclohexylene,
a is 0 or 1,
R3 denotes alkyl or alkenyl having up to 9 C atoms, and
R4 denotes alkyl having 1 to 12 C atoms, where, in addition, one or two non-adjacent CH2 groups may be replaced by —O—, —CH═CH—, —CO—, —OCO— or —COO— in such a way that O atoms are not linked directly to one another. 5. LC medium according to claim 1, characterised in that it additionally comprises one or more compounds selected from the group consisting of the following formulae:
in which
R0 denotes an alkyl or alkoxy radical having 1 to 15 C atoms, where, in addition, one or more CH2 groups in these radicals may each be replaced, independently of one another, by —C≡C—, —CF2O—, —CH═CH—,
—O—, —CO—O— or —O—CO— in such a way that O atoms are not linked directly to one another, and in which, in addition, one or more H atoms may be replaced by halogen,
X0 denotes F, Cl, CN, SF5, SCN, NCS, a halogenated alkyl radical, halogenated alkenyl radical, halogenated alkoxy radical or halogenated alkenyloxy radical, each having up to 6 C atoms,
Y1-6 each, independently of one another, denote H or F,
Z0 denotes —C2H4—, —(CH2)4—, —CH═CH—, —CF═CF—, —C2F4—, —CH2CF2—, —CF2CH2—, —CH2O—, —OCH2—, —COO—, —CF2O— or —OCF2—, in the formulae V and VI also a single bond, and
b and c each, independently of one another, denote 0 or 1. 6. LC medium according to claim 1, characterised in that it additionally comprises one or more compounds selected from the group consisting of the following formulae:
in which R0 , X0 and Y1-4 have the meanings indicated above, and
each, independently of one another, denote 7. LC medium according to claim 1, characterised in that the total concentration of the compounds of the formula II in the LC medium is in the range from 10 ppm to 10,000 ppm. 8. LC medium according to claim 1, characterised in that the compounds of the formula II are selected from the group of the compounds of the formulae I11 to I15, 9. LC medium according to claim 1, characterised in that the total concentration of the compounds of the formula I in the medium as a whole is 1% to 25%. 10. An electro-optical device comprising an LC medium according to claim 1. 11. LC display containing an LC medium according to claim 1. 12. Display according to claim 11, characterised in that it is based on the IPS or FFS effect. 13. Display according to claim 11, characterised in that it has an active-matrix addressing device. 14. Process for the preparation of an LC medium according to claim 1, characterised in that one or more compounds of the formula I are mixed with one or more compounds of the formula II and with one or more further mesogenic compounds. | 1,700 |
3,409 | 13,536,780 | 1,727 | An electric storage device includes: an electrode assembly including a positive electrode plate and a negative electrode plate that are insulated from each other; a pair of current collectors each of which includes a connecting portion and is connected to a corresponding one of the positive electrode plate and the negative electrode plate at the connecting portion; a case that houses the electrode assembly and the pair of current collectors, the electrode assembly being supported by the pair of current collectors in the case; and a distance retaining member that retains a distance between portions more distal than the respective connecting portions of the pair of current collectors. | 1. An electric storage device, comprising:
an electrode assembly including a positive electrode plate and a negative electrode plate that are insulated from each other; a pair of current collectors each of which includes a connecting portion and is connected to a corresponding one of the positive electrode plate and the negative electrode plate at the connecting portion; a case that houses the electrode assembly and the pair of current collectors, the electrode assembly being supported by the pair of current collectors in the case; and a distance retaining member that retains a distance between portions more distal than the respective connecting portions of the pair of current collectors. 2. The electric storage device according to claim 1, wherein:
the distance retaining member is a spacer that connects the pair of current collectors in the case. 3. The electric storage device according to claim 2, wherein:
the spacer is disposed in contact directly or indirectly with an inner surface of the case. 4. The electric storage device according to claim 3, wherein:
the spacer fits tightly against the inner surface of the case, and is fixed in the case. 5. The electric storage device according to claim 3, wherein:
the spacer is flexible, extends to a total length of an extent capable of fitting tightly against the inner surface of the case by bending, and is fixed in the case. 6. The electric storage device according to claim 5, wherein:
the spacer has opposite end portions and a central portion therebetween, the central portion being convex with reference to the opposite end portions; and the spacer is bent with the central portion being supported by the inner surface of the case and with the opposite end portions being applied with a force directly or indirectly from the pair of current collectors. 7. The electric storage device according to claim 3, wherein:
the spacer includes a pair of couplers, each of which is coupled to a corresponding one of the pair of current collectors; at least one of the pair of couplers includes a deformable portion that expands by cooperation with the current collector; and the spacer fits tightly against the inner surface of the case by expansion of the deformable portion, and is fixed in the case. 8. The electric storage device according to claim 7, wherein:
the spacer extends to a total length of an extent capable of fitting tightly against the inner surface of the case by expansion of the deformable portion, and is fixed in the case. 9. The electric storage device according to claim 7, wherein
at least one of the pair of couplers includes: a main wall portion; the deformable portion facing the main wall portion with a distance therebetween; and a side portion that connects the main wall portion and the deformable portion and allows a distal portion of the current collector to be inserted into between the main wall portion and the deformable portion, and the deformable portion expands by interfering with the distal portion of the current collector inserted into between the main wall portion and the deformable portion. 10. The electric storage device according to claim 9, wherein
at least one of the pair of couplers includes: the main wall portion; the deformable portion; the side portion; and a protrusion provided for at least one of the main wall portion and the deformable portion so as to protrude toward the remaining one of the at least one of the main wall portion and the deformable portion, and the deformable portion expands by interfering between the distal portion of the current collector inserted into between the main wall portion and the deformable portion and the protrusion. 11. The electric storage device according to claim 2, wherein:
the spacer includes a first coupler coupled to a predetermined portion of one of the pair of current collectors, and a second coupler coupled to a predetermined portion of the other of the pair of current collectors; and at least one of the first and second couplers can be coupled only to the predetermined portion of a corresponding one of the pair of current collectors. 12. The electric storage device according to claim 2, wherein:
the spacer includes a pair of couplers, each of which is coupled to a corresponding one of the pair of current collectors, and a bridge portion connecting the pair of couplers; the bridge portion includes: a pair of beam portions that connect the respective pair of couplers and are disposed with a distance from each other; and at least one beam connecting portion that connects the pair of beam portions to each other. 13. The electric storage device according to claim 1, wherein:
the distance retaining member a fixation structure that is formed in the case and fixes a surface of a portion on a distal end side of each of the pair of current collectors, the surface facing the opposite current collector. 14. The electric storage device according to claim 13, wherein:
the fixation structure further fixes a surface opposite to the surface of the portion on the distal end side of each of the pair of current collectors, the latter surface facing the opposite current collector. 15. The electric storage device according to claim 13, wherein;
the case includes an opening into which the electrode assembly and the pair of current collectors are inserted, and a bottom portion opposite to the opening, and the fixation structure is a step portion formed at the bottom portion. 16. A spacer for connecting a pair of current collectors each of which is connected to a corresponding one of a positive electrode plate and a negative electrode plate, comprising:
a pair of couplers coupled to the respective current collectors; and a bridge portion connecting the pair of couplers, wherein the bridge portion is flexible so that a total length of the bridge portion extends by bending. 17. The spacer according to claim 16, wherein:
the bridge portion has opposite end portions and a central portion therebetween, the central portion being convex with reference to the opposite end portions. 18. The spacer according to claim 16, wherein:
the bridge portion has opposite end portions and a central portion therebetween, the central portion being concave with reference to the opposite end portions. 19. A spacer for connecting a pair of current collectors each of which is connected to a corresponding one of a positive electrode plate and a negative electrode plate, comprising:
a pair of couplers coupled to the respective current collectors; and a bridge portion connecting the pair of couplers, wherein at least one of the pair of couplers includes a deformable portion that expands by cooperation with the current collector, and a total length of the spacer extends by expansion of the deformable portion. 20. The spacer according to claim 19, wherein:
at least one of the pair of couplers includes: a main wall portion; the deformable portion facing the main wall portion with a distance therebetween; and a side portion that connects the main wall portion and the deformable portion and allows a distal portion of the current collector to be inserted into between the main wall portion and the deformable portion, and the deformable portion expands by interfering with the distal portion of the current collector inserted into between the main wall portion and the deformable portion. | An electric storage device includes: an electrode assembly including a positive electrode plate and a negative electrode plate that are insulated from each other; a pair of current collectors each of which includes a connecting portion and is connected to a corresponding one of the positive electrode plate and the negative electrode plate at the connecting portion; a case that houses the electrode assembly and the pair of current collectors, the electrode assembly being supported by the pair of current collectors in the case; and a distance retaining member that retains a distance between portions more distal than the respective connecting portions of the pair of current collectors.1. An electric storage device, comprising:
an electrode assembly including a positive electrode plate and a negative electrode plate that are insulated from each other; a pair of current collectors each of which includes a connecting portion and is connected to a corresponding one of the positive electrode plate and the negative electrode plate at the connecting portion; a case that houses the electrode assembly and the pair of current collectors, the electrode assembly being supported by the pair of current collectors in the case; and a distance retaining member that retains a distance between portions more distal than the respective connecting portions of the pair of current collectors. 2. The electric storage device according to claim 1, wherein:
the distance retaining member is a spacer that connects the pair of current collectors in the case. 3. The electric storage device according to claim 2, wherein:
the spacer is disposed in contact directly or indirectly with an inner surface of the case. 4. The electric storage device according to claim 3, wherein:
the spacer fits tightly against the inner surface of the case, and is fixed in the case. 5. The electric storage device according to claim 3, wherein:
the spacer is flexible, extends to a total length of an extent capable of fitting tightly against the inner surface of the case by bending, and is fixed in the case. 6. The electric storage device according to claim 5, wherein:
the spacer has opposite end portions and a central portion therebetween, the central portion being convex with reference to the opposite end portions; and the spacer is bent with the central portion being supported by the inner surface of the case and with the opposite end portions being applied with a force directly or indirectly from the pair of current collectors. 7. The electric storage device according to claim 3, wherein:
the spacer includes a pair of couplers, each of which is coupled to a corresponding one of the pair of current collectors; at least one of the pair of couplers includes a deformable portion that expands by cooperation with the current collector; and the spacer fits tightly against the inner surface of the case by expansion of the deformable portion, and is fixed in the case. 8. The electric storage device according to claim 7, wherein:
the spacer extends to a total length of an extent capable of fitting tightly against the inner surface of the case by expansion of the deformable portion, and is fixed in the case. 9. The electric storage device according to claim 7, wherein
at least one of the pair of couplers includes: a main wall portion; the deformable portion facing the main wall portion with a distance therebetween; and a side portion that connects the main wall portion and the deformable portion and allows a distal portion of the current collector to be inserted into between the main wall portion and the deformable portion, and the deformable portion expands by interfering with the distal portion of the current collector inserted into between the main wall portion and the deformable portion. 10. The electric storage device according to claim 9, wherein
at least one of the pair of couplers includes: the main wall portion; the deformable portion; the side portion; and a protrusion provided for at least one of the main wall portion and the deformable portion so as to protrude toward the remaining one of the at least one of the main wall portion and the deformable portion, and the deformable portion expands by interfering between the distal portion of the current collector inserted into between the main wall portion and the deformable portion and the protrusion. 11. The electric storage device according to claim 2, wherein:
the spacer includes a first coupler coupled to a predetermined portion of one of the pair of current collectors, and a second coupler coupled to a predetermined portion of the other of the pair of current collectors; and at least one of the first and second couplers can be coupled only to the predetermined portion of a corresponding one of the pair of current collectors. 12. The electric storage device according to claim 2, wherein:
the spacer includes a pair of couplers, each of which is coupled to a corresponding one of the pair of current collectors, and a bridge portion connecting the pair of couplers; the bridge portion includes: a pair of beam portions that connect the respective pair of couplers and are disposed with a distance from each other; and at least one beam connecting portion that connects the pair of beam portions to each other. 13. The electric storage device according to claim 1, wherein:
the distance retaining member a fixation structure that is formed in the case and fixes a surface of a portion on a distal end side of each of the pair of current collectors, the surface facing the opposite current collector. 14. The electric storage device according to claim 13, wherein:
the fixation structure further fixes a surface opposite to the surface of the portion on the distal end side of each of the pair of current collectors, the latter surface facing the opposite current collector. 15. The electric storage device according to claim 13, wherein;
the case includes an opening into which the electrode assembly and the pair of current collectors are inserted, and a bottom portion opposite to the opening, and the fixation structure is a step portion formed at the bottom portion. 16. A spacer for connecting a pair of current collectors each of which is connected to a corresponding one of a positive electrode plate and a negative electrode plate, comprising:
a pair of couplers coupled to the respective current collectors; and a bridge portion connecting the pair of couplers, wherein the bridge portion is flexible so that a total length of the bridge portion extends by bending. 17. The spacer according to claim 16, wherein:
the bridge portion has opposite end portions and a central portion therebetween, the central portion being convex with reference to the opposite end portions. 18. The spacer according to claim 16, wherein:
the bridge portion has opposite end portions and a central portion therebetween, the central portion being concave with reference to the opposite end portions. 19. A spacer for connecting a pair of current collectors each of which is connected to a corresponding one of a positive electrode plate and a negative electrode plate, comprising:
a pair of couplers coupled to the respective current collectors; and a bridge portion connecting the pair of couplers, wherein at least one of the pair of couplers includes a deformable portion that expands by cooperation with the current collector, and a total length of the spacer extends by expansion of the deformable portion. 20. The spacer according to claim 19, wherein:
at least one of the pair of couplers includes: a main wall portion; the deformable portion facing the main wall portion with a distance therebetween; and a side portion that connects the main wall portion and the deformable portion and allows a distal portion of the current collector to be inserted into between the main wall portion and the deformable portion, and the deformable portion expands by interfering with the distal portion of the current collector inserted into between the main wall portion and the deformable portion. | 1,700 |
3,410 | 14,126,699 | 1,792 | A stock solution for making pelleted livestock feed or pet food, comprising: a) 20-50 wt %. of an organic acid selected from the group consisting of formic, acetic, propionic, butyric and mixtures thereof, b) 15-30 wt. % of ethoxylated castor oil surfactant having an HLB from 4 to 18 and a molar ratio of 1 molecule of castor oil to 40-60 molecules of ethylene oxide, c) 0-20 wt. % of propylene glycol, d) 0-50 wt. % of water, and a pelleted feed made therewith. | 1. A stock solution for making pelleted livestock feed or pet food, comprising:
a) 20-50 wt %. of an organic acid selected from the group consisting of formic, acetic, propionic, butyric and mixtures thereof, b) 15-30 wt. % of ethoxylated castor oil surfactant having an HLB from 4 to 18 and a molar ratio of 1 molecule of castor oil to 40-60 molecules of ethylene oxide, c) 0-20 wt. % of propylene glycol, d) 0-50 wt. % of water,
which is a solution at -10° C. 2. The stock solution of claim 1 diluted to an about 0.5 to 20.0 wt. % mixture in water. 3. The stock solution of claim 1, wherein the heat-treating composition is applied to the animal feed in an amount of 0.25 to 10 wt. % based on the weight of the feed. 4. The stock solution of claim 2, wherein energy consumption is improved at least 5% compared to a control sample treated with water. 5. The stock solution of claim 2, wherein pellet moisture is improved at least 0.4% compared to a control sample treated with water. 6. The stock solution of claim 2, wherein percent fines is improved at least 10% compared to a control sample treated with water. 7. The stock solution of claim 1, wherein a) contains acetic acid. 8. The stock solution of claim 1, wherein a) contains propionic acid. 9. The stock solution of claim 1, wherein a) contains butyric acid. 10. The stock solution of claim 1, wherein the acids of a) are unbuffered. 11. The stock solution of claim 1, wherein b) contains a second surfactant which is a non-ionic surfactant. 12. The stock solution of claim 1, wherein b) contains a second surfactant which is a non-ionic surfactant selected from polysorbates and polyoxyethylenes. 13. The stock solution of claim 1, which is a solution at −15° C. 14. A pelleted animal feed made by a process, comprising:
a stock solution containing a) 20-50 wt %. of an organic acid selected from the group consisting of formic, acetic, propionic, butyric and mixtures thereof, b) 15-30 wt. % of ethoxylated castor oil surfactant having an HLB from 4 to 18 and a molar ratio of 1 molecule of castor oil to 40-60 molecules of ethylene oxide, c) 0-20 wt. % of propylene glycol, d) 0-50 wt. % of water,
diluting said stock solution with 5 to 200 parts water to make a heat-treating composition, and applying an effective amount of the same to an animal feed or pet food, with sufficient heating to pelletize or extrude the feed. 15. The pelleted feed of claim 14, wherein the heat-treating composition is applied to the animal feed as an about 0.5 to 2.0 wt. % mixture in water. 16. The pelleted feed of claim 14, wherein the heat-treating composition is applied in an amount of 0.25 to 20 wt. % based on the weight of the animal feed. 17. The pelleted feed of claim 14, wherein energy consumption was improved at least 5% compared to a control sample treated with water. 18. The pelleted feed of claim 14, wherein pellet moisture is improved at least 0.4% compared to a control sample treated with water. 19. The pelleted feed of claim 14, wherein percent fines is improved at least 10% compared to a control sample treated with water. 20. The pelleted feed of claim 14, wherein a) contains acetic acid. 21. The pelleted feed of claim 14, wherein a) contains propionic acid. 22. The pelleted feed of claim 14, wherein a) contains butyric acid. 23. The pelleted feed of claim 14, wherein the acids of a) are unbuffered. 24. The pelleted feed of claim 14, wherein b) contains a second surfactant which is a non-ionic surfactant. 25. The pelleted feed of claim 14, wherein b) contains a second surfactant which is a non-ionic surfactant selected from polysorbates and polyoxyethylenes. | A stock solution for making pelleted livestock feed or pet food, comprising: a) 20-50 wt %. of an organic acid selected from the group consisting of formic, acetic, propionic, butyric and mixtures thereof, b) 15-30 wt. % of ethoxylated castor oil surfactant having an HLB from 4 to 18 and a molar ratio of 1 molecule of castor oil to 40-60 molecules of ethylene oxide, c) 0-20 wt. % of propylene glycol, d) 0-50 wt. % of water, and a pelleted feed made therewith.1. A stock solution for making pelleted livestock feed or pet food, comprising:
a) 20-50 wt %. of an organic acid selected from the group consisting of formic, acetic, propionic, butyric and mixtures thereof, b) 15-30 wt. % of ethoxylated castor oil surfactant having an HLB from 4 to 18 and a molar ratio of 1 molecule of castor oil to 40-60 molecules of ethylene oxide, c) 0-20 wt. % of propylene glycol, d) 0-50 wt. % of water,
which is a solution at -10° C. 2. The stock solution of claim 1 diluted to an about 0.5 to 20.0 wt. % mixture in water. 3. The stock solution of claim 1, wherein the heat-treating composition is applied to the animal feed in an amount of 0.25 to 10 wt. % based on the weight of the feed. 4. The stock solution of claim 2, wherein energy consumption is improved at least 5% compared to a control sample treated with water. 5. The stock solution of claim 2, wherein pellet moisture is improved at least 0.4% compared to a control sample treated with water. 6. The stock solution of claim 2, wherein percent fines is improved at least 10% compared to a control sample treated with water. 7. The stock solution of claim 1, wherein a) contains acetic acid. 8. The stock solution of claim 1, wherein a) contains propionic acid. 9. The stock solution of claim 1, wherein a) contains butyric acid. 10. The stock solution of claim 1, wherein the acids of a) are unbuffered. 11. The stock solution of claim 1, wherein b) contains a second surfactant which is a non-ionic surfactant. 12. The stock solution of claim 1, wherein b) contains a second surfactant which is a non-ionic surfactant selected from polysorbates and polyoxyethylenes. 13. The stock solution of claim 1, which is a solution at −15° C. 14. A pelleted animal feed made by a process, comprising:
a stock solution containing a) 20-50 wt %. of an organic acid selected from the group consisting of formic, acetic, propionic, butyric and mixtures thereof, b) 15-30 wt. % of ethoxylated castor oil surfactant having an HLB from 4 to 18 and a molar ratio of 1 molecule of castor oil to 40-60 molecules of ethylene oxide, c) 0-20 wt. % of propylene glycol, d) 0-50 wt. % of water,
diluting said stock solution with 5 to 200 parts water to make a heat-treating composition, and applying an effective amount of the same to an animal feed or pet food, with sufficient heating to pelletize or extrude the feed. 15. The pelleted feed of claim 14, wherein the heat-treating composition is applied to the animal feed as an about 0.5 to 2.0 wt. % mixture in water. 16. The pelleted feed of claim 14, wherein the heat-treating composition is applied in an amount of 0.25 to 20 wt. % based on the weight of the animal feed. 17. The pelleted feed of claim 14, wherein energy consumption was improved at least 5% compared to a control sample treated with water. 18. The pelleted feed of claim 14, wherein pellet moisture is improved at least 0.4% compared to a control sample treated with water. 19. The pelleted feed of claim 14, wherein percent fines is improved at least 10% compared to a control sample treated with water. 20. The pelleted feed of claim 14, wherein a) contains acetic acid. 21. The pelleted feed of claim 14, wherein a) contains propionic acid. 22. The pelleted feed of claim 14, wherein a) contains butyric acid. 23. The pelleted feed of claim 14, wherein the acids of a) are unbuffered. 24. The pelleted feed of claim 14, wherein b) contains a second surfactant which is a non-ionic surfactant. 25. The pelleted feed of claim 14, wherein b) contains a second surfactant which is a non-ionic surfactant selected from polysorbates and polyoxyethylenes. | 1,700 |
3,411 | 14,743,960 | 1,799 | Systems and methods for containing and manipulating liquids, including vessels and unit operations or components of cell culture, cell containment, bioreactor, and/or pharmaceutical manufacturing systems, are provided. In certain embodiments, such vessels and unit operations are directed to continuous perfusion reactor or bioreactor systems and may include one or more disposable components. For instance, in one aspect, a system includes an apparatus in the form of a bioreactor for harvesting cells which produce one or more products. The apparatus may include a disposable, collapsible bag adapted for containing a liquid, the collapsible bag in fluid communication with a liquid-solids (e.g., cell) separation device. For example, an outlet of the collapsible bag may be connected to an inlet of the separation device, and an outlet of the separation device may be connected to an inlet of the collapsible bag for recycle. Accordingly, after separating the cells from the liquid in the separation device, the cells can be flowed back into the collapsible bag where they can be re-harvested. Meanwhile, product contained in the liquid can be collected in a separate container. The efficiency of product formation in such a system may be enhanced by using mixing systems described herein. | 1. A system, comprising:
a first apparatus, comprising: a first collapsible bag adapted for containing a liquid, the first collapsible bag including at least one inlet, at least one outlet, and a base plate that is attached to the collapsible bag and configured to support an impeller; a first reusable support structure adapted for surrounding and supporting the first collapsible bag; and a second apparatus in fluid communication with the first apparatus, the second apparatus including at least one inlet and at least one outlet, wherein an outlet of the first collapsible bag is in fluid communication with an inlet of the second apparatus, and an outlet of the second apparatus is in fluid communication with an inlet of the first collapsible bag. 2. A system as in claim 1, wherein the second apparatus is configured to receive a first liquid comprising a first concentration of a component from the first apparatus and to deliver a second liquid comprising a second concentration of the component to the first apparatus, wherein the first and second concentrations are different. 3-6. (canceled) 7. A system as in claim 1, wherein the components include a solid object that comprises a cell. 8. (canceled) 9. A system as in claim 1, wherein the second apparatus comprises a second collapsible bag. 10. A system as in claim 1, wherein the second apparatus comprises a second reusable support structure adapted for surrounding and supporting the second collapsible bag. 11-12. (canceled) 13. A system as in claim 1, further comprising an impeller associated with the base plate wherein the impeller is magnetically-driven. 14-16. (canceled) 17. A system as in claim 1, wherein the first apparatus forms at least part of a bioreactor system. 18. A system as in claim 1, wherein the first apparatus forms at least part of a pharmaceutical manufacturing system. 19. (canceled) 20. A system as in claim 1, wherein the first collapsible bag has a volume of at least 40 L. 21. (canceled) 22. A system as in claim 1, wherein the second apparatus forms at least part of a separation device and the separation device is a liquid-solids separation device. 23. A system as in claim 1, wherein the second apparatus forms at least part of a separation device and the separation device comprises a centrifuge. 24. (canceled) 25. A system as in claim 1, wherein the second apparatus forms at least part of a separation device and the separation is adapted for separating cells from a liquid. 26. A system as in claim 1, wherein the second apparatus forms at least part of a separation device and the separation device comprises a hollow fiber filter. 27-31. (canceled) 32. A system as in claim 1, wherein the second apparatus forms at least part of a media or buffer storage tank. 33. A system as in claim 1, wherein the second apparatus forms at least part of a mixing system. 34. A system as in claim 1, wherein the second apparatus forms at least part of a batch harvesting tank. 35-38. (canceled) 39. A system, comprising:
a first apparatus in the form a portable module, comprising:
a first collapsible bag adapted for containing a liquid;
a first reusable support structure adapted for surrounding and supporting the collapsible bag; and
a second apparatus in the form a portable module, the second apparatus in fluid communication with the first apparatus, wherein the second apparatus comprises a liquid-solids separation device, wherein upon fluid communication between the first and second apparatuses, each apparatus can be moved relative to the other without breaking the connection. 40. A system as in claim 39, wherein the first collapsible bag comprises a base plate that is attached to the collapsible bag and configured to support an impeller. 41. A system as in claim 40, further comprising an impeller associated with the base plate wherein the impeller is magnetically-driven. 42-43. (canceled) 44. A system, comprising:
a first apparatus comprising:
a first collapsible bag adapted for containing a liquid, the first collapsible bag including at least one inlet and at least one outlet;
a first reusable support structure adapted for surrounding and supporting the first collapsible bag; and
a second apparatus in fluid communication with the first apparatus, the second apparatus comprising:
a second collapsible bag adapted for containing a liquid, the second collapsible bag including at least one inlet and at least one outlet; and
a second reusable support structure adapted for surrounding and supporting the second collapsible bag,
wherein an outlet of the first collapsible bag is in fluid communication with an inlet of the second collapsible bag, and an outlet of the second collapsible bag is in fluid communication with an inlet of the first collapsible bag. 45. A system as in claim 44, wherein the first collapsible bag comprises a base plate that is attached to the collapsible bag and configured to support an impeller. 46. A system as in claim 45, further comprising an impeller associated with the base plate wherein the impeller is magnetically-driven. 47-48. (canceled) 49. A system, comprising:
a first apparatus comprising:
a first collapsible bag adapted for containing a liquid;
a first reusable support structure adapted for surrounding and supporting the collapsible bag; and
a second apparatus in fluid communication with the first apparatus, the second apparatus comprising a centrifuge adapted for separating a plurality of particulates or solid objects from a liquid-solids mixture. 50. A method, comprising:
transferring a first liquid comprising a plurality of particulates or solid objects from a first collapsible bag to an apparatus including a liquid-solids separation device, wherein the first collapsible bag is supported by a first reusable support structure adapted for surrounding and supporting the first collapsible bag; separating at least a portion of the plurality of particulates or solid objects from the first liquid in the apparatus; and transferring a second liquid from the apparatus to the first collapsible bag,
wherein the first and second liquids have different concentrations of the particulates or solid objects. 51. A method as in claim 50, wherein the apparatus is external to the collapsible bag. 52. (canceled) 53. A method comprising:
continuously introducing a first liquid into a collapsible bag comprising an impeller, the first liquid having a first concentration of a particulate or solid objects, wherein the collapsible bag is supported by a reusable support structure adapted for surrounding and supporting the collapsible bag; continuously removing a second liquid from the collapsible bag, the second liquid having a second concentration of the particulate or solid objects, wherein the first and second concentrations of the particulate or solid objects is different; and maintaining a substantially constant volume within the collapsible bag during the introducing and removing steps. 55. (canceled) 56. A method, comprising:
introducing a first liquid into a collapsible bag comprising an impeller, the first liquid having a first concentration of a particulate or solid objects, wherein the collapsible bag is supported by a reusable support structure adapted for surrounding and supporting the collapsible bag; mixing the first liquid in the collapsible bag using the impeller; and removing a second liquid from the collapsible bag, the second liquid having a second concentration of the particulate or solid objects, wherein the first and second concentrations of the particulate or solid object is different, wherein the second liquid is substantially homogenous with respect to liquid remaining in the collapsible bag immediately after removal, such that the concentration of the particulate or solid objects in the second liquid removed from the collapsible bag is substantially equivalent to the concentration of the particulate or solid objects in the liquid remaining in the collapsible bag immediately after removal; causing a liquid to flow from the collapsible bag to an apparatus; and causing a liquid to flow from the apparatus to the collapsible bag. 57. A method as in claim 56, further comprising maintaining a substantially constant volume within the collapsible bag during the introducing and removing steps. | Systems and methods for containing and manipulating liquids, including vessels and unit operations or components of cell culture, cell containment, bioreactor, and/or pharmaceutical manufacturing systems, are provided. In certain embodiments, such vessels and unit operations are directed to continuous perfusion reactor or bioreactor systems and may include one or more disposable components. For instance, in one aspect, a system includes an apparatus in the form of a bioreactor for harvesting cells which produce one or more products. The apparatus may include a disposable, collapsible bag adapted for containing a liquid, the collapsible bag in fluid communication with a liquid-solids (e.g., cell) separation device. For example, an outlet of the collapsible bag may be connected to an inlet of the separation device, and an outlet of the separation device may be connected to an inlet of the collapsible bag for recycle. Accordingly, after separating the cells from the liquid in the separation device, the cells can be flowed back into the collapsible bag where they can be re-harvested. Meanwhile, product contained in the liquid can be collected in a separate container. The efficiency of product formation in such a system may be enhanced by using mixing systems described herein.1. A system, comprising:
a first apparatus, comprising: a first collapsible bag adapted for containing a liquid, the first collapsible bag including at least one inlet, at least one outlet, and a base plate that is attached to the collapsible bag and configured to support an impeller; a first reusable support structure adapted for surrounding and supporting the first collapsible bag; and a second apparatus in fluid communication with the first apparatus, the second apparatus including at least one inlet and at least one outlet, wherein an outlet of the first collapsible bag is in fluid communication with an inlet of the second apparatus, and an outlet of the second apparatus is in fluid communication with an inlet of the first collapsible bag. 2. A system as in claim 1, wherein the second apparatus is configured to receive a first liquid comprising a first concentration of a component from the first apparatus and to deliver a second liquid comprising a second concentration of the component to the first apparatus, wherein the first and second concentrations are different. 3-6. (canceled) 7. A system as in claim 1, wherein the components include a solid object that comprises a cell. 8. (canceled) 9. A system as in claim 1, wherein the second apparatus comprises a second collapsible bag. 10. A system as in claim 1, wherein the second apparatus comprises a second reusable support structure adapted for surrounding and supporting the second collapsible bag. 11-12. (canceled) 13. A system as in claim 1, further comprising an impeller associated with the base plate wherein the impeller is magnetically-driven. 14-16. (canceled) 17. A system as in claim 1, wherein the first apparatus forms at least part of a bioreactor system. 18. A system as in claim 1, wherein the first apparatus forms at least part of a pharmaceutical manufacturing system. 19. (canceled) 20. A system as in claim 1, wherein the first collapsible bag has a volume of at least 40 L. 21. (canceled) 22. A system as in claim 1, wherein the second apparatus forms at least part of a separation device and the separation device is a liquid-solids separation device. 23. A system as in claim 1, wherein the second apparatus forms at least part of a separation device and the separation device comprises a centrifuge. 24. (canceled) 25. A system as in claim 1, wherein the second apparatus forms at least part of a separation device and the separation is adapted for separating cells from a liquid. 26. A system as in claim 1, wherein the second apparatus forms at least part of a separation device and the separation device comprises a hollow fiber filter. 27-31. (canceled) 32. A system as in claim 1, wherein the second apparatus forms at least part of a media or buffer storage tank. 33. A system as in claim 1, wherein the second apparatus forms at least part of a mixing system. 34. A system as in claim 1, wherein the second apparatus forms at least part of a batch harvesting tank. 35-38. (canceled) 39. A system, comprising:
a first apparatus in the form a portable module, comprising:
a first collapsible bag adapted for containing a liquid;
a first reusable support structure adapted for surrounding and supporting the collapsible bag; and
a second apparatus in the form a portable module, the second apparatus in fluid communication with the first apparatus, wherein the second apparatus comprises a liquid-solids separation device, wherein upon fluid communication between the first and second apparatuses, each apparatus can be moved relative to the other without breaking the connection. 40. A system as in claim 39, wherein the first collapsible bag comprises a base plate that is attached to the collapsible bag and configured to support an impeller. 41. A system as in claim 40, further comprising an impeller associated with the base plate wherein the impeller is magnetically-driven. 42-43. (canceled) 44. A system, comprising:
a first apparatus comprising:
a first collapsible bag adapted for containing a liquid, the first collapsible bag including at least one inlet and at least one outlet;
a first reusable support structure adapted for surrounding and supporting the first collapsible bag; and
a second apparatus in fluid communication with the first apparatus, the second apparatus comprising:
a second collapsible bag adapted for containing a liquid, the second collapsible bag including at least one inlet and at least one outlet; and
a second reusable support structure adapted for surrounding and supporting the second collapsible bag,
wherein an outlet of the first collapsible bag is in fluid communication with an inlet of the second collapsible bag, and an outlet of the second collapsible bag is in fluid communication with an inlet of the first collapsible bag. 45. A system as in claim 44, wherein the first collapsible bag comprises a base plate that is attached to the collapsible bag and configured to support an impeller. 46. A system as in claim 45, further comprising an impeller associated with the base plate wherein the impeller is magnetically-driven. 47-48. (canceled) 49. A system, comprising:
a first apparatus comprising:
a first collapsible bag adapted for containing a liquid;
a first reusable support structure adapted for surrounding and supporting the collapsible bag; and
a second apparatus in fluid communication with the first apparatus, the second apparatus comprising a centrifuge adapted for separating a plurality of particulates or solid objects from a liquid-solids mixture. 50. A method, comprising:
transferring a first liquid comprising a plurality of particulates or solid objects from a first collapsible bag to an apparatus including a liquid-solids separation device, wherein the first collapsible bag is supported by a first reusable support structure adapted for surrounding and supporting the first collapsible bag; separating at least a portion of the plurality of particulates or solid objects from the first liquid in the apparatus; and transferring a second liquid from the apparatus to the first collapsible bag,
wherein the first and second liquids have different concentrations of the particulates or solid objects. 51. A method as in claim 50, wherein the apparatus is external to the collapsible bag. 52. (canceled) 53. A method comprising:
continuously introducing a first liquid into a collapsible bag comprising an impeller, the first liquid having a first concentration of a particulate or solid objects, wherein the collapsible bag is supported by a reusable support structure adapted for surrounding and supporting the collapsible bag; continuously removing a second liquid from the collapsible bag, the second liquid having a second concentration of the particulate or solid objects, wherein the first and second concentrations of the particulate or solid objects is different; and maintaining a substantially constant volume within the collapsible bag during the introducing and removing steps. 55. (canceled) 56. A method, comprising:
introducing a first liquid into a collapsible bag comprising an impeller, the first liquid having a first concentration of a particulate or solid objects, wherein the collapsible bag is supported by a reusable support structure adapted for surrounding and supporting the collapsible bag; mixing the first liquid in the collapsible bag using the impeller; and removing a second liquid from the collapsible bag, the second liquid having a second concentration of the particulate or solid objects, wherein the first and second concentrations of the particulate or solid object is different, wherein the second liquid is substantially homogenous with respect to liquid remaining in the collapsible bag immediately after removal, such that the concentration of the particulate or solid objects in the second liquid removed from the collapsible bag is substantially equivalent to the concentration of the particulate or solid objects in the liquid remaining in the collapsible bag immediately after removal; causing a liquid to flow from the collapsible bag to an apparatus; and causing a liquid to flow from the apparatus to the collapsible bag. 57. A method as in claim 56, further comprising maintaining a substantially constant volume within the collapsible bag during the introducing and removing steps. | 1,700 |
3,412 | 14,595,947 | 1,777 | An arrangement for mounting components in a heating chamber for heating a fluid of a fluid separation apparatus, wherein the arrangement comprises a mounting board having at least one mounting recess each configured for accommodating at least one component, and the at least one component each configured to be mountable in and/or on the at least one mounting recess. | 1. An arrangement for mounting components in a heating chamber for heating a fluid of a fluid separation apparatus, wherein the arrangement comprises:
a mounting board having at least one mounting recess each configured for accommodating at least one component; and the at least one component, wherein each of the at least one component is configured to be mountable in and/or on the at least one mounting recess, wherein each component comprises slanted surfaces corresponding to slanted surfaces of the respective mounting recess. 2. The arrangement of claim 1, wherein the at least one component comprises a pre-heater assembly for heating the fluid upstream of a separation unit of the fluid separation apparatus, wherein the pre-heater assembly comprises a capillary having a lumen and being configured for conducting the fluid and a thermal coupling body contacting at least part of the capillary and being arrangable so that heat generated by a heat source is supplied to the capillary via at least part of the thermal coupling body. 3. The arrangement of claim 1, further comprising a heat source, in particular a Peltier heat source, configured for generating heat for heating the mounting board. 4. The arrangement of claim 3, wherein the heat source is attached to the mounting board, in particular to a backside of the mounting board opposing a front side at which the at least one mounting recess is arranged. 5. The arrangement of claim 1, comprising at least one of the following features:
the mounting board is made of a material having a value of the thermal conductivity of at least 150 W/(m K), in particular comprises or consists of aluminum or copper; the at least one mounting recess is configured as at least one mounting groove within the, in particular substantially plate-shaped, mounting board; the at least one component comprises a holder configured for holding another one of the at least one component; the at least one component comprises at least one of a separation unit holder configured for holding a separation unit for separating the fluid in the fluid separation apparatus; the at least one component comprises a pre-heater assembly holder for holding a pre-heater assembly for pre-heating the fluid in the fluid separation apparatus. 6. The arrangement of claim 1, wherein the at least one mounting recess comprises an interior recess section configured for accommodating a first one of the at least one component and comprises an exterior recess section arranged between the interior recess section and a surrounding of the mounting board and being configured for accommodating a second one of the at least one component. 7. The arrangement of claim 6, comprising at least one of the following features:
the exterior recess section has an undercut, in particular one of a dovetail-type undercut, a triangular undercut, and a T-shaped undercut; the interior recess section, the exterior recess section, the first component and the second component are configured to match to one another so that the second component is mountable within the exterior recess section while the first component is already mounted in the interior recess section; the first component is a pre-heater assembly and the second component is a fastening element for fastening the pre-heater assembly to the mounting recess; the first component is a pre-heater assembly and the second component is a separation unit holder for holding a separation unit for separating the fluid in the fluid separation apparatus. 8. The arrangement of claim 1, further comprising a fastening element, in particular integrally formed with the component, configured for fastening the component in the mounting recess. 9. The arrangement of claim 8, wherein the fastening element is configured to be actuable by turning to thereby fasten the component in the mounting recess. 10. The arrangement of claim 9, wherein the fastening element is configured for fastening the component in the mounting recess by attaching the component to the mounting recess and subsequently actuating the fastening element to thereby fasten the fastening element in an undercut section of the mounting recess. 11. A heating chamber for heating a fluid of a fluid separation apparatus, wherein the heating chamber comprises an arrangement of claim 1. 12. The arrangement of claim 1, wherein each of the slanted surfaces is substantially V-shaped. 13. A fluid separation apparatus for separating a fluidic sample into a plurality of fractions, the apparatus comprising:
a fluid drive unit configured for driving a fluid comprising a mobile phase and the fluidic sample in the mobile phase; a separation unit configured for separating the fluidic sample into the plurality of fractions; and at least one of the group consisting of an arrangement of claim 1 for heating the fluid upstream of and/or in the separation unit. 14. A method of mounting components in a heating chamber for heating a fluid of a fluid separation apparatus, wherein the method comprises:
providing a mounting board having at least one mounting recess each configured for accommodating at least one component; and mounting the at least one component in and/or on the at least one mounting recess. | An arrangement for mounting components in a heating chamber for heating a fluid of a fluid separation apparatus, wherein the arrangement comprises a mounting board having at least one mounting recess each configured for accommodating at least one component, and the at least one component each configured to be mountable in and/or on the at least one mounting recess.1. An arrangement for mounting components in a heating chamber for heating a fluid of a fluid separation apparatus, wherein the arrangement comprises:
a mounting board having at least one mounting recess each configured for accommodating at least one component; and the at least one component, wherein each of the at least one component is configured to be mountable in and/or on the at least one mounting recess, wherein each component comprises slanted surfaces corresponding to slanted surfaces of the respective mounting recess. 2. The arrangement of claim 1, wherein the at least one component comprises a pre-heater assembly for heating the fluid upstream of a separation unit of the fluid separation apparatus, wherein the pre-heater assembly comprises a capillary having a lumen and being configured for conducting the fluid and a thermal coupling body contacting at least part of the capillary and being arrangable so that heat generated by a heat source is supplied to the capillary via at least part of the thermal coupling body. 3. The arrangement of claim 1, further comprising a heat source, in particular a Peltier heat source, configured for generating heat for heating the mounting board. 4. The arrangement of claim 3, wherein the heat source is attached to the mounting board, in particular to a backside of the mounting board opposing a front side at which the at least one mounting recess is arranged. 5. The arrangement of claim 1, comprising at least one of the following features:
the mounting board is made of a material having a value of the thermal conductivity of at least 150 W/(m K), in particular comprises or consists of aluminum or copper; the at least one mounting recess is configured as at least one mounting groove within the, in particular substantially plate-shaped, mounting board; the at least one component comprises a holder configured for holding another one of the at least one component; the at least one component comprises at least one of a separation unit holder configured for holding a separation unit for separating the fluid in the fluid separation apparatus; the at least one component comprises a pre-heater assembly holder for holding a pre-heater assembly for pre-heating the fluid in the fluid separation apparatus. 6. The arrangement of claim 1, wherein the at least one mounting recess comprises an interior recess section configured for accommodating a first one of the at least one component and comprises an exterior recess section arranged between the interior recess section and a surrounding of the mounting board and being configured for accommodating a second one of the at least one component. 7. The arrangement of claim 6, comprising at least one of the following features:
the exterior recess section has an undercut, in particular one of a dovetail-type undercut, a triangular undercut, and a T-shaped undercut; the interior recess section, the exterior recess section, the first component and the second component are configured to match to one another so that the second component is mountable within the exterior recess section while the first component is already mounted in the interior recess section; the first component is a pre-heater assembly and the second component is a fastening element for fastening the pre-heater assembly to the mounting recess; the first component is a pre-heater assembly and the second component is a separation unit holder for holding a separation unit for separating the fluid in the fluid separation apparatus. 8. The arrangement of claim 1, further comprising a fastening element, in particular integrally formed with the component, configured for fastening the component in the mounting recess. 9. The arrangement of claim 8, wherein the fastening element is configured to be actuable by turning to thereby fasten the component in the mounting recess. 10. The arrangement of claim 9, wherein the fastening element is configured for fastening the component in the mounting recess by attaching the component to the mounting recess and subsequently actuating the fastening element to thereby fasten the fastening element in an undercut section of the mounting recess. 11. A heating chamber for heating a fluid of a fluid separation apparatus, wherein the heating chamber comprises an arrangement of claim 1. 12. The arrangement of claim 1, wherein each of the slanted surfaces is substantially V-shaped. 13. A fluid separation apparatus for separating a fluidic sample into a plurality of fractions, the apparatus comprising:
a fluid drive unit configured for driving a fluid comprising a mobile phase and the fluidic sample in the mobile phase; a separation unit configured for separating the fluidic sample into the plurality of fractions; and at least one of the group consisting of an arrangement of claim 1 for heating the fluid upstream of and/or in the separation unit. 14. A method of mounting components in a heating chamber for heating a fluid of a fluid separation apparatus, wherein the method comprises:
providing a mounting board having at least one mounting recess each configured for accommodating at least one component; and mounting the at least one component in and/or on the at least one mounting recess. | 1,700 |
3,413 | 13,781,927 | 1,735 | Methods and systems for low-force, low-temperature thermocompression bonding. The present application teaches new methods and structures for three-dimensional integrated circuits, in which cold thermocompression bonding is used to provide reliable bonding. To achieve this, reduction and passivation steps are preferably both used to reduce native oxide on the contact metals and to prevent reformation of native oxide, preferably using atmospheric plasma treatments. Preferably the physical compression height of the elements is set to be only enough to reliably achieve at least some compression of each bonding element pair, compensating for any lack of flatness. Preferably the thermocompression bonding is performed well below the melting point. This not only avoids the deformation of lower levels which is induced by reflow techniques, but also provides a steep relation of force versus z-axis travel, so that a drastically-increasing resistance to compression helps to regulate the degree of thermocompression. | 1. A method for bonding microelectronic elements, comprising the steps of:
a) directing plasma-activated radical-enriched gas flow at substantially atmospheric pressure both to first contacting metallizations on a first element and also to second contacting metallizations on a second element, both to reduce native oxides from said contacting metallizations and also to passivate said contacting metallizations against re-oxidation; b) compressing said first and second contacting metallizations together, without any conductive liquid phase material, to thereby bond said second element to said first element; c) repeating said steps a) and b), to thereby bond contacting metallizations on subsequent elements to contacting metallizations on the previous element. 2. The method of claim 1, wherein said second element has contacting metallizations both on a first side and also on a second side. 3. The method of claim 1, wherein said directing step moves said plasma-activated radical-enriched gas flow across contacting metallizations on each said element. 4. The method of claim 1, wherein said directing step reduces native oxides from said contacting metallizations and passivates said contacting metallizations against re-oxidation simultaneously. 5. The method of claim 1, wherein said first contacting metallizations are contacting metallization pads, and said second contacting metallizations are contacting metallization bumps. 6. The method of claim 1, wherein said compressing step deforms said second contacting metallizations, but does not substantially deform said first contacting metallizations. 7. The method of claim 1, wherein said contacting metallizations are identical. 8. The method of claim 1, wherein said first contacting metallizations are contacting metallization bumps. 9. The method of claim 1, wherein said first contacting metallizations are contacting metallization pads. 10. The method of claim 1, wherein said first contacting metallizations are contacting metallization pillars. 11. The method of claim 1, wherein said first and second contacting metallizations have differing metallic compositions. 12. The method of claim 1, further comprising the step of bonding an additional element to the previous elements by said steps a) and b), wherein only one side of said additional element has contacting metallizations. 13. The method of claim 1, wherein said compressing step is performed at a temperature which is below the melting points of said contacting metallizations. 14. The method of claim 1, wherein said compressing step is performed at room temperature. 15. The method of claim 1, wherein said compressing step compresses said contacting metallizations by no more than 40% of the initial heights of said contacting metallizations. 16. The method of claim 1, wherein said compressing step compresses said contacting metallizations by no more than 30% of the initial heights of said contacting metallizations. 17. The method of claim 1, wherein the reducing and passivating steps occur sequentially for each surface. 18. The method of claim 1, further comprising heating said elements during said compressing step. 19.-24. (canceled) 25. A method for bonding microelectronic elements, comprising the steps of:
a) using plasma-activated radical-enriched gas flow at substantially atmospheric pressure: to reduce native oxides from the surfaces of first contacting metallizations on a first element; to passivate the surfaces of said first contacting metallizations against re-oxidation; to reduce native oxides from the surfaces of second contacting metallizations on a second element; and to passivate the surfaces of said second contacting metallizations against re-oxidation; b) compressing said first and second contacting metallizations together, without any conductive liquid phase material, to thereby bond said second element to said first element; c) repeating said steps a) and b), to thereby bond contacting metallizations on subsequent elements to contacting metallizations on the previous element; wherein said step of compressing said first and second contacting metallizations together joins one of said contacting metallizations which is of a first type together with another of said contacting metallizations which is of a second type. 26.-47. (canceled) 48. A method for bonding microelectronic elements, comprising:
forming a plurality of elements respectively having contacting metallizations both on a first side and also on a second side; forming at least one one-sided element having contacting metallizations on only one side; a) treating both first contacting metallizations on a first element and second contacting metallizations on a second element with plasma-activated radical-enriched gas flow at substantially atmospheric pressure; wherein said treating step reduces native oxides both from said first and second contacting metallizations, and also inhibits oxide re-formation thereupon; b) aligning and contacting said first and second contacting metallizations, without any conductive liquid phase material, to thereby bond said first and second elements; and c) repeating said steps a) and b), to thereby bond the contacting metallizations on subsequent elements to the contacting metallizations on the previous element; wherein said step of contacting said first and second contacting metallizations together joins one of said contacting metallizations which is of a first type together with another of said contacting metallizations which is of a second type; and repeating said steps a) and b), to thereby bond the contacting metallizations on an element to the contacting metallizations on a one-sided element. 49.-253. (canceled) | Methods and systems for low-force, low-temperature thermocompression bonding. The present application teaches new methods and structures for three-dimensional integrated circuits, in which cold thermocompression bonding is used to provide reliable bonding. To achieve this, reduction and passivation steps are preferably both used to reduce native oxide on the contact metals and to prevent reformation of native oxide, preferably using atmospheric plasma treatments. Preferably the physical compression height of the elements is set to be only enough to reliably achieve at least some compression of each bonding element pair, compensating for any lack of flatness. Preferably the thermocompression bonding is performed well below the melting point. This not only avoids the deformation of lower levels which is induced by reflow techniques, but also provides a steep relation of force versus z-axis travel, so that a drastically-increasing resistance to compression helps to regulate the degree of thermocompression.1. A method for bonding microelectronic elements, comprising the steps of:
a) directing plasma-activated radical-enriched gas flow at substantially atmospheric pressure both to first contacting metallizations on a first element and also to second contacting metallizations on a second element, both to reduce native oxides from said contacting metallizations and also to passivate said contacting metallizations against re-oxidation; b) compressing said first and second contacting metallizations together, without any conductive liquid phase material, to thereby bond said second element to said first element; c) repeating said steps a) and b), to thereby bond contacting metallizations on subsequent elements to contacting metallizations on the previous element. 2. The method of claim 1, wherein said second element has contacting metallizations both on a first side and also on a second side. 3. The method of claim 1, wherein said directing step moves said plasma-activated radical-enriched gas flow across contacting metallizations on each said element. 4. The method of claim 1, wherein said directing step reduces native oxides from said contacting metallizations and passivates said contacting metallizations against re-oxidation simultaneously. 5. The method of claim 1, wherein said first contacting metallizations are contacting metallization pads, and said second contacting metallizations are contacting metallization bumps. 6. The method of claim 1, wherein said compressing step deforms said second contacting metallizations, but does not substantially deform said first contacting metallizations. 7. The method of claim 1, wherein said contacting metallizations are identical. 8. The method of claim 1, wherein said first contacting metallizations are contacting metallization bumps. 9. The method of claim 1, wherein said first contacting metallizations are contacting metallization pads. 10. The method of claim 1, wherein said first contacting metallizations are contacting metallization pillars. 11. The method of claim 1, wherein said first and second contacting metallizations have differing metallic compositions. 12. The method of claim 1, further comprising the step of bonding an additional element to the previous elements by said steps a) and b), wherein only one side of said additional element has contacting metallizations. 13. The method of claim 1, wherein said compressing step is performed at a temperature which is below the melting points of said contacting metallizations. 14. The method of claim 1, wherein said compressing step is performed at room temperature. 15. The method of claim 1, wherein said compressing step compresses said contacting metallizations by no more than 40% of the initial heights of said contacting metallizations. 16. The method of claim 1, wherein said compressing step compresses said contacting metallizations by no more than 30% of the initial heights of said contacting metallizations. 17. The method of claim 1, wherein the reducing and passivating steps occur sequentially for each surface. 18. The method of claim 1, further comprising heating said elements during said compressing step. 19.-24. (canceled) 25. A method for bonding microelectronic elements, comprising the steps of:
a) using plasma-activated radical-enriched gas flow at substantially atmospheric pressure: to reduce native oxides from the surfaces of first contacting metallizations on a first element; to passivate the surfaces of said first contacting metallizations against re-oxidation; to reduce native oxides from the surfaces of second contacting metallizations on a second element; and to passivate the surfaces of said second contacting metallizations against re-oxidation; b) compressing said first and second contacting metallizations together, without any conductive liquid phase material, to thereby bond said second element to said first element; c) repeating said steps a) and b), to thereby bond contacting metallizations on subsequent elements to contacting metallizations on the previous element; wherein said step of compressing said first and second contacting metallizations together joins one of said contacting metallizations which is of a first type together with another of said contacting metallizations which is of a second type. 26.-47. (canceled) 48. A method for bonding microelectronic elements, comprising:
forming a plurality of elements respectively having contacting metallizations both on a first side and also on a second side; forming at least one one-sided element having contacting metallizations on only one side; a) treating both first contacting metallizations on a first element and second contacting metallizations on a second element with plasma-activated radical-enriched gas flow at substantially atmospheric pressure; wherein said treating step reduces native oxides both from said first and second contacting metallizations, and also inhibits oxide re-formation thereupon; b) aligning and contacting said first and second contacting metallizations, without any conductive liquid phase material, to thereby bond said first and second elements; and c) repeating said steps a) and b), to thereby bond the contacting metallizations on subsequent elements to the contacting metallizations on the previous element; wherein said step of contacting said first and second contacting metallizations together joins one of said contacting metallizations which is of a first type together with another of said contacting metallizations which is of a second type; and repeating said steps a) and b), to thereby bond the contacting metallizations on an element to the contacting metallizations on a one-sided element. 49.-253. (canceled) | 1,700 |
3,414 | 11,813,764 | 1,788 | A gasket material comprising a fibre component, a rubber component and a further resilient material is described. The further resilient material comprises chemically exfoliated vermiculite (CEV). A novel process of production is also described. The product has high stress retention and excellent sealing performance at high temperatures. Preferably, the gas permeability of the gasket material is less than 1.0 ml/min and the hot creep of the gasket material is less than 15%. | 1. A gasket material comprising a fiber component, a rubber component and a further resilient material, wherein the fiber component comprises a fibrillating fiber component and a further fiber component, wherein the further fiber component comprises 15-40% w/w of the final dried gasket and wherein the further resilient material comprises chemically exfoliated vermiculite (CEV) component. 2. A gasket material according to claim 1, wherein the rubber component is present at a level of less than 10% w/w in the final dried gasket material. 3. A gasket according to claim 1, wherein the gasket material is in the form of a sheet. 4. A gasket material according to claim 1, wherein the fiber component comprises a fibrillating fiber. 5. A gasket material according to claim 4, wherein the fiber component comprises a further fiber. 6. A gasket material according to claim 1, wherein the further resilient material comprises 1-95% w/w of the final dried gasket. 7. A gasket material according to claim 1, wherein the CEV component is at least partially derived from dry CEV. 8. A gasket material according to claim 1, wherein the further resilient material further comprises a plate like filler material. 9. A gasket material according to claim 1, wherein the fiber component is present at a level of 6-70% w/w. 10. A gasket material according to claim 1, wherein the fibrillating fiber component comprises between 1-25% w/w of the final dried gasket. 11. A gasket material according to claim 1, wherein the further fiber component comprises 5-45% w/w of the final dried gasket. 12. A process for the production of a gasket material comprising: mixing at least a fiber component and CEV into a wet dough, and calendaring the wet dough. 13. A process according to claim 12, wherein the mixing incorporates a rubber component. 14. A gasket material according to claim 1, wherein the gasket comprises a plurality of laminated layers. 15. A gasket material comprising a fibre component, a rubber component derived from a rubber solution and a further resilient material, wherein the further resilient material comprises chemically exfoliated vermiculite (CEV). | A gasket material comprising a fibre component, a rubber component and a further resilient material is described. The further resilient material comprises chemically exfoliated vermiculite (CEV). A novel process of production is also described. The product has high stress retention and excellent sealing performance at high temperatures. Preferably, the gas permeability of the gasket material is less than 1.0 ml/min and the hot creep of the gasket material is less than 15%.1. A gasket material comprising a fiber component, a rubber component and a further resilient material, wherein the fiber component comprises a fibrillating fiber component and a further fiber component, wherein the further fiber component comprises 15-40% w/w of the final dried gasket and wherein the further resilient material comprises chemically exfoliated vermiculite (CEV) component. 2. A gasket material according to claim 1, wherein the rubber component is present at a level of less than 10% w/w in the final dried gasket material. 3. A gasket according to claim 1, wherein the gasket material is in the form of a sheet. 4. A gasket material according to claim 1, wherein the fiber component comprises a fibrillating fiber. 5. A gasket material according to claim 4, wherein the fiber component comprises a further fiber. 6. A gasket material according to claim 1, wherein the further resilient material comprises 1-95% w/w of the final dried gasket. 7. A gasket material according to claim 1, wherein the CEV component is at least partially derived from dry CEV. 8. A gasket material according to claim 1, wherein the further resilient material further comprises a plate like filler material. 9. A gasket material according to claim 1, wherein the fiber component is present at a level of 6-70% w/w. 10. A gasket material according to claim 1, wherein the fibrillating fiber component comprises between 1-25% w/w of the final dried gasket. 11. A gasket material according to claim 1, wherein the further fiber component comprises 5-45% w/w of the final dried gasket. 12. A process for the production of a gasket material comprising: mixing at least a fiber component and CEV into a wet dough, and calendaring the wet dough. 13. A process according to claim 12, wherein the mixing incorporates a rubber component. 14. A gasket material according to claim 1, wherein the gasket comprises a plurality of laminated layers. 15. A gasket material comprising a fibre component, a rubber component derived from a rubber solution and a further resilient material, wherein the further resilient material comprises chemically exfoliated vermiculite (CEV). | 1,700 |
3,415 | 14,812,280 | 1,732 | Disclosed is a method/system for the production of titanium dioxide particles. The titanium dioxide particles are produced by oxidizing titanium tetrachloride in the presence of an agent which includes ultrafine titanium dioxide particles, and optionally, the presence of a Group 1 a metal compound. The presence of the agent, with or without the optional Group 1 a metal compound, also serves to control the particle size of the produced titanium dioxide particles. | 1. A method for producing titanium dioxide particles comprising:
a) introducing titanium tetrachloride, oxygen, and an agent to an oxidizer; wherein the agent comprises ultrafine titanium dioxide particles; and wherein the ultrafine titanium dioxide particles are in a form selected from the group consisting of anatase, rutile, amorphous, and combinations thereof; and b) oxidizing at least some of the titanium tetrachloride with at least some of the oxygen in the presence of the agent to form an oxidizer effluent comprising a titanium dioxide product having titanium dioxide particles. 2. The method of claim 1 wherein the agent provides an activity selected from the group consisting of nucleating activity, non-agglomerating activity, and both nucleating activity and non-agglomerating activity. 3. The method of claim 1 wherein:
c) at least some of the titanium dioxide product is separated from the oxidizer effluent. 4. The method of claim 1 wherein the oxidizer is operated at a temperature in the range of from about 900° C. to about 1600° C. 5. The method of claim 1 wherein the ultrafine titanium dioxide particles are introduced to the oxidizer in an amount of from about 50 ppmw to about 100 ppmw, based on the total weight of the titanium dioxide particles produced in step b). 6. The method of claim 1 wherein, at a target median titanium dioxide particle size, the rate of production of the titanium dioxide product is higher as compared to the rate of production of a second titanium dioxide product produced by a method which is the same as that used to produce the titanium dioxide product, but without the introduction of the ultrafine titanium dioxide particles to the oxidizer. 7. The method of claim 1 wherein, at a target titanium dioxide rate of production, the titanium dioxide product has a lower median titanium dioxide particle size and/or a narrower particle size distribution as compared to a third titanium dioxide product produced by a method which is the same as that used to produce the titanium dioxide product, but without the introduction of the ultrafine titanium dioxide particles to the oxidizer. 8. The method of claim 1 wherein the oxidizer comprises at least a first stage and a second stage, and wherein at least some of the titanium tetrachloride and at least some of the oxygen are introduced to the first stage. 9. The method of claim 8 wherein the oxidizer further comprises a third stage, and wherein at least some of the titanium tetrachloride is introduced to: i) the second stage or ii) the third stage or iii) both the second stage and the third stage. 10. The method of claim 8 wherein at least some of the ultrafine titanium dioxide particles are introduced to the first stage. 11. The method of claim 8 wherein at least some of the titanium tetrachloride and at least some of the oxygen are introduced to the second stage. 12. The method of claim 1 wherein a Group 1 a metal compound is also introduced as a part of the agent into the oxidizer in an amount from about 10 ppmw to about 950 ppmw, based on the total weight of the titanium dioxide particles produced in step b). 13. The method of claim 12 wherein the Group 1 a metal compound is a Group 1 a metal halide. 14. A method for controlling particle size of titanium dioxide particles comprising:
a) introducing titanium tetrachloride and oxygen to an oxidizer; b) introducing an agent comprising ultrafine titanium dioxide particles to the oxidizer in a controlled manner, wherein the ultrafine titanium dioxide particles are in a form selected from the group consisting of anatase, rutile, amorphous, and combinations thereof; and c) oxidizing at least some of the titanium tetrachloride with at least some of the oxygen in the presence of the agent to form an oxidizer effluent comprising a titanium dioxide product having titanium dioxide particles, and wherein the introduction of the agent to the oxidizer is controlled such that, at a target titanium dioxide rate of production, the manufacturing costs are lower and/or the titanium dioxide product has a lower median titanium dioxide particle size and/or a narrower particle size distribution as compared to a second titanium dioxide product produced by a method which is the same as that used to produce the titanium dioxide product, but without the controlled introduction of the agent to the oxidizer. 15. The method of claim 14 wherein the agent provides an activity selected from the group consisting of nucleating activity, non-agglomerating activity, and both nucleating activity and non-agglomerating activity. 16. The method of claim 14 wherein the oxidizer is operated at a temperature in the range of from about 900° C. to about 1600° C. 17. The method of claim 14 wherein the ultrafine titanium dioxide particles of the agent are introduced to the oxidizer in an amount of from about 50 ppmw to about 100 ppmw, based on the total weight of the titanium dioxide particles produced in step c). 18. The method of claim 14 wherein at least a portion of the ultrafine titanium dioxide particles of the agent are agglomerated ultrafine titanium dioxide particles having a median size range from about 2 nm to about 150 nm. 19. The method of claim 18 wherein at least a portion of the ultrafine titanium dioxide particles of the agent are maintained as discrete ultrafine titanium dioxide particles having a median discrete particle size from about 1 nm to about 60 nm. 20. The method of claim 14 wherein the oxidizer comprises at least a first stage and a second stage, and wherein at least some of the titanium tetrachloride and at least some of the oxygen are introduced to the first stage. 21. The method of claim 20 wherein the oxidizer further comprises a third stage, and wherein at least some of the titanium tetrachloride is introduced to: i) the second stage or ii) the third stage or iii) both the second stage and the third stage. 22. The method of claim 20 wherein at least some of the titanium tetrachloride and at least some of the oxygen are introduced to the second stage. 23. The method of claim 20 wherein at least some of the agent is introduced to the first stage. 24. The method of claim 14 wherein a Group 1 a metal compound is also introduced as a part of the agent into the oxidizer in a controlled manner in an amount from about 10 ppmw to about 950 ppmw, based on the total weight of the titanium dioxide particles produced in step c). 25. The method of claim 24 wherein the Group 1 a metal compound is a Group 1 a metal halide. 26. A method for producing titanium dioxide particles comprising:
a) introducing oxygen and a first titanium tetrachloride feed comprising titanium tetrachloride to a first stage of an oxidizer having at least two stages; b) oxidizing at least some of the first titanium tetrachloride feed with at least some of the oxygen in the first stage to form a first stage effluent; c) introducing the first stage effluent to a second stage of the oxidizer; d) introducing a second titanium tetrachloride feed comprising titanium tetrachloride to the second stage; e) oxidizing at least some of the second titanium tetrachloride feed with at least some of the oxygen from the first stage effluent in the second stage to form a second stage effluent comprising a titanium dioxide product, wherein the titanium dioxide product comprises the titanium dioxide particles; wherein an agent comprising ultrafine titanium dioxide particles is introduced to at least one stage of the oxidizer; and f) separating at least some of the titanium dioxide product from the second stage effluent. 27. The method of claim 26 wherein the agent provides an activity selected from the group consisting of nucleating activity, non-agglomerating activity, and both nucleating activity and non-agglomerating activity. 28. The method of claim 26 wherein the ultrafine titanium dioxide particles of the agent are in a form selected from the group consisting of anatase, rutile, amorphous, and combinations thereof. 29. The method of claim 26 wherein the ultrafine titanium dioxide particles of the agent are introduced to the oxidizer in an amount of from about 50 to about 100 ppmw, based on the total weight of the titanium dioxide particles produced in step e). 30. The method of claim 26 wherein at least a portion of the ultrafine titanium dioxide particles of the agent are agglomerated ultrafine titanium dioxide particles having a median size range from about 2 nm to about 150 nm. 31. The method of claim 30 wherein at least a portion of the ultrafine titanium dioxide particles of the agent are maintained as discrete ultrafine titanium dioxide particles having a median discrete particle size from about 1 nm to about 60 nm. 32. The method of claim 26 wherein the first stage is operated at a temperature in the range of from about 900° C. to about 1600° C., and the second stage is operated at a temperature in the range of from about 900° C. to about 1600° C. 33. The method of claim 26 wherein a Group 1 a metal compound is introduced as a part of the agent to at least one stage of the oxidizer in an amount from about 10 ppmw to about 950 ppmw, based on the total weight of the titanium dioxide particles produced in step e). 34. The method of claim 33 wherein the Group 1 a metal compound is a Group 1 a metal halide. | Disclosed is a method/system for the production of titanium dioxide particles. The titanium dioxide particles are produced by oxidizing titanium tetrachloride in the presence of an agent which includes ultrafine titanium dioxide particles, and optionally, the presence of a Group 1 a metal compound. The presence of the agent, with or without the optional Group 1 a metal compound, also serves to control the particle size of the produced titanium dioxide particles.1. A method for producing titanium dioxide particles comprising:
a) introducing titanium tetrachloride, oxygen, and an agent to an oxidizer; wherein the agent comprises ultrafine titanium dioxide particles; and wherein the ultrafine titanium dioxide particles are in a form selected from the group consisting of anatase, rutile, amorphous, and combinations thereof; and b) oxidizing at least some of the titanium tetrachloride with at least some of the oxygen in the presence of the agent to form an oxidizer effluent comprising a titanium dioxide product having titanium dioxide particles. 2. The method of claim 1 wherein the agent provides an activity selected from the group consisting of nucleating activity, non-agglomerating activity, and both nucleating activity and non-agglomerating activity. 3. The method of claim 1 wherein:
c) at least some of the titanium dioxide product is separated from the oxidizer effluent. 4. The method of claim 1 wherein the oxidizer is operated at a temperature in the range of from about 900° C. to about 1600° C. 5. The method of claim 1 wherein the ultrafine titanium dioxide particles are introduced to the oxidizer in an amount of from about 50 ppmw to about 100 ppmw, based on the total weight of the titanium dioxide particles produced in step b). 6. The method of claim 1 wherein, at a target median titanium dioxide particle size, the rate of production of the titanium dioxide product is higher as compared to the rate of production of a second titanium dioxide product produced by a method which is the same as that used to produce the titanium dioxide product, but without the introduction of the ultrafine titanium dioxide particles to the oxidizer. 7. The method of claim 1 wherein, at a target titanium dioxide rate of production, the titanium dioxide product has a lower median titanium dioxide particle size and/or a narrower particle size distribution as compared to a third titanium dioxide product produced by a method which is the same as that used to produce the titanium dioxide product, but without the introduction of the ultrafine titanium dioxide particles to the oxidizer. 8. The method of claim 1 wherein the oxidizer comprises at least a first stage and a second stage, and wherein at least some of the titanium tetrachloride and at least some of the oxygen are introduced to the first stage. 9. The method of claim 8 wherein the oxidizer further comprises a third stage, and wherein at least some of the titanium tetrachloride is introduced to: i) the second stage or ii) the third stage or iii) both the second stage and the third stage. 10. The method of claim 8 wherein at least some of the ultrafine titanium dioxide particles are introduced to the first stage. 11. The method of claim 8 wherein at least some of the titanium tetrachloride and at least some of the oxygen are introduced to the second stage. 12. The method of claim 1 wherein a Group 1 a metal compound is also introduced as a part of the agent into the oxidizer in an amount from about 10 ppmw to about 950 ppmw, based on the total weight of the titanium dioxide particles produced in step b). 13. The method of claim 12 wherein the Group 1 a metal compound is a Group 1 a metal halide. 14. A method for controlling particle size of titanium dioxide particles comprising:
a) introducing titanium tetrachloride and oxygen to an oxidizer; b) introducing an agent comprising ultrafine titanium dioxide particles to the oxidizer in a controlled manner, wherein the ultrafine titanium dioxide particles are in a form selected from the group consisting of anatase, rutile, amorphous, and combinations thereof; and c) oxidizing at least some of the titanium tetrachloride with at least some of the oxygen in the presence of the agent to form an oxidizer effluent comprising a titanium dioxide product having titanium dioxide particles, and wherein the introduction of the agent to the oxidizer is controlled such that, at a target titanium dioxide rate of production, the manufacturing costs are lower and/or the titanium dioxide product has a lower median titanium dioxide particle size and/or a narrower particle size distribution as compared to a second titanium dioxide product produced by a method which is the same as that used to produce the titanium dioxide product, but without the controlled introduction of the agent to the oxidizer. 15. The method of claim 14 wherein the agent provides an activity selected from the group consisting of nucleating activity, non-agglomerating activity, and both nucleating activity and non-agglomerating activity. 16. The method of claim 14 wherein the oxidizer is operated at a temperature in the range of from about 900° C. to about 1600° C. 17. The method of claim 14 wherein the ultrafine titanium dioxide particles of the agent are introduced to the oxidizer in an amount of from about 50 ppmw to about 100 ppmw, based on the total weight of the titanium dioxide particles produced in step c). 18. The method of claim 14 wherein at least a portion of the ultrafine titanium dioxide particles of the agent are agglomerated ultrafine titanium dioxide particles having a median size range from about 2 nm to about 150 nm. 19. The method of claim 18 wherein at least a portion of the ultrafine titanium dioxide particles of the agent are maintained as discrete ultrafine titanium dioxide particles having a median discrete particle size from about 1 nm to about 60 nm. 20. The method of claim 14 wherein the oxidizer comprises at least a first stage and a second stage, and wherein at least some of the titanium tetrachloride and at least some of the oxygen are introduced to the first stage. 21. The method of claim 20 wherein the oxidizer further comprises a third stage, and wherein at least some of the titanium tetrachloride is introduced to: i) the second stage or ii) the third stage or iii) both the second stage and the third stage. 22. The method of claim 20 wherein at least some of the titanium tetrachloride and at least some of the oxygen are introduced to the second stage. 23. The method of claim 20 wherein at least some of the agent is introduced to the first stage. 24. The method of claim 14 wherein a Group 1 a metal compound is also introduced as a part of the agent into the oxidizer in a controlled manner in an amount from about 10 ppmw to about 950 ppmw, based on the total weight of the titanium dioxide particles produced in step c). 25. The method of claim 24 wherein the Group 1 a metal compound is a Group 1 a metal halide. 26. A method for producing titanium dioxide particles comprising:
a) introducing oxygen and a first titanium tetrachloride feed comprising titanium tetrachloride to a first stage of an oxidizer having at least two stages; b) oxidizing at least some of the first titanium tetrachloride feed with at least some of the oxygen in the first stage to form a first stage effluent; c) introducing the first stage effluent to a second stage of the oxidizer; d) introducing a second titanium tetrachloride feed comprising titanium tetrachloride to the second stage; e) oxidizing at least some of the second titanium tetrachloride feed with at least some of the oxygen from the first stage effluent in the second stage to form a second stage effluent comprising a titanium dioxide product, wherein the titanium dioxide product comprises the titanium dioxide particles; wherein an agent comprising ultrafine titanium dioxide particles is introduced to at least one stage of the oxidizer; and f) separating at least some of the titanium dioxide product from the second stage effluent. 27. The method of claim 26 wherein the agent provides an activity selected from the group consisting of nucleating activity, non-agglomerating activity, and both nucleating activity and non-agglomerating activity. 28. The method of claim 26 wherein the ultrafine titanium dioxide particles of the agent are in a form selected from the group consisting of anatase, rutile, amorphous, and combinations thereof. 29. The method of claim 26 wherein the ultrafine titanium dioxide particles of the agent are introduced to the oxidizer in an amount of from about 50 to about 100 ppmw, based on the total weight of the titanium dioxide particles produced in step e). 30. The method of claim 26 wherein at least a portion of the ultrafine titanium dioxide particles of the agent are agglomerated ultrafine titanium dioxide particles having a median size range from about 2 nm to about 150 nm. 31. The method of claim 30 wherein at least a portion of the ultrafine titanium dioxide particles of the agent are maintained as discrete ultrafine titanium dioxide particles having a median discrete particle size from about 1 nm to about 60 nm. 32. The method of claim 26 wherein the first stage is operated at a temperature in the range of from about 900° C. to about 1600° C., and the second stage is operated at a temperature in the range of from about 900° C. to about 1600° C. 33. The method of claim 26 wherein a Group 1 a metal compound is introduced as a part of the agent to at least one stage of the oxidizer in an amount from about 10 ppmw to about 950 ppmw, based on the total weight of the titanium dioxide particles produced in step e). 34. The method of claim 33 wherein the Group 1 a metal compound is a Group 1 a metal halide. | 1,700 |
3,416 | 13,877,847 | 1,771 | Nutritional compositions and formulations that optimize nutritional contents are provided. Dietary compositions and methods for tailoring such compositions to optimize levels of nutrients that have beneficial effects within specific ranges are provided. Dietary plans, and formulations comprising dietary products that comprise optimized levels of nutrients derived from phytochemicals, antioxidants, vitamins, minerals, lipids, proteins, carbohydrates, probiotics, prebiotics, microorganisms and fiber. Diet plans and modular nutritional packages comprising food and drink items tailored according to consumer patterns typed by diet, age, size, gender, medical conditions, family history, climate and the like are provided. | 1-52. (canceled) 53. A method for selecting a nutritional formulation or plan for an individual, comprising:
determining for the individual a diet cohort, the cohort being high plant food, high meat, or high seafood; and supplementing the individual's diet with one or more nutritional modules comprising one or more of natural oils, butters, margarines, nuts, seeds, herbs, lipids, phytochemicals, antioxidants, vitamins, and minerals, so as to balance the individual's nutritional state. 54. The method of claim 53, which involves use of a kit comprising the formulation or modules, wherein one or more of the following apply:
(i) the kit comprises individual portions of food items for daily consumption; (ii) the kit comprises individual portions of food items for supplementation of daily diet of a subject; (iii) the kit comprises a label comprising at least one indication of the suitability of the modules or packages for a consumer with a specific dietary profile or cohort; (iv) the kit comprises an indication of the upper limit of average daily consumption of items in the kit or module; or (v) a label is attached to the packaging of the kit or module. 55. The method of claim 53, wherein the individual has signs or symptoms of a chronic disease. 56. A nutritional formulation for an individual comprising at least one module for consumption by a consumer, the formulation comprising:
one or more nutrients in each module, wherein the nutritional formulation comprises amounts and types of phytochemicals, antioxidants, vitamins, minerals, acid-base, lipids, proteins, carbohydrates, probiotics, prebiotics, microorganisms, fiber and other nutrients that are optimized and balanced to provide a health benefit when one or more servings of the nutritional formulation is used to provide at least 25% of the average daily calories to the consumer over one or more weeks. 57. The formulation of claim 56, wherein determination of the nutritional formulation comprises one or more of the following:
(i) determining a cohort of the individual based on primary dietary ingredients of the subject's daily or weekly diet by comparing levels of one or more of antioxidants, phytochemicals, vitamins, minerals, lipids, carbohydrates, and proteins from foods comprising the subject's diet with levels in a set of predetermined cohorts; (ii) determining a cohort based on average daily consumption of one or more of grains, vegetables, fruits, legumes, dairy, meats, seafood, herbs, sweeteners, and beverages; (iii) selecting a cohort from vegetable-based, meat-based and seafood-based; or (iv) selecting a cohort based on gender, age, genetic profile, family history, climactic temperature, or medical condition. 58. The formulation of claim 56, wherein the modules comprise one or more of:
(i) food items sufficient to supplement the consumer's diet and/or one or more nutrients selected to supplement a cohort; (ii) less than 500 calories or 25% of daily calories; (iii) vegetable or vegetable juice packs, fruit or fruit juice packs, dry grain packs, cereal packs, legume, grain, nuts, seeds packs, meat and/or seafood packs, herbs, lipids, meals, snack, side dish, salad, desserts, milks, powder, puree, and/or yogurt; (iv) nutrients selected from phytochemicals, lipids, antioxidants, vitamins, minerals, synbiotics, probiotics, prebiotics, microorganisms and fiber; (v) whole food items from natural sources; (vi) natural sources of lipids selected from oils, butters, margarines, nuts, and seeds; (vii) micronutrients derived entirely or partly from natural sources; or (viii) liquid, cream, or patch for topical use. 59. The formulation of claim 56, wherein the modules comprise one or more of:
(i) a part or entire daily dietary intake of nutrients for the subject; (ii) supplements, balances or replaces the subject's daily food consumption based on the subject's cohort or the subject's lipid consumption; (iii) at least 80% of daily or weekly total caloric intake for the subject; or (iv) suit satiety and dietary preference of the subject. 60. The formulation of claim 56, wherein food items are selected based on the methods of processing employed to prepare the food item and wherein optionally the processing is selected from hulling, removing a layer, drying, providing fresh, roasting, and grilling. 61. The formulation of claim 56, wherein one or more of the following apply:
(i) the omega-6 to omega-3 fatty acids ratio is greater than 1:1, or greater than 5:1, or greater than 10:1; (ii) the omega-9 to omega-6 fatty acids ratio is less than 4:1; (iii) the monounsaturated to polyunsaturated fatty acids ratio is less than 4:1; (iv) the omega-9 fatty acids are less than 60% or less than 50% of the total lipids; (v) the omega-6 fatty acids are greater than 20% or greater than 30% of the total lipids; (vi) the omega-3 fatty acids are less than 20% or less than 10% of the total lipids; (vii) the omega-6 fatty acids are less than 40 g or less than 25 g; or (viii) the omega-3 fatty acids are less than 2 g or less than 1 g. 62. The formulation of claim 56, which involves use of a kit comprising the formulation, modules or packages of food items, wherein one or more of the following apply:
(i) the kit comprises individual portions of food items for daily consumption; (ii) the kit comprises individual portions of food items for supplementation of daily diet of a subject; (iii) the kit comprises a label comprising at least one indication of the suitability of the modules or packages for a consumer with a specific dietary profile or cohort; (iv) the kit comprises an indication of the upper limit of average daily consumption of items in the kit or module; or (v) a label is attached to the packaging of the kit or module. 63. Use of the formulation of claim 56, wherein the module comprises a medicine for prophylaxis or therapy of a medical condition. 64. Use of the formulation of claim 56, wherein the individual has signs or symptoms of a chronic disease. 65. A formulation of claim 56, for use in the prophylaxis or treatment of a medical condition or disease or to ameliorate symptoms of a medical condition or disease, wherein optionally, the medical condition or disease is selected from menopause, aging, allergy, musculoskeletal disorders, vascular diseases, hypercholesterolemia, mood swing, reduced cognitive function, cancer, neural disorders, mental disorders, renal diseases, endocrine disorders, thyroid disturbances, weight gain, obesity, diabetes, digestive system disorders, reproductive disorders, infant abnormalities, pulmonary disorders, ophthalmologic disorders, dermatological disorders, sleep disorders, dental diseases, autoimmune diseases, infectious diseases, and inflammatory diseases. 66. A method of prophylaxis and/or treatment of a medical condition in a subject, comprising administering a formulation of claim 56. 67. The method of claim 66, wherein the medical condition or disease is selected from menopause, aging, allergy, musculoskeletal disorders, vascular diseases, hypercholesterolemia, mood swing, reduced cognitive function, cancer, neural disorders, mental disorders, renal diseases, endocrine disorders, thyroid disturbances, weight gain, obesity, diabetes, digestive system disorders, reproductive disorders, infant abnormalities, pulmonary disorders, ophthalmologic disorders, dermatological disorders, sleep disorders, dental diseases, autoimmune diseases, infectious diseases, and inflammatory diseases. 68. A process for developing a nutrient consumption program for an individual, the process comprising:
providing one or more lists of food items or modules comprising nutrients for average daily consumption by a subject, wherein the food items comprise at least 25% of the subject's average daily caloric intake over at least one week, wherein the food items further comprise a plurality of nutrients selected from phytochemicals, antioxidants, vitamins, minerals, synbiotics, probiotics, prebiotics, microorganisms and fiber in amounts that optimizes and balances the subject's total dietary intake of the nutrients over an extended period of time such that a beneficial effect is provided to the subject. 69. The process of claim 68, wherein determination of the process for developing a nutrient consumption program comprises one or more of the following:
(i) determining a cohort of the individual based on primary dietary ingredients of the subject's daily or weekly diet by comparing levels of one or more of antioxidants, phytochemicals, vitamins, minerals, lipids, carbohydrates, and proteins from foods comprising the subject's diet with levels in a set of predetermined cohorts; (ii) determining a cohort based on average daily consumption of one or more of grains, vegetables, fruits, legumes, dairy, meats, seafood, herbs, sweeteners, and beverages; (iii) selecting a cohort from vegetable-based, meat-based and seafood-based; or (iv) selecting a cohort based on gender, age, genetic profile, family history, climactic temperature, or medical condition. 70. The process of claim 68, wherein the module or one or more food items comprise one or more of:
(i) food items sufficient to supplement the consumer's diet and/or one or more nutrients selected to supplement a cohort; (ii) less than 500 calories or 25% of daily calories; (iii) vegetable or vegetable juice packs, fruit or fruit juice packs, dry grain packs, cereal packs, legume, grain, nuts, seeds packs, meat and/or seafood packs, herbs, lipids, meals, snack, side dish, salad, desserts, milks, powder, puree, and/or yogurt; (iv) nutrients selected from phytochemicals, lipids, antioxidants, vitamins, minerals, synbiotics, probiotics, prebiotics, microorganisms and fiber; (v) whole food items from natural sources; (vi) natural sources of lipids selected from oils, butters, margarines, nuts, and seeds; (vii) micronutrients derived entirely or partly from natural sources; or (viii) liquid, cream, or patch for topical use. 71. The process of claim 68, wherein the one or more modules or one or more food items comprise one or more of:
(i) a part or entire daily dietary intake of nutrients for the subject; (ii) supplements, balances or replaces the subject's daily food consumption based on the subject's cohort or the subject's lipid consumption; (iii) at least 80% of daily or weekly total caloric intake for the subject; or (iv) suit satiety and dietary preference of the subject. 72. The process of claim 68, wherein food items are selected based on the methods of processing employed to prepare the food item and wherein optionally the processing is selected from hulling, removing a layer, drying, providing fresh, roasting, and grilling. 73. The process of claim 68, wherein one or more of the following apply:
(i) the omega-6 to omega-3 fatty acids ratio is greater than 1:1, or greater than 5:1, or greater than 10:1; (ii) the omega-9 to omega-6 fatty acids ratio is less than 4:1; (iii) the monounsaturated to polyunsaturated fatty acids ratio is less than 4:1; (iv) the omega-9 fatty acids are less than 60% or less than 50% of the total lipids; (v) the omega-6 fatty acids are greater than 20% or greater than 30% of the total lipids; (vi) the omega-3 fatty acids are less than 20% or less than 10% of the total lipids; (vii) the omega-6 fatty acids are less than 40 g or less than 25 g; or (viii) the omega-3 fatty acids are less than 2 g or less than 1 g. 74. The process of claim 68, wherein the list provides one or more of the following:
(i) predetermined natural sources of lipids, the sources selected from oils, butters, margarines, nuts and seeds, and optionally one or more of nutrients selected from antioxidants, phytochemicals, vitamins and minerals in amounts that optimizes dietary nutrients such that the subject's lipid intake provides a beneficial effect to the subject; (ii) a recommendation for consumption of food items over at least one week; (iii) wherein the food items listed in the nutrient consumption program are optimized to suit satiety and dietary preferences of the subject; or (iv) the food items that should not be included in the subject's daily diet; should be limited in the subject's daily diet; or should be added to the subject's daily diet. 75. The process of claim 68, which involves use of a kit comprising the formulation, modules or packages of food items, wherein one or more of the following apply:
(i) the kit comprises individual portions of food items for daily consumption; (ii) the kit comprises individual portions of food items for supplementation of daily diet of a subject; (iii) the kit comprises a label comprising at least one indication of the suitability of the modules or packages for a consumer with a specific dietary profile or cohort; (iv) the kit comprises an indication of the upper limit of average daily consumption of items in the kit or module; or (v) a label is attached to the packaging of the kit or module. 76. A computer system for computationally implementing the process of claim 68, comprising:
(a) a computing device having a memory; (b) an input device for entering information regarding the subject's actual dietary intake into the memory; (c) a data base in the memory for storing the information; (d) a first application program, for execution in the computing device, for determining a dietary cohort of the subject corresponding to the subject's actual dietary intake; wherein optionally the dietary cohort of the subject is
(i) predetermined and entered directly in the computing device; and/or
(ii) determined either manually or computationally; and/or
(iii) selected from vegetable-based, seafood based and meat based;
(e) a nutrient database in the memory of the device for storing dietary guidelines relative to dietary cohorts of a subject; wherein optionally the nutrient database comprises suitable ranges for average daily dietary consumption of nutrients corresponding to each dietary cohort, and/or suitable ranges for daily dietary consumption of carbohydrates, protein, vitamins, minerals and phytochemicals; (f) a knowledge base in the memory having rules for manipulating the information in the data base to provide a recommended future dietary program for the user, the program comprising one or more of nutrients selected from antioxidants, phytochemicals, phytosterols, vitamins and minerals in amounts that optimize dietary nutrients to provide a beneficial effect to the subject, when at least 25% or optionally at least 70% of the subject's average daily calories are obtained from food listed in the program; (g) a second application program, for execution in the computing device, for applying the rules in the knowledge base to the information in the data base and to the guidelines in the nutrient base and for generating a nutrition program for the user in a result base; and (h) means for outputting the contents of the result base, under the direction of the application program, wherein the nutrition program contents comprise a listing of particular foods suggested for daily consumption by the subject. 77. Use of the process of claim 68, wherein the module comprises a medicine for prophylaxis or therapy of a medical condition. 78. Use of process of claims 68, wherein the individual has signs or symptoms of a chronic disease. 79. A formulation developed according to the process of claim 68, for use in the prophylaxis or treatment of a medical condition or disease or to ameliorate symptoms of a medical condition or disease, wherein optionally, the medical condition or disease is selected from menopause, aging, allergy, musculoskeletal disorders, vascular diseases, hypercholesterolemia, mood swing, reduced cognitive function, cancer, neural disorders, mental disorders, renal diseases, endocrine disorders, thyroid disturbances, weight gain, obesity, diabetes, digestive system disorders, reproductive disorders, infant abnormalities, pulmonary disorders, ophthalmologic disorders, dermatological disorders, sleep disorders, dental diseases, autoimmune diseases, infectious diseases, and inflammatory diseases. 80. A method of prophylaxis and/or treatment of a medical condition in a subject, comprising administering a formulation developed according to the process of claim 68. 81. The method of claim 80, wherein the medical condition or disease is selected from menopause, aging, allergy, musculoskeletal disorders, vascular diseases, hypercholesterolemia, mood swing, reduced cognitive function, cancer, neural disorders, mental disorders, renal diseases, endocrine disorders, thyroid disturbances, weight gain, obesity, diabetes, digestive system disorders, reproductive disorders, infant abnormalities, pulmonary disorders, ophthalmologic disorders, dermatological disorders, sleep disorders, dental diseases, autoimmune diseases, infectious diseases, and inflammatory diseases. | Nutritional compositions and formulations that optimize nutritional contents are provided. Dietary compositions and methods for tailoring such compositions to optimize levels of nutrients that have beneficial effects within specific ranges are provided. Dietary plans, and formulations comprising dietary products that comprise optimized levels of nutrients derived from phytochemicals, antioxidants, vitamins, minerals, lipids, proteins, carbohydrates, probiotics, prebiotics, microorganisms and fiber. Diet plans and modular nutritional packages comprising food and drink items tailored according to consumer patterns typed by diet, age, size, gender, medical conditions, family history, climate and the like are provided.1-52. (canceled) 53. A method for selecting a nutritional formulation or plan for an individual, comprising:
determining for the individual a diet cohort, the cohort being high plant food, high meat, or high seafood; and supplementing the individual's diet with one or more nutritional modules comprising one or more of natural oils, butters, margarines, nuts, seeds, herbs, lipids, phytochemicals, antioxidants, vitamins, and minerals, so as to balance the individual's nutritional state. 54. The method of claim 53, which involves use of a kit comprising the formulation or modules, wherein one or more of the following apply:
(i) the kit comprises individual portions of food items for daily consumption; (ii) the kit comprises individual portions of food items for supplementation of daily diet of a subject; (iii) the kit comprises a label comprising at least one indication of the suitability of the modules or packages for a consumer with a specific dietary profile or cohort; (iv) the kit comprises an indication of the upper limit of average daily consumption of items in the kit or module; or (v) a label is attached to the packaging of the kit or module. 55. The method of claim 53, wherein the individual has signs or symptoms of a chronic disease. 56. A nutritional formulation for an individual comprising at least one module for consumption by a consumer, the formulation comprising:
one or more nutrients in each module, wherein the nutritional formulation comprises amounts and types of phytochemicals, antioxidants, vitamins, minerals, acid-base, lipids, proteins, carbohydrates, probiotics, prebiotics, microorganisms, fiber and other nutrients that are optimized and balanced to provide a health benefit when one or more servings of the nutritional formulation is used to provide at least 25% of the average daily calories to the consumer over one or more weeks. 57. The formulation of claim 56, wherein determination of the nutritional formulation comprises one or more of the following:
(i) determining a cohort of the individual based on primary dietary ingredients of the subject's daily or weekly diet by comparing levels of one or more of antioxidants, phytochemicals, vitamins, minerals, lipids, carbohydrates, and proteins from foods comprising the subject's diet with levels in a set of predetermined cohorts; (ii) determining a cohort based on average daily consumption of one or more of grains, vegetables, fruits, legumes, dairy, meats, seafood, herbs, sweeteners, and beverages; (iii) selecting a cohort from vegetable-based, meat-based and seafood-based; or (iv) selecting a cohort based on gender, age, genetic profile, family history, climactic temperature, or medical condition. 58. The formulation of claim 56, wherein the modules comprise one or more of:
(i) food items sufficient to supplement the consumer's diet and/or one or more nutrients selected to supplement a cohort; (ii) less than 500 calories or 25% of daily calories; (iii) vegetable or vegetable juice packs, fruit or fruit juice packs, dry grain packs, cereal packs, legume, grain, nuts, seeds packs, meat and/or seafood packs, herbs, lipids, meals, snack, side dish, salad, desserts, milks, powder, puree, and/or yogurt; (iv) nutrients selected from phytochemicals, lipids, antioxidants, vitamins, minerals, synbiotics, probiotics, prebiotics, microorganisms and fiber; (v) whole food items from natural sources; (vi) natural sources of lipids selected from oils, butters, margarines, nuts, and seeds; (vii) micronutrients derived entirely or partly from natural sources; or (viii) liquid, cream, or patch for topical use. 59. The formulation of claim 56, wherein the modules comprise one or more of:
(i) a part or entire daily dietary intake of nutrients for the subject; (ii) supplements, balances or replaces the subject's daily food consumption based on the subject's cohort or the subject's lipid consumption; (iii) at least 80% of daily or weekly total caloric intake for the subject; or (iv) suit satiety and dietary preference of the subject. 60. The formulation of claim 56, wherein food items are selected based on the methods of processing employed to prepare the food item and wherein optionally the processing is selected from hulling, removing a layer, drying, providing fresh, roasting, and grilling. 61. The formulation of claim 56, wherein one or more of the following apply:
(i) the omega-6 to omega-3 fatty acids ratio is greater than 1:1, or greater than 5:1, or greater than 10:1; (ii) the omega-9 to omega-6 fatty acids ratio is less than 4:1; (iii) the monounsaturated to polyunsaturated fatty acids ratio is less than 4:1; (iv) the omega-9 fatty acids are less than 60% or less than 50% of the total lipids; (v) the omega-6 fatty acids are greater than 20% or greater than 30% of the total lipids; (vi) the omega-3 fatty acids are less than 20% or less than 10% of the total lipids; (vii) the omega-6 fatty acids are less than 40 g or less than 25 g; or (viii) the omega-3 fatty acids are less than 2 g or less than 1 g. 62. The formulation of claim 56, which involves use of a kit comprising the formulation, modules or packages of food items, wherein one or more of the following apply:
(i) the kit comprises individual portions of food items for daily consumption; (ii) the kit comprises individual portions of food items for supplementation of daily diet of a subject; (iii) the kit comprises a label comprising at least one indication of the suitability of the modules or packages for a consumer with a specific dietary profile or cohort; (iv) the kit comprises an indication of the upper limit of average daily consumption of items in the kit or module; or (v) a label is attached to the packaging of the kit or module. 63. Use of the formulation of claim 56, wherein the module comprises a medicine for prophylaxis or therapy of a medical condition. 64. Use of the formulation of claim 56, wherein the individual has signs or symptoms of a chronic disease. 65. A formulation of claim 56, for use in the prophylaxis or treatment of a medical condition or disease or to ameliorate symptoms of a medical condition or disease, wherein optionally, the medical condition or disease is selected from menopause, aging, allergy, musculoskeletal disorders, vascular diseases, hypercholesterolemia, mood swing, reduced cognitive function, cancer, neural disorders, mental disorders, renal diseases, endocrine disorders, thyroid disturbances, weight gain, obesity, diabetes, digestive system disorders, reproductive disorders, infant abnormalities, pulmonary disorders, ophthalmologic disorders, dermatological disorders, sleep disorders, dental diseases, autoimmune diseases, infectious diseases, and inflammatory diseases. 66. A method of prophylaxis and/or treatment of a medical condition in a subject, comprising administering a formulation of claim 56. 67. The method of claim 66, wherein the medical condition or disease is selected from menopause, aging, allergy, musculoskeletal disorders, vascular diseases, hypercholesterolemia, mood swing, reduced cognitive function, cancer, neural disorders, mental disorders, renal diseases, endocrine disorders, thyroid disturbances, weight gain, obesity, diabetes, digestive system disorders, reproductive disorders, infant abnormalities, pulmonary disorders, ophthalmologic disorders, dermatological disorders, sleep disorders, dental diseases, autoimmune diseases, infectious diseases, and inflammatory diseases. 68. A process for developing a nutrient consumption program for an individual, the process comprising:
providing one or more lists of food items or modules comprising nutrients for average daily consumption by a subject, wherein the food items comprise at least 25% of the subject's average daily caloric intake over at least one week, wherein the food items further comprise a plurality of nutrients selected from phytochemicals, antioxidants, vitamins, minerals, synbiotics, probiotics, prebiotics, microorganisms and fiber in amounts that optimizes and balances the subject's total dietary intake of the nutrients over an extended period of time such that a beneficial effect is provided to the subject. 69. The process of claim 68, wherein determination of the process for developing a nutrient consumption program comprises one or more of the following:
(i) determining a cohort of the individual based on primary dietary ingredients of the subject's daily or weekly diet by comparing levels of one or more of antioxidants, phytochemicals, vitamins, minerals, lipids, carbohydrates, and proteins from foods comprising the subject's diet with levels in a set of predetermined cohorts; (ii) determining a cohort based on average daily consumption of one or more of grains, vegetables, fruits, legumes, dairy, meats, seafood, herbs, sweeteners, and beverages; (iii) selecting a cohort from vegetable-based, meat-based and seafood-based; or (iv) selecting a cohort based on gender, age, genetic profile, family history, climactic temperature, or medical condition. 70. The process of claim 68, wherein the module or one or more food items comprise one or more of:
(i) food items sufficient to supplement the consumer's diet and/or one or more nutrients selected to supplement a cohort; (ii) less than 500 calories or 25% of daily calories; (iii) vegetable or vegetable juice packs, fruit or fruit juice packs, dry grain packs, cereal packs, legume, grain, nuts, seeds packs, meat and/or seafood packs, herbs, lipids, meals, snack, side dish, salad, desserts, milks, powder, puree, and/or yogurt; (iv) nutrients selected from phytochemicals, lipids, antioxidants, vitamins, minerals, synbiotics, probiotics, prebiotics, microorganisms and fiber; (v) whole food items from natural sources; (vi) natural sources of lipids selected from oils, butters, margarines, nuts, and seeds; (vii) micronutrients derived entirely or partly from natural sources; or (viii) liquid, cream, or patch for topical use. 71. The process of claim 68, wherein the one or more modules or one or more food items comprise one or more of:
(i) a part or entire daily dietary intake of nutrients for the subject; (ii) supplements, balances or replaces the subject's daily food consumption based on the subject's cohort or the subject's lipid consumption; (iii) at least 80% of daily or weekly total caloric intake for the subject; or (iv) suit satiety and dietary preference of the subject. 72. The process of claim 68, wherein food items are selected based on the methods of processing employed to prepare the food item and wherein optionally the processing is selected from hulling, removing a layer, drying, providing fresh, roasting, and grilling. 73. The process of claim 68, wherein one or more of the following apply:
(i) the omega-6 to omega-3 fatty acids ratio is greater than 1:1, or greater than 5:1, or greater than 10:1; (ii) the omega-9 to omega-6 fatty acids ratio is less than 4:1; (iii) the monounsaturated to polyunsaturated fatty acids ratio is less than 4:1; (iv) the omega-9 fatty acids are less than 60% or less than 50% of the total lipids; (v) the omega-6 fatty acids are greater than 20% or greater than 30% of the total lipids; (vi) the omega-3 fatty acids are less than 20% or less than 10% of the total lipids; (vii) the omega-6 fatty acids are less than 40 g or less than 25 g; or (viii) the omega-3 fatty acids are less than 2 g or less than 1 g. 74. The process of claim 68, wherein the list provides one or more of the following:
(i) predetermined natural sources of lipids, the sources selected from oils, butters, margarines, nuts and seeds, and optionally one or more of nutrients selected from antioxidants, phytochemicals, vitamins and minerals in amounts that optimizes dietary nutrients such that the subject's lipid intake provides a beneficial effect to the subject; (ii) a recommendation for consumption of food items over at least one week; (iii) wherein the food items listed in the nutrient consumption program are optimized to suit satiety and dietary preferences of the subject; or (iv) the food items that should not be included in the subject's daily diet; should be limited in the subject's daily diet; or should be added to the subject's daily diet. 75. The process of claim 68, which involves use of a kit comprising the formulation, modules or packages of food items, wherein one or more of the following apply:
(i) the kit comprises individual portions of food items for daily consumption; (ii) the kit comprises individual portions of food items for supplementation of daily diet of a subject; (iii) the kit comprises a label comprising at least one indication of the suitability of the modules or packages for a consumer with a specific dietary profile or cohort; (iv) the kit comprises an indication of the upper limit of average daily consumption of items in the kit or module; or (v) a label is attached to the packaging of the kit or module. 76. A computer system for computationally implementing the process of claim 68, comprising:
(a) a computing device having a memory; (b) an input device for entering information regarding the subject's actual dietary intake into the memory; (c) a data base in the memory for storing the information; (d) a first application program, for execution in the computing device, for determining a dietary cohort of the subject corresponding to the subject's actual dietary intake; wherein optionally the dietary cohort of the subject is
(i) predetermined and entered directly in the computing device; and/or
(ii) determined either manually or computationally; and/or
(iii) selected from vegetable-based, seafood based and meat based;
(e) a nutrient database in the memory of the device for storing dietary guidelines relative to dietary cohorts of a subject; wherein optionally the nutrient database comprises suitable ranges for average daily dietary consumption of nutrients corresponding to each dietary cohort, and/or suitable ranges for daily dietary consumption of carbohydrates, protein, vitamins, minerals and phytochemicals; (f) a knowledge base in the memory having rules for manipulating the information in the data base to provide a recommended future dietary program for the user, the program comprising one or more of nutrients selected from antioxidants, phytochemicals, phytosterols, vitamins and minerals in amounts that optimize dietary nutrients to provide a beneficial effect to the subject, when at least 25% or optionally at least 70% of the subject's average daily calories are obtained from food listed in the program; (g) a second application program, for execution in the computing device, for applying the rules in the knowledge base to the information in the data base and to the guidelines in the nutrient base and for generating a nutrition program for the user in a result base; and (h) means for outputting the contents of the result base, under the direction of the application program, wherein the nutrition program contents comprise a listing of particular foods suggested for daily consumption by the subject. 77. Use of the process of claim 68, wherein the module comprises a medicine for prophylaxis or therapy of a medical condition. 78. Use of process of claims 68, wherein the individual has signs or symptoms of a chronic disease. 79. A formulation developed according to the process of claim 68, for use in the prophylaxis or treatment of a medical condition or disease or to ameliorate symptoms of a medical condition or disease, wherein optionally, the medical condition or disease is selected from menopause, aging, allergy, musculoskeletal disorders, vascular diseases, hypercholesterolemia, mood swing, reduced cognitive function, cancer, neural disorders, mental disorders, renal diseases, endocrine disorders, thyroid disturbances, weight gain, obesity, diabetes, digestive system disorders, reproductive disorders, infant abnormalities, pulmonary disorders, ophthalmologic disorders, dermatological disorders, sleep disorders, dental diseases, autoimmune diseases, infectious diseases, and inflammatory diseases. 80. A method of prophylaxis and/or treatment of a medical condition in a subject, comprising administering a formulation developed according to the process of claim 68. 81. The method of claim 80, wherein the medical condition or disease is selected from menopause, aging, allergy, musculoskeletal disorders, vascular diseases, hypercholesterolemia, mood swing, reduced cognitive function, cancer, neural disorders, mental disorders, renal diseases, endocrine disorders, thyroid disturbances, weight gain, obesity, diabetes, digestive system disorders, reproductive disorders, infant abnormalities, pulmonary disorders, ophthalmologic disorders, dermatological disorders, sleep disorders, dental diseases, autoimmune diseases, infectious diseases, and inflammatory diseases. | 1,700 |
3,417 | 15,111,949 | 1,743 | A three-dimensional object may be generated. A controller may be to control an energy source to apply energy to a layer of build material on a support member or previous layer to cause a portion of the layer to coalesce and solidify to form a slice of the three-dimensional object. A radiation sensor may be to measure absorbance or gloss of the layer. The controller may be to receive, from the radiation sensor, data representing measured absorbance or measured gloss of the layer. The controller may be to control the apparatus to modify a process parameter if the measured absorbance or gloss indicates an incorrect degree of solidification of a part of the layer. | 1. An apparatus for generating a three-dimensional object, the apparatus comprising:
a radiation sensor to measure absorbance or gloss of build material; and a controller to:
control an energy source to apply energy to a layer of the build material to cause a portion of the layer to coalesce and solidify to form a slice of the three-dimensional object;
receive, from the radiation sensor, data representing measured absorbance or measured gloss of the layer; and
control the apparatus to modify a process parameter if the measured absorbance or measured gloss indicates an incorrect degree of solidification of a part of the layer. 2. The apparatus of claim 1 wherein the controller is to control an agent distributor to selectively deliver coalescing agent to the portion to cause the portion to coalesce when the energy is applied. 3. The apparatus of claim 2 wherein the radiation sensor is to measure the absorbance of the build material, wherein the coalescing agent is to absorb unfocused radiation used for measuring the absorbance, the unfocused radiation being received from the energy source or another radiation source. 4. The apparatus of claim 1 wherein the radiation sensor is part of a reflectometer, densitometer, colorimeter, digital camera, gloss meter, or haze meter. 5. The apparatus of claim 1 wherein the controller is to control the apparatus to modify the process parameter if the measured absorbance or measured gloss indicates that the part has under-solidified, the under-solidified part being in the portion that is to form the slice of the three-dimensional object. 6. The apparatus of claim 1 wherein the controller is to control the apparatus to modify the process parameter if the measured absorbance or measured gloss indicates that the part has over-solidified. 7. The apparatus of claim 1 further comprising an unfocused radiation source to apply unfocused radiation to the build material, the build material to reflect the unfocused radiation for detection by the radiation sensor to measure the absorbance of the build material, the unfocused radiation having a substantially different radiant spectrum than the energy applied by the energy source. 8. The apparatus of claim 1 further comprising a focused radiation source to apply focused radiation to the build material, the build material to reflect the focused radiation for detection by the radiation sensor to measure the specular reflection or gloss of the build material, the focused radiation having a substantially different radiant spectrum than the energy applied by the energy source. 9. The apparatus of claim 1 further comprising:
a first focused radiation source to apply first focused radiation to the build material at a first non-zero angle, the build material to specularly reflect the first focused radiation for detection by the radiation sensor to measure the gloss of the build material; and
a second radiation sensor to measure any of the first focused radiation that is reflected at a non-specular angle,
prior to controlling the apparatus to modify the process parameter, the controller to correct the gloss measurement by the first radiation sensor using the measurement by the second radiation sensor of the first focused radiation that is non-specularly reflected,
if the measured gloss, after being corrected, indicates the incorrect degree of solidification of the part of the layer, control the apparatus to modify the process parameter. 10. The apparatus of claim 1 wherein:
to measure the absorbance of the portion, the radiation sensor is to measure a reference absorbance or reference gloss of the portion prior to applying the energy to the portion, and is to measure a post-energy absorbance or post-energy gloss of the portion during or after applying the energy to the portion, and
the controller is to compare the reference absorbance or reference gloss and the post-energy absorbance or post-energy gloss to determine a calibrated absorbance or calibrated gloss, and to control the apparatus to modify the process parameter based on the calibrated absorbance or calibrated gloss. 11. The apparatus of claim 1 wherein modifying the process parameter comprises controlling an agent distributor to selectively deliver coalescence modifier agent to the part. 12. The apparatus of claim 1 wherein modifying the process parameter comprises the controller to control the energy source to vary temperature of the build material or vary duration or intensity of the energy applied to the build material. 13. The apparatus of claim 1 further comprising a radiation source to apply pulsed radiation to the build material, the build material to reflect the pulsed radiation for detection by the radiation sensor such that the detected pulsed radiation when the radiation source is in the on-state is compared by the radiation sensor or controller with detected background radiation when the radiation source is in the off-state, the comparison used to remove background noise from the measurement of the absorbance or the gloss. 14. An apparatus for generating a three-dimensional object, the apparatus comprising:
a radiation sensor to measure absorbance of build material; and a controller to:
control an energy source to apply energy to a layer of the build material to cause a portion of the layer to coalesce and solidify to form a slice of the three-dimensional object;
control the energy source or an unfocused radiation source to apply unfocused radiation to the build material,
receive, from the radiation sensor, data representing the measured absorbance of the layer, the measured absorbance based on detection by the radiation sensor of an amount of the unfocused radiation that is reflected by the build material, the measured absorbance positively correlated with a degree of solidification in the layer; and
if the measured absorbance indicates an incorrect degree of solidification of a part of the layer, control the apparatus to modify a process parameter. 15. An apparatus for generating a three-dimensional object, the apparatus comprising:
a radiation sensor to measure gloss of build material; and a controller to:
control an energy source to apply energy to a layer of the build material to cause a portion of the layer to coalesce and solidify to form a slice of the three-dimensional object;
control the energy source or a focused radiation source to apply focused radiation to the build material;
receive, from the radiation sensor, data representing the measured gloss of the layer, the measured gloss based on detection by the radiation sensor of an amount of the focused radiation that is reflected by the build material;
the measured gloss positively correlated with a degree of solidification in the layer; and
if the measured gloss indicates an incorrect degree of solidification of a part of the layer, control the apparatus to modify a process parameter. | A three-dimensional object may be generated. A controller may be to control an energy source to apply energy to a layer of build material on a support member or previous layer to cause a portion of the layer to coalesce and solidify to form a slice of the three-dimensional object. A radiation sensor may be to measure absorbance or gloss of the layer. The controller may be to receive, from the radiation sensor, data representing measured absorbance or measured gloss of the layer. The controller may be to control the apparatus to modify a process parameter if the measured absorbance or gloss indicates an incorrect degree of solidification of a part of the layer.1. An apparatus for generating a three-dimensional object, the apparatus comprising:
a radiation sensor to measure absorbance or gloss of build material; and a controller to:
control an energy source to apply energy to a layer of the build material to cause a portion of the layer to coalesce and solidify to form a slice of the three-dimensional object;
receive, from the radiation sensor, data representing measured absorbance or measured gloss of the layer; and
control the apparatus to modify a process parameter if the measured absorbance or measured gloss indicates an incorrect degree of solidification of a part of the layer. 2. The apparatus of claim 1 wherein the controller is to control an agent distributor to selectively deliver coalescing agent to the portion to cause the portion to coalesce when the energy is applied. 3. The apparatus of claim 2 wherein the radiation sensor is to measure the absorbance of the build material, wherein the coalescing agent is to absorb unfocused radiation used for measuring the absorbance, the unfocused radiation being received from the energy source or another radiation source. 4. The apparatus of claim 1 wherein the radiation sensor is part of a reflectometer, densitometer, colorimeter, digital camera, gloss meter, or haze meter. 5. The apparatus of claim 1 wherein the controller is to control the apparatus to modify the process parameter if the measured absorbance or measured gloss indicates that the part has under-solidified, the under-solidified part being in the portion that is to form the slice of the three-dimensional object. 6. The apparatus of claim 1 wherein the controller is to control the apparatus to modify the process parameter if the measured absorbance or measured gloss indicates that the part has over-solidified. 7. The apparatus of claim 1 further comprising an unfocused radiation source to apply unfocused radiation to the build material, the build material to reflect the unfocused radiation for detection by the radiation sensor to measure the absorbance of the build material, the unfocused radiation having a substantially different radiant spectrum than the energy applied by the energy source. 8. The apparatus of claim 1 further comprising a focused radiation source to apply focused radiation to the build material, the build material to reflect the focused radiation for detection by the radiation sensor to measure the specular reflection or gloss of the build material, the focused radiation having a substantially different radiant spectrum than the energy applied by the energy source. 9. The apparatus of claim 1 further comprising:
a first focused radiation source to apply first focused radiation to the build material at a first non-zero angle, the build material to specularly reflect the first focused radiation for detection by the radiation sensor to measure the gloss of the build material; and
a second radiation sensor to measure any of the first focused radiation that is reflected at a non-specular angle,
prior to controlling the apparatus to modify the process parameter, the controller to correct the gloss measurement by the first radiation sensor using the measurement by the second radiation sensor of the first focused radiation that is non-specularly reflected,
if the measured gloss, after being corrected, indicates the incorrect degree of solidification of the part of the layer, control the apparatus to modify the process parameter. 10. The apparatus of claim 1 wherein:
to measure the absorbance of the portion, the radiation sensor is to measure a reference absorbance or reference gloss of the portion prior to applying the energy to the portion, and is to measure a post-energy absorbance or post-energy gloss of the portion during or after applying the energy to the portion, and
the controller is to compare the reference absorbance or reference gloss and the post-energy absorbance or post-energy gloss to determine a calibrated absorbance or calibrated gloss, and to control the apparatus to modify the process parameter based on the calibrated absorbance or calibrated gloss. 11. The apparatus of claim 1 wherein modifying the process parameter comprises controlling an agent distributor to selectively deliver coalescence modifier agent to the part. 12. The apparatus of claim 1 wherein modifying the process parameter comprises the controller to control the energy source to vary temperature of the build material or vary duration or intensity of the energy applied to the build material. 13. The apparatus of claim 1 further comprising a radiation source to apply pulsed radiation to the build material, the build material to reflect the pulsed radiation for detection by the radiation sensor such that the detected pulsed radiation when the radiation source is in the on-state is compared by the radiation sensor or controller with detected background radiation when the radiation source is in the off-state, the comparison used to remove background noise from the measurement of the absorbance or the gloss. 14. An apparatus for generating a three-dimensional object, the apparatus comprising:
a radiation sensor to measure absorbance of build material; and a controller to:
control an energy source to apply energy to a layer of the build material to cause a portion of the layer to coalesce and solidify to form a slice of the three-dimensional object;
control the energy source or an unfocused radiation source to apply unfocused radiation to the build material,
receive, from the radiation sensor, data representing the measured absorbance of the layer, the measured absorbance based on detection by the radiation sensor of an amount of the unfocused radiation that is reflected by the build material, the measured absorbance positively correlated with a degree of solidification in the layer; and
if the measured absorbance indicates an incorrect degree of solidification of a part of the layer, control the apparatus to modify a process parameter. 15. An apparatus for generating a three-dimensional object, the apparatus comprising:
a radiation sensor to measure gloss of build material; and a controller to:
control an energy source to apply energy to a layer of the build material to cause a portion of the layer to coalesce and solidify to form a slice of the three-dimensional object;
control the energy source or a focused radiation source to apply focused radiation to the build material;
receive, from the radiation sensor, data representing the measured gloss of the layer, the measured gloss based on detection by the radiation sensor of an amount of the focused radiation that is reflected by the build material;
the measured gloss positively correlated with a degree of solidification in the layer; and
if the measured gloss indicates an incorrect degree of solidification of a part of the layer, control the apparatus to modify a process parameter. | 1,700 |
3,418 | 15,130,797 | 1,792 | The present invention relates to a method, device and apparatus for preparing a beverage with a liquid immersible bag with a desired steep time. The measurement and indication of the steep time of a beverage packaged in a disposable immersible bag is accomplished with the use of chromatography paper and color indicators. The proper combination of type, thickness, size and shape of chromatography paper used allows for the pre-setting of different desired steep times. Chromatography paper becomes translucent when wet and attached colors become visible to indicate the progress and the completion of the desired steep time. | 1. An apparatus for preparing a beverage, the beverage ingredients having a desired steep time, comprising:
a liquid immersible bag, said bag structured and arranged to hold the ingredients of the beverage, the bag structured and arranged to be immersed in liquid such that the ingredients of the beverage may steep in the liquid when immersed; a capillary action fluid transport device associated with the liquid immersible bag; and at least one flap carrying a steep timer device with at least one visual indicator of the expiration of a predetermined steeping time, said steep timer device being constructed with a wicking media, said wicking media being in contact with said capillary action fluid transport device. 2. The apparatus of claim 1, wherein said liquid immersible bag has at least one side fold, wherein said side fold acts as a stiffener to facilitate insertion through an opening of a lid of a cup. 3. The apparatus of claim 1, wherein said liquid immersible bag has rigid sides, wherein said rigid sides act as stiffeners to facilitate insertion through the opening of a lid of a cup. 4. The apparatus of claim 3, wherein said rigid sides comprise one of cardboard and plastic. 5. The apparatus of claim 1, wherein said wicking media is one of chromatography paper and filter paper. 6. The apparatus of claim 1, wherein said visual indicator has at least one continuous progress steep time indicator. 7. The apparatus of claim 1, wherein said visual indicator has at least one ornamental design steep time indicator. 8. The apparatus of claim 1, wherein said capillary fluid transport device is attached to the outside of the liquid immersible bag. 9. The apparatus of claim 1, wherein said capillary fluid transport device includes material with capillary action that is integrated into the material of the liquid immersible bag. 10. The apparatus of claim 1, wherein said capillary fluid transport device includes at least one cavity, said cavity adapted to carrying additional beverage ingredients or supplements. 11. The apparatus of claim 1, wherein said wicking media of said flap is comprised of two or more integrated materials with different capillary action characteristics. 12. An apparatus for preparing a beverage having a desired steep time, comprising:
beverage ingredients; a liquid immersible bag, said bag holding the beverage ingredient, said bag having an associated capillary fluid transport device; and a steep timer device with visual indicator of the expiration of a predetermined steep time, said visual indicator including a wicking media; and a handle, said bag being attached to said steep timer at said apparatus handle. 13. The apparatus of claim 12, wherein said liquid immersible bag has at least one side fold, said side fold acting as stiffener to facilitate insertion through an opening of a lid of a cup. 14. The apparatus of claim 12, wherein said liquid immersible bag has rigid sides, said rigid sides acting as stiffeners to facilitate insertion through an opening of a lid of a cup. 15. The apparatus of claim 14, wherein said rigid sides includes one of cardboard and plastic. 16. The apparatus of claim 12, wherein said visual indicator has at least one continuous progress steep time indicator. 17. The apparatus of claim 12, wherein said visual indicator has at least one ornamental design steep time indicator. 18. The apparatus of claim 12, wherein said capillary fluid transport device is attached to the outside of said liquid immersible bag. 19. The apparatus of claim 12, wherein said capillary fluid transport device has material with capillary action integrated into the material of said liquid immersible bag. 20. The apparatus of claim 12, wherein said capillary fluid transport device includes at least one cavity, said cavity carrying additional beverage ingredients or supplements. 21. The apparatus of claim 12, wherein said wicking media is one of chromatography paper and filter paper. 22. The apparatus of claim 12, wherein said upright steep timer device is comprised of two or more integrated materials with different capillary action characteristics. | The present invention relates to a method, device and apparatus for preparing a beverage with a liquid immersible bag with a desired steep time. The measurement and indication of the steep time of a beverage packaged in a disposable immersible bag is accomplished with the use of chromatography paper and color indicators. The proper combination of type, thickness, size and shape of chromatography paper used allows for the pre-setting of different desired steep times. Chromatography paper becomes translucent when wet and attached colors become visible to indicate the progress and the completion of the desired steep time.1. An apparatus for preparing a beverage, the beverage ingredients having a desired steep time, comprising:
a liquid immersible bag, said bag structured and arranged to hold the ingredients of the beverage, the bag structured and arranged to be immersed in liquid such that the ingredients of the beverage may steep in the liquid when immersed; a capillary action fluid transport device associated with the liquid immersible bag; and at least one flap carrying a steep timer device with at least one visual indicator of the expiration of a predetermined steeping time, said steep timer device being constructed with a wicking media, said wicking media being in contact with said capillary action fluid transport device. 2. The apparatus of claim 1, wherein said liquid immersible bag has at least one side fold, wherein said side fold acts as a stiffener to facilitate insertion through an opening of a lid of a cup. 3. The apparatus of claim 1, wherein said liquid immersible bag has rigid sides, wherein said rigid sides act as stiffeners to facilitate insertion through the opening of a lid of a cup. 4. The apparatus of claim 3, wherein said rigid sides comprise one of cardboard and plastic. 5. The apparatus of claim 1, wherein said wicking media is one of chromatography paper and filter paper. 6. The apparatus of claim 1, wherein said visual indicator has at least one continuous progress steep time indicator. 7. The apparatus of claim 1, wherein said visual indicator has at least one ornamental design steep time indicator. 8. The apparatus of claim 1, wherein said capillary fluid transport device is attached to the outside of the liquid immersible bag. 9. The apparatus of claim 1, wherein said capillary fluid transport device includes material with capillary action that is integrated into the material of the liquid immersible bag. 10. The apparatus of claim 1, wherein said capillary fluid transport device includes at least one cavity, said cavity adapted to carrying additional beverage ingredients or supplements. 11. The apparatus of claim 1, wherein said wicking media of said flap is comprised of two or more integrated materials with different capillary action characteristics. 12. An apparatus for preparing a beverage having a desired steep time, comprising:
beverage ingredients; a liquid immersible bag, said bag holding the beverage ingredient, said bag having an associated capillary fluid transport device; and a steep timer device with visual indicator of the expiration of a predetermined steep time, said visual indicator including a wicking media; and a handle, said bag being attached to said steep timer at said apparatus handle. 13. The apparatus of claim 12, wherein said liquid immersible bag has at least one side fold, said side fold acting as stiffener to facilitate insertion through an opening of a lid of a cup. 14. The apparatus of claim 12, wherein said liquid immersible bag has rigid sides, said rigid sides acting as stiffeners to facilitate insertion through an opening of a lid of a cup. 15. The apparatus of claim 14, wherein said rigid sides includes one of cardboard and plastic. 16. The apparatus of claim 12, wherein said visual indicator has at least one continuous progress steep time indicator. 17. The apparatus of claim 12, wherein said visual indicator has at least one ornamental design steep time indicator. 18. The apparatus of claim 12, wherein said capillary fluid transport device is attached to the outside of said liquid immersible bag. 19. The apparatus of claim 12, wherein said capillary fluid transport device has material with capillary action integrated into the material of said liquid immersible bag. 20. The apparatus of claim 12, wherein said capillary fluid transport device includes at least one cavity, said cavity carrying additional beverage ingredients or supplements. 21. The apparatus of claim 12, wherein said wicking media is one of chromatography paper and filter paper. 22. The apparatus of claim 12, wherein said upright steep timer device is comprised of two or more integrated materials with different capillary action characteristics. | 1,700 |
3,419 | 14,414,795 | 1,713 | A method for bonding of a first contact area of a first substrate to a second contact area of a second substrate, the second substrate having a least one reaction layer, and a device for carrying out said method. The method comprises: (a) accommodating the substrates between a first electrode and a second electrode, or within a coil, (b) formation of a reservoir on the first contact area by exposing the first contact area to a plasma (c) at least partially filling of the reservoir with a first educt or a first group of educts, (d) contacting the first contact area with the second contact area for formation of a pre-bond interconnection, (e) forming a permanent bond between the first and second contact areas at least partially strengthened by the reaction of the first educt with a second educt which is contained in the reaction layer of the second substrate. | 1. A method for bonding of a first contact area of a first substrate to a second contact area of a second substrate, the second substrate having at least one reaction layer, said method comprising:
receiving the substrates into a plasma chamber or into a substrate chamber which is connected to a plasma chamber, the plasma chamber having at least first and second generators for respectively generating alternating current at different first and second frequencies (f21, f22), to produce the plasma, forming a reservoir in a reservoir formation layer on the first contact area of the first substrate by applying a plasma, which has been produced in the plasma chamber, to the first contact area, at least partially filling the reservoir with a first educt or a first group of educts, contacting the first contact area of the first substrate with the second contact area of the second substrate to form a pre-bond interconnection, and forming a permanent bond between the first and second contact area at least partially strengthened by the reaction of the first educt with a second educt which is contained in the at least one reaction layer of the second substrate. 2. The method as claimed in claim 1, wherein the first frequency (f21) is between 1 Hz and 20 MHz. 3. The method as claimed in claim 1, wherein the second frequency (f22) is between 1 Hz and 20 MHz. 4. The method as claimed in claim 1, wherein a voltage amplitude of the first and/or second electrode is between 1 V and 1000 V. 5. A method for bonding of a first contact area of a first substrate to a second contact area of a second substrate, the second substrate having a least one reaction layer, the method comprising:
receiving the first and second substrates into an inductively coupled plasma chamber, forming a reservoir in a reservoir formation layer on the first contact area by exposing the first contact area to a plasma which has been produced by means of inductive coupling of, wherein a first generator generates alternating current at a first frequency (f21) different from a second frequency (f22) of an alternating current generated by a second generator during plasma production, at least partially filling the reservoir with a first educt or a first group of educts, contacting the first contact area with the second contact area to form a pre-bond interconnection, forming a permanent bond between the first and second contact areas at least partially strengthened by the reaction of the first educt with a second educt which is contained in the at least one reaction layer of the second substrate. 6. The method as claimed in claim 5, wherein the first frequency (f21) is between 0.001 kHz and 100000 kHz. 7. A device for bonding of a first contact area of a first substrate to a second contact area of a second substrate, the second substrate having a least one reaction layer, the device comprising:
a bonding chamber, a first electrode and a second electrode located opposite the first electrode, receiving means for receiving the substrates between the first electrode and the second electrode, reservoir formation means for forming a reservoir in a reservoir formation layer on the first contact area by exposing the first contact area to a plasma which has been produced by means of capacitive coupling of the first and second electrodes and, wherein an alternating current at a first frequency (f21) is applied to the first electrode during plasma production, wherein the first frequency is different from a second frequency (f22) of an alternating current applied to the second electrode, means for contacting the first contact area with the second contact area to form a pre-bond interconnection. 8. The device as claimed in claim 7, wherein the first and/or the second frequencies (f21, f22) are adjustable. 9. A device for bonding of a first contact area of a first substrate to a second contact area of a second substrate, the second substrate having a least one reaction layer, the device comprising:
a bonding chamber, a coil, receiving means for accommodating the substrates within the coil, reservoir formation means for forming a reservoir in a reservoir formation layer on the first contact area by exposing the first contact area to a plasma which has been produced by means of capacitive coupling of the electrodes, wherein an alternating current of a first frequency (f21) is applied to the first electrode during plasma production, wherein the first frequency is different from a second frequency (f22) of an alternating current applied to the second electrode, and means for contacting the first contact area with the second contact area to form a pre-bond interconnection. 10. The device as claimed in claim 9, wherein the first and/or the second frequencies (f21, f22) are adjustable. 11. The method as claimed in claim 1, wherein the method is carried out in a bonding chamber and the bonding chamber, at least in the formation of the reservoir, is exposed to a chamber pressure between 0.1 and 0.9 mbar. 12. The method as claimed in claim 11, wherein O2 gas and/or N2 gas and/or Ar gas predominates in the bonding chamber, at least when the reservoir is being formed. 13. A device for bonding of a first contact area of a first substrate to a second contact area of a second substrate, the second substrate having a least one reaction layer, the device comprising:
a plasma chamber for producing a plasma, the plasma chamber having at least two generators which can be respectively operated with different first and second frequencies (f21, f22), producing the plasma, a bonding chamber connected to the plasma chamber, reservoir formation means for forming a reservoir in a reservoir formation layer on the first contact area by exposing the first contact area to a plasma which has been produced in the plasma chamber, means for contacting the first contact area with the second contact area to form a pre-bond interconnection. 14. The device as claimed in claim 13, wherein a closable opening is located between the plasma chamber and the bonding chamber. 15. The method as claimed in claim 1, wherein an ac voltage applied to a first electrode of said plasma chamber has the first frequency (f21) in a frequency range between 1 Hz and 20 MHz. 16. The method as claimed in claim 1, wherein the first frequency (f21) is between 0.001 kHz and 100000 kHz. 17. The method as claimed in claim 1, wherein the second frequency (f22) is set in a frequency range between 0.001 kHz and 100000 kHz. 18. The method as claimed in claim 5, wherein the second frequency (f22) is set in a frequency range between 0.001 kHz and 100000 kHz. 19. The method as claimed in claim 5, wherein the method is carried out in a bonding chamber and the bonding chamber, at least in the formation of the reservoir, is exposed to a chamber pressure between 0.1 and 0.9 mbar. 20. The method as claimed in claim 1, wherein O2 gas and/or N2 gas and/or Ar gas predominates in the bonding chamber, at least when the reservoir is being formed. 21. The method as claimed in claim 5, wherein O2 gas and/or N2 gas and/or Ar gas predominates in the bonding chamber, at least when the reservoir is being formed. 22. The method as claimed in claim 1, wherein a closable opening is located between the plasma chamber and the bonding chamber. | A method for bonding of a first contact area of a first substrate to a second contact area of a second substrate, the second substrate having a least one reaction layer, and a device for carrying out said method. The method comprises: (a) accommodating the substrates between a first electrode and a second electrode, or within a coil, (b) formation of a reservoir on the first contact area by exposing the first contact area to a plasma (c) at least partially filling of the reservoir with a first educt or a first group of educts, (d) contacting the first contact area with the second contact area for formation of a pre-bond interconnection, (e) forming a permanent bond between the first and second contact areas at least partially strengthened by the reaction of the first educt with a second educt which is contained in the reaction layer of the second substrate.1. A method for bonding of a first contact area of a first substrate to a second contact area of a second substrate, the second substrate having at least one reaction layer, said method comprising:
receiving the substrates into a plasma chamber or into a substrate chamber which is connected to a plasma chamber, the plasma chamber having at least first and second generators for respectively generating alternating current at different first and second frequencies (f21, f22), to produce the plasma, forming a reservoir in a reservoir formation layer on the first contact area of the first substrate by applying a plasma, which has been produced in the plasma chamber, to the first contact area, at least partially filling the reservoir with a first educt or a first group of educts, contacting the first contact area of the first substrate with the second contact area of the second substrate to form a pre-bond interconnection, and forming a permanent bond between the first and second contact area at least partially strengthened by the reaction of the first educt with a second educt which is contained in the at least one reaction layer of the second substrate. 2. The method as claimed in claim 1, wherein the first frequency (f21) is between 1 Hz and 20 MHz. 3. The method as claimed in claim 1, wherein the second frequency (f22) is between 1 Hz and 20 MHz. 4. The method as claimed in claim 1, wherein a voltage amplitude of the first and/or second electrode is between 1 V and 1000 V. 5. A method for bonding of a first contact area of a first substrate to a second contact area of a second substrate, the second substrate having a least one reaction layer, the method comprising:
receiving the first and second substrates into an inductively coupled plasma chamber, forming a reservoir in a reservoir formation layer on the first contact area by exposing the first contact area to a plasma which has been produced by means of inductive coupling of, wherein a first generator generates alternating current at a first frequency (f21) different from a second frequency (f22) of an alternating current generated by a second generator during plasma production, at least partially filling the reservoir with a first educt or a first group of educts, contacting the first contact area with the second contact area to form a pre-bond interconnection, forming a permanent bond between the first and second contact areas at least partially strengthened by the reaction of the first educt with a second educt which is contained in the at least one reaction layer of the second substrate. 6. The method as claimed in claim 5, wherein the first frequency (f21) is between 0.001 kHz and 100000 kHz. 7. A device for bonding of a first contact area of a first substrate to a second contact area of a second substrate, the second substrate having a least one reaction layer, the device comprising:
a bonding chamber, a first electrode and a second electrode located opposite the first electrode, receiving means for receiving the substrates between the first electrode and the second electrode, reservoir formation means for forming a reservoir in a reservoir formation layer on the first contact area by exposing the first contact area to a plasma which has been produced by means of capacitive coupling of the first and second electrodes and, wherein an alternating current at a first frequency (f21) is applied to the first electrode during plasma production, wherein the first frequency is different from a second frequency (f22) of an alternating current applied to the second electrode, means for contacting the first contact area with the second contact area to form a pre-bond interconnection. 8. The device as claimed in claim 7, wherein the first and/or the second frequencies (f21, f22) are adjustable. 9. A device for bonding of a first contact area of a first substrate to a second contact area of a second substrate, the second substrate having a least one reaction layer, the device comprising:
a bonding chamber, a coil, receiving means for accommodating the substrates within the coil, reservoir formation means for forming a reservoir in a reservoir formation layer on the first contact area by exposing the first contact area to a plasma which has been produced by means of capacitive coupling of the electrodes, wherein an alternating current of a first frequency (f21) is applied to the first electrode during plasma production, wherein the first frequency is different from a second frequency (f22) of an alternating current applied to the second electrode, and means for contacting the first contact area with the second contact area to form a pre-bond interconnection. 10. The device as claimed in claim 9, wherein the first and/or the second frequencies (f21, f22) are adjustable. 11. The method as claimed in claim 1, wherein the method is carried out in a bonding chamber and the bonding chamber, at least in the formation of the reservoir, is exposed to a chamber pressure between 0.1 and 0.9 mbar. 12. The method as claimed in claim 11, wherein O2 gas and/or N2 gas and/or Ar gas predominates in the bonding chamber, at least when the reservoir is being formed. 13. A device for bonding of a first contact area of a first substrate to a second contact area of a second substrate, the second substrate having a least one reaction layer, the device comprising:
a plasma chamber for producing a plasma, the plasma chamber having at least two generators which can be respectively operated with different first and second frequencies (f21, f22), producing the plasma, a bonding chamber connected to the plasma chamber, reservoir formation means for forming a reservoir in a reservoir formation layer on the first contact area by exposing the first contact area to a plasma which has been produced in the plasma chamber, means for contacting the first contact area with the second contact area to form a pre-bond interconnection. 14. The device as claimed in claim 13, wherein a closable opening is located between the plasma chamber and the bonding chamber. 15. The method as claimed in claim 1, wherein an ac voltage applied to a first electrode of said plasma chamber has the first frequency (f21) in a frequency range between 1 Hz and 20 MHz. 16. The method as claimed in claim 1, wherein the first frequency (f21) is between 0.001 kHz and 100000 kHz. 17. The method as claimed in claim 1, wherein the second frequency (f22) is set in a frequency range between 0.001 kHz and 100000 kHz. 18. The method as claimed in claim 5, wherein the second frequency (f22) is set in a frequency range between 0.001 kHz and 100000 kHz. 19. The method as claimed in claim 5, wherein the method is carried out in a bonding chamber and the bonding chamber, at least in the formation of the reservoir, is exposed to a chamber pressure between 0.1 and 0.9 mbar. 20. The method as claimed in claim 1, wherein O2 gas and/or N2 gas and/or Ar gas predominates in the bonding chamber, at least when the reservoir is being formed. 21. The method as claimed in claim 5, wherein O2 gas and/or N2 gas and/or Ar gas predominates in the bonding chamber, at least when the reservoir is being formed. 22. The method as claimed in claim 1, wherein a closable opening is located between the plasma chamber and the bonding chamber. | 1,700 |
3,420 | 16,037,917 | 1,735 | A foam for use in a lost-foam casting process utilized in the manufacture of a component for a gas turbine engine, the foam having a void fraction less than or equal to ninety five percent, is disclosed. The foam may include a first layer comprising polymer foam having an open-cell structure and a void fraction greater than ninety five percent. A second layer, comprising adhesive, may be adhered to the first layer. A third layer comprising particulate material may be adhered to the second layer. | 1. A foam for forming a gas turbine engine fan blade using a lost-foam casting process, the foam having a void fraction less than or equal to ninety five percent, comprising:
a first layer, the first layer comprising a polymer foam having an open-cell structure and a void fraction greater than ninety five percent; a second layer, the second layer comprising an adhesive adhered to the first layer; and a third layer, the third layer comprising a particulate material, the third layer adhered to the second layer. 2. The modified foam according to claim 1, wherein the polymer foam is selected from the group consisting of polyurethane polymer foam, polyvinyl chloride polymer foam, polystyrene polymer foam, polyimide polymer foam, silicone polymer foam, polyethylene polymer foam, polyester polymer foam, polypropylene foam and combinations thereof. 3. The foam according to claim 1, wherein the adhesive is an adhesive polymer selected from the group consisting of acrylic polymer, alkyd polymer, styrene acrylic polymer, styrene butadiene polymer, vinyl acetate polymer, vinyl acetate homopolymer polymer, vinyl acrylic polymer, vinyl maleate polymer, vinyl versatate polymer, vinyl alcohol polymer, polyvinyl chloride polymer, polyvinylpyrrolidone polymer, casein and combinations thereof. 4. The foam according to claim 1, wherein the particulate material is selected from the group consisting of wax powder, wood flour, polymer powder and combinations thereof. 5. The foam according to claim 4, wherein the wax powder is selected from the group consisting of animal wax powder, vegetable wax powder, mineral wax powder, petroleum wax powder and combinations thereof. 6. The foam according to claim 4, wherein the polymer powder is selected from the group consisting of polyurethane polymer powder, polyvinyl chloride polymer powder, polystyrene polymer powder, polyimide polymer powder, polyethylene polymer powder, polyester polymer powder, polypropylene polymer powder and combinations thereof. 7. A method of manufacturing foam for forming a gas turbine engine fan blade using a lost-foam casting process, the foam having a void fraction less than or equal to ninety five percent, comprising:
providing a polymer foam having an open-cell structure and a void fraction greater than ninety five percent; coating the polymer foam with an adhesive; and applying a particulate material to the adhesive. 8. The method of manufacturing the foam according to claim 7, wherein the polymer foam is selected from the group consisting of polyurethane polymer foam, polyvinyl chloride polymer foam, polystyrene polymer foam, polyimide polymer foam, silicone polymer foam, polyethylene polymer foam, polyester polymer foam, polypropylene foam and combinations thereof. 9. The method of manufacturing the foam according to claim 7, wherein the adhesive comprises an adhesive polymer, the adhesive polymer selected from the group consisting of acrylic polymer, alkyd polymer, styrene acrylic polymer, styrene butadiene polymer, vinyl acetate polymer, vinyl acetate homopolymer polymer, vinyl acrylic polymer, vinyl maleate polymer, vinyl versatate polymer, vinyl alcohol polymer, polyvinyl chloride polymer, polyvinylpyrrolidone polymer, casein and combinations thereof. 10. The method of manufacturing the foam according to claim 7, wherein the particulate material is selected from the group consisting of wax powder, wood flour, polymer powder and combinations thereof. 11. The method of manufacturing the foam according to claim 10, wherein the wax powder is selected from the group consisting of animal wax powder, vegetable wax powder, mineral wax powder, petroleum wax powder and combinations thereof. 12. The method of manufacturing the foam according to claim 10, wherein the polymer powder is selected from the group consisting of polyurethane polymer powder, polyvinyl chloride polymer powder, polystyrene polymer powder, polyimide polymer powder, polyethylene polymer powder, polyester polymer powder, polypropylene polymer powder and combinations thereof. 13. The method of manufacturing the foam according to claim 7, wherein the coating the polymer foam with an adhesive step comprises applying an emulsion to the polymer foam, the emulsion comprising an adhesive polymer and solvent. 14. The method of manufacturing the foam according to claim 13, further comprising removing excess solvent from the polymer foam before applying a particulate material to the adhesive. 15. The method of manufacturing the foam according to claim 7, wherein the polymer foam comprises ligaments positioned between nodes, and further comprising heating the foam to a temperature above the melting temperature of the particulate material, followed by cooling the foam to a temperature below the melting temperature of the particulate material to form a substantially continuous coating of particulate material over the ligaments. 16. The method of manufacturing the foam according to claim 7, wherein the applying a particulate material to the adhesive includes passing the adhesive coated polymer foam through a fluidized bed of particulate material. | A foam for use in a lost-foam casting process utilized in the manufacture of a component for a gas turbine engine, the foam having a void fraction less than or equal to ninety five percent, is disclosed. The foam may include a first layer comprising polymer foam having an open-cell structure and a void fraction greater than ninety five percent. A second layer, comprising adhesive, may be adhered to the first layer. A third layer comprising particulate material may be adhered to the second layer.1. A foam for forming a gas turbine engine fan blade using a lost-foam casting process, the foam having a void fraction less than or equal to ninety five percent, comprising:
a first layer, the first layer comprising a polymer foam having an open-cell structure and a void fraction greater than ninety five percent; a second layer, the second layer comprising an adhesive adhered to the first layer; and a third layer, the third layer comprising a particulate material, the third layer adhered to the second layer. 2. The modified foam according to claim 1, wherein the polymer foam is selected from the group consisting of polyurethane polymer foam, polyvinyl chloride polymer foam, polystyrene polymer foam, polyimide polymer foam, silicone polymer foam, polyethylene polymer foam, polyester polymer foam, polypropylene foam and combinations thereof. 3. The foam according to claim 1, wherein the adhesive is an adhesive polymer selected from the group consisting of acrylic polymer, alkyd polymer, styrene acrylic polymer, styrene butadiene polymer, vinyl acetate polymer, vinyl acetate homopolymer polymer, vinyl acrylic polymer, vinyl maleate polymer, vinyl versatate polymer, vinyl alcohol polymer, polyvinyl chloride polymer, polyvinylpyrrolidone polymer, casein and combinations thereof. 4. The foam according to claim 1, wherein the particulate material is selected from the group consisting of wax powder, wood flour, polymer powder and combinations thereof. 5. The foam according to claim 4, wherein the wax powder is selected from the group consisting of animal wax powder, vegetable wax powder, mineral wax powder, petroleum wax powder and combinations thereof. 6. The foam according to claim 4, wherein the polymer powder is selected from the group consisting of polyurethane polymer powder, polyvinyl chloride polymer powder, polystyrene polymer powder, polyimide polymer powder, polyethylene polymer powder, polyester polymer powder, polypropylene polymer powder and combinations thereof. 7. A method of manufacturing foam for forming a gas turbine engine fan blade using a lost-foam casting process, the foam having a void fraction less than or equal to ninety five percent, comprising:
providing a polymer foam having an open-cell structure and a void fraction greater than ninety five percent; coating the polymer foam with an adhesive; and applying a particulate material to the adhesive. 8. The method of manufacturing the foam according to claim 7, wherein the polymer foam is selected from the group consisting of polyurethane polymer foam, polyvinyl chloride polymer foam, polystyrene polymer foam, polyimide polymer foam, silicone polymer foam, polyethylene polymer foam, polyester polymer foam, polypropylene foam and combinations thereof. 9. The method of manufacturing the foam according to claim 7, wherein the adhesive comprises an adhesive polymer, the adhesive polymer selected from the group consisting of acrylic polymer, alkyd polymer, styrene acrylic polymer, styrene butadiene polymer, vinyl acetate polymer, vinyl acetate homopolymer polymer, vinyl acrylic polymer, vinyl maleate polymer, vinyl versatate polymer, vinyl alcohol polymer, polyvinyl chloride polymer, polyvinylpyrrolidone polymer, casein and combinations thereof. 10. The method of manufacturing the foam according to claim 7, wherein the particulate material is selected from the group consisting of wax powder, wood flour, polymer powder and combinations thereof. 11. The method of manufacturing the foam according to claim 10, wherein the wax powder is selected from the group consisting of animal wax powder, vegetable wax powder, mineral wax powder, petroleum wax powder and combinations thereof. 12. The method of manufacturing the foam according to claim 10, wherein the polymer powder is selected from the group consisting of polyurethane polymer powder, polyvinyl chloride polymer powder, polystyrene polymer powder, polyimide polymer powder, polyethylene polymer powder, polyester polymer powder, polypropylene polymer powder and combinations thereof. 13. The method of manufacturing the foam according to claim 7, wherein the coating the polymer foam with an adhesive step comprises applying an emulsion to the polymer foam, the emulsion comprising an adhesive polymer and solvent. 14. The method of manufacturing the foam according to claim 13, further comprising removing excess solvent from the polymer foam before applying a particulate material to the adhesive. 15. The method of manufacturing the foam according to claim 7, wherein the polymer foam comprises ligaments positioned between nodes, and further comprising heating the foam to a temperature above the melting temperature of the particulate material, followed by cooling the foam to a temperature below the melting temperature of the particulate material to form a substantially continuous coating of particulate material over the ligaments. 16. The method of manufacturing the foam according to claim 7, wherein the applying a particulate material to the adhesive includes passing the adhesive coated polymer foam through a fluidized bed of particulate material. | 1,700 |
3,421 | 14,881,241 | 1,734 | A nanoparticle of a decomposition product of a transition metal aluminum hydride compound, a transition metal borohydride compound, or a transition metal gallium hydride compound. A process of: reacting a transition metal salt with an aluminum hydride compound, a borohydride compound, or a gallium hydride compound to produce one or more of the nanoparticles. The reaction occurs in solution while being sonicated at a temperature at which the metal hydride compound decomposes. A process of: reacting a nanoparticle with a compound containing at least two hydroxyl groups to form a coating having multi-dentate metal-alkoxides. | 1. A process comprising:
reacting a transition metal salt with an aluminum hydride compound, a borohydride compound, or a gallium hydride compound to produce one or more nanoparticles comprising a decomposition product of a metal hydride compound;
wherein the metal hydride compound is a transition metal aluminum hydride compound, a transition metal borohydride compound, or a transition metal gallium hydride compound; and
wherein the reaction occurs in solution while being sonicated at a temperature at which the metal hydride compound decomposes. 2. The process of claim 1, wherein the transition metal is zirconium, hafnium, titanium, vanadium, scandium, yttrium, niobium, chromium, tantalum, thorium, or uranium. 3. The process of claim 1, wherein the transition metal salt is ZrCl4, Zr(BH4)4, or Hf(BH4)4 and the aluminum hydride compound is LiAlH4. 4. The process of claim 1, further comprising:
annealing the nanoparticle. 5. The process of claim 1, further comprising:
reacting the nanoparticle with a compound containing at least two hydroxyl groups to form a coating comprising multi-dentate metal-alkoxides. 6. The process of claim 5, wherein the coating is a xerogel. 7. The process of claim 5, wherein the compound is glycerol, sorbitol, or a carbohydrate. 8. A process comprising:
reacting a nanoparticle with a compound containing at least two hydroxyl groups to form a coating comprising multi-dentate metal-alkoxides;
wherein the nanoparticle comprises a metal that reacts with hydroxyl groups to form the metal-alkoxides. 9. The process of claim 8, wherein the metal is aluminum, boron, silicon, zirconium, or hafnium. 10. The process of claim 8, wherein the coating is a xerogel. 11. The process of claim 8, wherein the compound is glycerol, sorbitol, or a carbohydrate. | A nanoparticle of a decomposition product of a transition metal aluminum hydride compound, a transition metal borohydride compound, or a transition metal gallium hydride compound. A process of: reacting a transition metal salt with an aluminum hydride compound, a borohydride compound, or a gallium hydride compound to produce one or more of the nanoparticles. The reaction occurs in solution while being sonicated at a temperature at which the metal hydride compound decomposes. A process of: reacting a nanoparticle with a compound containing at least two hydroxyl groups to form a coating having multi-dentate metal-alkoxides.1. A process comprising:
reacting a transition metal salt with an aluminum hydride compound, a borohydride compound, or a gallium hydride compound to produce one or more nanoparticles comprising a decomposition product of a metal hydride compound;
wherein the metal hydride compound is a transition metal aluminum hydride compound, a transition metal borohydride compound, or a transition metal gallium hydride compound; and
wherein the reaction occurs in solution while being sonicated at a temperature at which the metal hydride compound decomposes. 2. The process of claim 1, wherein the transition metal is zirconium, hafnium, titanium, vanadium, scandium, yttrium, niobium, chromium, tantalum, thorium, or uranium. 3. The process of claim 1, wherein the transition metal salt is ZrCl4, Zr(BH4)4, or Hf(BH4)4 and the aluminum hydride compound is LiAlH4. 4. The process of claim 1, further comprising:
annealing the nanoparticle. 5. The process of claim 1, further comprising:
reacting the nanoparticle with a compound containing at least two hydroxyl groups to form a coating comprising multi-dentate metal-alkoxides. 6. The process of claim 5, wherein the coating is a xerogel. 7. The process of claim 5, wherein the compound is glycerol, sorbitol, or a carbohydrate. 8. A process comprising:
reacting a nanoparticle with a compound containing at least two hydroxyl groups to form a coating comprising multi-dentate metal-alkoxides;
wherein the nanoparticle comprises a metal that reacts with hydroxyl groups to form the metal-alkoxides. 9. The process of claim 8, wherein the metal is aluminum, boron, silicon, zirconium, or hafnium. 10. The process of claim 8, wherein the coating is a xerogel. 11. The process of claim 8, wherein the compound is glycerol, sorbitol, or a carbohydrate. | 1,700 |
3,422 | 15,199,084 | 1,781 | An article includes a substrate that is substantially opaque to visible light and a coating disposed on the substrate. The coating includes a coating material having an inherent index of refraction, wherein the coating has an effective index of refraction that is less than the inherent index of refraction, and wherein the effective index of refraction is less than 1.8. | 1. An article, comprising:
a substrate that is substantially opaque to visible light; and a coating disposed on the substrate, wherein the coating comprises a coating material having an inherent index of refraction, wherein the coating has an effective index of refraction that is less than the inherent index of refraction, and wherein the effective index of refraction is less than 1.8, and wherein the coating comprises a plurality of columnar structures oriented such that a longitudinal axis of a columnar structure forms an angle with respect to a direction tangential to the substrate that is less than 90 degrees. 2. The article of claim 1, wherein the substrate comprises a metallic material, a ceramic material, or an intermetallic material. 3. The article of claim 1, wherein the substrate comprises a titanium alloy, a superalloy, or a ceramic-matrix composite. 4. The article of claim 1, wherein the article comprises a component for a turbine assembly. 5. The article of claim 4, wherein the component is a compressor blade or compressor vane. 6. The article of claim 1, wherein the coating comprises a plurality of columnar structures oriented such that a longitudinal axis of a columnar structure forms an angle with respect to a direction tangential to the substrate that is less than 90 degrees. 7. The article of claim 1, wherein the angle is less than 80 degrees. 8. The article of claim 1, wherein the angle is less than 60 degrees. 9. The article of claim 1, wherein the plurality of columnar structures has a nominal intercolumnar spacing of less than about 5 micrometers. 10. The article of claim 9, wherein the nominal intercolumnar spacing is less than about 2 micrometers. 11. The article of claim 9, wherein the nominal intercolumnar spacing is less than about 0.5 micrometer. 12. The article of claim 6, wherein the plurality of columnar structures has a nominal column width of less than about 2.5 micrometers. 13. The article of claim 12, wherein the nominal column width is less than about 1 micrometer. 14. The article of claim 12, wherein the nominal column width is less than about 0.25 micrometer. 15. The article of claim 1, wherein the coating has a coating stiffness value that is less than an inherent stiffness value of the coating material. 16. The article of claim 1, wherein the coating material comprises an oxide or a fluoride. 17. The article of claim 1, wherein the coating material comprises alumina, silica, zirconia, chromia, or a combination including one or more of these. 18. The article of claim 1, wherein the coating comprises a fluoride of one or more alkaline earth elements. 19. The article of claim 1, wherein the coating has a thickness of less than 100 micrometers. 20. The article of claim 1, wherein the coating has a thickness of less than 25 micrometers. 21. The article of claim 1, wherein the coating has a thickness of less than 10 micrometers. 22. The article of claim 1, wherein the substrate comprises an internal surface of the article. 23. The article of claim 1, wherein the substrate comprises an external surface of the article. 24. The article of claim 1, further comprising at least one intervening coating layer disposed between the substrate and the coating. 25. The article of claim 1, wherein the coating has a porosity of at least about 40 percent by volume. 26. An article comprising:
a substrate comprising a titanium alloy, a superalloy, or a ceramic-matrix composite; and a coating disposed on the substrate, the coating comprising (a) a fluoride of one or more alkaline earth elements, (b) alumina, silica, zirconia, or chromia, or (c) a combination including any one or more of the foregoing alternatives; wherein the coating further comprises a plurality of columnar structures oriented such that a longitudinal axis of a columnar structure forms an angle with respect to a direction tangential to the substrate that is less than 60 degrees. | An article includes a substrate that is substantially opaque to visible light and a coating disposed on the substrate. The coating includes a coating material having an inherent index of refraction, wherein the coating has an effective index of refraction that is less than the inherent index of refraction, and wherein the effective index of refraction is less than 1.8.1. An article, comprising:
a substrate that is substantially opaque to visible light; and a coating disposed on the substrate, wherein the coating comprises a coating material having an inherent index of refraction, wherein the coating has an effective index of refraction that is less than the inherent index of refraction, and wherein the effective index of refraction is less than 1.8, and wherein the coating comprises a plurality of columnar structures oriented such that a longitudinal axis of a columnar structure forms an angle with respect to a direction tangential to the substrate that is less than 90 degrees. 2. The article of claim 1, wherein the substrate comprises a metallic material, a ceramic material, or an intermetallic material. 3. The article of claim 1, wherein the substrate comprises a titanium alloy, a superalloy, or a ceramic-matrix composite. 4. The article of claim 1, wherein the article comprises a component for a turbine assembly. 5. The article of claim 4, wherein the component is a compressor blade or compressor vane. 6. The article of claim 1, wherein the coating comprises a plurality of columnar structures oriented such that a longitudinal axis of a columnar structure forms an angle with respect to a direction tangential to the substrate that is less than 90 degrees. 7. The article of claim 1, wherein the angle is less than 80 degrees. 8. The article of claim 1, wherein the angle is less than 60 degrees. 9. The article of claim 1, wherein the plurality of columnar structures has a nominal intercolumnar spacing of less than about 5 micrometers. 10. The article of claim 9, wherein the nominal intercolumnar spacing is less than about 2 micrometers. 11. The article of claim 9, wherein the nominal intercolumnar spacing is less than about 0.5 micrometer. 12. The article of claim 6, wherein the plurality of columnar structures has a nominal column width of less than about 2.5 micrometers. 13. The article of claim 12, wherein the nominal column width is less than about 1 micrometer. 14. The article of claim 12, wherein the nominal column width is less than about 0.25 micrometer. 15. The article of claim 1, wherein the coating has a coating stiffness value that is less than an inherent stiffness value of the coating material. 16. The article of claim 1, wherein the coating material comprises an oxide or a fluoride. 17. The article of claim 1, wherein the coating material comprises alumina, silica, zirconia, chromia, or a combination including one or more of these. 18. The article of claim 1, wherein the coating comprises a fluoride of one or more alkaline earth elements. 19. The article of claim 1, wherein the coating has a thickness of less than 100 micrometers. 20. The article of claim 1, wherein the coating has a thickness of less than 25 micrometers. 21. The article of claim 1, wherein the coating has a thickness of less than 10 micrometers. 22. The article of claim 1, wherein the substrate comprises an internal surface of the article. 23. The article of claim 1, wherein the substrate comprises an external surface of the article. 24. The article of claim 1, further comprising at least one intervening coating layer disposed between the substrate and the coating. 25. The article of claim 1, wherein the coating has a porosity of at least about 40 percent by volume. 26. An article comprising:
a substrate comprising a titanium alloy, a superalloy, or a ceramic-matrix composite; and a coating disposed on the substrate, the coating comprising (a) a fluoride of one or more alkaline earth elements, (b) alumina, silica, zirconia, or chromia, or (c) a combination including any one or more of the foregoing alternatives; wherein the coating further comprises a plurality of columnar structures oriented such that a longitudinal axis of a columnar structure forms an angle with respect to a direction tangential to the substrate that is less than 60 degrees. | 1,700 |
3,423 | 13,576,565 | 1,771 | A method for circulating a cooled regenerated catalyst comprises the following steps: a regenerated catalyst derived from a regenerator ( 5 ) is cooled to 200-720° C. by a catalyst cooler ( 8 A), which either directly enters into a riser reactor ( 2 ) without mixing with hot regenerated catalyst, or enters the same after mixing with another portion of uncooled hot regenerated catalyst and thereby obtaining a hybrid regenerated catalyst with its temperature lower than that of the regenerator; a contact reaction between a hydrocarbon raw materials and the catalyst is performed in the riser reactor ( 2 ); the reaction product is introduced into a settling vessel ( 1 ) to separated the catalyst and oil gas; the separated catalyst ready for regeneration is stream-stripped in a stream stripping phase ( 1 A) and enters the regenerator ( 5 ) for regeneration through charring; after cooling, the regenerated catalyst returns to the riser reactor ( 2 ) for recycling. | 1. A cycling method and its equipment of cold regenerated catalyst, characterized in that, including a FCC process: hydrocarbon materials react with catalyst in the riser reactor (with or without a fluidized bed reactor); the materials enter into a settler for the separation of catalyst from gas and oil; Separated catalyst will be stripped and enter into regenerator to burn for regeneration; The regenerated catalyst will be cold or/and not be cold to return the riser reactor directly for cycling use; The details are as follows:
the regenerator includes one, two, or more catalyst coolers, each connected to the riser reactor (or the fluidized bed reactor) is used to adjust the reaction temperature of the reaction zone, or/and to adjust regenerator temperatures, so as to keep them in the best value; the catalyst coolers connected with the riser reactor (or the fluidized set in the inside or outside of regenerator, or set under its riser reactor; The catalyst entrance of the shell of the described catalyst cooler directly (or through a pipeline) connects with the regenerator dense phase; there are internal components in the cooler for removing heat; there are fluidized media distribution facilities under the cooler; In the downstream, there is a buffer space for mixed buffer catalyst; the upper part is installed or not installed the gas channel to return to diluting phase of the regenerator; There are one, two or more catalyst exits set in the catalyst mixed buffer space in the downstream of the described catalyst cooler; One, two or more exits of catalysts are connected to the transmission channel of cold catalyst used to deliver cold-regenerated catalyst circulation to one, two or more of the riser (reactor or auxiliary riser); Another one, two or more (or not) catalyst exists are connected to the transmission channel of cold catalyst for conveying cold regenerated catalyst return to the regenerator; The described transmission channel of cold catalyst to the riser is set in the outside of the described catalyst cooler's shell, or all (or partly) set in the inside of the described catalyst cooler's shell; The return channel of the cooled catalyst back to the regenerator all set in the outside of the described catalyst cooler's shell, or all (or partly) set in the inside of the described catalyst cooler's shell. The described riser reactor is set one, two or more reaction zones with or without fluidized bed reactor; Before cold regenerated catalyst enters into the riser reactor or fluidized bed reactor, the riser reactor is set (or not set) a pre-lift section, with pre-lift media to send the cold regenerated catalyst to the riser reactor or the fluidized bed reactor; The described pre-lift section can all be set outside of the catalyst cooler shell, or all (or part) set inside. Part of regenerated catalysts coming from regenerator are cooled by catalyst cooler within 200 to 720° C. and enter into the pre-lift or directly into each reaction zone of riser reactor; Or these regenerated catalysts mix or/and with hot regenerated catalyst without cooling to get the regenerated catalyst mixture which temperature is lower than regenerator temperature and then the mixture enter into pre-lift or/and each reaction zone of the riser reactor; Or the cold and the hot regenerated catalysts enter into the pre-lift of riser separately and directly with pre-lift media for increasing the catalysts temperature to reach a proper temperature and then the mixture enter into each reaction zone of riser reactor; Or the regenerated catalyst without cooling by catalyst cooler enter into the pre-lift zone or/and each reaction zone of the riser reactor directly for cycling. 2. The method and its equipment of claim 1, wherein Setting (or not setting) one, two or more assistant risers, the described cold regenerated catalyst through the assistant risers with the pre-lift media are lifted to one, two or more riser reactors or fluidized bed reactor reaction zones as a cold shock agent for cycling. 3. The method and its equipment of claim 1, wherein the regenerated catalysts coming from regenerator as step (5) described are cooled by the catalyst cooler within 360 to 650° C. 4. The method and its equipment of claim 1, wherein the temperature of the described cold regenerated catalyst can be controlled by adjusting the flows of the fluidized media and/or taking-heat media or adjusting other parameters;
or controlled by adjusting the flows of the fluidized media and/or taking-heat media and/or adjusting the flows of cool catalyst returning regenerator or other parameters. 5. The method and its equipment of claim 1, wherein the temperature of the described regenerated catalysts mixture can be controlled by adjusting the ratio of cold and hot regenerated catalyst. 6. The method and its equipment of claim 1, wherein the reaction temperature of the described riser reactor or fluidized bed reactor reaction zones can be controlled by adjusting the ratio of the catalyst and feed, or/and by adjusting the temperature of the described cold regenerated catalyst or the temperature of the described regenerated catalyst mixture, or/and by using multi-point feeding technology, and/or by adding various cold shock agents to the riser reactor. 7. The method and its equipment of claim 1, wherein the described taking-heat medias in the catalyst cooler include water, steam, air and various oils. 8. The method and its equipment of claim 1, wherein the described cycling method and its equipment of the cold regenerated catalyst can be used widely for various FCC including tar catalytic cracking, wax oil catalytic cracking, gasoline catalytic modification for improving quality, or light hydrocarbon catalytic conversion, or for other burning process of gas-solid fluidized reaction including residue pre-processing, ethylene made by methanol, fluidize coking or flexible coking. 9. The method and its equipment of claim 1, wherein the cycling method and its equipment of cold regenerated catalyst can be implemented independently for each reaction zone of a riser reactor (or fluidized bed reactor) of all kinds of FCC; or jointed to implement for each reaction zone of one, two or more riser reactors (or fluidized bed reactor) including tar risers and gasoline risers of the dual risers FCC units or different feeds riser reactors. 10. The method and its equipment of claim 1, wherein the described catalyst in the catalyst cooler is the regenerated catalyst with any carbon content or the regenerated catalyst without completed regeneration or the contact agents with any carbon content or coking particles. 11. The method and its equipment of claim 2, wherein the regenerated catalysts coming from regenerator as step (5) described are cooled by the catalyst cooler within 360 to 650° C. | A method for circulating a cooled regenerated catalyst comprises the following steps: a regenerated catalyst derived from a regenerator ( 5 ) is cooled to 200-720° C. by a catalyst cooler ( 8 A), which either directly enters into a riser reactor ( 2 ) without mixing with hot regenerated catalyst, or enters the same after mixing with another portion of uncooled hot regenerated catalyst and thereby obtaining a hybrid regenerated catalyst with its temperature lower than that of the regenerator; a contact reaction between a hydrocarbon raw materials and the catalyst is performed in the riser reactor ( 2 ); the reaction product is introduced into a settling vessel ( 1 ) to separated the catalyst and oil gas; the separated catalyst ready for regeneration is stream-stripped in a stream stripping phase ( 1 A) and enters the regenerator ( 5 ) for regeneration through charring; after cooling, the regenerated catalyst returns to the riser reactor ( 2 ) for recycling.1. A cycling method and its equipment of cold regenerated catalyst, characterized in that, including a FCC process: hydrocarbon materials react with catalyst in the riser reactor (with or without a fluidized bed reactor); the materials enter into a settler for the separation of catalyst from gas and oil; Separated catalyst will be stripped and enter into regenerator to burn for regeneration; The regenerated catalyst will be cold or/and not be cold to return the riser reactor directly for cycling use; The details are as follows:
the regenerator includes one, two, or more catalyst coolers, each connected to the riser reactor (or the fluidized bed reactor) is used to adjust the reaction temperature of the reaction zone, or/and to adjust regenerator temperatures, so as to keep them in the best value; the catalyst coolers connected with the riser reactor (or the fluidized set in the inside or outside of regenerator, or set under its riser reactor; The catalyst entrance of the shell of the described catalyst cooler directly (or through a pipeline) connects with the regenerator dense phase; there are internal components in the cooler for removing heat; there are fluidized media distribution facilities under the cooler; In the downstream, there is a buffer space for mixed buffer catalyst; the upper part is installed or not installed the gas channel to return to diluting phase of the regenerator; There are one, two or more catalyst exits set in the catalyst mixed buffer space in the downstream of the described catalyst cooler; One, two or more exits of catalysts are connected to the transmission channel of cold catalyst used to deliver cold-regenerated catalyst circulation to one, two or more of the riser (reactor or auxiliary riser); Another one, two or more (or not) catalyst exists are connected to the transmission channel of cold catalyst for conveying cold regenerated catalyst return to the regenerator; The described transmission channel of cold catalyst to the riser is set in the outside of the described catalyst cooler's shell, or all (or partly) set in the inside of the described catalyst cooler's shell; The return channel of the cooled catalyst back to the regenerator all set in the outside of the described catalyst cooler's shell, or all (or partly) set in the inside of the described catalyst cooler's shell. The described riser reactor is set one, two or more reaction zones with or without fluidized bed reactor; Before cold regenerated catalyst enters into the riser reactor or fluidized bed reactor, the riser reactor is set (or not set) a pre-lift section, with pre-lift media to send the cold regenerated catalyst to the riser reactor or the fluidized bed reactor; The described pre-lift section can all be set outside of the catalyst cooler shell, or all (or part) set inside. Part of regenerated catalysts coming from regenerator are cooled by catalyst cooler within 200 to 720° C. and enter into the pre-lift or directly into each reaction zone of riser reactor; Or these regenerated catalysts mix or/and with hot regenerated catalyst without cooling to get the regenerated catalyst mixture which temperature is lower than regenerator temperature and then the mixture enter into pre-lift or/and each reaction zone of the riser reactor; Or the cold and the hot regenerated catalysts enter into the pre-lift of riser separately and directly with pre-lift media for increasing the catalysts temperature to reach a proper temperature and then the mixture enter into each reaction zone of riser reactor; Or the regenerated catalyst without cooling by catalyst cooler enter into the pre-lift zone or/and each reaction zone of the riser reactor directly for cycling. 2. The method and its equipment of claim 1, wherein Setting (or not setting) one, two or more assistant risers, the described cold regenerated catalyst through the assistant risers with the pre-lift media are lifted to one, two or more riser reactors or fluidized bed reactor reaction zones as a cold shock agent for cycling. 3. The method and its equipment of claim 1, wherein the regenerated catalysts coming from regenerator as step (5) described are cooled by the catalyst cooler within 360 to 650° C. 4. The method and its equipment of claim 1, wherein the temperature of the described cold regenerated catalyst can be controlled by adjusting the flows of the fluidized media and/or taking-heat media or adjusting other parameters;
or controlled by adjusting the flows of the fluidized media and/or taking-heat media and/or adjusting the flows of cool catalyst returning regenerator or other parameters. 5. The method and its equipment of claim 1, wherein the temperature of the described regenerated catalysts mixture can be controlled by adjusting the ratio of cold and hot regenerated catalyst. 6. The method and its equipment of claim 1, wherein the reaction temperature of the described riser reactor or fluidized bed reactor reaction zones can be controlled by adjusting the ratio of the catalyst and feed, or/and by adjusting the temperature of the described cold regenerated catalyst or the temperature of the described regenerated catalyst mixture, or/and by using multi-point feeding technology, and/or by adding various cold shock agents to the riser reactor. 7. The method and its equipment of claim 1, wherein the described taking-heat medias in the catalyst cooler include water, steam, air and various oils. 8. The method and its equipment of claim 1, wherein the described cycling method and its equipment of the cold regenerated catalyst can be used widely for various FCC including tar catalytic cracking, wax oil catalytic cracking, gasoline catalytic modification for improving quality, or light hydrocarbon catalytic conversion, or for other burning process of gas-solid fluidized reaction including residue pre-processing, ethylene made by methanol, fluidize coking or flexible coking. 9. The method and its equipment of claim 1, wherein the cycling method and its equipment of cold regenerated catalyst can be implemented independently for each reaction zone of a riser reactor (or fluidized bed reactor) of all kinds of FCC; or jointed to implement for each reaction zone of one, two or more riser reactors (or fluidized bed reactor) including tar risers and gasoline risers of the dual risers FCC units or different feeds riser reactors. 10. The method and its equipment of claim 1, wherein the described catalyst in the catalyst cooler is the regenerated catalyst with any carbon content or the regenerated catalyst without completed regeneration or the contact agents with any carbon content or coking particles. 11. The method and its equipment of claim 2, wherein the regenerated catalysts coming from regenerator as step (5) described are cooled by the catalyst cooler within 360 to 650° C. | 1,700 |
3,424 | 14,646,512 | 1,764 | Embodiments of the present disclosure are directed towards coating compositions comprising from 50 to 85 percent of an aqueous dispersion based on a total weight of the coating composition, an abrasion reducing composition, a solvent, a basic water composition, and a crosslinker. | 1. An coating composition comprising:
from 50 to 85 percent of an aqueous dispersion based on a total weight of the coating composition, wherein the aqueous dispersion comprises a melt blending product of (a) a base polymer comprising at least one polyolefin, (b) a polymeric stabilizing agent, and (c) a compatiblizer, wherein the aqueous dispersion has a solid content from 15 weight percent to 70 weight percent based on a total weight of the aqueous dispersion, the solid content comprises from 50 to 85 percent by weight of the base polymer based on a total weight of the solids content, from 10 to 35 percent by weight of the stabilizing agent based on the total weight of the solids content, and from 2 to 15 percent by weight of the compatiblizer based on the total weight of the solids content; an abrasion reducing composition comprising a polyethylene wax that is from 0.01 weight percent to 1.5 weight percent of the coating composition based on the total weight of the coating composition; a solvent, wherein the solvent is from 3 weight percent to 20 weight percent of the coating composition based on the total weight of the coating composition; a basic water composition comprising from 90 to 99.99 percent by weight of the water based on a total weight of the basic water composition and from 0.01 percent to 10 percent by weight of a base based on the total weight of the basic water composition, wherein the basic water composition is from 10 weight percent to 25 weight percent of the coating composition based on the total weight of the coating composition; and a crosslinker, wherein the crosslinker is from 0.01 weight percent to 40 weight percent of the coating composition based on the total weight of the coating composition. 2.-6. (canceled) 7. The coating composition of claim 1, wherein the polyethylene wax has a melting point of less than 129° C. as measured according to ASTM-D-127. 8. The coating composition of claim 1, wherein the at least one polyolefin comprises polypropylene. 9. The coating composition of claim 1, wherein the solvent is selected from the group of ethylene glycol, diethylene glycol monoethyl ether, dipropylene glycol dimethyl ether, propylene glycol methyl ether, ethanol, dipropylene glycol methyl ether, and combinations thereof. 10. The coating composition of claim 1, wherein the crosslinker is a hydroxyalkyl amide. 11. The coating composition of claim 1, wherein the stabilizing agent is selected from the group of ethylene-acrylic acid copolymer, ethylene-methacrylic acid copolymer, and combinations thereof. 12. The coating composition of claim 1, wherein the compatiblizer comprises a maleic anhydride grafted polypropylene polymer. 13. A coated article comprising a substrate and a coating on the substrate, wherein the coating includes the coating composition of claim 1. 14. The coated article of claim 13, wherein the substrate is a metal substrate. 15. A coated article comprising a substrate and a cured coating on the substrate, wherein the cured coating is formed by curing the coating composition of claim 1. | Embodiments of the present disclosure are directed towards coating compositions comprising from 50 to 85 percent of an aqueous dispersion based on a total weight of the coating composition, an abrasion reducing composition, a solvent, a basic water composition, and a crosslinker.1. An coating composition comprising:
from 50 to 85 percent of an aqueous dispersion based on a total weight of the coating composition, wherein the aqueous dispersion comprises a melt blending product of (a) a base polymer comprising at least one polyolefin, (b) a polymeric stabilizing agent, and (c) a compatiblizer, wherein the aqueous dispersion has a solid content from 15 weight percent to 70 weight percent based on a total weight of the aqueous dispersion, the solid content comprises from 50 to 85 percent by weight of the base polymer based on a total weight of the solids content, from 10 to 35 percent by weight of the stabilizing agent based on the total weight of the solids content, and from 2 to 15 percent by weight of the compatiblizer based on the total weight of the solids content; an abrasion reducing composition comprising a polyethylene wax that is from 0.01 weight percent to 1.5 weight percent of the coating composition based on the total weight of the coating composition; a solvent, wherein the solvent is from 3 weight percent to 20 weight percent of the coating composition based on the total weight of the coating composition; a basic water composition comprising from 90 to 99.99 percent by weight of the water based on a total weight of the basic water composition and from 0.01 percent to 10 percent by weight of a base based on the total weight of the basic water composition, wherein the basic water composition is from 10 weight percent to 25 weight percent of the coating composition based on the total weight of the coating composition; and a crosslinker, wherein the crosslinker is from 0.01 weight percent to 40 weight percent of the coating composition based on the total weight of the coating composition. 2.-6. (canceled) 7. The coating composition of claim 1, wherein the polyethylene wax has a melting point of less than 129° C. as measured according to ASTM-D-127. 8. The coating composition of claim 1, wherein the at least one polyolefin comprises polypropylene. 9. The coating composition of claim 1, wherein the solvent is selected from the group of ethylene glycol, diethylene glycol monoethyl ether, dipropylene glycol dimethyl ether, propylene glycol methyl ether, ethanol, dipropylene glycol methyl ether, and combinations thereof. 10. The coating composition of claim 1, wherein the crosslinker is a hydroxyalkyl amide. 11. The coating composition of claim 1, wherein the stabilizing agent is selected from the group of ethylene-acrylic acid copolymer, ethylene-methacrylic acid copolymer, and combinations thereof. 12. The coating composition of claim 1, wherein the compatiblizer comprises a maleic anhydride grafted polypropylene polymer. 13. A coated article comprising a substrate and a coating on the substrate, wherein the coating includes the coating composition of claim 1. 14. The coated article of claim 13, wherein the substrate is a metal substrate. 15. A coated article comprising a substrate and a cured coating on the substrate, wherein the cured coating is formed by curing the coating composition of claim 1. | 1,700 |
3,425 | 15,232,362 | 1,712 | Reflective luminescent markings on a road or sign surface are formed by applying onto the surface a base material which is liquid in an initial state for application and sets or cures to form a solid layer after application where the base material contains a fine/medium filler material of glass ground from recycled materials in a rotary mill. Coarse material from the grinder is separated out and supplied as a separate material to be applied onto the surface of the layer of base material and fine ground glass. The base material is connected or impregnated with a luminescent material such as photo luminescent 2 4 6 trichlorophenyl in a binder such as polyurea. | 1. A luminescent material comprising:
a base material comprising ground glass particles; wherein the particles are impregnated or coated with a material comprising a luminescent material and a binder. 2. The material according to claim 1 wherein the luminescent material is photo luminescent 2 4 6 trichlorophenyl. 3. The material according to claim 1 wherein the binder is polyurea. 4. The material according to claim 1 wherein the particles are colorless. 5. A method for manufacturing a material according to claim 1 comprising:
grinding glass material to form the ground glass and coating or impregnating the ground glass particles with the material in a process subsequent to said grinding. 6. The method according to claim 5 wherein the ground glass particles are impregnated with said material in a process including heating the ground glass particles to a temperature less than a melting temperature. 7. The method according to claim 5 wherein the ground glass includes a mixture of particles of different size. 8. The method according to claim 5 wherein the glass is ground from recycled glass material. 9. The method according to claim 1 wherein the glass is ground to provide finer particles and coarser particles and wherein the glass is ground in a rotary mill where the coarser particles are collected at a bottom of a discharge chamber and at least some of the finer particles are collected in an air stream at a top of the discharge chamber. 10. The method according to claim 9 wherein the particles collected from the bottom of the discharge material are separated into a medium grind, a coarse grind and a return for return to the rotary mill. 11. The method according to claim 9 wherein the material is impregnated or coated onto particles collected from the bottom of the discharge material. 12. A method for providing reflective luminescent markings on a surface comprising:
applying onto the surface a base material which is liquid in an initial state for application and sets or cures to form a solid layer after application; wherein the base material comprises a material according to claim 1. 13. The method according to claim 12 wherein at least part of the ground glass is mixed through the base material. 14. The method according to claim 12 wherein at least part of the ground glass is applied to the surface simultaneously with the base material. 15. The method according to claim 12 wherein the markings are applied to a road way. 16. The method according to claim 12 wherein the base material and the glass filler both are transparent or colorless to show through an underlying marking material over which the base material is applied. 17. The method according to claim 12 wherein the base material and the glass filler contain no pigment. 18. The method according to claim 12 wherein the base material includes a UN resistant material to prevent fading of an underlying marking. 19. The method according to claim 12 wherein the marking material is a layer plastics layer cut to form the markings and adhesively attached to the substrate. 20. The method according to claim 12 wherein the surface is mounted on a mast for presenting the substrate to passing viewers. | Reflective luminescent markings on a road or sign surface are formed by applying onto the surface a base material which is liquid in an initial state for application and sets or cures to form a solid layer after application where the base material contains a fine/medium filler material of glass ground from recycled materials in a rotary mill. Coarse material from the grinder is separated out and supplied as a separate material to be applied onto the surface of the layer of base material and fine ground glass. The base material is connected or impregnated with a luminescent material such as photo luminescent 2 4 6 trichlorophenyl in a binder such as polyurea.1. A luminescent material comprising:
a base material comprising ground glass particles; wherein the particles are impregnated or coated with a material comprising a luminescent material and a binder. 2. The material according to claim 1 wherein the luminescent material is photo luminescent 2 4 6 trichlorophenyl. 3. The material according to claim 1 wherein the binder is polyurea. 4. The material according to claim 1 wherein the particles are colorless. 5. A method for manufacturing a material according to claim 1 comprising:
grinding glass material to form the ground glass and coating or impregnating the ground glass particles with the material in a process subsequent to said grinding. 6. The method according to claim 5 wherein the ground glass particles are impregnated with said material in a process including heating the ground glass particles to a temperature less than a melting temperature. 7. The method according to claim 5 wherein the ground glass includes a mixture of particles of different size. 8. The method according to claim 5 wherein the glass is ground from recycled glass material. 9. The method according to claim 1 wherein the glass is ground to provide finer particles and coarser particles and wherein the glass is ground in a rotary mill where the coarser particles are collected at a bottom of a discharge chamber and at least some of the finer particles are collected in an air stream at a top of the discharge chamber. 10. The method according to claim 9 wherein the particles collected from the bottom of the discharge material are separated into a medium grind, a coarse grind and a return for return to the rotary mill. 11. The method according to claim 9 wherein the material is impregnated or coated onto particles collected from the bottom of the discharge material. 12. A method for providing reflective luminescent markings on a surface comprising:
applying onto the surface a base material which is liquid in an initial state for application and sets or cures to form a solid layer after application; wherein the base material comprises a material according to claim 1. 13. The method according to claim 12 wherein at least part of the ground glass is mixed through the base material. 14. The method according to claim 12 wherein at least part of the ground glass is applied to the surface simultaneously with the base material. 15. The method according to claim 12 wherein the markings are applied to a road way. 16. The method according to claim 12 wherein the base material and the glass filler both are transparent or colorless to show through an underlying marking material over which the base material is applied. 17. The method according to claim 12 wherein the base material and the glass filler contain no pigment. 18. The method according to claim 12 wherein the base material includes a UN resistant material to prevent fading of an underlying marking. 19. The method according to claim 12 wherein the marking material is a layer plastics layer cut to form the markings and adhesively attached to the substrate. 20. The method according to claim 12 wherein the surface is mounted on a mast for presenting the substrate to passing viewers. | 1,700 |
3,426 | 14,521,709 | 1,787 | The present invention provides a resin composition having a suitable melting temperature for molding, a resin sheet containing the resin composition, a cured resin product excellent in thermal conductivity and heat resistance, and a substrate. They are prepared in the way that in the resin composition containing epoxy compounds and curing agent selected from 1,3,5-tris(4-aminophenyl)benzene and 1,3,5-tris(4-hydroxyphenyl)benzene, the content of 1,3,5-triphenylbenzene that is the main skeleton of the curing agent is 15 mass % or more and 50 mass % or less of the total organic substances in the resin composition. | 1. A resin composition comprising epoxy compounds and a curing agent selected from 1,3,5-tris(4-aminophenyl)benzene and 1,3,5-tris(4-hydroxyphenyl)benzene,
wherein, the content of 1,3,5-triphenylbenzene which is the main skeleton of said curing agent, is 15 mass % or more and 50 mass % or less of the total organic substances in said resin composition. 2. A resin sheet comprising the resin composition according to claim 1. 3. A cured resin product obtained by curing the resin composition according to claim 1. 4. A substrate obtained by laminating, molding and curing one or several resin sheets according to claim 2. | The present invention provides a resin composition having a suitable melting temperature for molding, a resin sheet containing the resin composition, a cured resin product excellent in thermal conductivity and heat resistance, and a substrate. They are prepared in the way that in the resin composition containing epoxy compounds and curing agent selected from 1,3,5-tris(4-aminophenyl)benzene and 1,3,5-tris(4-hydroxyphenyl)benzene, the content of 1,3,5-triphenylbenzene that is the main skeleton of the curing agent is 15 mass % or more and 50 mass % or less of the total organic substances in the resin composition.1. A resin composition comprising epoxy compounds and a curing agent selected from 1,3,5-tris(4-aminophenyl)benzene and 1,3,5-tris(4-hydroxyphenyl)benzene,
wherein, the content of 1,3,5-triphenylbenzene which is the main skeleton of said curing agent, is 15 mass % or more and 50 mass % or less of the total organic substances in said resin composition. 2. A resin sheet comprising the resin composition according to claim 1. 3. A cured resin product obtained by curing the resin composition according to claim 1. 4. A substrate obtained by laminating, molding and curing one or several resin sheets according to claim 2. | 1,700 |
3,427 | 14,819,465 | 1,761 | A water-soluble laundry unit dose article comprising a liquid composition, wherein said composition comprises;
an anionic surfactant; an ethoxylated alcohol non-ionic surfactant; water; wherein the weight ratio of total anionic: non-ionic is between 5:1 and 23:1; and wherein the composition comprises between 0.1 wt % and 5 wt % of a perfume and between 0.1 wt % and 5 wt % of an encapsulated perfume. | 1. A water-soluble laundry unit dose article comprising a liquid composition, wherein said composition comprises;
an anionic surfactant; a non-ionic surfactant; water; wherein the weight ratio of total anionic: non-ionic is between about 5:1 and about 23:1; and wherein the composition comprises between about 0.1 wt % and about 5 wt % of a perfume and between about 0.1 wt % and about 5 wt % of an encapsulated perfume. 2. A unit dose article according to claim 1, wherein the anionic surfactant comprises linear alkylbenzene sulphonate. 3. A unit dose article according to claim 1, wherein the weight ratio of anionic to non-ionic surfactant is from about 5:1 to about 20:1. 4. A unit dose article according to claim 1, wherein the weight ratio of anionic to non-ionic surfactant is from about 5:1 to about 15:1. 5. A unit dose article according to claim 1, wherein the non-ionic surfactant comprises a fatty alcohol ethoxylate of formula R(EO)n, wherein R represents an alkyl chain between about 4 and about 30 carbon atoms, (EO) represents one unit of ethylene oxide monomer and n has an average value between about 0.5 and about 20. 6. A unit dose article according to claim 1 wherein the anionic surfactant comprises fatty acid. 7. A unit dose article according to claim 1 comprising an cationic hydroxyethyl cellulose polymer, preferably a cationic hydroxyethyl cellulose polymer derivatised with trimethyl ammonium substituted epoxide. 8. A unit dose article according to claim 1, wherein the cationic polymer has a molecular weight of between about 100,000 and about 800,000 daltons. 9. A unit dose article according to claim 7 wherein the polymer is present at a level of between about 0.05% and about 2%, by weight of the composition. 10. A unit dose article according to claim 7 wherein the polymer is present at a level of between about 0.6% and about 1% by weight of the of composition. 11. A unit dose article according to claim 1 wherein the encapsulated perfume comprises a core material and a wall material that at least partially surrounds said core, wherein said core comprises the perfume. 12. A unit dose article according to claim 1 wherein the ratio of total surfactant to water is between about 3:1 to about 20:1. 13. A unit dose article according to claim 1 comprising between about 0.5 wt % and about 25 wt % water. 14. A unit dose article according to claim 1 comprising an adjunct laundry detergent ingredient, wherein the adjunct laundry detergent ingredient is selected from bleach, bleach catalyst, dye, hueing agents, cleaning polymers, alkoxylated polyamines, polyethyleneimines, alkoxylated polyethyleneimines, soil release polymers, amphiphilic graft polymers, surfactants, solvents, dye transfer inhibitors, chelants, enzymes, perfumes, encapsulated perfumes, perfume delivery agents, suds suppressor, brighteners, polycarboxylates, structurants, anti-oxidants, deposition aids and mixtures thereof. 15. A unit dose article according to claim 1 comprising at least two compartments. 16. A unit dose article according to claim 1 comprising at least three compartments. 17. The unit dose article according to claim 12 where the compartments are arranged in a superposed orientation or in a side-by-side orientation. | A water-soluble laundry unit dose article comprising a liquid composition, wherein said composition comprises;
an anionic surfactant; an ethoxylated alcohol non-ionic surfactant; water; wherein the weight ratio of total anionic: non-ionic is between 5:1 and 23:1; and wherein the composition comprises between 0.1 wt % and 5 wt % of a perfume and between 0.1 wt % and 5 wt % of an encapsulated perfume.1. A water-soluble laundry unit dose article comprising a liquid composition, wherein said composition comprises;
an anionic surfactant; a non-ionic surfactant; water; wherein the weight ratio of total anionic: non-ionic is between about 5:1 and about 23:1; and wherein the composition comprises between about 0.1 wt % and about 5 wt % of a perfume and between about 0.1 wt % and about 5 wt % of an encapsulated perfume. 2. A unit dose article according to claim 1, wherein the anionic surfactant comprises linear alkylbenzene sulphonate. 3. A unit dose article according to claim 1, wherein the weight ratio of anionic to non-ionic surfactant is from about 5:1 to about 20:1. 4. A unit dose article according to claim 1, wherein the weight ratio of anionic to non-ionic surfactant is from about 5:1 to about 15:1. 5. A unit dose article according to claim 1, wherein the non-ionic surfactant comprises a fatty alcohol ethoxylate of formula R(EO)n, wherein R represents an alkyl chain between about 4 and about 30 carbon atoms, (EO) represents one unit of ethylene oxide monomer and n has an average value between about 0.5 and about 20. 6. A unit dose article according to claim 1 wherein the anionic surfactant comprises fatty acid. 7. A unit dose article according to claim 1 comprising an cationic hydroxyethyl cellulose polymer, preferably a cationic hydroxyethyl cellulose polymer derivatised with trimethyl ammonium substituted epoxide. 8. A unit dose article according to claim 1, wherein the cationic polymer has a molecular weight of between about 100,000 and about 800,000 daltons. 9. A unit dose article according to claim 7 wherein the polymer is present at a level of between about 0.05% and about 2%, by weight of the composition. 10. A unit dose article according to claim 7 wherein the polymer is present at a level of between about 0.6% and about 1% by weight of the of composition. 11. A unit dose article according to claim 1 wherein the encapsulated perfume comprises a core material and a wall material that at least partially surrounds said core, wherein said core comprises the perfume. 12. A unit dose article according to claim 1 wherein the ratio of total surfactant to water is between about 3:1 to about 20:1. 13. A unit dose article according to claim 1 comprising between about 0.5 wt % and about 25 wt % water. 14. A unit dose article according to claim 1 comprising an adjunct laundry detergent ingredient, wherein the adjunct laundry detergent ingredient is selected from bleach, bleach catalyst, dye, hueing agents, cleaning polymers, alkoxylated polyamines, polyethyleneimines, alkoxylated polyethyleneimines, soil release polymers, amphiphilic graft polymers, surfactants, solvents, dye transfer inhibitors, chelants, enzymes, perfumes, encapsulated perfumes, perfume delivery agents, suds suppressor, brighteners, polycarboxylates, structurants, anti-oxidants, deposition aids and mixtures thereof. 15. A unit dose article according to claim 1 comprising at least two compartments. 16. A unit dose article according to claim 1 comprising at least three compartments. 17. The unit dose article according to claim 12 where the compartments are arranged in a superposed orientation or in a side-by-side orientation. | 1,700 |
3,428 | 14,330,547 | 1,784 | In one aspect, composite articles are described comprising multifunctional coatings. A composite article described herein, in some embodiments, comprises a substrate and a coating adhered to the substrate, the coating comprising an inner layer and an outer layer, the inner layer comprising a presintered metal or alloy and the outer layer comprising particles disposed in a metal or alloy matrix. | 1. A composite article comprising:
a substrate; and a coating adhered to the substrate, the coating comprising an inner layer and an outer layer, the inner layer being substantially fully dense and comprising sintered metal or alloy, and the outer layer comprising hard particles disposed in matrix metal or matrix alloy, wherein the matrix metal or matrix alloy does not infiltrate the inner layer. 2. The composite article of claim 1, wherein the inner layer is metallurgically bonded to the substrate. 3. The composite article of claim 1, wherein the hard particles of the outer layer comprise one or more metal carbides, metal nitrides, metal borides, metal silicides, ceramics, cemented carbides, cast carbides or mixtures thereof. 4. The composite article of claim 1, wherein the inner layer has hardness on the Rockwell C scale lower than the outer layer. 5. The composite article of claim 4, wherein the outer layer has an abrasion resistance greater than the inner layer as measured according to ASTM G65-04. 6. The composite article of claim 1, wherein the outer layer further comprises metal carbide tiles or ceramic tiles disposed in the matrix metal or matrix alloy. 7. The composite article of claim 1, wherein the inner layer further comprises particles disposed in the sintered metal or alloy, the particles selected from the group consisting of metal carbides, metal nitrides, metal borides, metal silicides, ceramics, cemented carbides, cast carbides and mixtures thereof. 8. The composite article of claim 1, wherein the coating further comprises at least one layer of refractory material deposited over the outer layer by chemical vapor deposition or physical vapor deposition of a combination thereof. 9. The composite article of claim 1, wherein the inner layer of the coating has corrosion resistant and crack arrest functionalities, and the outer layer of the coating has an abrasion resistant functionality, erosion resistant functionality or combination thereof. 10. The composite article of claim 1, wherein the substrate comprises steel. 11. The composite article of claim 1, further comprising an interfacial transition region between the inner layer and the outer layer. 12. The composite article of claim 1, wherein the inner layer comprises sintered nickel-based alloy. 13. The composite article of claim 12, wherein the nickel-based alloy is of composition 0-15 wt. % cobalt, 1-30 wt. % chromium, 2-28 wt. % molybdenum, 0-5 wt. % tungsten, 0-50 wt. % iron, 0-6 wt. % niobium, 0-1 wt. % silicon, 0-2 wt. % manganese, 0-3 wt. % copper, 0-1 wt. % aluminum, 0-2 wt. % titanium and the balance nickel. 14. A composite article comprising:
a substrate; and a coating adhered to the substrate, the coating comprising an inner layer and an outer layer, the outer layer comprising hard particles disposed in matrix metal or matrix alloy, and the inner layer being substantially fully dense and formed of a porous sintered metal or sintered alloy scaffold infiltrated with the matrix metal or matrix alloy of the outer layer. 15. The composite article of claim 14, wherein the inner layer is metallurgically bonded to the substrate. 16. The composite article of claim 14, wherein the particles of the outer layer comprise one or more metal carbides, metal nitrides, metal borides, metal silicides, ceramics, cemented carbides, cast carbides or mixtures thereof. 17. The composite article of claim 14, wherein the inner layer has hardness on the Rockwell C scale lower than the outer layer. 18. The composite article of claim 17, wherein the outer layer has an abrasion resistance greater than the inner layer as measured according to ASTM G65-04. 19. The composite article of claim 14, wherein the substrate comprises steel. 20. The composite article of claim 14, wherein the inner layer of the coating has corrosion resistant and crack arrest functionalities, and the outer layer of the coating has an abrasion resistant functionality, erosion resistant functionality or combination thereof. | In one aspect, composite articles are described comprising multifunctional coatings. A composite article described herein, in some embodiments, comprises a substrate and a coating adhered to the substrate, the coating comprising an inner layer and an outer layer, the inner layer comprising a presintered metal or alloy and the outer layer comprising particles disposed in a metal or alloy matrix.1. A composite article comprising:
a substrate; and a coating adhered to the substrate, the coating comprising an inner layer and an outer layer, the inner layer being substantially fully dense and comprising sintered metal or alloy, and the outer layer comprising hard particles disposed in matrix metal or matrix alloy, wherein the matrix metal or matrix alloy does not infiltrate the inner layer. 2. The composite article of claim 1, wherein the inner layer is metallurgically bonded to the substrate. 3. The composite article of claim 1, wherein the hard particles of the outer layer comprise one or more metal carbides, metal nitrides, metal borides, metal silicides, ceramics, cemented carbides, cast carbides or mixtures thereof. 4. The composite article of claim 1, wherein the inner layer has hardness on the Rockwell C scale lower than the outer layer. 5. The composite article of claim 4, wherein the outer layer has an abrasion resistance greater than the inner layer as measured according to ASTM G65-04. 6. The composite article of claim 1, wherein the outer layer further comprises metal carbide tiles or ceramic tiles disposed in the matrix metal or matrix alloy. 7. The composite article of claim 1, wherein the inner layer further comprises particles disposed in the sintered metal or alloy, the particles selected from the group consisting of metal carbides, metal nitrides, metal borides, metal silicides, ceramics, cemented carbides, cast carbides and mixtures thereof. 8. The composite article of claim 1, wherein the coating further comprises at least one layer of refractory material deposited over the outer layer by chemical vapor deposition or physical vapor deposition of a combination thereof. 9. The composite article of claim 1, wherein the inner layer of the coating has corrosion resistant and crack arrest functionalities, and the outer layer of the coating has an abrasion resistant functionality, erosion resistant functionality or combination thereof. 10. The composite article of claim 1, wherein the substrate comprises steel. 11. The composite article of claim 1, further comprising an interfacial transition region between the inner layer and the outer layer. 12. The composite article of claim 1, wherein the inner layer comprises sintered nickel-based alloy. 13. The composite article of claim 12, wherein the nickel-based alloy is of composition 0-15 wt. % cobalt, 1-30 wt. % chromium, 2-28 wt. % molybdenum, 0-5 wt. % tungsten, 0-50 wt. % iron, 0-6 wt. % niobium, 0-1 wt. % silicon, 0-2 wt. % manganese, 0-3 wt. % copper, 0-1 wt. % aluminum, 0-2 wt. % titanium and the balance nickel. 14. A composite article comprising:
a substrate; and a coating adhered to the substrate, the coating comprising an inner layer and an outer layer, the outer layer comprising hard particles disposed in matrix metal or matrix alloy, and the inner layer being substantially fully dense and formed of a porous sintered metal or sintered alloy scaffold infiltrated with the matrix metal or matrix alloy of the outer layer. 15. The composite article of claim 14, wherein the inner layer is metallurgically bonded to the substrate. 16. The composite article of claim 14, wherein the particles of the outer layer comprise one or more metal carbides, metal nitrides, metal borides, metal silicides, ceramics, cemented carbides, cast carbides or mixtures thereof. 17. The composite article of claim 14, wherein the inner layer has hardness on the Rockwell C scale lower than the outer layer. 18. The composite article of claim 17, wherein the outer layer has an abrasion resistance greater than the inner layer as measured according to ASTM G65-04. 19. The composite article of claim 14, wherein the substrate comprises steel. 20. The composite article of claim 14, wherein the inner layer of the coating has corrosion resistant and crack arrest functionalities, and the outer layer of the coating has an abrasion resistant functionality, erosion resistant functionality or combination thereof. | 1,700 |
3,429 | 14,649,551 | 1,784 | Provided is a multilayer thin film for a cutting tool, in which micro-scale thin films having a thickness of a few nanometers to tens of nanometers are alternately stacked, having less quality variations and being capable of realizing excellent wear resistance. The multilayer thin film according to the present disclosure is a multilayer thin film for a cutting tool, in which unit thin films which are respectively formed of thin layers A, B, C, and D are stacked more than once, wherein elastic moduluses k of the thin layers satisfy relationships of k A >k B , k D >k C or k C >k B , k D >k A , lattice parameters L of the thin layers satisfy relationships of L A , L C >L B , L D or L B , L D >L A , L C , and a difference between maximum and minimum values of the lattice parameter L is 20% or less. | 1. A multilayer thin film for a cutting tool, in which unit thin films which are respectively formed of thin layers A, B, C, and D are stacked more than once, wherein elastic moduluses k of the thin layers satisfy relationships of kA>kB, kD>kC or kC>kB, kD>kA,
lattice parameters L of the thin layers satisfy relationships of LA, LC>LB, LD or LB, LD>LA, LC, and a difference between maximum and minimum values of the lattice parameter L is 20% or less. 2. The multilayer thin film of claim 1, wherein an average lattice parameter period λL of the multilayer thin film is one half of an average elastic modulus period λk thereof. 3. The multilayer thin film of claim 1, wherein the unit thin film has a thickness of 4 to 50 nm. 4. The multilayer thin film of claim 1, wherein the thin layers B and D are formed of the same material. 5. A cutting tool coated with the multilayer thin film of claim 1. 6. The multilayer thin film of claim 2, wherein the unit thin film has a thickness of 4 to 50 nm. 7. The multilayer thin film of claim 2, wherein the thin layers B and D are formed of the same material. 8. A cutting tool coated with the multilayer thin film of claim 2. | Provided is a multilayer thin film for a cutting tool, in which micro-scale thin films having a thickness of a few nanometers to tens of nanometers are alternately stacked, having less quality variations and being capable of realizing excellent wear resistance. The multilayer thin film according to the present disclosure is a multilayer thin film for a cutting tool, in which unit thin films which are respectively formed of thin layers A, B, C, and D are stacked more than once, wherein elastic moduluses k of the thin layers satisfy relationships of k A >k B , k D >k C or k C >k B , k D >k A , lattice parameters L of the thin layers satisfy relationships of L A , L C >L B , L D or L B , L D >L A , L C , and a difference between maximum and minimum values of the lattice parameter L is 20% or less.1. A multilayer thin film for a cutting tool, in which unit thin films which are respectively formed of thin layers A, B, C, and D are stacked more than once, wherein elastic moduluses k of the thin layers satisfy relationships of kA>kB, kD>kC or kC>kB, kD>kA,
lattice parameters L of the thin layers satisfy relationships of LA, LC>LB, LD or LB, LD>LA, LC, and a difference between maximum and minimum values of the lattice parameter L is 20% or less. 2. The multilayer thin film of claim 1, wherein an average lattice parameter period λL of the multilayer thin film is one half of an average elastic modulus period λk thereof. 3. The multilayer thin film of claim 1, wherein the unit thin film has a thickness of 4 to 50 nm. 4. The multilayer thin film of claim 1, wherein the thin layers B and D are formed of the same material. 5. A cutting tool coated with the multilayer thin film of claim 1. 6. The multilayer thin film of claim 2, wherein the unit thin film has a thickness of 4 to 50 nm. 7. The multilayer thin film of claim 2, wherein the thin layers B and D are formed of the same material. 8. A cutting tool coated with the multilayer thin film of claim 2. | 1,700 |
3,430 | 13,408,810 | 1,716 | Embodiments of the present disclosure generally relate to vacuum processing chambers having different pumping requirements and connected to a shared pumping system through a single foreline. In one embodiment, the vacuum processing chambers include a high conductance pumping conduit and a low conductance pumping conduit coupled to a single high conductance foreline. In another embodiment, a plurality of unbalanced chamber groups may be connected to a common pumping system by a final foreline. | 1. A system for processing substrates, comprising:
a chamber body having a first substrate transfer chamber isolated from a second substrate transfer chamber; a vacuum pump; a high conductance foreline coupled to the pump; a high conductance pumping conduit coupling the foreline to the first substrate transfer chamber; and a low conductance pumping conduit coupling the foreline to the second substrate transfer chamber. 2. The system of claim 1, further comprising: a second vacuum pump coupled to the high conductance foreline. 3. The system of claim 1, wherein each substrate transfer chamber has two substrate transfer ports. 4. The system of claim 1, further comprising: a showerhead disposed within the first substrate transfer chamber. 5. The system of claim 1, further comprising:
a substrate support disposed within the first substrate transfer chamber; and a heater configured to heat the substrate support. 6. The system of claim 1, wherein the first substrate transfer chamber is coupled to a remote plasma source. 7. A system for processing substrates, comprising:
a chamber body having a first substrate transfer chamber and a second substrate transfer chamber formed therein, wherein the first substrate transfer chamber is isolated from the second substrate transfer chamber; a vacuum pump; a high conductance foreline coupled to the pump; a high conductance pumping conduit coupling the foreline to the first substrate transfer chamber; and a low conductance pumping conduit coupling the foreline to the second substrate transfer chamber. 8. The system of claim 7, wherein each substrate transfer chamber has two substrate transfer ports. 9. The system of claim 7, further comprising: a showerhead disposed within the first substrate transfer chamber. 10. The system of claim 7, further comprising:
a substrate support disposed within the first substrate transfer chamber; and a heater configured to heat the substrate support. 11. The system of claim 7, further comprising: a second vacuum pump coupled to the high conductance foreline. 12. The system of claim 7, wherein the first substrate transfer chamber is coupled to a remote plasma source. 13. A system for processing substrates, comprising:
a first chamber body having a first substrate transfer chamber isolated from a second first substrate transfer chamber; a second chamber body having a third substrate transfer chamber isolated from a fourth first substrate transfer chamber; a vacuum pump; a high conductance common exhaust coupled to the pump; a high conductance common exhaust coupled to the high conductance foreline; a first high conductance pumping conduit coupling the high conductance common exhaust to the first substrate transfer chamber; a second high conductance pumping conduit coupling the high conductance common exhaust to the third substrate transfer chamber; a low conductance common exhaust coupled to the high conductance foreline; a first low conductance pumping conduit coupling the low conductance common exhaust to the second substrate transfer chamber; and a second low conductance pumping conduit coupling the low conductance common exhaust to the fourth substrate transfer chamber. 14. The system of claim 13, wherein first and second high conductance pumping conduits have equal conductance. 15. The system of claim 13, wherein first and second high conductance pumping conduits are arranged in a mirror image. 16. The system of claim 13, wherein first substrate transfer chamber is a plasma processing chamber and the second substrate transfer chamber is a load lock chamber. 17. The system of claim 13, further comprising a second pump coupled to the high conductance foreline. 18. The system of claim 13, wherein the high conductance pumping conduits are coupled to the high conductance foreline by a bellows. 19. The system of claim 13, wherein each substrate transfer chamber has two substrate transfer ports. 20. The system of claim 14, wherein the first substrate transfer chamber has a substrate support heater and is coupled to a remote plasma source. | Embodiments of the present disclosure generally relate to vacuum processing chambers having different pumping requirements and connected to a shared pumping system through a single foreline. In one embodiment, the vacuum processing chambers include a high conductance pumping conduit and a low conductance pumping conduit coupled to a single high conductance foreline. In another embodiment, a plurality of unbalanced chamber groups may be connected to a common pumping system by a final foreline.1. A system for processing substrates, comprising:
a chamber body having a first substrate transfer chamber isolated from a second substrate transfer chamber; a vacuum pump; a high conductance foreline coupled to the pump; a high conductance pumping conduit coupling the foreline to the first substrate transfer chamber; and a low conductance pumping conduit coupling the foreline to the second substrate transfer chamber. 2. The system of claim 1, further comprising: a second vacuum pump coupled to the high conductance foreline. 3. The system of claim 1, wherein each substrate transfer chamber has two substrate transfer ports. 4. The system of claim 1, further comprising: a showerhead disposed within the first substrate transfer chamber. 5. The system of claim 1, further comprising:
a substrate support disposed within the first substrate transfer chamber; and a heater configured to heat the substrate support. 6. The system of claim 1, wherein the first substrate transfer chamber is coupled to a remote plasma source. 7. A system for processing substrates, comprising:
a chamber body having a first substrate transfer chamber and a second substrate transfer chamber formed therein, wherein the first substrate transfer chamber is isolated from the second substrate transfer chamber; a vacuum pump; a high conductance foreline coupled to the pump; a high conductance pumping conduit coupling the foreline to the first substrate transfer chamber; and a low conductance pumping conduit coupling the foreline to the second substrate transfer chamber. 8. The system of claim 7, wherein each substrate transfer chamber has two substrate transfer ports. 9. The system of claim 7, further comprising: a showerhead disposed within the first substrate transfer chamber. 10. The system of claim 7, further comprising:
a substrate support disposed within the first substrate transfer chamber; and a heater configured to heat the substrate support. 11. The system of claim 7, further comprising: a second vacuum pump coupled to the high conductance foreline. 12. The system of claim 7, wherein the first substrate transfer chamber is coupled to a remote plasma source. 13. A system for processing substrates, comprising:
a first chamber body having a first substrate transfer chamber isolated from a second first substrate transfer chamber; a second chamber body having a third substrate transfer chamber isolated from a fourth first substrate transfer chamber; a vacuum pump; a high conductance common exhaust coupled to the pump; a high conductance common exhaust coupled to the high conductance foreline; a first high conductance pumping conduit coupling the high conductance common exhaust to the first substrate transfer chamber; a second high conductance pumping conduit coupling the high conductance common exhaust to the third substrate transfer chamber; a low conductance common exhaust coupled to the high conductance foreline; a first low conductance pumping conduit coupling the low conductance common exhaust to the second substrate transfer chamber; and a second low conductance pumping conduit coupling the low conductance common exhaust to the fourth substrate transfer chamber. 14. The system of claim 13, wherein first and second high conductance pumping conduits have equal conductance. 15. The system of claim 13, wherein first and second high conductance pumping conduits are arranged in a mirror image. 16. The system of claim 13, wherein first substrate transfer chamber is a plasma processing chamber and the second substrate transfer chamber is a load lock chamber. 17. The system of claim 13, further comprising a second pump coupled to the high conductance foreline. 18. The system of claim 13, wherein the high conductance pumping conduits are coupled to the high conductance foreline by a bellows. 19. The system of claim 13, wherein each substrate transfer chamber has two substrate transfer ports. 20. The system of claim 14, wherein the first substrate transfer chamber has a substrate support heater and is coupled to a remote plasma source. | 1,700 |
3,431 | 14,377,952 | 1,792 | Provided are a production method for an edible fermented dairy product using, as a raw material, sterile full fat soy flour, which has a very high nutritional value and has a markedly improved taste evaluation that includes flavor and smooth texture, and a fermented dairy product produced by the method. A production method for a fermented dairy product includes the steps of: producing sterile full fat soy flour having a grain size of from 100 to 1,000 meshes by pulverizing sterile dehulled soybeans prepared so as to have a bacterial count of 300 cells/g or less by using a method of separating whole soybeans into cotyledons, germs, and hulls; adding water to the sterile full fat soy flour to prepare a powdered soy juice, followed by sterilizing the powdered soy juice by heating; homogenizing the powdered soy juice to prepare a homogenized powdered soy juice; and adding a lactic acid bacterium to the homogenized powdered soy juice, followed by fermentation to prepare fermented milk. | 1. A production method for a fermented dairy product using sterile full fat soy flour as a raw material, comprising the steps of:
producing sterile full fat soy flour having a grain size of from 100 to 1,000 meshes by pulverizing sterile dehulled soybeans prepared so as to have a bacterial count of 300 cells/g or less by using a method of separating whole soybeans into cotyledons, germs, and hulls; adding water to the sterile full fat soy flour to prepare a powdered soy juice, followed by sterilizing the powdered soy juice by heating; homogenizing the powdered soy juice to prepare a homogenized powdered soy juice; and adding a lactic acid bacterium to the homogenized powdered soy juice, followed by fermentation to prepare fermented milk. 2. A production method for a fermented dairy product according to claim 1, wherein the step of homogenizing the powdered soy juice is conducted after the step of sterilizing the powdered soy juice by heating or during the step of sterilizing the powdered soy juice by heating. 3. A production method for a fermented dairy product according to claim 1, wherein the lactic acid bacterium comprises a lactic acid bacterium that grows actively in steamed soybean soup or soy milk. 4. A production method for a fermented dairy product according to claim 3, wherein the lactic acid bacterium comprises a plant origin lactic acid bacterium or a dairy lactic acid bacterium. 5. A production method for a fermented dairy product according to claim 1, wherein a starter medium for the lactic acid bacterium comprises the homogenized powdered soy juice. 6. A production method for a fermented dairy product according to claim 4, wherein the plant origin lactic acid bacterium is a lactic acid bacterium separated from sake yeast mash. 7. A production method for a fermented dairy product according to claim 1, wherein the fermented milk comprises a yogurt. 8. A production method for a fermented dairy product according to claim 1, further comprising the step of removing whey from the fermented milk to produce a cheese. 9. A production method for a fermented dairy product according to claim 1, further comprising the step of adding a sweetener to the fermented milk, followed by sterilizing the milk to produce a sterilized dairy product lactic acid bacteria beverage. 10. A production method for a fermented dairy product according to claim 1, further comprising the step of mixing a stabilizer and sugar in the fermented milk, followed by homogenizing the mixture to produce a lactic acid bacteria beverage. 11. A production method for a fermented dairy product according to claim 1, wherein the fermented dairy product is produced. 12. A production method for a fermented dairy product according to claim 1, wherein a yogurt is produced. 13. A production method for a fermented dairy product according to claim 12, wherein the yogurt has a hardness, determined by hardness measurement using a creep test device, of from 30 gf/cm2 to 200 gf/cm2. 14. A production method for a fermented dairy product according to claim 1, wherein a cheese is produced. 15. A production method for a fermented dairy product according to claim 1, wherein a sterilized dairy product lactic acid bacteria beverage is produced. 16. A production method for a fermented dairy product according to claim 1, wherein a lactic acid bacteria beverage is produced. 17. A method for producing yogurt, comprising:
producing sterile full fat soy flour having a grain size of from 100 to 1,000 meshes by pulverizing sterile dehulled soybeans prepared so as to have a bacterial count of 300 cells/g or less by using a method of separating whole soybeans into cotyledons, germs, and hulls; adding water to the sterile full fat soy flour to prepare a powdered soy juice, followed by sterilizing the powdered soy juice by heating; homogenizing the powdered soy juice to prepare a homogenized powdered soy juice; and adding a lactic acid bacterium to the homogenized powdered soy juice, followed by fermentation to prepare fermented milk. 18. A method for producing cheese, comprising:
producing sterile full fat soy flour having a grain size of from 100 to 1,000 meshes by pulverizing sterile dehulled soybeans prepared so as to have a bacterial count of 300 cells/g or less by using a method of separating whole soybeans into cotyledons, germs, and hulls; adding water to the sterile full fat soy flour to prepare a powdered soy juice, followed by sterilizing the powdered soy juice by heating; homogenizing the powdered soy juice to prepare a homogenized powdered soy juice; and adding a lactic acid bacterium to the homogenized powdered soy juice, followed by fermentation to prepare fermented milk. 19. A method according to claim 18, further comprising:
removing whey from the fermented milk | Provided are a production method for an edible fermented dairy product using, as a raw material, sterile full fat soy flour, which has a very high nutritional value and has a markedly improved taste evaluation that includes flavor and smooth texture, and a fermented dairy product produced by the method. A production method for a fermented dairy product includes the steps of: producing sterile full fat soy flour having a grain size of from 100 to 1,000 meshes by pulverizing sterile dehulled soybeans prepared so as to have a bacterial count of 300 cells/g or less by using a method of separating whole soybeans into cotyledons, germs, and hulls; adding water to the sterile full fat soy flour to prepare a powdered soy juice, followed by sterilizing the powdered soy juice by heating; homogenizing the powdered soy juice to prepare a homogenized powdered soy juice; and adding a lactic acid bacterium to the homogenized powdered soy juice, followed by fermentation to prepare fermented milk.1. A production method for a fermented dairy product using sterile full fat soy flour as a raw material, comprising the steps of:
producing sterile full fat soy flour having a grain size of from 100 to 1,000 meshes by pulverizing sterile dehulled soybeans prepared so as to have a bacterial count of 300 cells/g or less by using a method of separating whole soybeans into cotyledons, germs, and hulls; adding water to the sterile full fat soy flour to prepare a powdered soy juice, followed by sterilizing the powdered soy juice by heating; homogenizing the powdered soy juice to prepare a homogenized powdered soy juice; and adding a lactic acid bacterium to the homogenized powdered soy juice, followed by fermentation to prepare fermented milk. 2. A production method for a fermented dairy product according to claim 1, wherein the step of homogenizing the powdered soy juice is conducted after the step of sterilizing the powdered soy juice by heating or during the step of sterilizing the powdered soy juice by heating. 3. A production method for a fermented dairy product according to claim 1, wherein the lactic acid bacterium comprises a lactic acid bacterium that grows actively in steamed soybean soup or soy milk. 4. A production method for a fermented dairy product according to claim 3, wherein the lactic acid bacterium comprises a plant origin lactic acid bacterium or a dairy lactic acid bacterium. 5. A production method for a fermented dairy product according to claim 1, wherein a starter medium for the lactic acid bacterium comprises the homogenized powdered soy juice. 6. A production method for a fermented dairy product according to claim 4, wherein the plant origin lactic acid bacterium is a lactic acid bacterium separated from sake yeast mash. 7. A production method for a fermented dairy product according to claim 1, wherein the fermented milk comprises a yogurt. 8. A production method for a fermented dairy product according to claim 1, further comprising the step of removing whey from the fermented milk to produce a cheese. 9. A production method for a fermented dairy product according to claim 1, further comprising the step of adding a sweetener to the fermented milk, followed by sterilizing the milk to produce a sterilized dairy product lactic acid bacteria beverage. 10. A production method for a fermented dairy product according to claim 1, further comprising the step of mixing a stabilizer and sugar in the fermented milk, followed by homogenizing the mixture to produce a lactic acid bacteria beverage. 11. A production method for a fermented dairy product according to claim 1, wherein the fermented dairy product is produced. 12. A production method for a fermented dairy product according to claim 1, wherein a yogurt is produced. 13. A production method for a fermented dairy product according to claim 12, wherein the yogurt has a hardness, determined by hardness measurement using a creep test device, of from 30 gf/cm2 to 200 gf/cm2. 14. A production method for a fermented dairy product according to claim 1, wherein a cheese is produced. 15. A production method for a fermented dairy product according to claim 1, wherein a sterilized dairy product lactic acid bacteria beverage is produced. 16. A production method for a fermented dairy product according to claim 1, wherein a lactic acid bacteria beverage is produced. 17. A method for producing yogurt, comprising:
producing sterile full fat soy flour having a grain size of from 100 to 1,000 meshes by pulverizing sterile dehulled soybeans prepared so as to have a bacterial count of 300 cells/g or less by using a method of separating whole soybeans into cotyledons, germs, and hulls; adding water to the sterile full fat soy flour to prepare a powdered soy juice, followed by sterilizing the powdered soy juice by heating; homogenizing the powdered soy juice to prepare a homogenized powdered soy juice; and adding a lactic acid bacterium to the homogenized powdered soy juice, followed by fermentation to prepare fermented milk. 18. A method for producing cheese, comprising:
producing sterile full fat soy flour having a grain size of from 100 to 1,000 meshes by pulverizing sterile dehulled soybeans prepared so as to have a bacterial count of 300 cells/g or less by using a method of separating whole soybeans into cotyledons, germs, and hulls; adding water to the sterile full fat soy flour to prepare a powdered soy juice, followed by sterilizing the powdered soy juice by heating; homogenizing the powdered soy juice to prepare a homogenized powdered soy juice; and adding a lactic acid bacterium to the homogenized powdered soy juice, followed by fermentation to prepare fermented milk. 19. A method according to claim 18, further comprising:
removing whey from the fermented milk | 1,700 |
3,432 | 12,861,077 | 1,798 | Described are methods of removing phospholipids and other off-flavor-causing compounds from edible proteins using a cyclodextrin treatment. The methods include treating soy protein with cyclodextrins such as β-cyclodextrin to form cyclodextrin-compound complexes and then separating the resulting complexes from the protein. Optionally, prior to treating the protein with cyclodextrin, the protein is sonicated and then treated with a phospholipase, such as phospholipase A 2 . Versions of the methods described herein are capable of removing more than 99% of phospholipids from soy protein. | 1. A method for removing compounds that cause off-flavors in proteins, the method comprising:
contacting a protein-containing solution with a cyclodextrin for a time and under conditions wherein the cyclodextrin binds to an off-flavor-causing compound in the solution, thereby yielding a cyclodextrin-compound complex; and then separating the cyclodextrin-compound complex from the protein-containing solution. 2. The method of claim 1 wherein the protein-containing solution is derived from oilseeds or oil-bearing cereal grain. 3. The method of claim 1 wherein the protein-containing solution includes soy protein. 4. The method of claim 1 wherein the contacting step includes contacting the protein-containing solution with an unsubstituted or substituted β-cyclodextrin. 5. The method of claim 4 wherein the β-cyclodextrin in the contacting step is immobilized on a solid support. 6. The method of claim 1 further comprising, prior to the contacting step, treating the protein-containing solution with a lipid hydrolase. 7. The method of claim 6 wherein the treating step includes treating the protein-containing solution with a phospholipase. 8. The method of claim 6 wherein the treating step includes treating the protein-containing solution with a phospholipase A2. 9. The method of claim 6 wherein the treating step includes treating the protein-containing solution with a phospholipase A2 at a temperature of from about 20° C. to about 50° C. and at a concentration of from about 50 units to about 200 units phospholipase A2 per gram of protein in the protein-containing solution. 10. The method of claim 6 further comprising, prior to the treating step, sonicating the protein-containing solution. 11. The method of claim 10 wherein the sonicating step includes sonicating the protein-containing solution for at least about 2 minutes, at a temperature of from about 20° C. to about 70° C., at a frequency of from about 10 kHz to about 30 kHz, and at a power of from about 30 W to about 100 W. 12. The method of claim 11 wherein the sonicating step includes sonicating the protein-containing solution for at least about 5 minutes. 13. The method of claim 1 wherein the separating step includes separating the cyclodextrin-compound complexes from the protein-containing solution via ultrafiltration, dialysis, or precipitation. 14. The method of claim 1 wherein the separating step includes separating the cyclodextrin-compound complexes from the protein-containing solution via isoelectric precipitation at a pH of from about 4 to 5. 15. The method of claim 1 wherein the separating step includes separating the cyclodextrin-compound complexes from the protein-containing solution via ultrafiltration, wherein the ultrafiltration includes diafiltration. 16. The method of claim 1 wherein the diafiltration is performed with a diafiltration ratio of at least 2×. 17. The method of claim 1 wherein the diafiltration is performed with a diluent of water that includes a cyclodextrin. 18. The method of claim 1 wherein the off-flavor-causing compound consists of a lipid containing a fatty acid moiety. 19. The method of claim 1 wherein the off-flavor-causing compound is selected from the group consisting of a free fatty acid, a phospholipid, a glyceride, and a cholesterol ester. 20. A method for removing compounds that cause off-flavors in proteins, the method comprising:
(a) sonicating a protein-containing solution; then (b) treating the protein-containing solution with a lipid hydrolase; then (c) contacting the protein-containing solution with a cyclodextrin for a time and under conditions wherein the cyclodextrin binds to an off-flavor-causing compound in the protein-containing solution, thereby yielding a cyclodextrin-compound complex; and then (d) separating the cyclodextrin-compound complex from the protein-containing solution. 21. The method of claim 20 wherein the protein-containing solution includes soy protein. 22. The method of claim 20 wherein the contacting step includes contacting the protein-containing solution with an unsubstituted or substituted β-cyclodextrin. 23. The method of claim 22 wherein the f3-cyclodextrin is immobilized on a solid support. 24. The method of claim 20 wherein the sonicating step includes sonicating the protein-containing solution for at least about 5 minutes, at a temperature of from about 20° C. to about 70° C., at a frequency of from about 10 kHz to about 30 kHz, and at a power of from about 30 W to about 100 W. 25. The method of claim 20 wherein the treating step includes treating the protein-containing solution with a phospholipase. 26. The method of claim 20 wherein the treating step includes treating the protein-containing solution with a phospholipase A2 at a temperature of from about 20° C. to about 50° C. and at a concentration of from about 50 units to about 200 units phospholipase A2 per gram of protein in the protein-containing solution. 27. The method of claim 20 wherein the separating step includes separating the cyclodextrin-compound complexes from the protein-containing solution via ultrafiltration using diafiltration at a diafiltration ratio of at least 2× or isoelectric precipitation at a pH of from about 4 to 5. 28. The method of claim 20 wherein the off-flavor-causing compound is selected from the group consisting of a free fatty acid, a phospholipid, a glyceride, and a cholesterol ester. 29. A protein product produced according to claim 1. 30. The protein product of claim 29 wherein the protein product includes soy protein. 31. The protein product of claim 29 wherein the protein product has a phospholipid content less than about 10 mg phospholipid/g protein. 32. The protein product of claim 29 wherein the protein product has a phospholipid content less than about 1 mg phospholipid/g protein. 33. The protein product of claim 29 wherein the protein product has a free fatty acid content less than about 1 mg fatty acid/g protein. 34. The protein product of claim 29 wherein the protein product is edible. | Described are methods of removing phospholipids and other off-flavor-causing compounds from edible proteins using a cyclodextrin treatment. The methods include treating soy protein with cyclodextrins such as β-cyclodextrin to form cyclodextrin-compound complexes and then separating the resulting complexes from the protein. Optionally, prior to treating the protein with cyclodextrin, the protein is sonicated and then treated with a phospholipase, such as phospholipase A 2 . Versions of the methods described herein are capable of removing more than 99% of phospholipids from soy protein.1. A method for removing compounds that cause off-flavors in proteins, the method comprising:
contacting a protein-containing solution with a cyclodextrin for a time and under conditions wherein the cyclodextrin binds to an off-flavor-causing compound in the solution, thereby yielding a cyclodextrin-compound complex; and then separating the cyclodextrin-compound complex from the protein-containing solution. 2. The method of claim 1 wherein the protein-containing solution is derived from oilseeds or oil-bearing cereal grain. 3. The method of claim 1 wherein the protein-containing solution includes soy protein. 4. The method of claim 1 wherein the contacting step includes contacting the protein-containing solution with an unsubstituted or substituted β-cyclodextrin. 5. The method of claim 4 wherein the β-cyclodextrin in the contacting step is immobilized on a solid support. 6. The method of claim 1 further comprising, prior to the contacting step, treating the protein-containing solution with a lipid hydrolase. 7. The method of claim 6 wherein the treating step includes treating the protein-containing solution with a phospholipase. 8. The method of claim 6 wherein the treating step includes treating the protein-containing solution with a phospholipase A2. 9. The method of claim 6 wherein the treating step includes treating the protein-containing solution with a phospholipase A2 at a temperature of from about 20° C. to about 50° C. and at a concentration of from about 50 units to about 200 units phospholipase A2 per gram of protein in the protein-containing solution. 10. The method of claim 6 further comprising, prior to the treating step, sonicating the protein-containing solution. 11. The method of claim 10 wherein the sonicating step includes sonicating the protein-containing solution for at least about 2 minutes, at a temperature of from about 20° C. to about 70° C., at a frequency of from about 10 kHz to about 30 kHz, and at a power of from about 30 W to about 100 W. 12. The method of claim 11 wherein the sonicating step includes sonicating the protein-containing solution for at least about 5 minutes. 13. The method of claim 1 wherein the separating step includes separating the cyclodextrin-compound complexes from the protein-containing solution via ultrafiltration, dialysis, or precipitation. 14. The method of claim 1 wherein the separating step includes separating the cyclodextrin-compound complexes from the protein-containing solution via isoelectric precipitation at a pH of from about 4 to 5. 15. The method of claim 1 wherein the separating step includes separating the cyclodextrin-compound complexes from the protein-containing solution via ultrafiltration, wherein the ultrafiltration includes diafiltration. 16. The method of claim 1 wherein the diafiltration is performed with a diafiltration ratio of at least 2×. 17. The method of claim 1 wherein the diafiltration is performed with a diluent of water that includes a cyclodextrin. 18. The method of claim 1 wherein the off-flavor-causing compound consists of a lipid containing a fatty acid moiety. 19. The method of claim 1 wherein the off-flavor-causing compound is selected from the group consisting of a free fatty acid, a phospholipid, a glyceride, and a cholesterol ester. 20. A method for removing compounds that cause off-flavors in proteins, the method comprising:
(a) sonicating a protein-containing solution; then (b) treating the protein-containing solution with a lipid hydrolase; then (c) contacting the protein-containing solution with a cyclodextrin for a time and under conditions wherein the cyclodextrin binds to an off-flavor-causing compound in the protein-containing solution, thereby yielding a cyclodextrin-compound complex; and then (d) separating the cyclodextrin-compound complex from the protein-containing solution. 21. The method of claim 20 wherein the protein-containing solution includes soy protein. 22. The method of claim 20 wherein the contacting step includes contacting the protein-containing solution with an unsubstituted or substituted β-cyclodextrin. 23. The method of claim 22 wherein the f3-cyclodextrin is immobilized on a solid support. 24. The method of claim 20 wherein the sonicating step includes sonicating the protein-containing solution for at least about 5 minutes, at a temperature of from about 20° C. to about 70° C., at a frequency of from about 10 kHz to about 30 kHz, and at a power of from about 30 W to about 100 W. 25. The method of claim 20 wherein the treating step includes treating the protein-containing solution with a phospholipase. 26. The method of claim 20 wherein the treating step includes treating the protein-containing solution with a phospholipase A2 at a temperature of from about 20° C. to about 50° C. and at a concentration of from about 50 units to about 200 units phospholipase A2 per gram of protein in the protein-containing solution. 27. The method of claim 20 wherein the separating step includes separating the cyclodextrin-compound complexes from the protein-containing solution via ultrafiltration using diafiltration at a diafiltration ratio of at least 2× or isoelectric precipitation at a pH of from about 4 to 5. 28. The method of claim 20 wherein the off-flavor-causing compound is selected from the group consisting of a free fatty acid, a phospholipid, a glyceride, and a cholesterol ester. 29. A protein product produced according to claim 1. 30. The protein product of claim 29 wherein the protein product includes soy protein. 31. The protein product of claim 29 wherein the protein product has a phospholipid content less than about 10 mg phospholipid/g protein. 32. The protein product of claim 29 wherein the protein product has a phospholipid content less than about 1 mg phospholipid/g protein. 33. The protein product of claim 29 wherein the protein product has a free fatty acid content less than about 1 mg fatty acid/g protein. 34. The protein product of claim 29 wherein the protein product is edible. | 1,700 |
3,433 | 14,554,984 | 1,788 | The present application relates to gas barrier film having excellent adhesive strength and a method of manufacturing the same. Particularly, the present application is directed to providing a gas barrier film having excellent adhesion performance between an inorganic layer and a protective coating layer under harsh conditions by protective coating layer including inorganic nano particles surface-modified with organic silane on the inorganic layer | 1. A gas barrier film, comprising:
an organic-inorganic hybrid coating layer; an inorganic layer; and a protective coating layer including inorganic nano particles surface-modified with organic silane, which are sequentially stacked on one or both surface of a base. 2. The film according to claim 1, which satisfies Equation 1:
[Equation 1] X≧48
wherein X represents a time (h) for which adhesive strength between the inorganic layer and the protective coating layer is maintained to be 90% or more at 85° C. and a relative humidity of 85% as verified by performing a cross hatch cut test. 3. The film according to claim 1, wherein the organic silane is a compound represented by Formula 1:
[Formula 1] R1 mSiX4-m wherein X is the same as or different from each other, and represents hydrogen, halogen, an alkoxy group having 1 to 12 carbon atoms, an acyloxy group, an alkylcarbonyl group, an alkoxycarbonyl group, or N(R2)2 (here, R2 is hydrogen or an alkyl group having 1 to 12 carbon atoms), R1 is the same as or different from each other, and represents an alkyl group having 1 to 12 carbon atoms, an alkenyl group, an alkynyl group, an aryl group, an arylalkyl group, an alkylaryl group, an arylalkenyl group, an alkenylaryl group, an arylalkynyl group, an alkynylaryl group, or an alkylcarbonyl group, and have an amino group, an amide group, an aldehyde group, a keto group, a carboxyl group, a mercapto group, a cyano group, a hydroxyl group, an alkoxy group having 1 to 12 carbon atoms, an alkoxycarbonyl group having 1 to 12 carbon atoms, a sulfonic acid, a phosphoric acid, an acryl group, a methacryl group, an epoxy group or a vinyl group as a substituent, and m is an integer from 1 to 3. 4. The film according to claim 1, wherein the protective coating layer includes at 10 to 500 parts by weight of organic silane with respect to 100 parts by weight of the inorganic nano particles. 5. The film according to claim 1, wherein the base is a plastic film. 6. The film according to claim 5, wherein the plastic film is at least one selected from the group consisting of a homopolymer, at least one of polymer blends, and a polymer composite material containing an organic or inorganic additive. 7. The film according to claim 1, wherein the inorganic layer includes a metal oxide or nitride. 8. The film according to claim 7, wherein the metal is at least one selected from the group consisting of Al, Zr, Ti, Hf, Ta, In, Sn, Zn and Si. 9. The film according to claim 1, wherein the inorganic nano particles are at least one selected from the group consisting of alumina nano particles, silica nano particles, zinc oxide nano particles, antimony oxide nano particles, titanium oxide nano particles, and zirconium oxide nano particles. 10. The film according to claim 1, wherein the organic-inorganic hybrid coating layer has a thickness of 0.1 to 10 μm. 11. The film according to claim 1, wherein the inorganic layer has a thickness of 5 to 1000 nm. 12. The film according to claim 1, wherein the protective coating layer has a thickness of 0.1 to 10 μm. 13. A method of manufacturing a gas barrier film, comprising:
forming an organic-inorganic hybrid coating layer with a sol-type coating composition on one or both surfaces of a base; forming an inorganic layer on the organic-inorganic hybrid coating layer; and forming a protective coating layer with a solution prepared by mixing a sol-type hydrolyzing solution and a solution including inorganic nano particles surface-modified with organic silane on the inorganic layer. 14. The method according to claim 13, wherein the organic silane is a gas barrier film represented by Formula 1:
[Formula 1] R1 mSiX4-m where X is the same as or different from each other, and represents hydrogen, halogen, an alkoxy group having 1 to 12 carbon atoms, an acyloxy group, an alkylcarbonyl group, an alkoxycarbonyl group, or N(R2)2 (here, R2 is hydrogen or an alkyl group having 1 to 12 carbon atoms), R1 is the same as or different from each other, and represents an alkyl group having 1 to 12 carbon atoms, an alkenyl group, an alkynyl group, an aryl group, an arylalkyl group, an alkylaryl group, an arylalkenyl group, an alkenylaryl group, an arylalkynyl group, an alkynylaryl group, or an alkylcarbonyl group, and have an amino group, an amide group, an aldehyde group, a keto group, a carboxyl group, a mercapto group, a cyano group, a hydroxyl group, an alkoxy group having 1 to 12 carbon atoms, an alkoxycarbonyl group having 1 to 12 carbon atoms, a sulfonic acid, a phosphoric acid, an acryl group, a methacryl group, an epoxy group or a vinyl group as a substituent, and m is an integer from 1 to 3. 15. A display device, comprising:
the gas barrier film according to claim 1. 16. A photovoltaic cell according to claim 1, comprising:
the gas barrier film according to claim 1. 17. A food packaging material, comprising:
the gas barrier film according to claim 1. | The present application relates to gas barrier film having excellent adhesive strength and a method of manufacturing the same. Particularly, the present application is directed to providing a gas barrier film having excellent adhesion performance between an inorganic layer and a protective coating layer under harsh conditions by protective coating layer including inorganic nano particles surface-modified with organic silane on the inorganic layer1. A gas barrier film, comprising:
an organic-inorganic hybrid coating layer; an inorganic layer; and a protective coating layer including inorganic nano particles surface-modified with organic silane, which are sequentially stacked on one or both surface of a base. 2. The film according to claim 1, which satisfies Equation 1:
[Equation 1] X≧48
wherein X represents a time (h) for which adhesive strength between the inorganic layer and the protective coating layer is maintained to be 90% or more at 85° C. and a relative humidity of 85% as verified by performing a cross hatch cut test. 3. The film according to claim 1, wherein the organic silane is a compound represented by Formula 1:
[Formula 1] R1 mSiX4-m wherein X is the same as or different from each other, and represents hydrogen, halogen, an alkoxy group having 1 to 12 carbon atoms, an acyloxy group, an alkylcarbonyl group, an alkoxycarbonyl group, or N(R2)2 (here, R2 is hydrogen or an alkyl group having 1 to 12 carbon atoms), R1 is the same as or different from each other, and represents an alkyl group having 1 to 12 carbon atoms, an alkenyl group, an alkynyl group, an aryl group, an arylalkyl group, an alkylaryl group, an arylalkenyl group, an alkenylaryl group, an arylalkynyl group, an alkynylaryl group, or an alkylcarbonyl group, and have an amino group, an amide group, an aldehyde group, a keto group, a carboxyl group, a mercapto group, a cyano group, a hydroxyl group, an alkoxy group having 1 to 12 carbon atoms, an alkoxycarbonyl group having 1 to 12 carbon atoms, a sulfonic acid, a phosphoric acid, an acryl group, a methacryl group, an epoxy group or a vinyl group as a substituent, and m is an integer from 1 to 3. 4. The film according to claim 1, wherein the protective coating layer includes at 10 to 500 parts by weight of organic silane with respect to 100 parts by weight of the inorganic nano particles. 5. The film according to claim 1, wherein the base is a plastic film. 6. The film according to claim 5, wherein the plastic film is at least one selected from the group consisting of a homopolymer, at least one of polymer blends, and a polymer composite material containing an organic or inorganic additive. 7. The film according to claim 1, wherein the inorganic layer includes a metal oxide or nitride. 8. The film according to claim 7, wherein the metal is at least one selected from the group consisting of Al, Zr, Ti, Hf, Ta, In, Sn, Zn and Si. 9. The film according to claim 1, wherein the inorganic nano particles are at least one selected from the group consisting of alumina nano particles, silica nano particles, zinc oxide nano particles, antimony oxide nano particles, titanium oxide nano particles, and zirconium oxide nano particles. 10. The film according to claim 1, wherein the organic-inorganic hybrid coating layer has a thickness of 0.1 to 10 μm. 11. The film according to claim 1, wherein the inorganic layer has a thickness of 5 to 1000 nm. 12. The film according to claim 1, wherein the protective coating layer has a thickness of 0.1 to 10 μm. 13. A method of manufacturing a gas barrier film, comprising:
forming an organic-inorganic hybrid coating layer with a sol-type coating composition on one or both surfaces of a base; forming an inorganic layer on the organic-inorganic hybrid coating layer; and forming a protective coating layer with a solution prepared by mixing a sol-type hydrolyzing solution and a solution including inorganic nano particles surface-modified with organic silane on the inorganic layer. 14. The method according to claim 13, wherein the organic silane is a gas barrier film represented by Formula 1:
[Formula 1] R1 mSiX4-m where X is the same as or different from each other, and represents hydrogen, halogen, an alkoxy group having 1 to 12 carbon atoms, an acyloxy group, an alkylcarbonyl group, an alkoxycarbonyl group, or N(R2)2 (here, R2 is hydrogen or an alkyl group having 1 to 12 carbon atoms), R1 is the same as or different from each other, and represents an alkyl group having 1 to 12 carbon atoms, an alkenyl group, an alkynyl group, an aryl group, an arylalkyl group, an alkylaryl group, an arylalkenyl group, an alkenylaryl group, an arylalkynyl group, an alkynylaryl group, or an alkylcarbonyl group, and have an amino group, an amide group, an aldehyde group, a keto group, a carboxyl group, a mercapto group, a cyano group, a hydroxyl group, an alkoxy group having 1 to 12 carbon atoms, an alkoxycarbonyl group having 1 to 12 carbon atoms, a sulfonic acid, a phosphoric acid, an acryl group, a methacryl group, an epoxy group or a vinyl group as a substituent, and m is an integer from 1 to 3. 15. A display device, comprising:
the gas barrier film according to claim 1. 16. A photovoltaic cell according to claim 1, comprising:
the gas barrier film according to claim 1. 17. A food packaging material, comprising:
the gas barrier film according to claim 1. | 1,700 |
3,434 | 14,426,208 | 1,798 | Embodiments of the present invention provide for assessing the state of an 82 Rb elution system. In certain embodiments, a system begins an assessment that comprises an elution, and a metric may be measured. This metric may be a concentration of 82 Rb, 82 Sr, or 85 Sr in a fluid that is eluted from the generator, the volume of the fluid that is eluted from the generator, or the pressure of the fluid flowing through at least one portion of the system. If the assessment is completed, an output may be generated on a user interface that recommends a course of action, or no course of action, based on a result of the assessment. Should the assessment not complete successfully because it is interrupted, a 82 Sr/ 82 Rb generator of the system may be halted so as to prevent a user from performing an end-run around these quality control mechanisms of the 82 Rb elution system. | 1. An 82Sr/82Rb elution system, comprising:
a 82Sr/82Rb generator; a processor; and a memory communicatively coupled to the processor when the system is operational, the memory bearing processor-executable instructions that, when executed on the processor, cause the system to at least:
begin to assess a concentration of 82Rb, 82Sr, or 85Sr in a fluid that is eluted from the generator, the volume of the fluid that is eluted from the generator, or the pressure of the fluid flowing through at least one portion of the system;
when the assessment is completed,
generate an output on a user interface that recommends a course of action or no course of action, based on a result of the assessment, or
store an indication of the result of the assessment in a memory location, and upload the indication of the result of the assessment to a computer via a communications network; and
when the assessment is interrupted, halting the generator to prevent user end-run around quality control. 2. The system of claim 1, further comprising:
a pump; and a controller communicatively coupled with the pump and the processor, the controller shutting down the pump in response to determining that communication with the processor has been lost. 3. The system of claim 1, wherein the memory further bears instructions that, when executed on the processor, cause the system to at least:
in response to determining that a total volume of the fluid eluted exceeds a limit threshold, preventing elution until the generator is replaced with a new generator. 4. The system of claim 1, wherein the memory further bears instructions that, when executed on the processor, cause the system to at least:
in response to determining that a ratio of 82Sr to 82Rb, or 85Sr to 82Rb is greater than a maximum threshold of USP, preventing elution until the generator is replaced with a new generator. 5. The system of claim 1, wherein the memory further bears instructions that, when executed on the processor, cause the system to at least:
in response to determining that a ratio of 82Sr to 82Rb, or 85Sr to 82Rb is greater than a warning threshold of USP, performing an additional assessment after a delimited number of patients are treated with the system since determining that the ratio of 82Sr to 82Rb, or 85Sr to 82Rb is greater than a warning threshold of USP. 6. The system of claim 1, further comprising:
a pump; and where in the memory further bears processor-executable instructions that, when executed on the processor, cause the system to at least:
in response to determining that the in-line pressure of the fluid is outside an acceptable range, stopping the pump. 7. The system of claim 1, further comprising:
a pump, a positron detector, and a generator valve or a patient valve; and
wherein the memory further bears processor-executable instructions that, when executed on the processor, cause the system to stop the pump in response to identifying a malfunction of the pump, the pressure sensor, the valve, or the positron detector. 8. The system of claim 1, wherein the memory further bears instructions that, when executed on the processor, cause the system to at least:
in response to determining that a half-life of an isotope in the fluid eluted is not indicative of 82Rb, perform an assessment where the elution is not provided to a patient before performing an assessment where an elution is provided to the patient. 9. The system of claim 1, wherein the assessment comprises:
determining a ratio of 82Sr to 82Rb and a ratio of 85Sr to 82Rb in the fluid. 10. The system of claim 1, further comprising:
a portable cart that houses the generator, the processor, a pump, the memory, a patient line, a bypass line, a positron detector, and a dose calibrator. 11. The system of claim 10, wherein the cart comprises an interior that is coated with a vibration-absorbing material. 12. The system of claim 1, wherein the memory further bears instructions that, when executed on the processor on a given day, cause the system to at least:
in response to determining that the assessment has not been performed within a predetermined period of time preceding the execution of said instructions, perform the assessment check before performing an additional patient elution. 13. The system of claim 12, wherein the memory further bears instructions that, when executed on the processor, cause the system to at least:
in response to determining from the assessment performed on the given day that the 82Sr or 85Sr concentration is above a threshold, perform a flush elution and a calibration elution before performing a patient elution. 14. The system of claim 1, wherein the instructions that, when executed upon the processor, cause the system to at least upload the indication of the result of the assessment to a computer via a communications network further cause the system to at least:
upload the indication of the result of the assessment to a computer via a communications network, the computer combining the result of the assessment with a result of an assessment of another 82Sr/82Rb elution system. | Embodiments of the present invention provide for assessing the state of an 82 Rb elution system. In certain embodiments, a system begins an assessment that comprises an elution, and a metric may be measured. This metric may be a concentration of 82 Rb, 82 Sr, or 85 Sr in a fluid that is eluted from the generator, the volume of the fluid that is eluted from the generator, or the pressure of the fluid flowing through at least one portion of the system. If the assessment is completed, an output may be generated on a user interface that recommends a course of action, or no course of action, based on a result of the assessment. Should the assessment not complete successfully because it is interrupted, a 82 Sr/ 82 Rb generator of the system may be halted so as to prevent a user from performing an end-run around these quality control mechanisms of the 82 Rb elution system.1. An 82Sr/82Rb elution system, comprising:
a 82Sr/82Rb generator; a processor; and a memory communicatively coupled to the processor when the system is operational, the memory bearing processor-executable instructions that, when executed on the processor, cause the system to at least:
begin to assess a concentration of 82Rb, 82Sr, or 85Sr in a fluid that is eluted from the generator, the volume of the fluid that is eluted from the generator, or the pressure of the fluid flowing through at least one portion of the system;
when the assessment is completed,
generate an output on a user interface that recommends a course of action or no course of action, based on a result of the assessment, or
store an indication of the result of the assessment in a memory location, and upload the indication of the result of the assessment to a computer via a communications network; and
when the assessment is interrupted, halting the generator to prevent user end-run around quality control. 2. The system of claim 1, further comprising:
a pump; and a controller communicatively coupled with the pump and the processor, the controller shutting down the pump in response to determining that communication with the processor has been lost. 3. The system of claim 1, wherein the memory further bears instructions that, when executed on the processor, cause the system to at least:
in response to determining that a total volume of the fluid eluted exceeds a limit threshold, preventing elution until the generator is replaced with a new generator. 4. The system of claim 1, wherein the memory further bears instructions that, when executed on the processor, cause the system to at least:
in response to determining that a ratio of 82Sr to 82Rb, or 85Sr to 82Rb is greater than a maximum threshold of USP, preventing elution until the generator is replaced with a new generator. 5. The system of claim 1, wherein the memory further bears instructions that, when executed on the processor, cause the system to at least:
in response to determining that a ratio of 82Sr to 82Rb, or 85Sr to 82Rb is greater than a warning threshold of USP, performing an additional assessment after a delimited number of patients are treated with the system since determining that the ratio of 82Sr to 82Rb, or 85Sr to 82Rb is greater than a warning threshold of USP. 6. The system of claim 1, further comprising:
a pump; and where in the memory further bears processor-executable instructions that, when executed on the processor, cause the system to at least:
in response to determining that the in-line pressure of the fluid is outside an acceptable range, stopping the pump. 7. The system of claim 1, further comprising:
a pump, a positron detector, and a generator valve or a patient valve; and
wherein the memory further bears processor-executable instructions that, when executed on the processor, cause the system to stop the pump in response to identifying a malfunction of the pump, the pressure sensor, the valve, or the positron detector. 8. The system of claim 1, wherein the memory further bears instructions that, when executed on the processor, cause the system to at least:
in response to determining that a half-life of an isotope in the fluid eluted is not indicative of 82Rb, perform an assessment where the elution is not provided to a patient before performing an assessment where an elution is provided to the patient. 9. The system of claim 1, wherein the assessment comprises:
determining a ratio of 82Sr to 82Rb and a ratio of 85Sr to 82Rb in the fluid. 10. The system of claim 1, further comprising:
a portable cart that houses the generator, the processor, a pump, the memory, a patient line, a bypass line, a positron detector, and a dose calibrator. 11. The system of claim 10, wherein the cart comprises an interior that is coated with a vibration-absorbing material. 12. The system of claim 1, wherein the memory further bears instructions that, when executed on the processor on a given day, cause the system to at least:
in response to determining that the assessment has not been performed within a predetermined period of time preceding the execution of said instructions, perform the assessment check before performing an additional patient elution. 13. The system of claim 12, wherein the memory further bears instructions that, when executed on the processor, cause the system to at least:
in response to determining from the assessment performed on the given day that the 82Sr or 85Sr concentration is above a threshold, perform a flush elution and a calibration elution before performing a patient elution. 14. The system of claim 1, wherein the instructions that, when executed upon the processor, cause the system to at least upload the indication of the result of the assessment to a computer via a communications network further cause the system to at least:
upload the indication of the result of the assessment to a computer via a communications network, the computer combining the result of the assessment with a result of an assessment of another 82Sr/82Rb elution system. | 1,700 |
3,435 | 13,737,050 | 1,786 | The present invention is generally directed to a liquid entrapping device having the capacity to absorb liquids. More particularly, the present invention is directed to a liquid entrapping device comprising an absorbent component, hydrophilic elastomeric fibrous component in fluid communication therewith, and optionally an adhesive component. The present invention is also directed to a liquid entrapping device having the capacity to absorb liquids while maintaining a suitable degree of mechanical strength. Furthermore, the present invention is generally directed to methods for making and using the foregoing devices and materials. | 1. A liquid entrapping device comprising:
an absorbent component; and a hydrophilic elastomeric fibrous component, wherein the absorbent component and the hydrophilic elastomeric fibrous component are in physical proximity thereby resulting in fluid communication, wherein the absorbent component is more absorbent than the hydrophilic elastomeric fibrous component but wherein the hydrophilic elastomeric fibrous component absorbs more quickly than and has a smaller holding capacity than the absorbent component, wherein the liquid entrapping device, including the hydrophilic fibrous component is formed from at least one electrospun nanofiber where the at least one electrospun nanofiber comprises both the absorbent component and the hydrophilic elastomeric fibrous component in the nanofiber body, where wherein the absorbent component is mechanically entangled by the electrospun hydrophilic elastomeric fibrous component. 2. The liquid entrapping device of claim 1, wherein the absorbent component is selected from polyesters, polyethers, polyester-polyethers, polymers having pendant carboxylic acids or pendant hydroxyls, polysiloxanes, polyacrylamides, kaolins, serpentines, smectites, glauconite, chlorites, vermiculites, attapulgite, sepiolite, allophane and imogolite, sodium polyacrylates, 2-propenamide-co-2-propenoic acid, and any combination thereof. 3. The liquid entrapping device of claim 1, wherein the absorbent component is selected from zein protein, polyester elastomers, polydimethylsiloxane, hydrophilic poly(ether-co-ester) elastomers, silicone-co-polyethyleneglycol elastomers, polyacrylates, thermoplastic polyurethanes, poly(ether-co-urethanes), and any combination thereof. 4. The liquid entrapping device of claim 1, wherein the absorbent component is present in an amount from about 1% (w/w) to about 85% (w/w). 5. The liquid entrapping device of claim 1, wherein the absorbent component is present in an amount from about 5% (w/w) to about 50% (w/w). 6. The liquid entrapping device of claim 1, wherein the absorbent component is present in an amount from about 30% (w/w) to about 50% (w/w). 7. The liquid entrapping device of claim 1, wherein the hydrophilic elastomeric fibrous component is selected from polyurethanes, poly ether-co-urethanes, and any combination thereof. 8. The liquid entrapping device of claim 1, wherein the liquid entrapping device comprises a device selected from a diaper, a tampon, a sanitary napkin, a sanitary wipe, a spill absorbing device, a mop head, and a floor waxing device. 9. The liquid entrapping device of claim 1, wherein the liquid entrapping device further comprises an absorbency of water from about 400% to about 6000%, wherein absorbency is defined as Q=(W2−W1)/W1. 10. The liquid entrapping device of claim 9, wherein the liquid entrapping device further comprises an absorbency of water from about 500% to about 5500%. 11. The liquid entrapping device of claim 1, wherein the liquid entrapping device further comprises an absorbency of urine from about 500% to about 1250%, wherein absorbency is defined as Q=(W2−W1)W1. 12. The liquid entrapping device of claim 11, wherein the liquid entrapping device further comprises an absorbency of urine from about 500% to about 1000%. 13. The liquid entrapping device of claim 12, wherein the liquid entrapping device further comprises an absorbency of urine from about 600% to about 1000%, wherein absorbency is defined as Q=(W2−W1)/W1. 14. The liquid entrapping device of claim 1, wherein the liquid entrapping device further comprises a capacity to absorb about 100% of its equilibrium capacity in about 5 seconds. 15. The liquid entrapping device of claim 14, wherein the liquid entrapping device further comprises a capacity to absorb greater than about 73% of its equilibrium capacity in about 5 seconds. 16. The liquid entrapping device of claim 15, wherein the liquid entrapping device further comprises a capacity to absorb greater than about 75% of its equilibrium capacity in about two minutes. 17. The liquid entrapping device of claim 1, wherein the liquid entrapping device further comprises a tensile strength from about 0 to about 3.0 MPa when the device is wetted with water. 18. The liquid entrapping device of claim 17, wherein the liquid entrapping device further comprises a tensile strength from about 0.25 to about 3.0 MPa when the device is wetted with water. 19. The liquid entrapping device of claim 18, wherein the liquid entrapping device further comprises a tensile strength from about 0.2 to about 2.8 MPa when the device is wetted with water. 20. The liquid entrapping device of claim 19, wherein the liquid entrapping device further comprises a tensile strength from about 0.25 to about 2.8 MPa when the device is wetted with water. 21. The liquid entrapping device of claim 1, wherein the liquid entrapping device further comprises a breaking point at about 850% to about 900% strain. 22. The liquid entrapping device of claim 1, wherein the liquid entrapping device further comprises a breaking point at about 600% strain. 23. The liquid entrapping device of claim 1, wherein the liquid entrapping device further comprises from about 1% (w/w) to about 5% (w/w) leachable matter. 24. The liquid entrapping device of claim 23, wherein the liquid entrapping device further comprises from about 1.6% (w/w) to about 4.5% (w/w) leachable matter. 25. The liquid entrapping device of claim 24, wherein the liquid entrapping device further comprises from about 1% (w/w) to about 4% (w/w) leachable matter. 26. The liquid entrapping device of claim 1, wherein the absorbent component is a super absorbent. 27. The liquid entrapping device of claim 1, wherein the absorbent component is capable of holding at least about 50 times its own weight in liquid. 28. The liquid entrapping device of claim 1, wherein the nanofibers are electrospun nanofibers having a fiber diameter of about 1 nanometer to about 3,000 nanometers. 29. A non-woven liquid entrapping device comprising:
a super absorbent component; and a hydrophilic elastomeric fibrous component, wherein the super absorbent component and the hydrophilic elastomeric fibrous component are in physical proximity thereby resulting in fluid communication, wherein the super absorbent component is more absorbent than the hydrophilic elastomeric fibrous component, but wherein the hydrophilic elastomeric fibrous component absorbs more quickly than and has a smaller holding capacity than the super absorbent component, wherein the non-woven liquid entrapping device, including the hydrophilic elastomeric fibrous component, is formed from at least one electrospun nanofiber where the at least one electrospun nanofiber comprises both the absorbent component and the hydrophilic elastomeric fibrous component in the nanofiber body, wherein the super absorbent component is mechanically entangled by the electrospunhydrophilic elastomeric fibrous component, and wherein the super absorbent component is present in an amount from about 1% (w/w) to about 85% (w/w). 30. The non-woven liquid entrapping device of claim 29, wherein the hydrophilic elastomeric fibrous component is selected from zein protein, polyester elastomers, polydimethylsiloxane, hydrophilic poly(ether-co-ester) elastomers, silicone-co-polyethyleneglycol elastomers, polyacrylates, thermoplastic polyurethanes, poly(ether-co-urethanes), and any combination thereof. 31. The non-woven liquid entrapping device of claim 29, wherein the absorbent component is present in an amount from about 5% (w/w) to about 50% (w/w). 32. The non-woven liquid entrapping device of claim 29, wherein the absorbent component is present in an amount from about 30% (w/w) to about 50% (w/w). 33. The non-woven liquid entrapping device of claim 29, wherein the hydrophilic elastomeric fibrous component is selected from polyurethanes, poly ether-co-urethanes, and any combination thereof. 34. The non-woven liquid entrapping device of claim 29, wherein the liquid entrapping device comprises a device selected from a diaper, a tampon, a sanitary napkin, a sanitary wipe, a spill absorbing device, a mop head, and a floor waxing device. 35. The non-woven liquid entrapping device of claim 29, wherein the nanofibers are electrospun nanofibers having a fiber diameter of about 1 nanometer to about 3,000 nanometers. 36. The non-woven liquid entrapping device of claim 29, wherein the nanofibers are electrospun nanofibers having a fiber diameter of about 10 nanometers to about 2,000 nanometers. 37. A non-woven liquid entrapping device comprising:
an absorbent component; and a hydrophilic elastomeric fibrous component, wherein the absorbent component and the hydrophilic elastomeric fibrous component are in physical proximity thereby resulting in fluid communication, wherein the absorbent component is more absorbent than the hydrophilic elastomeric fibrous component, but wherein the hydrophilic elastomeric fibrous component absorbs more quickly than and has a smaller holding capacity than the absorbent component, wherein the non-woven liquid entrapping device, including the hydrophilic elastomeric fibrous component, is formed from at least one electrospun nanofiber where the at least one electrospun nanofiber comprises both the absorbent component and the hydrophilic elastomeric fibrous component in the electrospun nanofiber body, wherein the absorbent component is mechanically entangled by the electrospun hydrophilic elastomeric fibrous component, wherein the non-woven liquid entrapping device, including the hydrophilic elastomeric fibrous component, is formed from nanofibers having a fiber diameter of about 1 nanometer to about 3,000 nanometers, and wherein the absorbent component is capable of holding at least about 50 times its own weight in liquid. 38. The non-woven liquid entrapping device of claim 37, wherein the hydrophilic elastomeric fibrous component is selected from zein protein, polyester elastomers, polydimethylsiloxane, hydrophilic poly(ether-co-ester) elastomers, silicone-co-polyethyleneglycol elastomers, polyacrylates, thermoplastic polyurethanes, poly(ether-co-urethanes), and any combination thereof. 39. The non-woven liquid entrapping device of claim 37, wherein the absorbent component is present in an amount from about 5% (w/w) to about 50% (w/w). 40. The non-woven liquid entrapping device of claim 37, wherein the absorbent component is present in an amount from about 30% (w/w) to about 50% (w/w). 41. The non-woven liquid entrapping device of claim 37, wherein the hydrophilic elastomeric fibrous component is selected from polyurethanes, poly ether-co-urethanes, and any combination thereof. 42. The non-woven liquid entrapping device of claim 37, wherein the liquid entrapping device comprises a device selected from a diaper, a tampon, a sanitary napkin, a sanitary wipe, a spill absorbing device, a mop head, and a floor waxing device. 43. The non-woven liquid entrapping device of claim 37, wherein the nanofibers are electrospun nanofibers having a fiber diameter of about 10 nanometers to about 2,000 nanometers. | The present invention is generally directed to a liquid entrapping device having the capacity to absorb liquids. More particularly, the present invention is directed to a liquid entrapping device comprising an absorbent component, hydrophilic elastomeric fibrous component in fluid communication therewith, and optionally an adhesive component. The present invention is also directed to a liquid entrapping device having the capacity to absorb liquids while maintaining a suitable degree of mechanical strength. Furthermore, the present invention is generally directed to methods for making and using the foregoing devices and materials.1. A liquid entrapping device comprising:
an absorbent component; and a hydrophilic elastomeric fibrous component, wherein the absorbent component and the hydrophilic elastomeric fibrous component are in physical proximity thereby resulting in fluid communication, wherein the absorbent component is more absorbent than the hydrophilic elastomeric fibrous component but wherein the hydrophilic elastomeric fibrous component absorbs more quickly than and has a smaller holding capacity than the absorbent component, wherein the liquid entrapping device, including the hydrophilic fibrous component is formed from at least one electrospun nanofiber where the at least one electrospun nanofiber comprises both the absorbent component and the hydrophilic elastomeric fibrous component in the nanofiber body, where wherein the absorbent component is mechanically entangled by the electrospun hydrophilic elastomeric fibrous component. 2. The liquid entrapping device of claim 1, wherein the absorbent component is selected from polyesters, polyethers, polyester-polyethers, polymers having pendant carboxylic acids or pendant hydroxyls, polysiloxanes, polyacrylamides, kaolins, serpentines, smectites, glauconite, chlorites, vermiculites, attapulgite, sepiolite, allophane and imogolite, sodium polyacrylates, 2-propenamide-co-2-propenoic acid, and any combination thereof. 3. The liquid entrapping device of claim 1, wherein the absorbent component is selected from zein protein, polyester elastomers, polydimethylsiloxane, hydrophilic poly(ether-co-ester) elastomers, silicone-co-polyethyleneglycol elastomers, polyacrylates, thermoplastic polyurethanes, poly(ether-co-urethanes), and any combination thereof. 4. The liquid entrapping device of claim 1, wherein the absorbent component is present in an amount from about 1% (w/w) to about 85% (w/w). 5. The liquid entrapping device of claim 1, wherein the absorbent component is present in an amount from about 5% (w/w) to about 50% (w/w). 6. The liquid entrapping device of claim 1, wherein the absorbent component is present in an amount from about 30% (w/w) to about 50% (w/w). 7. The liquid entrapping device of claim 1, wherein the hydrophilic elastomeric fibrous component is selected from polyurethanes, poly ether-co-urethanes, and any combination thereof. 8. The liquid entrapping device of claim 1, wherein the liquid entrapping device comprises a device selected from a diaper, a tampon, a sanitary napkin, a sanitary wipe, a spill absorbing device, a mop head, and a floor waxing device. 9. The liquid entrapping device of claim 1, wherein the liquid entrapping device further comprises an absorbency of water from about 400% to about 6000%, wherein absorbency is defined as Q=(W2−W1)/W1. 10. The liquid entrapping device of claim 9, wherein the liquid entrapping device further comprises an absorbency of water from about 500% to about 5500%. 11. The liquid entrapping device of claim 1, wherein the liquid entrapping device further comprises an absorbency of urine from about 500% to about 1250%, wherein absorbency is defined as Q=(W2−W1)W1. 12. The liquid entrapping device of claim 11, wherein the liquid entrapping device further comprises an absorbency of urine from about 500% to about 1000%. 13. The liquid entrapping device of claim 12, wherein the liquid entrapping device further comprises an absorbency of urine from about 600% to about 1000%, wherein absorbency is defined as Q=(W2−W1)/W1. 14. The liquid entrapping device of claim 1, wherein the liquid entrapping device further comprises a capacity to absorb about 100% of its equilibrium capacity in about 5 seconds. 15. The liquid entrapping device of claim 14, wherein the liquid entrapping device further comprises a capacity to absorb greater than about 73% of its equilibrium capacity in about 5 seconds. 16. The liquid entrapping device of claim 15, wherein the liquid entrapping device further comprises a capacity to absorb greater than about 75% of its equilibrium capacity in about two minutes. 17. The liquid entrapping device of claim 1, wherein the liquid entrapping device further comprises a tensile strength from about 0 to about 3.0 MPa when the device is wetted with water. 18. The liquid entrapping device of claim 17, wherein the liquid entrapping device further comprises a tensile strength from about 0.25 to about 3.0 MPa when the device is wetted with water. 19. The liquid entrapping device of claim 18, wherein the liquid entrapping device further comprises a tensile strength from about 0.2 to about 2.8 MPa when the device is wetted with water. 20. The liquid entrapping device of claim 19, wherein the liquid entrapping device further comprises a tensile strength from about 0.25 to about 2.8 MPa when the device is wetted with water. 21. The liquid entrapping device of claim 1, wherein the liquid entrapping device further comprises a breaking point at about 850% to about 900% strain. 22. The liquid entrapping device of claim 1, wherein the liquid entrapping device further comprises a breaking point at about 600% strain. 23. The liquid entrapping device of claim 1, wherein the liquid entrapping device further comprises from about 1% (w/w) to about 5% (w/w) leachable matter. 24. The liquid entrapping device of claim 23, wherein the liquid entrapping device further comprises from about 1.6% (w/w) to about 4.5% (w/w) leachable matter. 25. The liquid entrapping device of claim 24, wherein the liquid entrapping device further comprises from about 1% (w/w) to about 4% (w/w) leachable matter. 26. The liquid entrapping device of claim 1, wherein the absorbent component is a super absorbent. 27. The liquid entrapping device of claim 1, wherein the absorbent component is capable of holding at least about 50 times its own weight in liquid. 28. The liquid entrapping device of claim 1, wherein the nanofibers are electrospun nanofibers having a fiber diameter of about 1 nanometer to about 3,000 nanometers. 29. A non-woven liquid entrapping device comprising:
a super absorbent component; and a hydrophilic elastomeric fibrous component, wherein the super absorbent component and the hydrophilic elastomeric fibrous component are in physical proximity thereby resulting in fluid communication, wherein the super absorbent component is more absorbent than the hydrophilic elastomeric fibrous component, but wherein the hydrophilic elastomeric fibrous component absorbs more quickly than and has a smaller holding capacity than the super absorbent component, wherein the non-woven liquid entrapping device, including the hydrophilic elastomeric fibrous component, is formed from at least one electrospun nanofiber where the at least one electrospun nanofiber comprises both the absorbent component and the hydrophilic elastomeric fibrous component in the nanofiber body, wherein the super absorbent component is mechanically entangled by the electrospunhydrophilic elastomeric fibrous component, and wherein the super absorbent component is present in an amount from about 1% (w/w) to about 85% (w/w). 30. The non-woven liquid entrapping device of claim 29, wherein the hydrophilic elastomeric fibrous component is selected from zein protein, polyester elastomers, polydimethylsiloxane, hydrophilic poly(ether-co-ester) elastomers, silicone-co-polyethyleneglycol elastomers, polyacrylates, thermoplastic polyurethanes, poly(ether-co-urethanes), and any combination thereof. 31. The non-woven liquid entrapping device of claim 29, wherein the absorbent component is present in an amount from about 5% (w/w) to about 50% (w/w). 32. The non-woven liquid entrapping device of claim 29, wherein the absorbent component is present in an amount from about 30% (w/w) to about 50% (w/w). 33. The non-woven liquid entrapping device of claim 29, wherein the hydrophilic elastomeric fibrous component is selected from polyurethanes, poly ether-co-urethanes, and any combination thereof. 34. The non-woven liquid entrapping device of claim 29, wherein the liquid entrapping device comprises a device selected from a diaper, a tampon, a sanitary napkin, a sanitary wipe, a spill absorbing device, a mop head, and a floor waxing device. 35. The non-woven liquid entrapping device of claim 29, wherein the nanofibers are electrospun nanofibers having a fiber diameter of about 1 nanometer to about 3,000 nanometers. 36. The non-woven liquid entrapping device of claim 29, wherein the nanofibers are electrospun nanofibers having a fiber diameter of about 10 nanometers to about 2,000 nanometers. 37. A non-woven liquid entrapping device comprising:
an absorbent component; and a hydrophilic elastomeric fibrous component, wherein the absorbent component and the hydrophilic elastomeric fibrous component are in physical proximity thereby resulting in fluid communication, wherein the absorbent component is more absorbent than the hydrophilic elastomeric fibrous component, but wherein the hydrophilic elastomeric fibrous component absorbs more quickly than and has a smaller holding capacity than the absorbent component, wherein the non-woven liquid entrapping device, including the hydrophilic elastomeric fibrous component, is formed from at least one electrospun nanofiber where the at least one electrospun nanofiber comprises both the absorbent component and the hydrophilic elastomeric fibrous component in the electrospun nanofiber body, wherein the absorbent component is mechanically entangled by the electrospun hydrophilic elastomeric fibrous component, wherein the non-woven liquid entrapping device, including the hydrophilic elastomeric fibrous component, is formed from nanofibers having a fiber diameter of about 1 nanometer to about 3,000 nanometers, and wherein the absorbent component is capable of holding at least about 50 times its own weight in liquid. 38. The non-woven liquid entrapping device of claim 37, wherein the hydrophilic elastomeric fibrous component is selected from zein protein, polyester elastomers, polydimethylsiloxane, hydrophilic poly(ether-co-ester) elastomers, silicone-co-polyethyleneglycol elastomers, polyacrylates, thermoplastic polyurethanes, poly(ether-co-urethanes), and any combination thereof. 39. The non-woven liquid entrapping device of claim 37, wherein the absorbent component is present in an amount from about 5% (w/w) to about 50% (w/w). 40. The non-woven liquid entrapping device of claim 37, wherein the absorbent component is present in an amount from about 30% (w/w) to about 50% (w/w). 41. The non-woven liquid entrapping device of claim 37, wherein the hydrophilic elastomeric fibrous component is selected from polyurethanes, poly ether-co-urethanes, and any combination thereof. 42. The non-woven liquid entrapping device of claim 37, wherein the liquid entrapping device comprises a device selected from a diaper, a tampon, a sanitary napkin, a sanitary wipe, a spill absorbing device, a mop head, and a floor waxing device. 43. The non-woven liquid entrapping device of claim 37, wherein the nanofibers are electrospun nanofibers having a fiber diameter of about 10 nanometers to about 2,000 nanometers. | 1,700 |
3,436 | 15,110,418 | 1,793 | A freeform fabrication system for the production of an edible three-dimensional food product from digital input data is disclosed. Food products are produced in a layer-by-layer manner without object-specific tooling or human intervention. Color, flavor, texture and/or other characteristics may be independently modulated throughout the food product. In addition, in some cases, the food products may further undergo one or more post-processing steps. | 1. A method for making an edible component comprising:
depositing successive layers of a food material according to digital data that describes the edible component; and applying to one or more regions of the successive layers of food material one or more edible binders that bond the food material at said one or more regions to form said edible component,
wherein the food material comprises 25-75% by weight polysaccharide and 25-75% by weight monosaccharide and/or disaccharide, based on the total weight of the food material. 2. The method of claim 1, wherein the polysaccharide comprises a starch or modified starch. 3. The method of claim 2, wherein the modified starch is a modified food starch. 4. The method of claim 1, wherein the polysaccharide comprises maltodextrin. 5. The method of claim 1, wherein the monosaccharide and/or disaccharide comprises fructose, glucose, sucrose, or a combination thereof. 6. The method of claim 1, wherein the monosaccharide and/or disaccharide comprises confectioner's sugar. 7. The method of claim 1, wherein the monosaccharide and/or disaccharide comprises fructose. 8. The method of claim 1, wherein the food material further comprises 1-30% by weight sugar alcohol, based on the total weight of the food material. 9. The method of claim 8, wherein the sugar alcohol comprises one or more of glycerol, erythritol, xylitol, mannitol, sorbitol, inositol, volemitol, isomalt, maltitol, and lactitol. 10. The method of claim 1, wherein the edible component exhibits a flexural strength between about 0.5 MPa and about 2.0 MPa, when measured according to ASTM D790. 11. The method of claim 1, wherein the food material further comprises one or more flavorants. 12. The method of claim 1, wherein the digital data describes sequential cross-sectional layers of the edible component, the cross-sectional layers comprising a plurality of voxels. 13. The method of claim 12, wherein the sequential cross-sectional layers are generated from CAD data. 14. The method of claim 12, wherein the plurality of voxels vary in food material composition, color, flavor, or a combination thereof. 15. The method of claim 1, wherein one or more edible binders are applied to one or more regions of each of the successive layers of food material. 16. The method of claim 1, wherein unbound food material supports the edible component during formation of the edible component. 17. The method of claim 1 further comprising infiltrating the edible component with an infiltrant. 18. A method for making an edible component comprising:
depositing successive layers of a food material according to digital data that describes the edible component; and applying to one or more regions of the successive layers of food material one or more edible binders that bond the food material at said one or more regions to form said edible component,
wherein the food material comprises 1-25% by weight seed crystals. 19. The method of claim 18, wherein the seed crystals comprise cocoa butter seed crystals. 20. The method of claim 18, wherein the cocoa butter seed crystals have a Type V crystal structure. | A freeform fabrication system for the production of an edible three-dimensional food product from digital input data is disclosed. Food products are produced in a layer-by-layer manner without object-specific tooling or human intervention. Color, flavor, texture and/or other characteristics may be independently modulated throughout the food product. In addition, in some cases, the food products may further undergo one or more post-processing steps.1. A method for making an edible component comprising:
depositing successive layers of a food material according to digital data that describes the edible component; and applying to one or more regions of the successive layers of food material one or more edible binders that bond the food material at said one or more regions to form said edible component,
wherein the food material comprises 25-75% by weight polysaccharide and 25-75% by weight monosaccharide and/or disaccharide, based on the total weight of the food material. 2. The method of claim 1, wherein the polysaccharide comprises a starch or modified starch. 3. The method of claim 2, wherein the modified starch is a modified food starch. 4. The method of claim 1, wherein the polysaccharide comprises maltodextrin. 5. The method of claim 1, wherein the monosaccharide and/or disaccharide comprises fructose, glucose, sucrose, or a combination thereof. 6. The method of claim 1, wherein the monosaccharide and/or disaccharide comprises confectioner's sugar. 7. The method of claim 1, wherein the monosaccharide and/or disaccharide comprises fructose. 8. The method of claim 1, wherein the food material further comprises 1-30% by weight sugar alcohol, based on the total weight of the food material. 9. The method of claim 8, wherein the sugar alcohol comprises one or more of glycerol, erythritol, xylitol, mannitol, sorbitol, inositol, volemitol, isomalt, maltitol, and lactitol. 10. The method of claim 1, wherein the edible component exhibits a flexural strength between about 0.5 MPa and about 2.0 MPa, when measured according to ASTM D790. 11. The method of claim 1, wherein the food material further comprises one or more flavorants. 12. The method of claim 1, wherein the digital data describes sequential cross-sectional layers of the edible component, the cross-sectional layers comprising a plurality of voxels. 13. The method of claim 12, wherein the sequential cross-sectional layers are generated from CAD data. 14. The method of claim 12, wherein the plurality of voxels vary in food material composition, color, flavor, or a combination thereof. 15. The method of claim 1, wherein one or more edible binders are applied to one or more regions of each of the successive layers of food material. 16. The method of claim 1, wherein unbound food material supports the edible component during formation of the edible component. 17. The method of claim 1 further comprising infiltrating the edible component with an infiltrant. 18. A method for making an edible component comprising:
depositing successive layers of a food material according to digital data that describes the edible component; and applying to one or more regions of the successive layers of food material one or more edible binders that bond the food material at said one or more regions to form said edible component,
wherein the food material comprises 1-25% by weight seed crystals. 19. The method of claim 18, wherein the seed crystals comprise cocoa butter seed crystals. 20. The method of claim 18, wherein the cocoa butter seed crystals have a Type V crystal structure. | 1,700 |
3,437 | 12,019,445 | 1,797 | A composition, method and device for the preparation of biological samples for subsequent LC-MS analysis using a combined and concurrent protein precipitation and solid phase extraction (SPE) process is described. Through an integrated combination of protein precipitation, filtration, and SPE using a novel zirconia-coated chromatographic media, interfering compounds, such as proteins and phosphate-containing compounds, are eliminated from the biological samples, affording a higher degree of analyte response during LC-MS analysis. | 1. A solid phase extraction (SPE) media for the selective removal of phosphate-containing compounds from a biological composition prior to bioanalytical analysis, the SPE media comprising:
a. a substrate; and, b. a transition metal oxide bonded onto the substrate. 2. The SPE media of claim 1, wherein the substrate is selected from the group comprised of porous silica, porous alumina, non-porous silica, non-porous alumina, carbon, zirconia, diatomaceous earth, controlled pore glass, porous polymer, and combinations thereof. 3. The SPE media of claim 1, wherein the particle size of the substrate ranges between about 10 nm and about 1000 μm. 4. The SPE media of claim 1, wherein the particle size of the substrate ranges between about 5 μm and about 70 μm. 5. The SPE media of claim 1, wherein the pore size of the substrate ranges between about 30 Å and about 1000 Å. 6. The SPE media of claim 1, wherein the pore size of the substrate ranges between about 60 Å and about 400 Å. 7. The SPE media of claim 1, wherein the surface area of the substrate ranges between about 5 m2/g and about 1000 m2/g. 8. The SPE media of claim 1, wherein the surface area of the substrate ranges between about 100 m2/g and about 600 m2/g. 9. The SPE media of claim 1, wherein the transitional metal oxide bonded to the substrate is selected from the group consisting of zirconia, titania, ceria, and combinations thereof. 10. A solid phase extraction (SPE) media for the selective removal of phosphate-containing compounds from a biological composition prior to bioanalytical analysis, the SPE media comprising:
a. a porous silica substrate with a particle size ranging between about 10 nm and about 1000 μm, a pore size ranging between about 30 Å and about 1000 Å, and a surface area ranging between about 5 m2/g and about 1000 m2/g; and, b. zirconia bonded onto the outer surface of the silica substrate. 11. The SPE media of claim 10, wherein the particle size of the substrate ranges between about 5 μm and about 70 μm. 12. The SPE media of claim 10, wherein the pore size of the substrate ranges between about 60 Å and about 400 Å. 13. The SPE media of claim 10, wherein the surface area of the substrate ranges between about 100 m2/g and about 600 m2/g. 14. The SPE media of claim 10, wherein the media is comprised of porous silica particles bonded to a transition metal oxide selected from the group consisting of zirconia, titania, ceria, and combinations thereof. 15. A method of bonding a transition metal oxide to a substrate, yielding a solid phase extraction media possessing a selective binding affinity for phosphate-containing compounds in aqueous solution, the method comprising:
a. drying the substrate to a constant weight; b. combining a transition metal alkoxide with the substrate, at an alkoxide:substrate molar ratio ranging between about 0.1 and about 10, in an excess of anhydrous solvent, and heating the reaction mixture to a temperature ranging between about 50° C. and about 120° C. for a period of time ranging between about 4 hours and about 24 hours; and, c. terminating the transition metal alkoxide-substrate reaction and removing excess reactants and byproducts, yielding a bonded transition metal-substrate composition. 16. The method of claim 15, wherein the substrate particles are made from materials selected from the group comprised of porous silica, porous alumina, non-porous silica, non-porous alumina, carbon, zirconia, diatomaceous earth, controlled pore glass, porous polymer, and combinations thereof. 17. The method of claim 15, wherein the substrate materials are dried using methods selected from room temperature drying, oven drying, vacuum oven drying, azeotropic drying, and combinations thereof. 18. The method of claim 15, wherein the substrate particles are dried to constant weight using a vacuum oven at a temperature ranging between about 30° C. and about 300° C. 19. The method of claim 15, wherein the substrate particles are dried azeotropically by adding the substrate particles to HPLC-grade toluene in a round bottom flask with a Dean Stark trap attached, heating the mixture to a temperature ranging between about 100° C. and 140° C., and then draining the flask through the Dean Stark trap, repeating the process up to 5 times. 20. The method of claim 15, wherein the transition metal alkoxide is selected from the group comprised of zirconium butoxide, zirconium ethoxide, zirconium isopropoxide, zirconium methoxide, titanium butoxide, titanium ethoxide, titanium isopropoxide, titanium methoxide, cerium butoxide, cerium ethoxide, cerium isopropoxide, cerium methoxide, and combinations thereof. 21. The method of claim 15, wherein the anhydrous solvent is selected from the group comprising anhydrous toluene, 1,2-dichloroethane, 1-methyl-2-pyrrolidinone, acetonitrile, benzene, butyl ether, chloroform, dimethyl sulfoxide, ethyl acetate, heptane, isopropyl alcohol, methyl alcohol, methylene chloride, N,N-dimethylacetamide, N,N-dimethylformamide, p-dioxane, pentane, petroleum ether, pyridine, tetrahydrofuran, xylene, ethyl benzene, and combinations thereof. 22. The method of claim 15, wherein the transition metal alkoxide is added to the substrate at an alkoxide:substrate molar ratio ranging between about 0.5 and about 3. 23. The method of claim 15, wherein the mixture is heated for a time period ranging between about 8 hours and about 16 hours. 24. The method of claim 15, wherein the reaction is terminated by hydrolysis in an aqueous environment using an organic or inorganic acid at a concentration of no more than 10% and a temperature ranging between about 20° C. and about 150° C. 25. The method of claim 15, wherein the reaction is terminated by hydrolysis in an aqueous environment using an organic or inorganic acid at a concentration of no more than about 5% and a temperature ranging between about 20° C. and about 100° C. 26. The method of claim 15, wherein the bonded transition metal-substrate composition is separated from the solvents and excess reactants by filtration through a sintered-glass Buchner funnel with a pore size ranging between about 10 μm and about 100 μm. 27. The method of claim 15, wherein the excess reactants and byproducts are removed using solvent extraction methods. 28. The method of claim 15, wherein the bonded transition metal-substrate composition is dried to constant weight in a vacuum oven at a temperature ranging between about 20° C. and about 150° C. 29. The method of claim 15, wherein the bonded transition metal-substrate composition is dried to constant weight in a vacuum oven at a temperature ranging between about 50° C. and about 150° C. 30. A method of bonding zirconia to porous silica, yielding a solid phase extraction media possessing a selective binding affinity for phosphate-containing compounds in aqueous solution, the method comprising:
a. drying the porous silica particles to constant weight in a vacuum oven at a temperature ranging between about 30° C. and about 300° C.; b. azeotropically drying the oven-dried porous silica particles by adding the particles to HPLC-grade toluene in a round bottom flask with a Dean Stark trap attached, heating the mixture to a temperature of about 112° C., and then draining the flask through the Dean Stark trap, repeating the process up to 5 times; c. combining the porous silica particles with zirconium alkoxide at a molar ratio ranging between about 0.5 and about 3.0 moles of zirconium alkoxide per mole of porous silica, in an excess of anhydrous solvent, forming a reaction mixture; d. heating the reaction mixture to a temperature ranging between about 50° C. and about 120° C. for a period of time ranging between about 8 hours and about 16 hours; e. terminating the reaction by hydrolysis in an aqueous environment using an organic or inorganic acid at a concentration of no more than about 5% and a temperature ranging between about 20° C. and about 100° C.; f. cooling and then filtering the reaction mixture; g. removing unreacted zirconium alkoxide from the reaction mixture by solvent extraction; h. washing the zirconia-coated silica particles; and, i. drying the washed zirconia-coated silica particles in a vacuum oven at a temperature ranging between about 50° C. and about 120° C. to constant weight. 31. The method of claim 30, wherein the particle size of the porous silica particles ranges between about 5 μm and about 70 μm. 32. The method of claim 30, wherein the pore size of the porous silica particles ranges between about 60 Å and about 400 Å. 33. The method of claim 30, wherein the surface area of the porous silica particles ranges between about 100 m2/g and about 600 m2/g. 34. The method of claim 30, wherein the zirconium alkoxide is selected from the group comprised of zirconium butoxide, zirconium ethoxide, zirconium isopropoxide, zirconium methoxide, and combinations thereof. 35. A method for the selective removal of interfering components from a biological composition prior to bioanalytical analysis, the method comprising:
a. mixing a biological sample with an organic acid in solution with a protein precipitating agent to form a biological composition with precipitated proteins; b. separating the precipitated proteins from the biological composition; and, c. contacting the biological composition with a transition metal oxide, resulting in an eluate. 36. The method of claim 35, wherein the organic acid is selected from the list comprised of formic acid, acetic acid, citric acid, oxalic acid, maleic acid, malic acid, pyromellitic acid, and combinations thereof. 37. The method of claim 35, wherein the protein precipitating agent is selected from the list comprised of acetonitrile, formic acid, acetic acid, trichloroacetic acid, acetone, ethanol, hydrochloric acid, methanol, chloroform, ammonium sulfate, sodium citrate, sulfuric acid, polyethylene glycol, dextran, alginate, carboxymethycellulose, polyacrylic acid, tannic acid, polyphosphates, potassium chloride, ethanol, zinc chloride, t-butanol, and combinations thereof. 38. The method of claim 35, wherein the organic acid is in solution with the protein precipitating agent at a concentration of no more than about 5% by volume. 39. The method of claim 35, wherein the organic acid/protein precipitation agent solution is mixed with the biological sample at a solution:sample volume ratio ranging between about 2:1 and about 5:1. 40. The method of claim 35, wherein the precipitated proteins are separated from the biological composition using techniques from the list comprising centrifugation, filtration, and combinations thereof. 41. The method of claim 35, wherein the precipitated proteins are separated from the biological composition by centrifugation, and the supernate of the biological composition is contacted with the transition metal oxide. 42. The method of claim 35, wherein the precipitated proteins are separated from the biological composition using filtration, and the filtrate of the biological composition is contacted with the transition metal oxide. 43. The method of claim 35, wherein the transition metal oxide is selected from the list comprised of zirconia, titania, ceria, and combinations thereof. 44. The method of claim 35, wherein the transition metal oxide is zirconia bonded to porous silica substrate particles. 45. The method of claim 35, wherein the eluate is essentially free of interfering components selected from the group comprising phosphate-containing compounds, proteins, and combinations thereof. 46. The method of claim 35, wherein the eluate is subjected to LC-MS or LC-MS-MS measurements to determine the presence of analytes. 47. A method for the selective removal of interfering components from a biological composition prior to bioanalytical analysis, the method comprising:
a. mixing a biological sample with formic acid in solution with acetonitrile at a percent acid concentration ranging between about 0% and about 2%, and at a acid/acetonitrile:sample volume ratio ranging between about 2:1 and about 5:1; b. centrifuging the biological composition to form precipitated proteins and supernate; and, c. passing the supernate through a SPE cartridge with a volume ranging between about 0.5 ml and about 60 ml having zirconia-bonded silica particles packed between an upper PTFE frit with a nominal porosity of 5 μm and a lower filter with a nominal porosity of 0.2 μm to separate phosphate-containing interfering components from the supernate, resulting in an eluate essentially free of interfering components. 48. The method of claim 47, wherein the formic acid is in solution with the acetonitrile at an acid concentration of about 1% by volume. 49. The method of claim 47, wherein the formic acid/acetonitrile solution is mixed with the biological sample at a solution:sample volume ratio of about 3:1. 50. The method of claim 47, wherein the transition metal oxide is selected from the list comprised of zirconia, titania, ceria, and combinations thereof. 51. The method of claim 47, wherein the eluate is subjected to LC-MS or LC-MS-MS measurements to determine the presence of analytes. 52. The method of claim 47, wherein the SPE cartridge has a volume of 1 ml, 3 ml, or 6 ml. 53. The method of claim 47, wherein the cartridge is a well in a 96 well tray with a headspace volume capacity ranging between about 0.5 ml and about 2 ml. 54. A method for the selective removal of interfering components from a biological sample prior to bioanalytical analysis, the method comprising:
a. mixing a biological sample with formic acid in solution with acetonitrile at a percent acid concentration ranging between about 0% and about 2%, and at a acid/acetonitrile:sample volume ratio ranging between about 2:1 and about 5:1, forming a biological composition; and, b. passing the biological composition through a SPE cartridge with a volume ranging between about 0.5 ml and about 60 ml having zirconia-bonded silica particles packed between an upper PTFE frit with a nominal porosity of 5 μm and a lower filter with a nominal porosity of 0.2 μm to separate phosphate-containing interfering components from the supernate, resulting in an eluate essentially free of interfering components. 55. The method of claim 54, wherein the formic acid is in solution with the acetonitrile at an acid concentration of about 1% by volume. 56. The method of claim 54, wherein the formic acid/acetonitrile solution is mixed with the biological sample at a solution:sample volume ratio of about 3:1. 57. The method of claim 54, wherein the eluate is subjected to LC-MS or LC-MS-MS measurements to determine the presence of analytes. 58. The method of claim 54, wherein the SPE cartridge has a volume of 1 ml, 3 ml, or 6 ml. 59. The method of claim 54, wherein the cartridge is a 1 ml well in a 96 well tray. 60. A system for the selective removal of interfering components from a biological composition prior to bioanalytical analysis, the system comprising:
a. at least one cartridge having a volume ranging between about 0.5 ml and about 60 ml, the cartridge having; b. a top filter with a porosity ranging between about 0.1 μm and about 50 μm inside the cartridge near the cartridge entrance; c. a bottom filter with a porosity ranging between about 0.1 μm and about 50 μm inside the cartridge near the cartridge exit; and, d. a transition metal oxide bonded to substrate particles packed inside of the cartridge between the top filter/frit and the bottom filter. 61. The system of claim 60, wherein the lower filter is a filter possessing a nominal porosity of about 0.2 μm. 62. The system of claim 60, wherein the upper filter is a PTFE frit with a nominal porosity of about 5 μm. 63. The system of claim 60, wherein the transition metal oxide is selected from the list comprised of zirconia, titania, ceria, and combinations thereof. 64. The system of claim 60, wherein the transition metal oxide is zirconia bonded to porous silica particles. 65. The system of claim 60, wherein the cartridge is a 1 ml syringe barrel. 66. The system of claim 60, wherein the system includes a 96 well tray with well headspace volume capacities ranging between about 0.5 ml and about 2 ml. 67. The system of claim 60, wherein the system includes a LC-MS or LC-MS-MS measurement apparatus. 68. A system for the selective removal of interfering components from a biological composition prior to bioanalytical analysis, the system comprising:
a. a cartridge having a volume of about 1 ml; b. a top PTFE filter with a porosity of about 5 μm inside the cartridge near the cartridge entrance; c. a bottom filter with a porosity of about 0.2 μm inside the cartridge near the cartridge exit; and, d. a quantity of zirconia bonded to porous silica particles, with a mass ranging between about 20 mg and about 80 mg, packed inside of the cartridge between the top filter/frit and the bottom filter. 69. The system of claim 68, wherein the cartridge is packed with about 50 mg of zirconia bonded to porous silica particles between the upper frit and the lower filter. 70. The system of claim 68, wherein the cartridge is a 1 ml syringe barrel. 71. The system of claim 68, wherein the system includes a 96 well tray with well headspace volume capacities ranging between about 0.5 ml and about 2 ml. | A composition, method and device for the preparation of biological samples for subsequent LC-MS analysis using a combined and concurrent protein precipitation and solid phase extraction (SPE) process is described. Through an integrated combination of protein precipitation, filtration, and SPE using a novel zirconia-coated chromatographic media, interfering compounds, such as proteins and phosphate-containing compounds, are eliminated from the biological samples, affording a higher degree of analyte response during LC-MS analysis.1. A solid phase extraction (SPE) media for the selective removal of phosphate-containing compounds from a biological composition prior to bioanalytical analysis, the SPE media comprising:
a. a substrate; and, b. a transition metal oxide bonded onto the substrate. 2. The SPE media of claim 1, wherein the substrate is selected from the group comprised of porous silica, porous alumina, non-porous silica, non-porous alumina, carbon, zirconia, diatomaceous earth, controlled pore glass, porous polymer, and combinations thereof. 3. The SPE media of claim 1, wherein the particle size of the substrate ranges between about 10 nm and about 1000 μm. 4. The SPE media of claim 1, wherein the particle size of the substrate ranges between about 5 μm and about 70 μm. 5. The SPE media of claim 1, wherein the pore size of the substrate ranges between about 30 Å and about 1000 Å. 6. The SPE media of claim 1, wherein the pore size of the substrate ranges between about 60 Å and about 400 Å. 7. The SPE media of claim 1, wherein the surface area of the substrate ranges between about 5 m2/g and about 1000 m2/g. 8. The SPE media of claim 1, wherein the surface area of the substrate ranges between about 100 m2/g and about 600 m2/g. 9. The SPE media of claim 1, wherein the transitional metal oxide bonded to the substrate is selected from the group consisting of zirconia, titania, ceria, and combinations thereof. 10. A solid phase extraction (SPE) media for the selective removal of phosphate-containing compounds from a biological composition prior to bioanalytical analysis, the SPE media comprising:
a. a porous silica substrate with a particle size ranging between about 10 nm and about 1000 μm, a pore size ranging between about 30 Å and about 1000 Å, and a surface area ranging between about 5 m2/g and about 1000 m2/g; and, b. zirconia bonded onto the outer surface of the silica substrate. 11. The SPE media of claim 10, wherein the particle size of the substrate ranges between about 5 μm and about 70 μm. 12. The SPE media of claim 10, wherein the pore size of the substrate ranges between about 60 Å and about 400 Å. 13. The SPE media of claim 10, wherein the surface area of the substrate ranges between about 100 m2/g and about 600 m2/g. 14. The SPE media of claim 10, wherein the media is comprised of porous silica particles bonded to a transition metal oxide selected from the group consisting of zirconia, titania, ceria, and combinations thereof. 15. A method of bonding a transition metal oxide to a substrate, yielding a solid phase extraction media possessing a selective binding affinity for phosphate-containing compounds in aqueous solution, the method comprising:
a. drying the substrate to a constant weight; b. combining a transition metal alkoxide with the substrate, at an alkoxide:substrate molar ratio ranging between about 0.1 and about 10, in an excess of anhydrous solvent, and heating the reaction mixture to a temperature ranging between about 50° C. and about 120° C. for a period of time ranging between about 4 hours and about 24 hours; and, c. terminating the transition metal alkoxide-substrate reaction and removing excess reactants and byproducts, yielding a bonded transition metal-substrate composition. 16. The method of claim 15, wherein the substrate particles are made from materials selected from the group comprised of porous silica, porous alumina, non-porous silica, non-porous alumina, carbon, zirconia, diatomaceous earth, controlled pore glass, porous polymer, and combinations thereof. 17. The method of claim 15, wherein the substrate materials are dried using methods selected from room temperature drying, oven drying, vacuum oven drying, azeotropic drying, and combinations thereof. 18. The method of claim 15, wherein the substrate particles are dried to constant weight using a vacuum oven at a temperature ranging between about 30° C. and about 300° C. 19. The method of claim 15, wherein the substrate particles are dried azeotropically by adding the substrate particles to HPLC-grade toluene in a round bottom flask with a Dean Stark trap attached, heating the mixture to a temperature ranging between about 100° C. and 140° C., and then draining the flask through the Dean Stark trap, repeating the process up to 5 times. 20. The method of claim 15, wherein the transition metal alkoxide is selected from the group comprised of zirconium butoxide, zirconium ethoxide, zirconium isopropoxide, zirconium methoxide, titanium butoxide, titanium ethoxide, titanium isopropoxide, titanium methoxide, cerium butoxide, cerium ethoxide, cerium isopropoxide, cerium methoxide, and combinations thereof. 21. The method of claim 15, wherein the anhydrous solvent is selected from the group comprising anhydrous toluene, 1,2-dichloroethane, 1-methyl-2-pyrrolidinone, acetonitrile, benzene, butyl ether, chloroform, dimethyl sulfoxide, ethyl acetate, heptane, isopropyl alcohol, methyl alcohol, methylene chloride, N,N-dimethylacetamide, N,N-dimethylformamide, p-dioxane, pentane, petroleum ether, pyridine, tetrahydrofuran, xylene, ethyl benzene, and combinations thereof. 22. The method of claim 15, wherein the transition metal alkoxide is added to the substrate at an alkoxide:substrate molar ratio ranging between about 0.5 and about 3. 23. The method of claim 15, wherein the mixture is heated for a time period ranging between about 8 hours and about 16 hours. 24. The method of claim 15, wherein the reaction is terminated by hydrolysis in an aqueous environment using an organic or inorganic acid at a concentration of no more than 10% and a temperature ranging between about 20° C. and about 150° C. 25. The method of claim 15, wherein the reaction is terminated by hydrolysis in an aqueous environment using an organic or inorganic acid at a concentration of no more than about 5% and a temperature ranging between about 20° C. and about 100° C. 26. The method of claim 15, wherein the bonded transition metal-substrate composition is separated from the solvents and excess reactants by filtration through a sintered-glass Buchner funnel with a pore size ranging between about 10 μm and about 100 μm. 27. The method of claim 15, wherein the excess reactants and byproducts are removed using solvent extraction methods. 28. The method of claim 15, wherein the bonded transition metal-substrate composition is dried to constant weight in a vacuum oven at a temperature ranging between about 20° C. and about 150° C. 29. The method of claim 15, wherein the bonded transition metal-substrate composition is dried to constant weight in a vacuum oven at a temperature ranging between about 50° C. and about 150° C. 30. A method of bonding zirconia to porous silica, yielding a solid phase extraction media possessing a selective binding affinity for phosphate-containing compounds in aqueous solution, the method comprising:
a. drying the porous silica particles to constant weight in a vacuum oven at a temperature ranging between about 30° C. and about 300° C.; b. azeotropically drying the oven-dried porous silica particles by adding the particles to HPLC-grade toluene in a round bottom flask with a Dean Stark trap attached, heating the mixture to a temperature of about 112° C., and then draining the flask through the Dean Stark trap, repeating the process up to 5 times; c. combining the porous silica particles with zirconium alkoxide at a molar ratio ranging between about 0.5 and about 3.0 moles of zirconium alkoxide per mole of porous silica, in an excess of anhydrous solvent, forming a reaction mixture; d. heating the reaction mixture to a temperature ranging between about 50° C. and about 120° C. for a period of time ranging between about 8 hours and about 16 hours; e. terminating the reaction by hydrolysis in an aqueous environment using an organic or inorganic acid at a concentration of no more than about 5% and a temperature ranging between about 20° C. and about 100° C.; f. cooling and then filtering the reaction mixture; g. removing unreacted zirconium alkoxide from the reaction mixture by solvent extraction; h. washing the zirconia-coated silica particles; and, i. drying the washed zirconia-coated silica particles in a vacuum oven at a temperature ranging between about 50° C. and about 120° C. to constant weight. 31. The method of claim 30, wherein the particle size of the porous silica particles ranges between about 5 μm and about 70 μm. 32. The method of claim 30, wherein the pore size of the porous silica particles ranges between about 60 Å and about 400 Å. 33. The method of claim 30, wherein the surface area of the porous silica particles ranges between about 100 m2/g and about 600 m2/g. 34. The method of claim 30, wherein the zirconium alkoxide is selected from the group comprised of zirconium butoxide, zirconium ethoxide, zirconium isopropoxide, zirconium methoxide, and combinations thereof. 35. A method for the selective removal of interfering components from a biological composition prior to bioanalytical analysis, the method comprising:
a. mixing a biological sample with an organic acid in solution with a protein precipitating agent to form a biological composition with precipitated proteins; b. separating the precipitated proteins from the biological composition; and, c. contacting the biological composition with a transition metal oxide, resulting in an eluate. 36. The method of claim 35, wherein the organic acid is selected from the list comprised of formic acid, acetic acid, citric acid, oxalic acid, maleic acid, malic acid, pyromellitic acid, and combinations thereof. 37. The method of claim 35, wherein the protein precipitating agent is selected from the list comprised of acetonitrile, formic acid, acetic acid, trichloroacetic acid, acetone, ethanol, hydrochloric acid, methanol, chloroform, ammonium sulfate, sodium citrate, sulfuric acid, polyethylene glycol, dextran, alginate, carboxymethycellulose, polyacrylic acid, tannic acid, polyphosphates, potassium chloride, ethanol, zinc chloride, t-butanol, and combinations thereof. 38. The method of claim 35, wherein the organic acid is in solution with the protein precipitating agent at a concentration of no more than about 5% by volume. 39. The method of claim 35, wherein the organic acid/protein precipitation agent solution is mixed with the biological sample at a solution:sample volume ratio ranging between about 2:1 and about 5:1. 40. The method of claim 35, wherein the precipitated proteins are separated from the biological composition using techniques from the list comprising centrifugation, filtration, and combinations thereof. 41. The method of claim 35, wherein the precipitated proteins are separated from the biological composition by centrifugation, and the supernate of the biological composition is contacted with the transition metal oxide. 42. The method of claim 35, wherein the precipitated proteins are separated from the biological composition using filtration, and the filtrate of the biological composition is contacted with the transition metal oxide. 43. The method of claim 35, wherein the transition metal oxide is selected from the list comprised of zirconia, titania, ceria, and combinations thereof. 44. The method of claim 35, wherein the transition metal oxide is zirconia bonded to porous silica substrate particles. 45. The method of claim 35, wherein the eluate is essentially free of interfering components selected from the group comprising phosphate-containing compounds, proteins, and combinations thereof. 46. The method of claim 35, wherein the eluate is subjected to LC-MS or LC-MS-MS measurements to determine the presence of analytes. 47. A method for the selective removal of interfering components from a biological composition prior to bioanalytical analysis, the method comprising:
a. mixing a biological sample with formic acid in solution with acetonitrile at a percent acid concentration ranging between about 0% and about 2%, and at a acid/acetonitrile:sample volume ratio ranging between about 2:1 and about 5:1; b. centrifuging the biological composition to form precipitated proteins and supernate; and, c. passing the supernate through a SPE cartridge with a volume ranging between about 0.5 ml and about 60 ml having zirconia-bonded silica particles packed between an upper PTFE frit with a nominal porosity of 5 μm and a lower filter with a nominal porosity of 0.2 μm to separate phosphate-containing interfering components from the supernate, resulting in an eluate essentially free of interfering components. 48. The method of claim 47, wherein the formic acid is in solution with the acetonitrile at an acid concentration of about 1% by volume. 49. The method of claim 47, wherein the formic acid/acetonitrile solution is mixed with the biological sample at a solution:sample volume ratio of about 3:1. 50. The method of claim 47, wherein the transition metal oxide is selected from the list comprised of zirconia, titania, ceria, and combinations thereof. 51. The method of claim 47, wherein the eluate is subjected to LC-MS or LC-MS-MS measurements to determine the presence of analytes. 52. The method of claim 47, wherein the SPE cartridge has a volume of 1 ml, 3 ml, or 6 ml. 53. The method of claim 47, wherein the cartridge is a well in a 96 well tray with a headspace volume capacity ranging between about 0.5 ml and about 2 ml. 54. A method for the selective removal of interfering components from a biological sample prior to bioanalytical analysis, the method comprising:
a. mixing a biological sample with formic acid in solution with acetonitrile at a percent acid concentration ranging between about 0% and about 2%, and at a acid/acetonitrile:sample volume ratio ranging between about 2:1 and about 5:1, forming a biological composition; and, b. passing the biological composition through a SPE cartridge with a volume ranging between about 0.5 ml and about 60 ml having zirconia-bonded silica particles packed between an upper PTFE frit with a nominal porosity of 5 μm and a lower filter with a nominal porosity of 0.2 μm to separate phosphate-containing interfering components from the supernate, resulting in an eluate essentially free of interfering components. 55. The method of claim 54, wherein the formic acid is in solution with the acetonitrile at an acid concentration of about 1% by volume. 56. The method of claim 54, wherein the formic acid/acetonitrile solution is mixed with the biological sample at a solution:sample volume ratio of about 3:1. 57. The method of claim 54, wherein the eluate is subjected to LC-MS or LC-MS-MS measurements to determine the presence of analytes. 58. The method of claim 54, wherein the SPE cartridge has a volume of 1 ml, 3 ml, or 6 ml. 59. The method of claim 54, wherein the cartridge is a 1 ml well in a 96 well tray. 60. A system for the selective removal of interfering components from a biological composition prior to bioanalytical analysis, the system comprising:
a. at least one cartridge having a volume ranging between about 0.5 ml and about 60 ml, the cartridge having; b. a top filter with a porosity ranging between about 0.1 μm and about 50 μm inside the cartridge near the cartridge entrance; c. a bottom filter with a porosity ranging between about 0.1 μm and about 50 μm inside the cartridge near the cartridge exit; and, d. a transition metal oxide bonded to substrate particles packed inside of the cartridge between the top filter/frit and the bottom filter. 61. The system of claim 60, wherein the lower filter is a filter possessing a nominal porosity of about 0.2 μm. 62. The system of claim 60, wherein the upper filter is a PTFE frit with a nominal porosity of about 5 μm. 63. The system of claim 60, wherein the transition metal oxide is selected from the list comprised of zirconia, titania, ceria, and combinations thereof. 64. The system of claim 60, wherein the transition metal oxide is zirconia bonded to porous silica particles. 65. The system of claim 60, wherein the cartridge is a 1 ml syringe barrel. 66. The system of claim 60, wherein the system includes a 96 well tray with well headspace volume capacities ranging between about 0.5 ml and about 2 ml. 67. The system of claim 60, wherein the system includes a LC-MS or LC-MS-MS measurement apparatus. 68. A system for the selective removal of interfering components from a biological composition prior to bioanalytical analysis, the system comprising:
a. a cartridge having a volume of about 1 ml; b. a top PTFE filter with a porosity of about 5 μm inside the cartridge near the cartridge entrance; c. a bottom filter with a porosity of about 0.2 μm inside the cartridge near the cartridge exit; and, d. a quantity of zirconia bonded to porous silica particles, with a mass ranging between about 20 mg and about 80 mg, packed inside of the cartridge between the top filter/frit and the bottom filter. 69. The system of claim 68, wherein the cartridge is packed with about 50 mg of zirconia bonded to porous silica particles between the upper frit and the lower filter. 70. The system of claim 68, wherein the cartridge is a 1 ml syringe barrel. 71. The system of claim 68, wherein the system includes a 96 well tray with well headspace volume capacities ranging between about 0.5 ml and about 2 ml. | 1,700 |
3,438 | 14,441,913 | 1,782 | The present invention relates to foodstuffs packaging containing a polyolefin-based film with properties providing a barrier to mineral oils. | 1.-24. (canceled) 25. A foodstuff packaging comprising:
a) a foodstuff, b) a polyolefin-based film which film encases the foodstuff, c) a cardboard based on recycled cardboard, which encases the polyolefin-based film, in particular the film based on biaxially oriented polypropylene (boPP) films, containing the foodstuff, wherein the polyolefin-based film comprises at least one coating comprising (i) acrylate polymer and/or (ii) halogen-containing vinyl polymers and/or vinylidene polymers and/or (iii) polymers based on vinyl alcohol (VOH), and the coating is present at least on the side of the film facing towards the cardboard based on recycled cardboard. 26. The foodstuff packaging according to claim 25, wherein the film and/or the cardboard does not have any metallization preventing the migration of mineral oils into the packaged foodstuff). 27. The foodstuff packaging according to claim 25, wherein the film is monolayered or multi-layered and comprises a base layer containing at least 70% by weight of the polyolefin in relation to the weight of the layer. 28. The foodstuff packaging according to claim 27, wherein the polyolefin-based film is a film based on biaxially oriented polypropylene (boPP) films and the base layer contains 85 to 95% by weight, of the polyolefin, in each case in relation to the weight of the layer. 29. The foodstuff packaging according to claim 28, wherein the film is monolayered and contains 90 to 100% by weight, of propylene polymers of which the melting point is 120° C. and which have a melt flow index from 1 to 10 g/10 min at 230° C. and a force of 21.6 N (DIN 53735). 30. The foodstuff packaging according to claim 25, wherein the propylene polymer is a mixture of propylene homopolymers and/or copolymers and/or terpolymers and other polyolefins wherein the mixture contains at least 50% by weight of propylene polymer. 31. The foodstuff packaging according claim 25, wherein the polyolefin film contains pigments in a quantity from 0.5 to 10% by weight. 32. The foodstuff packaging according to claim 25, wherein the polyolefin-based film has a thickness from 20 to 100 μm. 33. The foodstuff packaging according to claim 25, wherein the polyolefin-based film comprises, on one or both sides, an adhesion promoter made of polyethylene imine, to which the coating/s is/are applied. 34. The foodstuff packaging according to claim 34, wherein the coating is present on both sides of the film. 35. The foodstuff packaging according to claim 25, wherein the coating of the film on each side has in each case a total thickness between 0.4-5 μm. 36. The foodstuff packaging according to claim 35, wherein the coating is multi-layered and, with a coating made of halogen-containing vinyl polymers and/or vinylidene polymers, initially has a secondary primer layer based on vinyl acetate/acrylate, and the layer thickness of the secondary primer layer comprises 50-100% of the layer thickness of the coating made of halogen-containing vinyl polymers and/or vinylidene polymers. 37. The foodstuff packaging according to claim 25, wherein acrylate is an acrylate homopolymer and/or acrylate copolymer based on alkyl acrylates. 38. The foodstuff packaging according to claim 25, wherein the halogen-containing vinyl polymer and/or vinylidene polymer is based on vinyl chloride and/or is vinyl chloride, which preferably comprises a copolymer based on vinyl acetate or acrylate. 39. The foodstuff packaging according to claim 25, wherein the coating material made of a polymer based on vinyl alcohol (VOH) comprises a mixture of ethylene vinyl alcohol (EVOH) and polyvinyl alcohol, and said mixture comprising 5-15% by weight of a mixture of ethylene vinyl alcohol and polyvinyl alcohol, in the ratio 0.8-1.2 to 1.2-0.8 (ratios by weight). 40. The foodstuff packaging according to claim 25, wherein the quantity of coating per side of the film (after drying) is between 0.5 and 1.0 g/m2 for coating materials made of polymers based on vinyl alcohol (VOH), and the layer thickness is 1 to 1.5 μm (±0.2 μm). 41. The foodstuff packaging according to claim 25, wherein the quantity of coating per side of the film after drying is between 0.5 and 1.5 g/m2 for coating materials based on acrylate, and the layer thickness is 1 to 1.5 μm. 42. The foodstuff packaging according to claim 25, wherein the quantity of coating per side of the film after drying is between 2.5 and 4 g/m2 for coating materials based on halogen-containing vinyl polymers and/or vinylidene polymers, wherein the above quantity includes the secondary primer layer based on vinyl acetate/acrylate, and the layer thickness is 1.5 to 2.0 μm (±0.2 μm). 43. The foodstuff packaging according to claim 25, wherein the recycled cardboard contains at least 300-1000 mg/kg mineral oil. 44. The foodstuff packaging according to claim 25, wherein the film comprises a barrier for the mineral oils present in the recycled cardboard and at most 1%, of the MOSH 14-24 fraction present in the recycled cardboard diffuses into a foodstuff′ simulant when the proportion of the fraction MOSH 14-24 in the mineral oil of the recycled cardboard is at least 30% by weight. 45. The foodstuff packaging according to claim 25, wherein the film comprises a barrier for the mineral oils present in the recycled cardboard and at most 1.6% of the MOSH 24-35 fraction present in the recycled cardboard diffuse into a foodstuff simulant when the proportion of the fraction MOSH 24-35 in the mineral oil of the recycled cardboard is at least 10% by weight. 46. The foodstuff packaging according to claim 25, wherein the film comprises a barrier for the mineral oils present in the recycled cardboard and at most 0.5% of the MOAH 14-24 fraction present in the recycled cardboard diffuses into as foodstuff simulant when the proportion of the fraction MOAH 14-24 in the mineral oil of the recycled cardboard is at least 10% by weight. 47. The foodstuff packaging according to claim 25, wherein the film comprises a barrier for the mineral oils present in the recycled cardboard and at most 3.5%, of the MOAH 24-35 fraction present in the recycled cardboard diffuse into a foodstuff simulant when the proportion of the fraction MOAH 24-35 in the mineral oil of the recycled cardboard is at least 1% by weight. 48. The foodstuff packaging according to claim 25, wherein the foodstuffs packaging consists of the cardboard and the film and does not comprise any further metal layer. | The present invention relates to foodstuffs packaging containing a polyolefin-based film with properties providing a barrier to mineral oils.1.-24. (canceled) 25. A foodstuff packaging comprising:
a) a foodstuff, b) a polyolefin-based film which film encases the foodstuff, c) a cardboard based on recycled cardboard, which encases the polyolefin-based film, in particular the film based on biaxially oriented polypropylene (boPP) films, containing the foodstuff, wherein the polyolefin-based film comprises at least one coating comprising (i) acrylate polymer and/or (ii) halogen-containing vinyl polymers and/or vinylidene polymers and/or (iii) polymers based on vinyl alcohol (VOH), and the coating is present at least on the side of the film facing towards the cardboard based on recycled cardboard. 26. The foodstuff packaging according to claim 25, wherein the film and/or the cardboard does not have any metallization preventing the migration of mineral oils into the packaged foodstuff). 27. The foodstuff packaging according to claim 25, wherein the film is monolayered or multi-layered and comprises a base layer containing at least 70% by weight of the polyolefin in relation to the weight of the layer. 28. The foodstuff packaging according to claim 27, wherein the polyolefin-based film is a film based on biaxially oriented polypropylene (boPP) films and the base layer contains 85 to 95% by weight, of the polyolefin, in each case in relation to the weight of the layer. 29. The foodstuff packaging according to claim 28, wherein the film is monolayered and contains 90 to 100% by weight, of propylene polymers of which the melting point is 120° C. and which have a melt flow index from 1 to 10 g/10 min at 230° C. and a force of 21.6 N (DIN 53735). 30. The foodstuff packaging according to claim 25, wherein the propylene polymer is a mixture of propylene homopolymers and/or copolymers and/or terpolymers and other polyolefins wherein the mixture contains at least 50% by weight of propylene polymer. 31. The foodstuff packaging according claim 25, wherein the polyolefin film contains pigments in a quantity from 0.5 to 10% by weight. 32. The foodstuff packaging according to claim 25, wherein the polyolefin-based film has a thickness from 20 to 100 μm. 33. The foodstuff packaging according to claim 25, wherein the polyolefin-based film comprises, on one or both sides, an adhesion promoter made of polyethylene imine, to which the coating/s is/are applied. 34. The foodstuff packaging according to claim 34, wherein the coating is present on both sides of the film. 35. The foodstuff packaging according to claim 25, wherein the coating of the film on each side has in each case a total thickness between 0.4-5 μm. 36. The foodstuff packaging according to claim 35, wherein the coating is multi-layered and, with a coating made of halogen-containing vinyl polymers and/or vinylidene polymers, initially has a secondary primer layer based on vinyl acetate/acrylate, and the layer thickness of the secondary primer layer comprises 50-100% of the layer thickness of the coating made of halogen-containing vinyl polymers and/or vinylidene polymers. 37. The foodstuff packaging according to claim 25, wherein acrylate is an acrylate homopolymer and/or acrylate copolymer based on alkyl acrylates. 38. The foodstuff packaging according to claim 25, wherein the halogen-containing vinyl polymer and/or vinylidene polymer is based on vinyl chloride and/or is vinyl chloride, which preferably comprises a copolymer based on vinyl acetate or acrylate. 39. The foodstuff packaging according to claim 25, wherein the coating material made of a polymer based on vinyl alcohol (VOH) comprises a mixture of ethylene vinyl alcohol (EVOH) and polyvinyl alcohol, and said mixture comprising 5-15% by weight of a mixture of ethylene vinyl alcohol and polyvinyl alcohol, in the ratio 0.8-1.2 to 1.2-0.8 (ratios by weight). 40. The foodstuff packaging according to claim 25, wherein the quantity of coating per side of the film (after drying) is between 0.5 and 1.0 g/m2 for coating materials made of polymers based on vinyl alcohol (VOH), and the layer thickness is 1 to 1.5 μm (±0.2 μm). 41. The foodstuff packaging according to claim 25, wherein the quantity of coating per side of the film after drying is between 0.5 and 1.5 g/m2 for coating materials based on acrylate, and the layer thickness is 1 to 1.5 μm. 42. The foodstuff packaging according to claim 25, wherein the quantity of coating per side of the film after drying is between 2.5 and 4 g/m2 for coating materials based on halogen-containing vinyl polymers and/or vinylidene polymers, wherein the above quantity includes the secondary primer layer based on vinyl acetate/acrylate, and the layer thickness is 1.5 to 2.0 μm (±0.2 μm). 43. The foodstuff packaging according to claim 25, wherein the recycled cardboard contains at least 300-1000 mg/kg mineral oil. 44. The foodstuff packaging according to claim 25, wherein the film comprises a barrier for the mineral oils present in the recycled cardboard and at most 1%, of the MOSH 14-24 fraction present in the recycled cardboard diffuses into a foodstuff′ simulant when the proportion of the fraction MOSH 14-24 in the mineral oil of the recycled cardboard is at least 30% by weight. 45. The foodstuff packaging according to claim 25, wherein the film comprises a barrier for the mineral oils present in the recycled cardboard and at most 1.6% of the MOSH 24-35 fraction present in the recycled cardboard diffuse into a foodstuff simulant when the proportion of the fraction MOSH 24-35 in the mineral oil of the recycled cardboard is at least 10% by weight. 46. The foodstuff packaging according to claim 25, wherein the film comprises a barrier for the mineral oils present in the recycled cardboard and at most 0.5% of the MOAH 14-24 fraction present in the recycled cardboard diffuses into as foodstuff simulant when the proportion of the fraction MOAH 14-24 in the mineral oil of the recycled cardboard is at least 10% by weight. 47. The foodstuff packaging according to claim 25, wherein the film comprises a barrier for the mineral oils present in the recycled cardboard and at most 3.5%, of the MOAH 24-35 fraction present in the recycled cardboard diffuse into a foodstuff simulant when the proportion of the fraction MOAH 24-35 in the mineral oil of the recycled cardboard is at least 1% by weight. 48. The foodstuff packaging according to claim 25, wherein the foodstuffs packaging consists of the cardboard and the film and does not comprise any further metal layer. | 1,700 |
3,439 | 13,496,207 | 1,765 | The present invention provides a composition comprising (i) a polymer, (ii) an organic compound A carrying at least two amide functionalities, and (iii) 12 to 1'000 parts per million (ppm) of a compound B selected from the group consisting of an organic compound C carrying at least two amide functionalities, sugar alcohol acetals and derivatives thereof, metal salts of organic acids and precursor-systems thereof, metal salts of organic phosphoric acids and precursor-systems thereof and metal salts of polyols and precursor-systems thereof, and mixtures thereof, based on the weight of the polymer, as well as shaped articles obtainable from this composition. | 1. A composition comprising
(i) a polymer, (ii) an organic compound A carrying at least two amide functionalities and (iii) 12 to 1,000 parts per million, based on the weight of the polymer, of a compound B selected from the group consisting of an organic compound C carrying at least two amide functionalities, sugar alcohol acetals or derivatives thereof, metal salts of organic acids or precursor-systems thereof, metal salts of organic phosphoric acids or precursor-systems thereof, -metal salts of polyols or precursor-systems thereof and mixtures thereof. 2. The composition of claim 1, wherein the organic compound A carrying at least two amide functionalities is a compound of formula 1
wherein
R1 is —NHC(O)R4,
R2 is —NHC(O)R6 and
R3 is —NHC(O)R8,
wherein R4, R6 and R8 are the same and different and are branched C3-20-alkyl. 3. The composition of claim 1, wherein the organic compound A carrying at least two amide functionalities is 1,3,5-tris[2,2-dimethylpropionylamino]benzene. 4. The composition of claim 1, wherein compound B is selected from the group consisting of sugar alcohol acetals or derivatives thereof, metal salts of organic acids or precursor-systems thereof, metal salts of organic phosphoric acids or precursor-systems thereof and metal salts of polyols or precursor-systems thereof. 5. The composition of claim 1, wherein compound B is selected from the group consisting of metal salts of organic acids, metal salts of organic phosphoric acids, metal salts of polyols and precursor-systems thereof. 6. The composition of claim 1, wherein compound B is a sugar alcohol acetal or a derivative thereof of formula 3
wherein R19, R20, R21, R22, R23, R24, R25, R26, R27, R28, R29 and R30 are the same or different and are hydrogen or C1-20-alkyl unsubstituted or substituted by one or more hydroxyl. 7. The composition of claim 1, wherein compound B is 1,3:2,4-bis(3,4-dimethylbenzylidene)sorbitol. 8. The composition of claim 1, wherein compound B is a metal salt of an organic acid selected from the group consisting of
i) compounds of formula 4
wherein M1 and M2 are the same or different and are selected from the group consisting of calcium, strontium, lithium, sodium and monobasic aluminum, and wherein R31, R32, R33, R34, R35, R36, R37, R38, R39 and R40 are individually selected from the group consisting of hydrogen, C1-9-alkyl, wherein any two vicinal (neighboring) or geminal (same carbon) alkyl groups may be combined to form a carbocyclic ring of up to six carbon atoms, hydroxy, C1-9-alkoxy, C1-9-alkyleneoxy, amino, C1-9-alkylamino, halogeno, and phenyl,
ii) compounds of formula 5
wherein M3 and M4 are independently selected from the group consisting of metal cations and organic cations, or M3 and M4 together represent a bivalent metal ion and wherein R41, R42, R43, R44, R45, R46, R47, R48, R49 and R50 are individually selected from the group consisting of hydrogen, C1-9-alkyl, wherein any two vicinal (neighboring) or geminal (same carbon) alkyl groups may be combined to form a carbocyclic ring of up to six carbon atoms, hydroxy, C1-9-alkoxy, C1-9-alkyleneoxy, amino, C1-9-alkylamino, halogeno phenyl and alkylphenyl,
iii) sodium benzoate
and precursors-systems thereof. 9. The composition of claim 1, wherein compound B is cis-endo-bicyclo[2.2.1]heptane-2,3-dicarboxylic acid disodium salt or a precursor-system thereof. 10. The composition of claim 1, wherein compound B is sodium 2,2′-methylene bis(4,6-di-tert-butylphenyl)phosphate, lithium 2,2′-methylene-bis(4,6-di-tert-butylphenyl)phosphate, aluminium-hydroxy-bis[2,2′-methylene-bis(4,6-di-tert-butylphenyl)phosphate or a precursor-system thereof. 11. The composition of claim 1, wherein compound B is a metal salt of a polyol selected from the group consisting of divalent metal salts of polyhydroxylated C2-20-alkanes or a precursor-system thereof, wherein the divalent metal is zinc, calcium, cobalt, boron, manganese, iron, magnesium, titanium or copper. 12. The composition of claim 1, wherein compound B is zinc glycerolate or a precursor-system thereof. 13. The composition of claim 1, wherein the polymer is a polypropylene homopolymer or a polypropylene random copolymer, alternating or segmented copolymer or block copolymer containing one or more comonomers selected from the group consisting of ethylene, C4-C20-α-olefin, vinylcyclohexane, vinylcyclohexene, C4-C20alkandiene, C5-C12cycloalkandiene and norbornene derivatives; the total amount of propylene and the comonomer(s) being 100%. 14. The composition of claim 1 comprising 12 to 10,000 parts per million, of the organic compound A carrying at least two amide functionalities based on the weight of the polymer. 15. The composition of claim 1, wherein the composition comprises 12 to 500 parts per million of compound B based on the weight of the polymer. 16. A shaped article obtained from the composition of claim 1. 17-20. (canceled) 21. The composition of claim 1 comprising
(i) a polypropylene homopolymer or a polypropylene random copolymer, alternating or segmented copolymer or block copolymer containing one or more comonomers selected from the group consisting of ethylene, C4-C20-α-olefin, vinylcyclohexane, vinylcyclohexene, C4-C20alkandiene, C5-C12cycloalkandiene and norbornene derivatives; the total amount of propylene and the comonomer(s) being 100%,
(ii) a compound of formula 1
wherein
R1 is —NHC(O)R4,
R2 is —NHC(O)R6 and
R3 is —NHC(O)R8,
wherein R4, R6 and R8 are the same and different and are branched C3-20-alkyl
and
(iii) a compound of formula 3
wherein R19, R20, R21, R22, R23, R24, R25, R26, R27, R28, R29 and R30 are the same or different and are hydrogen or C1-20-alkyl unsubstituted or substituted by one or more hydroxyl,
a compound of formula 5
wherein M3 and M4 are independently selected from the group consisting of metal cations and organic cations, or M3 and M4 together represent a bivalent metal ion and wherein R41, R42, R43, R44, R45, R46, R47, R48, R49 and R50 are individually selected from the group consisting of hydrogen, C1-9-alkyl, wherein any two vicinal (neighboring) or geminal (same carbon) alkyl groups may be combined to form a carbocyclic ring of up to six carbon atoms, hydroxy, C1-9-alkoxy, C1-9-alkyleneoxy, amino, C1-9-alkylamino, halogeno, phenyl and alkylphenyl,
a metal salt of 2,2′-methylene bis(4,6-di-tert-butylphenyl)phosphate or
a divalent metal salt of a polyhydroxylated C2-20-alkane wherein the divalent metal is zinc, calcium, cobalt, boron, manganese, iron, magnesium, titanium or copper. 22. The composition of claim 1 comprising
(i) a polypropylene homopolymer or a polypropylene random copolymer, alternating or segmented copolymer or block copolymer containing one or more comonomers selected from the group consisting of ethylene, C4-C20-α-olefin, vinylcyclohexane, vinylcyclohexene, C4-C20alkandiene, C5-C12cycloalkandiene and norbornene derivatives; the total amount of propylene and the comonomer(s) being 100%,
(ii) 1,3,5-tris[2,2-dimethylpropionylamino]benzene and
(iii) 1,3:2,4-bis(3,4-dimethylbenzylidene)sorbitol, cis-endo-bicyclo[2.2.1]heptane-2,3-dicarboxylic acid disodium salt, sodium 2,2′-methylene bis(4,6-di-tert-butylphenyl)phosphate, lithium 2,2′-methylene-bis(4,6-di-tert-butylphenyl)phosphate, aluminium-hydroxy-bis[2,2′-methylene-bis(4,6-di-tert-butylphenyl) phosphate] or zinc glycerolate. | The present invention provides a composition comprising (i) a polymer, (ii) an organic compound A carrying at least two amide functionalities, and (iii) 12 to 1'000 parts per million (ppm) of a compound B selected from the group consisting of an organic compound C carrying at least two amide functionalities, sugar alcohol acetals and derivatives thereof, metal salts of organic acids and precursor-systems thereof, metal salts of organic phosphoric acids and precursor-systems thereof and metal salts of polyols and precursor-systems thereof, and mixtures thereof, based on the weight of the polymer, as well as shaped articles obtainable from this composition.1. A composition comprising
(i) a polymer, (ii) an organic compound A carrying at least two amide functionalities and (iii) 12 to 1,000 parts per million, based on the weight of the polymer, of a compound B selected from the group consisting of an organic compound C carrying at least two amide functionalities, sugar alcohol acetals or derivatives thereof, metal salts of organic acids or precursor-systems thereof, metal salts of organic phosphoric acids or precursor-systems thereof, -metal salts of polyols or precursor-systems thereof and mixtures thereof. 2. The composition of claim 1, wherein the organic compound A carrying at least two amide functionalities is a compound of formula 1
wherein
R1 is —NHC(O)R4,
R2 is —NHC(O)R6 and
R3 is —NHC(O)R8,
wherein R4, R6 and R8 are the same and different and are branched C3-20-alkyl. 3. The composition of claim 1, wherein the organic compound A carrying at least two amide functionalities is 1,3,5-tris[2,2-dimethylpropionylamino]benzene. 4. The composition of claim 1, wherein compound B is selected from the group consisting of sugar alcohol acetals or derivatives thereof, metal salts of organic acids or precursor-systems thereof, metal salts of organic phosphoric acids or precursor-systems thereof and metal salts of polyols or precursor-systems thereof. 5. The composition of claim 1, wherein compound B is selected from the group consisting of metal salts of organic acids, metal salts of organic phosphoric acids, metal salts of polyols and precursor-systems thereof. 6. The composition of claim 1, wherein compound B is a sugar alcohol acetal or a derivative thereof of formula 3
wherein R19, R20, R21, R22, R23, R24, R25, R26, R27, R28, R29 and R30 are the same or different and are hydrogen or C1-20-alkyl unsubstituted or substituted by one or more hydroxyl. 7. The composition of claim 1, wherein compound B is 1,3:2,4-bis(3,4-dimethylbenzylidene)sorbitol. 8. The composition of claim 1, wherein compound B is a metal salt of an organic acid selected from the group consisting of
i) compounds of formula 4
wherein M1 and M2 are the same or different and are selected from the group consisting of calcium, strontium, lithium, sodium and monobasic aluminum, and wherein R31, R32, R33, R34, R35, R36, R37, R38, R39 and R40 are individually selected from the group consisting of hydrogen, C1-9-alkyl, wherein any two vicinal (neighboring) or geminal (same carbon) alkyl groups may be combined to form a carbocyclic ring of up to six carbon atoms, hydroxy, C1-9-alkoxy, C1-9-alkyleneoxy, amino, C1-9-alkylamino, halogeno, and phenyl,
ii) compounds of formula 5
wherein M3 and M4 are independently selected from the group consisting of metal cations and organic cations, or M3 and M4 together represent a bivalent metal ion and wherein R41, R42, R43, R44, R45, R46, R47, R48, R49 and R50 are individually selected from the group consisting of hydrogen, C1-9-alkyl, wherein any two vicinal (neighboring) or geminal (same carbon) alkyl groups may be combined to form a carbocyclic ring of up to six carbon atoms, hydroxy, C1-9-alkoxy, C1-9-alkyleneoxy, amino, C1-9-alkylamino, halogeno phenyl and alkylphenyl,
iii) sodium benzoate
and precursors-systems thereof. 9. The composition of claim 1, wherein compound B is cis-endo-bicyclo[2.2.1]heptane-2,3-dicarboxylic acid disodium salt or a precursor-system thereof. 10. The composition of claim 1, wherein compound B is sodium 2,2′-methylene bis(4,6-di-tert-butylphenyl)phosphate, lithium 2,2′-methylene-bis(4,6-di-tert-butylphenyl)phosphate, aluminium-hydroxy-bis[2,2′-methylene-bis(4,6-di-tert-butylphenyl)phosphate or a precursor-system thereof. 11. The composition of claim 1, wherein compound B is a metal salt of a polyol selected from the group consisting of divalent metal salts of polyhydroxylated C2-20-alkanes or a precursor-system thereof, wherein the divalent metal is zinc, calcium, cobalt, boron, manganese, iron, magnesium, titanium or copper. 12. The composition of claim 1, wherein compound B is zinc glycerolate or a precursor-system thereof. 13. The composition of claim 1, wherein the polymer is a polypropylene homopolymer or a polypropylene random copolymer, alternating or segmented copolymer or block copolymer containing one or more comonomers selected from the group consisting of ethylene, C4-C20-α-olefin, vinylcyclohexane, vinylcyclohexene, C4-C20alkandiene, C5-C12cycloalkandiene and norbornene derivatives; the total amount of propylene and the comonomer(s) being 100%. 14. The composition of claim 1 comprising 12 to 10,000 parts per million, of the organic compound A carrying at least two amide functionalities based on the weight of the polymer. 15. The composition of claim 1, wherein the composition comprises 12 to 500 parts per million of compound B based on the weight of the polymer. 16. A shaped article obtained from the composition of claim 1. 17-20. (canceled) 21. The composition of claim 1 comprising
(i) a polypropylene homopolymer or a polypropylene random copolymer, alternating or segmented copolymer or block copolymer containing one or more comonomers selected from the group consisting of ethylene, C4-C20-α-olefin, vinylcyclohexane, vinylcyclohexene, C4-C20alkandiene, C5-C12cycloalkandiene and norbornene derivatives; the total amount of propylene and the comonomer(s) being 100%,
(ii) a compound of formula 1
wherein
R1 is —NHC(O)R4,
R2 is —NHC(O)R6 and
R3 is —NHC(O)R8,
wherein R4, R6 and R8 are the same and different and are branched C3-20-alkyl
and
(iii) a compound of formula 3
wherein R19, R20, R21, R22, R23, R24, R25, R26, R27, R28, R29 and R30 are the same or different and are hydrogen or C1-20-alkyl unsubstituted or substituted by one or more hydroxyl,
a compound of formula 5
wherein M3 and M4 are independently selected from the group consisting of metal cations and organic cations, or M3 and M4 together represent a bivalent metal ion and wherein R41, R42, R43, R44, R45, R46, R47, R48, R49 and R50 are individually selected from the group consisting of hydrogen, C1-9-alkyl, wherein any two vicinal (neighboring) or geminal (same carbon) alkyl groups may be combined to form a carbocyclic ring of up to six carbon atoms, hydroxy, C1-9-alkoxy, C1-9-alkyleneoxy, amino, C1-9-alkylamino, halogeno, phenyl and alkylphenyl,
a metal salt of 2,2′-methylene bis(4,6-di-tert-butylphenyl)phosphate or
a divalent metal salt of a polyhydroxylated C2-20-alkane wherein the divalent metal is zinc, calcium, cobalt, boron, manganese, iron, magnesium, titanium or copper. 22. The composition of claim 1 comprising
(i) a polypropylene homopolymer or a polypropylene random copolymer, alternating or segmented copolymer or block copolymer containing one or more comonomers selected from the group consisting of ethylene, C4-C20-α-olefin, vinylcyclohexane, vinylcyclohexene, C4-C20alkandiene, C5-C12cycloalkandiene and norbornene derivatives; the total amount of propylene and the comonomer(s) being 100%,
(ii) 1,3,5-tris[2,2-dimethylpropionylamino]benzene and
(iii) 1,3:2,4-bis(3,4-dimethylbenzylidene)sorbitol, cis-endo-bicyclo[2.2.1]heptane-2,3-dicarboxylic acid disodium salt, sodium 2,2′-methylene bis(4,6-di-tert-butylphenyl)phosphate, lithium 2,2′-methylene-bis(4,6-di-tert-butylphenyl)phosphate, aluminium-hydroxy-bis[2,2′-methylene-bis(4,6-di-tert-butylphenyl) phosphate] or zinc glycerolate. | 1,700 |
3,440 | 13,823,971 | 1,787 | The claimed invention provides an antistatic hard coat film that is extremely excellent in white muddiness resistance and antistatic properties and sufficiently prevents an interference fringe pattern. The claimed invention provides an antistatic hard coat film including a triacetyl cellulose substrate and a hard coat layer formed on the triacetyl cellulose substrate, the hard coat layer including an antistatic agent, a (meth)acrylate resin, and a polymer of a (meth)acrylate monomer, the triacetyl cellulose substrate including a permeation layer formed by permeation of the (meth)acrylate monomer from the hard coat layer side of the interface toward the opposite side of the hard coat layer, the antistatic hard coat film satisfying Formulas (1), (2), and (3):
3 μm≦ T ≦18 μm Formula (1)
0.3 T≦t ≦0.9 T Formula (2)
2 μm≦ T−t ≦11 μm Formula (3)
where T denotes the total thickness (μm) of the permeation layer and the hard coat layer, and t denotes the thickness (μm) of the permeation layer. | 1. An antistatic hard coat film comprising
a triacetyl cellulose substrate, and a hard coat layer formed on the triacetyl cellulose substrate, wherein the hard coat layer comprises an antistatic agent, a (meth)acrylate resin, and a polymer of a (meth)acrylate monomer, the triacetyl cellulose substrate comprises a permeation layer formed by permeation of the (meth)acrylate monomer from the hard coat layer side of the interface toward the opposite side of the hard coat layer, the antistatic hard coat film satisfies Formulas (1), (2), and (3):
3 μm≦T≦18 μm Formula (1)
0.3T≦t≦0.9T Formula (2)
2 μm≦T−t≦11 μm Formula (3)
where T denotes the total thickness (μm) of the permeation layer and the hard coat layer, and t denotes the thickness (μm) of the permeation layer. 2. The antistatic hard coat film according to claim 1,
wherein the thickness of the permeation layer (t) is 2 to 8 μm. 3. The antistatic hard coat film according to claim 1,
wherein the hard coat layer is a cured product formed by applying a composition for producing a hard coat layer on the triacetyl cellulose substrate, the composition comprising the antistatic agent, the (meth)acrylate resin, and the (meth)acrylate monomer, and the permeation layer is formed by permeation of the (meth)acrylate monomer in the composition into the triacetyl cellulose substrate. 4. The antistatic hard coat film according to claim 1,
wherein the antistatic agent contains a quaternary ammonium salt oligomer. 5. The antistatic hard coat film according to claim 1,
wherein the (meth)acrylate monomer has a weight-average molecular weight of less than 1,000. 6. The antistatic hard coat film according to claim 1,
wherein the (meth)acrylate monomer is at least one selected from the group consisting of pentaerythritol tri(meth)acrylate, dipentaerythritol hexa(meth)acrylate, pentaerythritol tetra(meth)acrylate, dipentaerythritol penta(meth)acrylate, trimethylolpropane tri(meth)acrylate, dipentaerythritol tetra(meth)acrylate, and isocyanuric acid EO-modified tri(meth)acrylate. 7. A polarizer comprising a polarizing element,
wherein said polarizer has the antistatic hard coat film according to claim 1, on the polarizing element surface. 8. An image display device comprising a the antistatic hard coat film comprising
a triacetyl cellulose substrate, and a hard coat layer formed on the triacetyl cellulose substrate, wherein the hard coat layer comprises an antistatic agent, a (meth)acrylate resin, and a polymer of a (meth)acrylate monomer, the triacetyl cellulose substrate comprises a permeation layer formed by permeation of the (meth)acrylate monomer from the hard coat layer side of the interface toward the opposite side of the hard coat layer, the antistatic hard coat film satisfies Formulas (1), (2), and (3):
3 μm≦T≦18 μm Formula (1)
0.3T≦t≦0.9T Formula (2)
2 μm≦T−t≦11 μm Formula (3)
where T denotes the total thickness (μm) of the permeation layer and the hard coat layer, and t denotes the thickness (μm) of the permeation layer or the polarizer according to claim 7 on an outermost surface thereof. 9. A method for producing an antistatic hard coat film that contains a triacetyl cellulose substrate and a hard coat layer formed on the triacetyl cellulose substrate, the method comprising:
forming a film by applying a composition for producing a hard coat layer on the triacetyl cellulose substrate, the composition including an antistatic agent, a (meth)acrylate resin, and a (meth)acrylate monomer; drying the film under the drying conditions below within 20 seconds from completion of the application of the composition; and curing the dried film, the drying conditions being: Drying temperature: 40 to 80° C.; Drying time: 20 to 70 seconds; and Wind velocity: to 20 m/min. 10. The antistatic hard coat film according to claim 2,
wherein the hard coat layer is a cured product formed by applying a composition for producing a hard coat layer on the triacetyl cellulose substrate, the composition comprising the antistatic agent, the (meth)acrylate resin, and the (meth)acrylate monomer, and the permeation layer is formed by permeation of the (meth)acrylate monomer in the composition into the triacetyl cellulose substrate. 11. The antistatic hard coat film according to claim 2, wherein the antistatic agent contains a quaternary ammonium salt oligomer. 12. The antistatic hard coat film according to claim 3, wherein the antistatic agent contains a quaternary ammonium salt oligomer. 13. The antistatic hard coat film according to claim 2, wherein the (meth)acrylate monomer has a weight-average molecular weight of less than 1,000. 14. The antistatic hard coat film according to claim 3, wherein the (meth)acrylate monomer has a weight-average molecular weight of less than 1,000. 15. The antistatic hard coat film according to claim 4, wherein the (meth)acrylate monomer has a weight-average molecular weight of less than 1,000. 16. The antistatic hard coat film according to claim 2, wherein the (meth)acrylate monomer is at least one selected from the group consisting of pentaerythritol tri(meth)acrylate, dipentaerythritol hexa(meth)acrylate, pentaerythritol tetra(meth)acrylate, dipentaerythritol penta(meth)acrylate, trimethylolpropane tri(meth)acrylate, dipentaerythritol tetra(meth)acrylate, and isocyanuric acid EO-modified tri(meth)acrylate. 17. The antistatic hard coat film according to claim 3, wherein the (meth)acrylate monomer is at least one selected from the group consisting of pentaerythritol tri(meth)acrylate, dipentaerythritol hexa(meth)acrylate, pentaerythritol tetra(meth)acrylate, dipentaerythritol penta(meth)acrylate, trimethylolpropane tri(meth)acrylate, dipentaerythritol tetra(meth)acrylate, and isocyanuric acid EO-modified tri(meth)acrylate. 18. The antistatic hard coat film according to claim 4, wherein the (meth)acrylate monomer is at least one selected from the group consisting of pentaerythritol tri(meth)acrylate, dipentaerythritol hexa(meth)acrylate, pentaerythritol tetra(meth)acrylate, dipentaerythritol penta(meth)acrylate, trimethylolpropane tri(meth)acrylate, dipentaerythritol tetra(meth)acrylate, and isocyanuric acid EO-modified tri(meth)acrylate. 19. The antistatic hard coat film according to claim 5, wherein the (meth)acrylate monomer is at least one selected from the group consisting of pentaerythritol tri(meth)acrylate, dipentaerythritol hexa(meth)acrylate, pentaerythritol tetra(meth)acrylate, dipentaerythritol penta(meth)acrylate, trimethylolpropane tri(meth)acrylate, dipentaerythritol tetra(meth)acrylate, and isocyanuric acid EO-modified tri(meth)acrylate. 20. A polarizer comprising a polarizing element, wherein said polarizer has the antistatic hard coat film according to claim 2 on the polarizing element surface. | The claimed invention provides an antistatic hard coat film that is extremely excellent in white muddiness resistance and antistatic properties and sufficiently prevents an interference fringe pattern. The claimed invention provides an antistatic hard coat film including a triacetyl cellulose substrate and a hard coat layer formed on the triacetyl cellulose substrate, the hard coat layer including an antistatic agent, a (meth)acrylate resin, and a polymer of a (meth)acrylate monomer, the triacetyl cellulose substrate including a permeation layer formed by permeation of the (meth)acrylate monomer from the hard coat layer side of the interface toward the opposite side of the hard coat layer, the antistatic hard coat film satisfying Formulas (1), (2), and (3):
3 μm≦ T ≦18 μm Formula (1)
0.3 T≦t ≦0.9 T Formula (2)
2 μm≦ T−t ≦11 μm Formula (3)
where T denotes the total thickness (μm) of the permeation layer and the hard coat layer, and t denotes the thickness (μm) of the permeation layer.1. An antistatic hard coat film comprising
a triacetyl cellulose substrate, and a hard coat layer formed on the triacetyl cellulose substrate, wherein the hard coat layer comprises an antistatic agent, a (meth)acrylate resin, and a polymer of a (meth)acrylate monomer, the triacetyl cellulose substrate comprises a permeation layer formed by permeation of the (meth)acrylate monomer from the hard coat layer side of the interface toward the opposite side of the hard coat layer, the antistatic hard coat film satisfies Formulas (1), (2), and (3):
3 μm≦T≦18 μm Formula (1)
0.3T≦t≦0.9T Formula (2)
2 μm≦T−t≦11 μm Formula (3)
where T denotes the total thickness (μm) of the permeation layer and the hard coat layer, and t denotes the thickness (μm) of the permeation layer. 2. The antistatic hard coat film according to claim 1,
wherein the thickness of the permeation layer (t) is 2 to 8 μm. 3. The antistatic hard coat film according to claim 1,
wherein the hard coat layer is a cured product formed by applying a composition for producing a hard coat layer on the triacetyl cellulose substrate, the composition comprising the antistatic agent, the (meth)acrylate resin, and the (meth)acrylate monomer, and the permeation layer is formed by permeation of the (meth)acrylate monomer in the composition into the triacetyl cellulose substrate. 4. The antistatic hard coat film according to claim 1,
wherein the antistatic agent contains a quaternary ammonium salt oligomer. 5. The antistatic hard coat film according to claim 1,
wherein the (meth)acrylate monomer has a weight-average molecular weight of less than 1,000. 6. The antistatic hard coat film according to claim 1,
wherein the (meth)acrylate monomer is at least one selected from the group consisting of pentaerythritol tri(meth)acrylate, dipentaerythritol hexa(meth)acrylate, pentaerythritol tetra(meth)acrylate, dipentaerythritol penta(meth)acrylate, trimethylolpropane tri(meth)acrylate, dipentaerythritol tetra(meth)acrylate, and isocyanuric acid EO-modified tri(meth)acrylate. 7. A polarizer comprising a polarizing element,
wherein said polarizer has the antistatic hard coat film according to claim 1, on the polarizing element surface. 8. An image display device comprising a the antistatic hard coat film comprising
a triacetyl cellulose substrate, and a hard coat layer formed on the triacetyl cellulose substrate, wherein the hard coat layer comprises an antistatic agent, a (meth)acrylate resin, and a polymer of a (meth)acrylate monomer, the triacetyl cellulose substrate comprises a permeation layer formed by permeation of the (meth)acrylate monomer from the hard coat layer side of the interface toward the opposite side of the hard coat layer, the antistatic hard coat film satisfies Formulas (1), (2), and (3):
3 μm≦T≦18 μm Formula (1)
0.3T≦t≦0.9T Formula (2)
2 μm≦T−t≦11 μm Formula (3)
where T denotes the total thickness (μm) of the permeation layer and the hard coat layer, and t denotes the thickness (μm) of the permeation layer or the polarizer according to claim 7 on an outermost surface thereof. 9. A method for producing an antistatic hard coat film that contains a triacetyl cellulose substrate and a hard coat layer formed on the triacetyl cellulose substrate, the method comprising:
forming a film by applying a composition for producing a hard coat layer on the triacetyl cellulose substrate, the composition including an antistatic agent, a (meth)acrylate resin, and a (meth)acrylate monomer; drying the film under the drying conditions below within 20 seconds from completion of the application of the composition; and curing the dried film, the drying conditions being: Drying temperature: 40 to 80° C.; Drying time: 20 to 70 seconds; and Wind velocity: to 20 m/min. 10. The antistatic hard coat film according to claim 2,
wherein the hard coat layer is a cured product formed by applying a composition for producing a hard coat layer on the triacetyl cellulose substrate, the composition comprising the antistatic agent, the (meth)acrylate resin, and the (meth)acrylate monomer, and the permeation layer is formed by permeation of the (meth)acrylate monomer in the composition into the triacetyl cellulose substrate. 11. The antistatic hard coat film according to claim 2, wherein the antistatic agent contains a quaternary ammonium salt oligomer. 12. The antistatic hard coat film according to claim 3, wherein the antistatic agent contains a quaternary ammonium salt oligomer. 13. The antistatic hard coat film according to claim 2, wherein the (meth)acrylate monomer has a weight-average molecular weight of less than 1,000. 14. The antistatic hard coat film according to claim 3, wherein the (meth)acrylate monomer has a weight-average molecular weight of less than 1,000. 15. The antistatic hard coat film according to claim 4, wherein the (meth)acrylate monomer has a weight-average molecular weight of less than 1,000. 16. The antistatic hard coat film according to claim 2, wherein the (meth)acrylate monomer is at least one selected from the group consisting of pentaerythritol tri(meth)acrylate, dipentaerythritol hexa(meth)acrylate, pentaerythritol tetra(meth)acrylate, dipentaerythritol penta(meth)acrylate, trimethylolpropane tri(meth)acrylate, dipentaerythritol tetra(meth)acrylate, and isocyanuric acid EO-modified tri(meth)acrylate. 17. The antistatic hard coat film according to claim 3, wherein the (meth)acrylate monomer is at least one selected from the group consisting of pentaerythritol tri(meth)acrylate, dipentaerythritol hexa(meth)acrylate, pentaerythritol tetra(meth)acrylate, dipentaerythritol penta(meth)acrylate, trimethylolpropane tri(meth)acrylate, dipentaerythritol tetra(meth)acrylate, and isocyanuric acid EO-modified tri(meth)acrylate. 18. The antistatic hard coat film according to claim 4, wherein the (meth)acrylate monomer is at least one selected from the group consisting of pentaerythritol tri(meth)acrylate, dipentaerythritol hexa(meth)acrylate, pentaerythritol tetra(meth)acrylate, dipentaerythritol penta(meth)acrylate, trimethylolpropane tri(meth)acrylate, dipentaerythritol tetra(meth)acrylate, and isocyanuric acid EO-modified tri(meth)acrylate. 19. The antistatic hard coat film according to claim 5, wherein the (meth)acrylate monomer is at least one selected from the group consisting of pentaerythritol tri(meth)acrylate, dipentaerythritol hexa(meth)acrylate, pentaerythritol tetra(meth)acrylate, dipentaerythritol penta(meth)acrylate, trimethylolpropane tri(meth)acrylate, dipentaerythritol tetra(meth)acrylate, and isocyanuric acid EO-modified tri(meth)acrylate. 20. A polarizer comprising a polarizing element, wherein said polarizer has the antistatic hard coat film according to claim 2 on the polarizing element surface. | 1,700 |
3,441 | 14,130,978 | 1,782 | Aqueous polyurethane coating compositions are disclosed in this specification. The aqueous polyurethane coating compositions contain a polycarbonate-polyurethane resin component and a water-dilutable, ethylenically unsaturated polyurethane polyol component. | 1. An aqueous polyurethane coating composition comprising:
(a) a water-dilutable free radically curable polyurethane resin comprising a reaction product of:
(A1) 40-90 wt. % of one or more acrylate prepolymers containing hydroxyl groups and having an OH content of 40-120 mg of KOH/g and
(B1) 0.1-20 wt. % of one or more mono- and/or difunctional compounds reactive towards isocyanate groups, which compounds contain groups which are cationic, anionic and/or have a dispersant action due to ether groups with
(C1) 10-50 wt. % of one or more polyisocyanates
(D1) 0.0-30.0 Wt. % of one or more polyols together with a subsequent reaction with
(E1) 0.1-10 wt. % of one or more di- and/or polyamines, and
(b) a water-dilutable polycarbonate-polyurethane resin,
wherein the polycarbonate-polyurethane resin is non-functional. 2. The aqueous polyurethane coating composition of claim 1, wherein the polycarbonate-polyurethane resin component (b) comprises a reaction product of:
(A1′) a polyisocyanate; (A2′) a polycarbonate polyol; and (A3′) an isocyanate-reactive compound comprising at least one ionic group or potentially ionic group. 3. The aqueous polyurethane coating composition of claim 1, wherein the polycarbonate-polyurethane resin component (b) further comprises:
(A4′) isocyanate-reactive chain extender and/or chain terminator. 4. The aqueous polyurethane coating composition of claim 1, wherein acrylate prepolymers containing hydroxyl groups (A1) are selected from the group consisting of polyester acrylate prepolymers, polyether acrylate prepolymers, or polycarbonate acrylate prepolymers containing hydroxyl groups. 5. The aqueous polyurethane coating composition of claim 1, wherein one or more mono- and/or difunctional compounds reactive towards isocyanate groups, which compounds contain groups which are cationic, anionic and/or have a dispersant action due to ether groups (B1) are selected from the group consisting of bis(hydroxymethyl)propionic acid, malic acid, glycolic acid, lactic acid, glycine, alanine, taurine, 2-aminoethylaminoethanesulphonic acid, polyethylene glycols and polypropylene glycols started on alcohols. 6. The aqueous polyurethane coating composition of claim 1, wherein the one or more polyisocyanates (C1) are selected from the group consisting of aromatic, araliphatic, aliphatic, cycloaliphatic polyisocyanates and mixtures thereof. 7. The aqueous polyurethane coating composition of claim 6, wherein the one or more polyisocyanates (C1) are selected from the group consisting of hexamethylene diisocyanate and isophorone diisocyanate. 8. The aqueous polyurethane coating composition of claim 1, wherein the one or more polyols (D1) are selected from the group consisting of propylene glycol, ethylene glycol, neopentyl glycol, 1,6-hexane diol, polyesterpolyols having an average OH-functionality of 1.8-2.2, polyetherpolyols having an average OH-functionality of 1.8-2.2, polycarbonatepolyols having an average OH-functionality of 1.8-2.2, ethanol and butanol. 9. The aqueous polyurethane coating composition of claim 1, wherein the one or more di- and/or polyamines (E1) are selected from the group consisting of ethylenediamine, 1,6-hexamethylenediamine, isophoronediamine, 1,3- and 1,4-phenylenediamine, 4,4′-diphenylmethanediamine, aminofunctional polyethylene oxide, polypropylene oxide, triethylenetetramine and hydrazine. 10. The aqueous polyurethane coating composition of claim 1, wherein the polyisocyanate (A1′) is selected from the group consisting of monomeric organic diisocyanate, monomeric isocyanate comprising three or more isocyanate groups, and diisocyanate adducts and/or oligomers comprising urethane groups, urea groups, uretdione groups, uretonimine groups, isocyanurate groups, iminooxadiazine dione groups, oxadiazine trione groups, carbodiimide groups, acyl urea groups, biuret groups, and/or allophanate groups. 11. The aqueous polyurethane coating composition of claim 1, wherein the polycarbonate polyol (A2′) is selected from the group consisting of a polycondensation reaction product of polyhydric alcohols and phosgene and a polycondensation reaction product of polyhydric alcohols and diesters of carbonic acid. 12. The aqueous polyurethane coating composition of claim 11, wherein the polyhydric alcohol is selected from the group consisting of 1,3-propanediol, ethylene glycol, propylene glycol, 1,4-propanediol, diethylene glycol, triethylene glycol, tetraethylene glycol, 1,4-butanediol, 1,6-hexanediol, trimethylenepentanediol, 1,4-cyclohexanediol, 1,4-cyclohexanedimethanol, neopentyl glycol, 1,8-octanediol, glycerol, trimethylolpropane, trimethylolethane, hexanetriol, pentaerythritol, and mixtures thereof. 13. A glass substrate coated with the aqueous polyurethane coating composition of claim 1. 14. A glass container coated with the aqueous polyurethane coating composition of claim 1. 15. A glass bottle coated with the aqueous polyurethane coating composition of claim 1. 16. A method of coating a glass substrate comprising 1) providing a glass substrate, 2) applying the aqueous polyurethane coating composition of claim 1 to at least a portion of the glass substrate and 3) exposing the aqueous polyurethane coating composition of claim 1 to a source of actinic radiation for a time sufficient to cure the aqueous polyurethane coating composition of claim 1. | Aqueous polyurethane coating compositions are disclosed in this specification. The aqueous polyurethane coating compositions contain a polycarbonate-polyurethane resin component and a water-dilutable, ethylenically unsaturated polyurethane polyol component.1. An aqueous polyurethane coating composition comprising:
(a) a water-dilutable free radically curable polyurethane resin comprising a reaction product of:
(A1) 40-90 wt. % of one or more acrylate prepolymers containing hydroxyl groups and having an OH content of 40-120 mg of KOH/g and
(B1) 0.1-20 wt. % of one or more mono- and/or difunctional compounds reactive towards isocyanate groups, which compounds contain groups which are cationic, anionic and/or have a dispersant action due to ether groups with
(C1) 10-50 wt. % of one or more polyisocyanates
(D1) 0.0-30.0 Wt. % of one or more polyols together with a subsequent reaction with
(E1) 0.1-10 wt. % of one or more di- and/or polyamines, and
(b) a water-dilutable polycarbonate-polyurethane resin,
wherein the polycarbonate-polyurethane resin is non-functional. 2. The aqueous polyurethane coating composition of claim 1, wherein the polycarbonate-polyurethane resin component (b) comprises a reaction product of:
(A1′) a polyisocyanate; (A2′) a polycarbonate polyol; and (A3′) an isocyanate-reactive compound comprising at least one ionic group or potentially ionic group. 3. The aqueous polyurethane coating composition of claim 1, wherein the polycarbonate-polyurethane resin component (b) further comprises:
(A4′) isocyanate-reactive chain extender and/or chain terminator. 4. The aqueous polyurethane coating composition of claim 1, wherein acrylate prepolymers containing hydroxyl groups (A1) are selected from the group consisting of polyester acrylate prepolymers, polyether acrylate prepolymers, or polycarbonate acrylate prepolymers containing hydroxyl groups. 5. The aqueous polyurethane coating composition of claim 1, wherein one or more mono- and/or difunctional compounds reactive towards isocyanate groups, which compounds contain groups which are cationic, anionic and/or have a dispersant action due to ether groups (B1) are selected from the group consisting of bis(hydroxymethyl)propionic acid, malic acid, glycolic acid, lactic acid, glycine, alanine, taurine, 2-aminoethylaminoethanesulphonic acid, polyethylene glycols and polypropylene glycols started on alcohols. 6. The aqueous polyurethane coating composition of claim 1, wherein the one or more polyisocyanates (C1) are selected from the group consisting of aromatic, araliphatic, aliphatic, cycloaliphatic polyisocyanates and mixtures thereof. 7. The aqueous polyurethane coating composition of claim 6, wherein the one or more polyisocyanates (C1) are selected from the group consisting of hexamethylene diisocyanate and isophorone diisocyanate. 8. The aqueous polyurethane coating composition of claim 1, wherein the one or more polyols (D1) are selected from the group consisting of propylene glycol, ethylene glycol, neopentyl glycol, 1,6-hexane diol, polyesterpolyols having an average OH-functionality of 1.8-2.2, polyetherpolyols having an average OH-functionality of 1.8-2.2, polycarbonatepolyols having an average OH-functionality of 1.8-2.2, ethanol and butanol. 9. The aqueous polyurethane coating composition of claim 1, wherein the one or more di- and/or polyamines (E1) are selected from the group consisting of ethylenediamine, 1,6-hexamethylenediamine, isophoronediamine, 1,3- and 1,4-phenylenediamine, 4,4′-diphenylmethanediamine, aminofunctional polyethylene oxide, polypropylene oxide, triethylenetetramine and hydrazine. 10. The aqueous polyurethane coating composition of claim 1, wherein the polyisocyanate (A1′) is selected from the group consisting of monomeric organic diisocyanate, monomeric isocyanate comprising three or more isocyanate groups, and diisocyanate adducts and/or oligomers comprising urethane groups, urea groups, uretdione groups, uretonimine groups, isocyanurate groups, iminooxadiazine dione groups, oxadiazine trione groups, carbodiimide groups, acyl urea groups, biuret groups, and/or allophanate groups. 11. The aqueous polyurethane coating composition of claim 1, wherein the polycarbonate polyol (A2′) is selected from the group consisting of a polycondensation reaction product of polyhydric alcohols and phosgene and a polycondensation reaction product of polyhydric alcohols and diesters of carbonic acid. 12. The aqueous polyurethane coating composition of claim 11, wherein the polyhydric alcohol is selected from the group consisting of 1,3-propanediol, ethylene glycol, propylene glycol, 1,4-propanediol, diethylene glycol, triethylene glycol, tetraethylene glycol, 1,4-butanediol, 1,6-hexanediol, trimethylenepentanediol, 1,4-cyclohexanediol, 1,4-cyclohexanedimethanol, neopentyl glycol, 1,8-octanediol, glycerol, trimethylolpropane, trimethylolethane, hexanetriol, pentaerythritol, and mixtures thereof. 13. A glass substrate coated with the aqueous polyurethane coating composition of claim 1. 14. A glass container coated with the aqueous polyurethane coating composition of claim 1. 15. A glass bottle coated with the aqueous polyurethane coating composition of claim 1. 16. A method of coating a glass substrate comprising 1) providing a glass substrate, 2) applying the aqueous polyurethane coating composition of claim 1 to at least a portion of the glass substrate and 3) exposing the aqueous polyurethane coating composition of claim 1 to a source of actinic radiation for a time sufficient to cure the aqueous polyurethane coating composition of claim 1. | 1,700 |
3,442 | 14,539,215 | 1,743 | An aerosol delivery device is provided that includes a housing, microelectromechanical systems-based (MEMS-based) sensor and microprocessor. The MEMS-based sensor is within the housing and configured to detect a pressure on the MEMS-based sensor caused by airflow through at least a portion of the housing. The MEMS-based sensor is configured to convert the pressure to an electrical signal, and output the electrical signal. The microprocessor is configured to receive the electrical signal from the MEMS-based sensor, and control operation of at least one functional element of the aerosol delivery device based thereon. | 1. An aerosol delivery device comprising:
a housing; a microelectromechanical systems-based (MEMS-based) sensor within the housing and configured to detect a pressure on the MEMS-based sensor caused by airflow through at least a portion of the housing, the MEMS-based sensor being configured to convert the pressure to an electrical signal, and output the electrical signal; and a microprocessor configured to receive the electrical signal from the MEMS-based sensor, and control operation of at least one functional element of the aerosol delivery device based thereon. 2. The aerosol delivery device of claim 1, wherein the MEMS-based sensor being configured to convert the pressure includes being configured to convert the pressure to the electrical signal that varies with a corresponding variation in the pressure relative to an ambient pressure on the MEMS-based sensor, the corresponding variation being caused by variation in the airflow. 3. The aerosol delivery device of claim 2, wherein the corresponding variation in the pressure is caused by variation in a rate of the airflow. 4. The aerosol delivery device of claim 1, wherein the MEMS-based sensor is a MEMS microphone including:
a die with a micromachined, pressure-sensitive diaphragm and a backplate that form a variable capacitor; wherein in an instance in which an input voltage is applied to the variable capacitor, the pressure causes movement of the diaphragm and thereby a change in a capacitance of the variable capacitor, the change in capacitance causing a change in an output voltage across the variable capacitor, the output voltage or a digital representation thereof being output by the MEMS microphone as the electrical signal. 5. The aerosol delivery device of claim 4, wherein the MEMS microphone further comprises another die wire bonded to the die and including a bias generator circuit configured to bias the variable capacitor with the input voltage. 6. The aerosol delivery device of claim 1, wherein the MEMS-based sensor is a MEMS pressure sensor including:
a die with a micromachined, pressure-sensitive diaphragm, and one or more piezoresistors disposed on the diaphragm, wherein in an instance in which an input voltage is applied to the one or more piezoresistors, the pressure causes movement of the diaphragm and thereby a change in a resistance of the one or more piezoresistors, the change in resistance causing a change in an output voltage across the one or more piezoresistors, the output voltage or a digital representation thereof being output by the MEMS pressure sensor as the electrical signal. 7. The aerosol delivery device of claim 6, wherein the MEMS pressure sensor further comprises another die wire bonded to the die and including a bias generator circuit configured to bias the one or more piezoresistors with the input voltage. 8. The aerosol delivery device of claim 1, wherein the microprocessor being configured to control the operation of at least one functional element includes being configured to control the operation of a heater, fluid-delivery member, sensory-feedback member or any combination thereof. 9. A method for controlling operation of an aerosol delivery device including a microelectromechanical systems-based (MEMS-based) sensor within a housing thereof, the method comprising:
detecting an pressure on the MEMS-based sensor caused by airflow through at least a portion of the housing, the MEMS-based sensor converting the pressure to an electrical signal; and controlling operation of at least one functional element of the aerosol delivery device based on the electrical signal. 10. The method of claim 9, wherein the MEMS-based sensor converting the pressure includes converting the pressure to the electrical signal that varies with a corresponding variation in the pressure relative to an ambient pressure on the MEMS-based sensor, the corresponding variation being caused by variation in the airflow. 11. The method delivery device of claim 10, wherein the corresponding variation in the pressure is caused by variation in a rate of the airflow. 12. The method of claim 9, wherein the MEMS-based sensor is a MEMS microphone including a die with a micromachined, pressure-sensitive diaphragm and a backplate that form a variable capacitor, and
wherein in an instance in which an input voltage is applied to the variable capacitor, the pressure causes movement of the diaphragm and thereby a change in a capacitance of the variable capacitor, the change in capacitance causing a change in an output voltage across the variable capacitor, the MEMS microphone outputting the output voltage or a digital representation thereof as the electrical signal. 13. The method of claim 9, wherein the MEMS-based sensor is a MEMS pressure sensor including a die with a micromachined, pressure-sensitive diaphragm, and one or more piezoresistors disposed on the diaphragm,
wherein in an instance in which an input voltage is applied to the one or more piezoresistors, the pressure causes movement of the diaphragm and thereby a change in a resistance of the one or more piezoresistors, the change in resistance causing a change in an output voltage across the one or more piezoresistors, the MEMS pressure sensor outputting the output voltage or a digital representation thereof as the electrical signal. 14. The method of claim 9, wherein controlling the operation of at least one functional element includes controlling the operation of a heater, fluid-delivery member, sensory-feedback member or any combination thereof. | An aerosol delivery device is provided that includes a housing, microelectromechanical systems-based (MEMS-based) sensor and microprocessor. The MEMS-based sensor is within the housing and configured to detect a pressure on the MEMS-based sensor caused by airflow through at least a portion of the housing. The MEMS-based sensor is configured to convert the pressure to an electrical signal, and output the electrical signal. The microprocessor is configured to receive the electrical signal from the MEMS-based sensor, and control operation of at least one functional element of the aerosol delivery device based thereon.1. An aerosol delivery device comprising:
a housing; a microelectromechanical systems-based (MEMS-based) sensor within the housing and configured to detect a pressure on the MEMS-based sensor caused by airflow through at least a portion of the housing, the MEMS-based sensor being configured to convert the pressure to an electrical signal, and output the electrical signal; and a microprocessor configured to receive the electrical signal from the MEMS-based sensor, and control operation of at least one functional element of the aerosol delivery device based thereon. 2. The aerosol delivery device of claim 1, wherein the MEMS-based sensor being configured to convert the pressure includes being configured to convert the pressure to the electrical signal that varies with a corresponding variation in the pressure relative to an ambient pressure on the MEMS-based sensor, the corresponding variation being caused by variation in the airflow. 3. The aerosol delivery device of claim 2, wherein the corresponding variation in the pressure is caused by variation in a rate of the airflow. 4. The aerosol delivery device of claim 1, wherein the MEMS-based sensor is a MEMS microphone including:
a die with a micromachined, pressure-sensitive diaphragm and a backplate that form a variable capacitor; wherein in an instance in which an input voltage is applied to the variable capacitor, the pressure causes movement of the diaphragm and thereby a change in a capacitance of the variable capacitor, the change in capacitance causing a change in an output voltage across the variable capacitor, the output voltage or a digital representation thereof being output by the MEMS microphone as the electrical signal. 5. The aerosol delivery device of claim 4, wherein the MEMS microphone further comprises another die wire bonded to the die and including a bias generator circuit configured to bias the variable capacitor with the input voltage. 6. The aerosol delivery device of claim 1, wherein the MEMS-based sensor is a MEMS pressure sensor including:
a die with a micromachined, pressure-sensitive diaphragm, and one or more piezoresistors disposed on the diaphragm, wherein in an instance in which an input voltage is applied to the one or more piezoresistors, the pressure causes movement of the diaphragm and thereby a change in a resistance of the one or more piezoresistors, the change in resistance causing a change in an output voltage across the one or more piezoresistors, the output voltage or a digital representation thereof being output by the MEMS pressure sensor as the electrical signal. 7. The aerosol delivery device of claim 6, wherein the MEMS pressure sensor further comprises another die wire bonded to the die and including a bias generator circuit configured to bias the one or more piezoresistors with the input voltage. 8. The aerosol delivery device of claim 1, wherein the microprocessor being configured to control the operation of at least one functional element includes being configured to control the operation of a heater, fluid-delivery member, sensory-feedback member or any combination thereof. 9. A method for controlling operation of an aerosol delivery device including a microelectromechanical systems-based (MEMS-based) sensor within a housing thereof, the method comprising:
detecting an pressure on the MEMS-based sensor caused by airflow through at least a portion of the housing, the MEMS-based sensor converting the pressure to an electrical signal; and controlling operation of at least one functional element of the aerosol delivery device based on the electrical signal. 10. The method of claim 9, wherein the MEMS-based sensor converting the pressure includes converting the pressure to the electrical signal that varies with a corresponding variation in the pressure relative to an ambient pressure on the MEMS-based sensor, the corresponding variation being caused by variation in the airflow. 11. The method delivery device of claim 10, wherein the corresponding variation in the pressure is caused by variation in a rate of the airflow. 12. The method of claim 9, wherein the MEMS-based sensor is a MEMS microphone including a die with a micromachined, pressure-sensitive diaphragm and a backplate that form a variable capacitor, and
wherein in an instance in which an input voltage is applied to the variable capacitor, the pressure causes movement of the diaphragm and thereby a change in a capacitance of the variable capacitor, the change in capacitance causing a change in an output voltage across the variable capacitor, the MEMS microphone outputting the output voltage or a digital representation thereof as the electrical signal. 13. The method of claim 9, wherein the MEMS-based sensor is a MEMS pressure sensor including a die with a micromachined, pressure-sensitive diaphragm, and one or more piezoresistors disposed on the diaphragm,
wherein in an instance in which an input voltage is applied to the one or more piezoresistors, the pressure causes movement of the diaphragm and thereby a change in a resistance of the one or more piezoresistors, the change in resistance causing a change in an output voltage across the one or more piezoresistors, the MEMS pressure sensor outputting the output voltage or a digital representation thereof as the electrical signal. 14. The method of claim 9, wherein controlling the operation of at least one functional element includes controlling the operation of a heater, fluid-delivery member, sensory-feedback member or any combination thereof. | 1,700 |
3,443 | 15,117,641 | 1,791 | Provided is wheat flour that can be shaken out of a shaker-type container onto a foodstuff in small amounts with little scattering and lumping. Provided is a packaged wheat flour including wheat flour packed in a shaker-type container having one or more shaker holes having a maximum width of 2 to 20 mm, the wheat flour having a particle diameter at 10%, D10, of 18 μm or more and a particle diameter at 90%, D90, of 500 μm or less. | 1. A packaged wheat flour, comprising a wheat flour packed in a shaker-type container having one or more shaker holes having a maximum width of 2 to 20 mm, the wheat flour having a particle diameter at 10%, D10 of 18 μm or more and a particle diameter at 90%, D90, of 500 μm or less. 2. The packaged wheat flour according to claim 1, wherein the shaker-type container has 2 to 9 shaker holes. 3. The packaged wheat flour according to claim 1, wherein the wheat flour is a granulated wheat flour or a mixture of a granulated wheat flour and a non-granulated wheat flour. 4. The packaged wheat flour according to claim 1, wherein the wheat flour has a D10 of 25 μm or more and a D90 of 400 μm or less. 5. The packaged wheat flour according to claim 1, wherein D90/D10 is 3 to 12. 6. The packaged wheat flour according to claim 1, wherein the wheat flour has a mean particle diameter of 40 to 200 μm. 7. A method of applying a wheat flour, comprising shaking out a wheat flour through shaker holes to apply the wheat flour to an object, wherein the wheat flour is packed in a shaker-type container having 2 to 9 shaker holes having a maximum width of 2 to 20 mm, and the wheat flour has a particle diameter at 10%, D10, of 18 μm or more and a particle diameter at 90%, D90, of 500 μm or less. 8. A method of suppressing scattering and formation of lumps of a wheat flour, comprising shaking out a wheat flour thorough shaker holes to apply the wheat flour to an object, wherein the wheat flour is packed in a shaker-type container having 2 to 9 shaker holes having a maximum width of 2 to 20 mm, and the wheat flour having a particle diameter at 10%, D10, of 18 μm or more and a particle diameter at 90%, D90, of 500 μm or less. 9. The method according to claim 7, wherein the wheat flour is a granulated wheat flour or a mixture of a granulated wheat flour and a non-granulated wheat flour. 10. The method according to claim 7, wherein D90/D10 is 3 to 12. 11. The method according to claim 7, wherein the wheat flour has a mean particle diameter of 40 to 200 μm. 12. The method according to claim 8, wherein the wheat flour is a granulated wheat flour or a mixture of a granulated wheat flour and a non-granulated wheat flour. 13. The method according to claim 8, wherein D90/D10 is 3 to 12. 14. The method according to claim 8, wherein the wheat flour has a mean particle diameter of 40 to 200 μm. | Provided is wheat flour that can be shaken out of a shaker-type container onto a foodstuff in small amounts with little scattering and lumping. Provided is a packaged wheat flour including wheat flour packed in a shaker-type container having one or more shaker holes having a maximum width of 2 to 20 mm, the wheat flour having a particle diameter at 10%, D10, of 18 μm or more and a particle diameter at 90%, D90, of 500 μm or less.1. A packaged wheat flour, comprising a wheat flour packed in a shaker-type container having one or more shaker holes having a maximum width of 2 to 20 mm, the wheat flour having a particle diameter at 10%, D10 of 18 μm or more and a particle diameter at 90%, D90, of 500 μm or less. 2. The packaged wheat flour according to claim 1, wherein the shaker-type container has 2 to 9 shaker holes. 3. The packaged wheat flour according to claim 1, wherein the wheat flour is a granulated wheat flour or a mixture of a granulated wheat flour and a non-granulated wheat flour. 4. The packaged wheat flour according to claim 1, wherein the wheat flour has a D10 of 25 μm or more and a D90 of 400 μm or less. 5. The packaged wheat flour according to claim 1, wherein D90/D10 is 3 to 12. 6. The packaged wheat flour according to claim 1, wherein the wheat flour has a mean particle diameter of 40 to 200 μm. 7. A method of applying a wheat flour, comprising shaking out a wheat flour through shaker holes to apply the wheat flour to an object, wherein the wheat flour is packed in a shaker-type container having 2 to 9 shaker holes having a maximum width of 2 to 20 mm, and the wheat flour has a particle diameter at 10%, D10, of 18 μm or more and a particle diameter at 90%, D90, of 500 μm or less. 8. A method of suppressing scattering and formation of lumps of a wheat flour, comprising shaking out a wheat flour thorough shaker holes to apply the wheat flour to an object, wherein the wheat flour is packed in a shaker-type container having 2 to 9 shaker holes having a maximum width of 2 to 20 mm, and the wheat flour having a particle diameter at 10%, D10, of 18 μm or more and a particle diameter at 90%, D90, of 500 μm or less. 9. The method according to claim 7, wherein the wheat flour is a granulated wheat flour or a mixture of a granulated wheat flour and a non-granulated wheat flour. 10. The method according to claim 7, wherein D90/D10 is 3 to 12. 11. The method according to claim 7, wherein the wheat flour has a mean particle diameter of 40 to 200 μm. 12. The method according to claim 8, wherein the wheat flour is a granulated wheat flour or a mixture of a granulated wheat flour and a non-granulated wheat flour. 13. The method according to claim 8, wherein D90/D10 is 3 to 12. 14. The method according to claim 8, wherein the wheat flour has a mean particle diameter of 40 to 200 μm. | 1,700 |
3,444 | 15,042,909 | 1,797 | Methods, devices, systems, and kits useful for the collection and analysis of samples obtained by swabs are disclosed. Swab containers configured for receiving a swab containing a sample; cartridges for holding one or more of: a swab container, a swab, assay units, pipette tips, vessels, transport units, and implements; systems (which may include a sample processing device); kits; and methods for their use are disclosed. A swab container may include an entry port; an assay chamber having an assay port; a conduit comprising an interior channel connecting the entry port; and an interior channel providing fluidic communication between the entry port and assay chamber. An interior channel may be configured to squeeze a portion of a swab placed in or through the conduit. A cartridge may include a cartridge frame configured to receive one or more of swab containers, assay units, transport units, pipette tips, vessels or implements. | 1-100. (canceled) 101. A system comprising:
a sample analysis device; an implement; and a cartridge comprising a swab container, said swab container comprising an entry port and an assay chamber, effective that passing a swab through said entry port allows at least a portion of said swab to be placed within said assay chamber, said cartridge further comprising: a cartridge frame configured for insertion into said sample analysis device, said cartridge frame comprising a plurality of receptacles, wherein said receptacles comprise: a sample receptacle configured to receive a sample collection vessel for holding a fluid sample; and an implement receptacle configured to receive an implement for use by said automatic sample analysis device, wherein said implement is disposed in said implement receptacle. 102. The system of claim 101, wherein a sample collection vessel is disposed in said sample receptacle. 103. The system of claim 102, wherein said sample collection vessel disposed in said sample receptacle comprises a sample. 104. The system of claim 101, wherein said cartridge comprising a swab container comprises a swab for obtaining a swab sample. 105. The system of claim 102, wherein said cartridge comprising a swab container comprises a swab for obtaining a swab sample. 106. The system of claim 104, wherein said swab further comprises a swab sample. 107. The system of claim 105, wherein said swab further comprises a swab sample. 108. The system of claim 101, wherein said cartridge frame comprises a swab container receptacle configured to receive a swab container for holding a swab for obtaining a swab sample, and wherein said swab container is disposed in said swab container receptacle. 109. The system of claim 101, wherein said swab container comprises a conduit comprising an interior channel connecting said entry port with said assay chamber. 110. The system of claim 109, wherein said conduit provides fluidic communication between said entry port and said assay chamber effective that passing a swab having a handle through said entry port into said conduit allows said swab to be placed within said assay chamber. 111. The system of claim 101, wherein said swab container comprises an entry port, said entry port configured to receive a swab having a handle; an assay chamber having an assay port, said assay chamber being configured to receive at least a portion of a swab; and a conduit comprising an interior channel connecting said entry port with said assay chamber, said conduit being configured to accept a least a portion of said swab handle therein, wherein said conduit provides fluidic communication between said entry port and said assay chamber effective that passing a swab through said entry port into said conduit allows the swab to be placed within said assay chamber. 112. The system of claim 101, wherein said sample analysis device comprises an automatic sample analysis device. 113. The system of claim 101, wherein said implement is a cuvette. 114. The system of claim 101, wherein said implement is a pipette tip. 115. The system of claim 101, wherein said implement is a transport unit. 116. The system of claim 101, wherein said implement is a swab. 117. The system of claim 101, wherein said implement is a magnet. 118. The system of claim 101, wherein said cartridge frame comprises a receptacle configured to receive a vessel. 119. The system of claim 118, wherein said cartridge further comprises one or more vessels selected from the group of vessels consisting of a sample collection vessel, an empty vessel, a reagent vessel containing reagent, a mixing vessel, and a waste vessel. 120. The system of claim 101, wherein said swab container contains a reagent for bathing a swab within said assay chamber, wherein said reagent for bathing a swab is effective to receive sample material from said swab into said reagent. 121. The system of claim 101, wherein said swab container comprises a conduit interior channel configured to squeeze a portion of a swab placed in or through a portion of the conduit interior channel adjacent to said assay chamber. 122. The system of claim 101, wherein said swab container comprises a conduit having a plurality of interior channels or a plurality of conduits each of which comprise at least one interior channel. 123. The system of claim 101, wherein said swab container comprises a body portion and a cover portion, wherein said cover portion is flexibly connected to said body portion of the swab container. 124. The system of claim 101, wherein said assay chamber of said swab container contains a volume of reagent for bathing a swab, wherein said volume of reagent is less than about 500 μL. 125. The system of claim 124, wherein said volume of reagent is selected from the group of volumes of less than about 250 μL, or less than 150 μL, or less than about 100 μL, or less than about 50 μL, or less than about 25 μL, or less than about 10 μL, or less than about 5 μL, or less than about 1 μL. 126. The system of claim 102, wherein said sample collection vessel disposed in said sample receptacle contains a fluid sample. 127. The system of claim 101, wherein said cartridge frame comprises a reagent vessel containing reagent disposed in a receptacle configured to receive a reagent vessel, wherein said reagent and reagent vessel are suitable for use for use by said sample analysis device. 128. The system of claim 101, wherein said cartridge frame comprises an assay unit disposed in a receptacle configured to receive an assay unit, wherein said assay unit is suitable for use for use by said sample analysis device. 129. The system of claim 101, wherein said cartridge frame comprises a mixing vessel receptacle configured to receive a mixing vessel, and a mixing vessel disposed in said mixing vessel receptacle, wherein said mixing vessel is suitable for use for use by said sample analysis device. 130. The system of claim 101, wherein said cartridge frame comprises a waste vessel receptacle configured to receive a waste vessel, and a waste vessel disposed in said waste vessel receptacle, wherein said waste vessel is suitable for use for use by said sample analysis device. | Methods, devices, systems, and kits useful for the collection and analysis of samples obtained by swabs are disclosed. Swab containers configured for receiving a swab containing a sample; cartridges for holding one or more of: a swab container, a swab, assay units, pipette tips, vessels, transport units, and implements; systems (which may include a sample processing device); kits; and methods for their use are disclosed. A swab container may include an entry port; an assay chamber having an assay port; a conduit comprising an interior channel connecting the entry port; and an interior channel providing fluidic communication between the entry port and assay chamber. An interior channel may be configured to squeeze a portion of a swab placed in or through the conduit. A cartridge may include a cartridge frame configured to receive one or more of swab containers, assay units, transport units, pipette tips, vessels or implements.1-100. (canceled) 101. A system comprising:
a sample analysis device; an implement; and a cartridge comprising a swab container, said swab container comprising an entry port and an assay chamber, effective that passing a swab through said entry port allows at least a portion of said swab to be placed within said assay chamber, said cartridge further comprising: a cartridge frame configured for insertion into said sample analysis device, said cartridge frame comprising a plurality of receptacles, wherein said receptacles comprise: a sample receptacle configured to receive a sample collection vessel for holding a fluid sample; and an implement receptacle configured to receive an implement for use by said automatic sample analysis device, wherein said implement is disposed in said implement receptacle. 102. The system of claim 101, wherein a sample collection vessel is disposed in said sample receptacle. 103. The system of claim 102, wherein said sample collection vessel disposed in said sample receptacle comprises a sample. 104. The system of claim 101, wherein said cartridge comprising a swab container comprises a swab for obtaining a swab sample. 105. The system of claim 102, wherein said cartridge comprising a swab container comprises a swab for obtaining a swab sample. 106. The system of claim 104, wherein said swab further comprises a swab sample. 107. The system of claim 105, wherein said swab further comprises a swab sample. 108. The system of claim 101, wherein said cartridge frame comprises a swab container receptacle configured to receive a swab container for holding a swab for obtaining a swab sample, and wherein said swab container is disposed in said swab container receptacle. 109. The system of claim 101, wherein said swab container comprises a conduit comprising an interior channel connecting said entry port with said assay chamber. 110. The system of claim 109, wherein said conduit provides fluidic communication between said entry port and said assay chamber effective that passing a swab having a handle through said entry port into said conduit allows said swab to be placed within said assay chamber. 111. The system of claim 101, wherein said swab container comprises an entry port, said entry port configured to receive a swab having a handle; an assay chamber having an assay port, said assay chamber being configured to receive at least a portion of a swab; and a conduit comprising an interior channel connecting said entry port with said assay chamber, said conduit being configured to accept a least a portion of said swab handle therein, wherein said conduit provides fluidic communication between said entry port and said assay chamber effective that passing a swab through said entry port into said conduit allows the swab to be placed within said assay chamber. 112. The system of claim 101, wherein said sample analysis device comprises an automatic sample analysis device. 113. The system of claim 101, wherein said implement is a cuvette. 114. The system of claim 101, wherein said implement is a pipette tip. 115. The system of claim 101, wherein said implement is a transport unit. 116. The system of claim 101, wherein said implement is a swab. 117. The system of claim 101, wherein said implement is a magnet. 118. The system of claim 101, wherein said cartridge frame comprises a receptacle configured to receive a vessel. 119. The system of claim 118, wherein said cartridge further comprises one or more vessels selected from the group of vessels consisting of a sample collection vessel, an empty vessel, a reagent vessel containing reagent, a mixing vessel, and a waste vessel. 120. The system of claim 101, wherein said swab container contains a reagent for bathing a swab within said assay chamber, wherein said reagent for bathing a swab is effective to receive sample material from said swab into said reagent. 121. The system of claim 101, wherein said swab container comprises a conduit interior channel configured to squeeze a portion of a swab placed in or through a portion of the conduit interior channel adjacent to said assay chamber. 122. The system of claim 101, wherein said swab container comprises a conduit having a plurality of interior channels or a plurality of conduits each of which comprise at least one interior channel. 123. The system of claim 101, wherein said swab container comprises a body portion and a cover portion, wherein said cover portion is flexibly connected to said body portion of the swab container. 124. The system of claim 101, wherein said assay chamber of said swab container contains a volume of reagent for bathing a swab, wherein said volume of reagent is less than about 500 μL. 125. The system of claim 124, wherein said volume of reagent is selected from the group of volumes of less than about 250 μL, or less than 150 μL, or less than about 100 μL, or less than about 50 μL, or less than about 25 μL, or less than about 10 μL, or less than about 5 μL, or less than about 1 μL. 126. The system of claim 102, wherein said sample collection vessel disposed in said sample receptacle contains a fluid sample. 127. The system of claim 101, wherein said cartridge frame comprises a reagent vessel containing reagent disposed in a receptacle configured to receive a reagent vessel, wherein said reagent and reagent vessel are suitable for use for use by said sample analysis device. 128. The system of claim 101, wherein said cartridge frame comprises an assay unit disposed in a receptacle configured to receive an assay unit, wherein said assay unit is suitable for use for use by said sample analysis device. 129. The system of claim 101, wherein said cartridge frame comprises a mixing vessel receptacle configured to receive a mixing vessel, and a mixing vessel disposed in said mixing vessel receptacle, wherein said mixing vessel is suitable for use for use by said sample analysis device. 130. The system of claim 101, wherein said cartridge frame comprises a waste vessel receptacle configured to receive a waste vessel, and a waste vessel disposed in said waste vessel receptacle, wherein said waste vessel is suitable for use for use by said sample analysis device. | 1,700 |
3,445 | 15,152,950 | 1,737 | Provided is a method for patterning a substrate, comprising: forming a layer of radiation-sensitive material on a substrate; preparing a pattern in the layer of radiation-sensitive material using a lithographic process, the pattern being characterized by a critical dimension (CD) and a roughness; following the preparing the pattern, performing a CD shrink process to reduce the CD to a reduced CD; and performing a growth process to grow the reduced CD to a target CD. Roughness includes a line edge roughness (LER), a line width roughness (LWR), or both LER and LWR. Performing the CD shrink process comprises: coating the pattern with a hard mask, the coating generating a hard mask coated resist; baking the hard mask coated resist in a temperature range for a time period, the baking generating a baked coated resist; and developing the baked coated resist in deionized water. | 1. A method for patterning a substrate in a patterning system having a throughput in substrates per hour, the method comprising:
forming a layer of radiation-sensitive material on a substrate; preparing a pattern in the layer of radiation-sensitive material using an extreme ultra violet (EUV) lithographic process, the pattern being characterized by a critical dimension (CD) and a roughness; following the preparing the pattern, performing a CD shrink process to reduce the CD to a reduced CD; and following the performing the CD shrink process, performing a growth process to grow the reduced CD to a target CD; wherein the throughput is 50 substrates per hour or more while controlling the line wide roughness (LWR) and line edge roughness (LER) of the substrate. 2. The method of claim 1 wherein the performing the CD shrink process comprises:
coating the pattern with a hard mask, the coating generating a hard mask coated resist;
baking the hard mask coated resist in a temperature range for a selected time period, the baking generating a baked coated resist; and
developing the baked coated resist in deionized water (DIW). 3. The method of claim 2 wherein the baking the hard mask coated resist is performed in a temperature range from 110 to 170 degrees C. for 70 seconds or less. 4. The method of claim 3 wherein the CD shrink process reduces the CD by 10 to 15 nm. 5. The method of claim 3 wherein the hard mask coating is performed with a film thickness in a range from 60 to 150 nm. 6. The method of claim 3 wherein the developing the baked coated resist is performed in 60 sec or less. 7. The method of claim 1 wherein the growth process is performed preceding, following, or during the CD shrink process. 8. The method of claim 1 wherein the shrink process is performed using solvent vapor process or a chemical spin coating process. 9. The method of claim 1, wherein the shrink process is performed using resist development process or an etch process. 10. The method of claim 1, wherein the performing the growth process is performed using a solvent vapor process, a chemical spin coating process, or an etch process. 11. The method of claim 1 further comprising:
concurrently controlling two or more selected operating variables in order to meet patterning targets. 12. The method of claim 11 wherein the two or more selected operating variables comprise coating time, coating spin speed, coating acceleration, etchant dispense rate, deionized water dispense rate, depth of focus (DOF) margin, shrinkage range (nm), mixing bake temperature, and hard mask film thickness range. 13. The method of claim 12 wherein the LER and LWR after the growth process is lower by 11 to 20% compared to the LER and LWR after the shrink process. 14. A method for patterning a substrate, comprising:
forming a layer of radiation-sensitive material on a substrate; preparing a contact hole (C/H) pattern in the layer of radiation-sensitive material using a lithographic process, the pattern being characterized by a critical dimension (CD) and a contact edge roughness (CER); following the preparing the C/H pattern, performing an exposure process to a lower energy than the target energy, the exposure process forming a smaller C/H CD than the expected C/H CD, performing a growth process to create a C/H CD larger than the expected C/H CD; and performing a shrink back process to reduce the C/H CD to a target CD. 15. The method of claim 14 wherein the performing the growth process is performed using a solvent vapor process, a chemical spin coating process, a resist development process or an etch process. 16. The method of claim 14 wherein the performing the shrink back process is performed using a solvent vapor process, a chemical spin coating process, or an etch process. 17. The method of claim 14 further comprising:
concurrently controlling two or more selected operating variables in order to meet patterning targets comprising sensitivity reduction, CER and/or CD uniformity (CDU). 18. The method of claim 17 wherein the two or more selected operating variables comprise coating time, coating spin speed, coating acceleration, etchant dispense rate, deionized water dispense rate, depth of focus (DOF) margin, mixing bake degrees per 60 sec, shrinkage (nm), mixing bake temperature, hard mask film thickness range, growth process time, and/or shrink back process time. 19. The method of claim 14 wherein the CER is reduced by 15 to 33% and the throughput is 50 or more substrates per hour. 20. The method of claim 14 further comprising:
utilizing the pattern in the layer of radiation-sensitive material as a mandrel for performing a sidewall image transfer process and the layer of radiation-sensitive material comprises an EUV (extreme ultraviolet) resist. | Provided is a method for patterning a substrate, comprising: forming a layer of radiation-sensitive material on a substrate; preparing a pattern in the layer of radiation-sensitive material using a lithographic process, the pattern being characterized by a critical dimension (CD) and a roughness; following the preparing the pattern, performing a CD shrink process to reduce the CD to a reduced CD; and performing a growth process to grow the reduced CD to a target CD. Roughness includes a line edge roughness (LER), a line width roughness (LWR), or both LER and LWR. Performing the CD shrink process comprises: coating the pattern with a hard mask, the coating generating a hard mask coated resist; baking the hard mask coated resist in a temperature range for a time period, the baking generating a baked coated resist; and developing the baked coated resist in deionized water.1. A method for patterning a substrate in a patterning system having a throughput in substrates per hour, the method comprising:
forming a layer of radiation-sensitive material on a substrate; preparing a pattern in the layer of radiation-sensitive material using an extreme ultra violet (EUV) lithographic process, the pattern being characterized by a critical dimension (CD) and a roughness; following the preparing the pattern, performing a CD shrink process to reduce the CD to a reduced CD; and following the performing the CD shrink process, performing a growth process to grow the reduced CD to a target CD; wherein the throughput is 50 substrates per hour or more while controlling the line wide roughness (LWR) and line edge roughness (LER) of the substrate. 2. The method of claim 1 wherein the performing the CD shrink process comprises:
coating the pattern with a hard mask, the coating generating a hard mask coated resist;
baking the hard mask coated resist in a temperature range for a selected time period, the baking generating a baked coated resist; and
developing the baked coated resist in deionized water (DIW). 3. The method of claim 2 wherein the baking the hard mask coated resist is performed in a temperature range from 110 to 170 degrees C. for 70 seconds or less. 4. The method of claim 3 wherein the CD shrink process reduces the CD by 10 to 15 nm. 5. The method of claim 3 wherein the hard mask coating is performed with a film thickness in a range from 60 to 150 nm. 6. The method of claim 3 wherein the developing the baked coated resist is performed in 60 sec or less. 7. The method of claim 1 wherein the growth process is performed preceding, following, or during the CD shrink process. 8. The method of claim 1 wherein the shrink process is performed using solvent vapor process or a chemical spin coating process. 9. The method of claim 1, wherein the shrink process is performed using resist development process or an etch process. 10. The method of claim 1, wherein the performing the growth process is performed using a solvent vapor process, a chemical spin coating process, or an etch process. 11. The method of claim 1 further comprising:
concurrently controlling two or more selected operating variables in order to meet patterning targets. 12. The method of claim 11 wherein the two or more selected operating variables comprise coating time, coating spin speed, coating acceleration, etchant dispense rate, deionized water dispense rate, depth of focus (DOF) margin, shrinkage range (nm), mixing bake temperature, and hard mask film thickness range. 13. The method of claim 12 wherein the LER and LWR after the growth process is lower by 11 to 20% compared to the LER and LWR after the shrink process. 14. A method for patterning a substrate, comprising:
forming a layer of radiation-sensitive material on a substrate; preparing a contact hole (C/H) pattern in the layer of radiation-sensitive material using a lithographic process, the pattern being characterized by a critical dimension (CD) and a contact edge roughness (CER); following the preparing the C/H pattern, performing an exposure process to a lower energy than the target energy, the exposure process forming a smaller C/H CD than the expected C/H CD, performing a growth process to create a C/H CD larger than the expected C/H CD; and performing a shrink back process to reduce the C/H CD to a target CD. 15. The method of claim 14 wherein the performing the growth process is performed using a solvent vapor process, a chemical spin coating process, a resist development process or an etch process. 16. The method of claim 14 wherein the performing the shrink back process is performed using a solvent vapor process, a chemical spin coating process, or an etch process. 17. The method of claim 14 further comprising:
concurrently controlling two or more selected operating variables in order to meet patterning targets comprising sensitivity reduction, CER and/or CD uniformity (CDU). 18. The method of claim 17 wherein the two or more selected operating variables comprise coating time, coating spin speed, coating acceleration, etchant dispense rate, deionized water dispense rate, depth of focus (DOF) margin, mixing bake degrees per 60 sec, shrinkage (nm), mixing bake temperature, hard mask film thickness range, growth process time, and/or shrink back process time. 19. The method of claim 14 wherein the CER is reduced by 15 to 33% and the throughput is 50 or more substrates per hour. 20. The method of claim 14 further comprising:
utilizing the pattern in the layer of radiation-sensitive material as a mandrel for performing a sidewall image transfer process and the layer of radiation-sensitive material comprises an EUV (extreme ultraviolet) resist. | 1,700 |
3,446 | 14,726,864 | 1,734 | The disclosure provides Au—Al-Rare-Earth metallic glass-forming alloys and metallic glasses comprising various other additions including but not limited to Cu, Pd, Sn and Mg. In certain embodiments, the metallic glasses according to the disclosure satisfy the 18-Karat Gold Alloy Hallmark, and demonstrate colors that include yellow and pink/rose. | 1. An alloy capable of forming a metallic glass, the alloy comprising:
an atomic fraction of Au in the range of 40 to 90 percent, an atomic fraction of Al in the range of 0.5 to 40 percent, and an atomic fraction of RE is in the range of 1 to 20 percent; and wherein RE is a rare earth metal. 2. The alloy of claim 1 wherein RE is selected from Y, Er, Dy and a combination thereof. 3. The alloy of claim 1, wherein the atomic fraction of Al is in the range of 2 to 20 percent. 4. The alloy of claim 2, wherein RE comprises Y in an atomic fraction of 3 to 15 percent. 5. The alloy of claim 1, further comprising an atomic fraction of Cu of up to 20 percent. 6. The alloy of claim 1, further comprising an atomic fraction of Pd of up to 25 percent. 7. The alloy of claim 1, further comprising Sn in an atomic fraction of up to 10 percent. 8. The alloy of claim 1, further comprising Mg in an atomic fraction of up to 20 percent. 9. The alloy of claim 1, further comprising at least one additional element selected from Ag, Pt, Rh, Ir, Fe, Ni, Co, Ru, Cr, Mo, Mn, Ti, Zr, Hf, W, Re, Be, Ca, Si, P, S, Ge, Ga, In, Sb, and Bi, or combinations thereof, in an atomic fraction of up to 10 percent. 10. The alloy of claim 1, wherein the alloy has a critical casting thickness of at least 1 micrometer. 11. A metallic glass comprising an alloy of claim 1. 12. The metallic glass of claim 11, wherein the metallic glass has a glass transition temperature of at least 150° C. 13. The metallic glass of claim 11, wherein the metallic glass has a Vicker's hardness of at least 400 kgf/mm2. 14. The metallic glass of claim 11, wherein the metallic glass has a color having CIELAB coordinates with L* in the range of 65 to 120, a* in the range of −5 to 15, and b* in the range of 5 to 40. 15. A metallic glass-forming alloy having a composition represented by the following formula (subscripts denote atomic percentages):
Au(100-a-b-c-d)AlaREbCucPdd where: a ranges from 0.5 to 40; b ranges from 1 to 20; c is up to 20; d up to 25; and wherein RE is a rare earth metal. 16. The metallic glass-forming alloy of claim 15, where a ranges from 2 to 20. 17. The metallic glass-forming alloy of claim 15, where b ranges from 3 to 15. 18. The metallic glass-forming alloy of claim 15, where c ranges from 0.5 to 10. 19. The metallic glass-forming alloy of claim 15, where d ranges from 0.5 to 20. 20. The metallic glass-forming alloy of claim 15, where the weight fraction of Au is at least 75 percent. 21. The metallic glass-forming alloy of claim 15, wherein the alloy has a critical casting thickness of at least 1 micrometer. 22. A metallic glass comprising an alloy of claim 15. 23. The metallic glass of claim 22, wherein the metallic glass has a glass transition temperature of at least 150° C. 24. The metallic glass of claim 22, wherein the metallic glass has a Vicker's hardness of at least 400 kgf/mm2. 25. The metallic glass of claim 22, wherein the metallic glass has a color having CIELAB coordinates with L* in the range of 65 to 120, a* in the range of −5 to 15, and b* in the range of 5 to 40. 26. A method of producing a metallic glass comprising:
melting an alloy comprising:
an atomic fraction of Au in the range of 40 to 90 percent,
an atomic fraction of Al in the range of 0.5 to 40 percent, and
an atomic fraction of RE is in the range of 1 to 20 percent; and
wherein RE is a rare earth metal into a molten state; and
quenching the melt at a cooling rate sufficiently high to prevent crystallization of the alloy. | The disclosure provides Au—Al-Rare-Earth metallic glass-forming alloys and metallic glasses comprising various other additions including but not limited to Cu, Pd, Sn and Mg. In certain embodiments, the metallic glasses according to the disclosure satisfy the 18-Karat Gold Alloy Hallmark, and demonstrate colors that include yellow and pink/rose.1. An alloy capable of forming a metallic glass, the alloy comprising:
an atomic fraction of Au in the range of 40 to 90 percent, an atomic fraction of Al in the range of 0.5 to 40 percent, and an atomic fraction of RE is in the range of 1 to 20 percent; and wherein RE is a rare earth metal. 2. The alloy of claim 1 wherein RE is selected from Y, Er, Dy and a combination thereof. 3. The alloy of claim 1, wherein the atomic fraction of Al is in the range of 2 to 20 percent. 4. The alloy of claim 2, wherein RE comprises Y in an atomic fraction of 3 to 15 percent. 5. The alloy of claim 1, further comprising an atomic fraction of Cu of up to 20 percent. 6. The alloy of claim 1, further comprising an atomic fraction of Pd of up to 25 percent. 7. The alloy of claim 1, further comprising Sn in an atomic fraction of up to 10 percent. 8. The alloy of claim 1, further comprising Mg in an atomic fraction of up to 20 percent. 9. The alloy of claim 1, further comprising at least one additional element selected from Ag, Pt, Rh, Ir, Fe, Ni, Co, Ru, Cr, Mo, Mn, Ti, Zr, Hf, W, Re, Be, Ca, Si, P, S, Ge, Ga, In, Sb, and Bi, or combinations thereof, in an atomic fraction of up to 10 percent. 10. The alloy of claim 1, wherein the alloy has a critical casting thickness of at least 1 micrometer. 11. A metallic glass comprising an alloy of claim 1. 12. The metallic glass of claim 11, wherein the metallic glass has a glass transition temperature of at least 150° C. 13. The metallic glass of claim 11, wherein the metallic glass has a Vicker's hardness of at least 400 kgf/mm2. 14. The metallic glass of claim 11, wherein the metallic glass has a color having CIELAB coordinates with L* in the range of 65 to 120, a* in the range of −5 to 15, and b* in the range of 5 to 40. 15. A metallic glass-forming alloy having a composition represented by the following formula (subscripts denote atomic percentages):
Au(100-a-b-c-d)AlaREbCucPdd where: a ranges from 0.5 to 40; b ranges from 1 to 20; c is up to 20; d up to 25; and wherein RE is a rare earth metal. 16. The metallic glass-forming alloy of claim 15, where a ranges from 2 to 20. 17. The metallic glass-forming alloy of claim 15, where b ranges from 3 to 15. 18. The metallic glass-forming alloy of claim 15, where c ranges from 0.5 to 10. 19. The metallic glass-forming alloy of claim 15, where d ranges from 0.5 to 20. 20. The metallic glass-forming alloy of claim 15, where the weight fraction of Au is at least 75 percent. 21. The metallic glass-forming alloy of claim 15, wherein the alloy has a critical casting thickness of at least 1 micrometer. 22. A metallic glass comprising an alloy of claim 15. 23. The metallic glass of claim 22, wherein the metallic glass has a glass transition temperature of at least 150° C. 24. The metallic glass of claim 22, wherein the metallic glass has a Vicker's hardness of at least 400 kgf/mm2. 25. The metallic glass of claim 22, wherein the metallic glass has a color having CIELAB coordinates with L* in the range of 65 to 120, a* in the range of −5 to 15, and b* in the range of 5 to 40. 26. A method of producing a metallic glass comprising:
melting an alloy comprising:
an atomic fraction of Au in the range of 40 to 90 percent,
an atomic fraction of Al in the range of 0.5 to 40 percent, and
an atomic fraction of RE is in the range of 1 to 20 percent; and
wherein RE is a rare earth metal into a molten state; and
quenching the melt at a cooling rate sufficiently high to prevent crystallization of the alloy. | 1,700 |
3,447 | 14,235,420 | 1,784 | The invention relates principally to a welded steel part with a very high mechanical strength characteristics obtained by heating followed by hot forming, then cooling of at least one welded blank obtained by butt welding of at least one first and one second sheet consisting at least in part of a steel substrate and a pre-coating which is constituted by an intermetallic alloy layer in contact with the steel substrate, topped by a metal alloy layer of aluminum or aluminum-based alloy.
This welded steel part claimed by the invention is essentially characterized in that the metal alloy layer ( 19, 20 ) has been removed from the edges ( 36 ) in direct proximity to the weld metal zone ( 35 ), while the intermetallic alloy layer ( 17, 18 ) has been left in place, and in that over at least a portion of the length of the weld metal zone ( 35 ), the ratio between the carbon content of the weld metal zone ( 35 ) and the carbon content of the substrate ( 25, 26 ) of either the first or the second sheet ( 11, 12 ) having the higher carbon content (Cmax) is between 1.27 and 1.59.
The invention likewise relates to a method for the fabrication of a welded steel part as well as the use of this welded steel part for the fabrication of structural or safety parts for automotive vehicles. | 1-29. (canceled) 30. A welded steel part obtained by heating in the austenitic range followed by hot forming, then cooling, of at least one welded blank obtained by a butt welding of at least a first and a second sheet comprising:
a steel substrate; and a pre-coating including an intermetallic alloy layer and a metal alloy layer of an aluminum or aluminum-base alloy, the intermetallic alloy layer contacting the steel substrate, the metal alloy layer topping the intermetallic alloy layer; a weld metal zone resulting from the welding operation and forming a bond between the first and second sheets; the metal alloy layer being removed from edges peripheral to the weld metal zone while the intermetallic alloy layer remains; over at least a portion of the weld metal zone, a ratio between a carbon content of the weld metal zone and a carbon content of the steel substrate of the first or second sheet having a higher carbon content Cmax, is between 1.27 and 1.59; a composition of the steel substrate of at least the first or the second sheet, comprises the following elements, expressed in per cent by weight: 0.10%≦C≦0.5% 0.5%≦Mn≦3% 0.1%≦Si≦1% 0.01%≦Cr≦1% Ti≦0.2% Al≦0.1% S≦0.05% P≦0.1% 0.0002%≦B≦0.010%,
the balance being iron and unavoidable impurities from processing. 31. The steel part as recited in claim 30, wherein the ratio between the hardness of the welded metal zone and the hardness of the substrate of one of the first or second sheets having a higher carbon content is greater than 1.029+(0.36 Cmax), whereby Cmax is expressed in per cent by weight. 32. The steel part as recited in claim 30, wherein the composition of the steel substrate of at least the first or second sheet includes the following elements, expressed in per cent by weight:
0.15%≦C≦0.4% 0.8%≦Mn≦2.3% 0.1%≦Si≦0.35% 0.01%≦Cr≦1% Ti≦0.1% Al≦0.1% S≦0.03% P≦0.05% 0.0005%≦B≦0.010%,
the balance being iron and unavoidable impurities from processing. 33. The steel part as recited in claim 30, wherein the composition of the steel substrate of at least the first or second sheet includes the following elements, expressed in per cent by weight:
0.15%≦C≦0.25% 0.8%≦Mn≦1.8% 0.1%≦Si≦0.35% 0.01%≦Cr≦0.5% Ti≦0.1% Al≦0.1% S≦0.05% P≦0.1% 0.0002%≦B≦0.005%,
the balance being iron and unavoidable impurities from processing. 34. The steel part as recited in claim 30, wherein the carbon content of the weld metal zone is less than or equal to 0.35% by weight. 35. The steel part as recited in claim 30, wherein the metal alloy layer of the pre-coating includes, expressed in per cent by weight, between 8 and 11% silicon and between 2 and 4% iron, the remainder of the metal alloy layer composition consisting of aluminum and unavoidable impurities. 36. The steel part as recited claim 30, wherein a microstructure of the weld metal zone includes no ferrite. 37. The steel part as recited in claim 30, wherein a microstructure of the weld metal zone is martensitic. 38. The steel part as recited in claim 30, wherein hot forming of the welded blank is performed by a hot stamping operation. 39. The steel part as recited in claim 30, wherein the aluminum or aluminum alloy of the metal alloy layer is removed from respective cut edges (of peripheral edges of the first and second sheets destined to undergo the welding operation. 40. A method for the fabrication of a welded steel part as recited in claim 30, comprising the steps of:
providing at least the first and the second steel sheet; removing the metal alloy layer from at least one surface of a portion of the peripheral edges of each of the first and second steel sheets; butt welding the first and the second steel sheets at a level of the respective edges of the first and second steel sheets from which the metal alloy layer has been removed with a laser source and using a filler metal wire over at least a portion of the welded metal zone, the filler metal wire having a carbon content higher than that of the steel substrates of at least one of the first or second sheets to obtain a welded blank; heating the welded blank to give the weld metal zone an austenitic structure; hot forming and heating the welded blank to obtain a steel part; and cooling the steel part at a controlled rate to obtain specified mechanical strength characteristics. 41. The method as recited in claim 40, wherein the metal alloy layer has been removed from each of the facing surfaces of the respective peripheral edges of each of the first and second steel sheets leaving the intermetallic alloy layer in place. 42. The method as recited in claim 40, wherein a width of a zone from which the metal alloy layer has been removed at the level of the peripheral edge of the first and second sheets destined to undergo the welding operation is between 0.2 and 2.2 mm. 43. The method as recited in claim 40, wherein a composition of the steel substrate of at least the first or second sheet includes the following elements, expressed in per cent by weight
0.15%≦C≦0.4% 0.8%≦Mn≦2.3% 0.1%≦Si≦0.35% 0.01%≦Cr≦1% Ti≦0.1% Al≦0.1% S≦0.03% P≦0.05% 0.0005%≦B≦0.010%,
the balance being iron and unavoidable impurities from processing. 44. The method as recited in claim 40, wherein the composition of the steel substrate of at least the first or the second sheet includes the following elements, expressed in per cent by weight:
0.15%≦C≦0.25% 0.8%≦Mn≦1.8% 0.1%≦Si≦0.35% 0.01%≦Cr≦0.5% Ti≦0.1% Al≦0.1% S≦0.05% P≦0.1% 0.0002%≦B≦0.005%,
the balance being iron and unavoidable impurities from processing. 45. The method as recited in claim 40, wherein during the step of butt welding, the peripheral edges of the first and second steel sheets to be welded are located at a distance of 0.1 mm or less from each other. 46. The method as recited in claim 40, wherein a linear welding energy of the laser source during the welding operation is greater than 0.3 kJ/cm. 47. The method as recited in claim 46, wherein the laser source is a CO2 gas laser type, which delivers a linear welding energy greater than 1.4 kJ/cm, or a solid-state laser type which delivers a linear welding energy greater than 0.3 kJ/cm. 48. The method as recited in claim 47, wherein a welding speed is between 3 meters/minute and 8 meters/minute, and a power of the CO2 gas laser is greater than or equal to 7 kW and a power of the solid state laser is greater than or equal to 4 kW. 49. The method as recited in claim 40, wherein the butt welding step is performed under a helium or argon cover gas. 50. The method as recited in claim 49, wherein a flow rate of helium or argon during the butt welding step is greater than or equal to 15 liters per minute. 51. The method as recited in claim 40, wherein the filler metal wire comprises the following elements, expressed in per cent by weight:
0.6%≦C≦1.5% 1%≦Mn≦4% 0.1%≦Si≦0.6% Cr≦2% Ti≦0.2%
the balance being iron and unavoidable impurities from processing. 52. The method as recited in claim 51, wherein the filler metal wire includes the following elements, expressed in per cent by weight:
0.65%≦C≦0.75% 1.95%≦Mn≦2.05% 0.35%≦Si≦0.45% 0.95%≦Cr≦1.05% 0.15%≦Ti≦0.25%
the balance being iron and unavoidable impurities from processing. 53. The method as recited in claim 52, wherein a proportion of filler metal relative to a volume of the weld metal zone is between 12% and 26% and the welding speed is between 3 and 7 meters/minute. 54. The method as recited in claim 53, wherein filler metal relative to the volume of the weld metal zone and the welding speed are within a range (50) illustrated in FIG. 8. 55. The method as recited in claim 54, wherein a proportion of filler metal relative to the volume of the weld metal zone is between 12% and 26%, the welding speed is between 3 and 7 meters per minute and when the welding speed is greater than 3.5 meters per minute, the proportion of filler metal relative to the volume of the weld metal zone and the welding speed is such that Y≦−3.86X+39.5, whereby Y designates the proportion of filler metal expressed as a volume per cent and X designates the welding speed expressed in meters per minute. 56. The method as recited in claim 53, wherein the proportion of filler metal relative to the volume of the weld metal zone is between 14 and 16%, a helium or argon flow rate is between 13 and 17 liters per minute, a diameter at a point of impact on the sheet of the laser beam is between 500 and 700 μm, and an extremity of the filler wire is at a distance from the point of impact of the laser beam on the sheet of between 2 and 3 mm. 57. The method as recited in claim 40, wherein a cooling rate of the weld metal zone during the hot forming step is greater than or equal to a critical martensitic hardening rate of the weld metal zone. 58. A structural or safety part for an automotive vehicle comprising:
a welded steel part as recited in claim 30. 59. The method as recited in claim 40, wherein the steps are performed successively. 60. The method as recited in claim 40, wherein the structure of the weld metal zone is completely austenitic. 61. The method as recited in claim 40, wherein on respective cut edges of the peripheral edges of the first and second sheets destined to be welded, the metal alloy layer is removed during a previous cutting operation of each of the first and second sheets. 62. The steel part as recited in claim 30, wherein the welded steel part includes a mechanical strength greater than 1230 MPa. | The invention relates principally to a welded steel part with a very high mechanical strength characteristics obtained by heating followed by hot forming, then cooling of at least one welded blank obtained by butt welding of at least one first and one second sheet consisting at least in part of a steel substrate and a pre-coating which is constituted by an intermetallic alloy layer in contact with the steel substrate, topped by a metal alloy layer of aluminum or aluminum-based alloy.
This welded steel part claimed by the invention is essentially characterized in that the metal alloy layer ( 19, 20 ) has been removed from the edges ( 36 ) in direct proximity to the weld metal zone ( 35 ), while the intermetallic alloy layer ( 17, 18 ) has been left in place, and in that over at least a portion of the length of the weld metal zone ( 35 ), the ratio between the carbon content of the weld metal zone ( 35 ) and the carbon content of the substrate ( 25, 26 ) of either the first or the second sheet ( 11, 12 ) having the higher carbon content (Cmax) is between 1.27 and 1.59.
The invention likewise relates to a method for the fabrication of a welded steel part as well as the use of this welded steel part for the fabrication of structural or safety parts for automotive vehicles.1-29. (canceled) 30. A welded steel part obtained by heating in the austenitic range followed by hot forming, then cooling, of at least one welded blank obtained by a butt welding of at least a first and a second sheet comprising:
a steel substrate; and a pre-coating including an intermetallic alloy layer and a metal alloy layer of an aluminum or aluminum-base alloy, the intermetallic alloy layer contacting the steel substrate, the metal alloy layer topping the intermetallic alloy layer; a weld metal zone resulting from the welding operation and forming a bond between the first and second sheets; the metal alloy layer being removed from edges peripheral to the weld metal zone while the intermetallic alloy layer remains; over at least a portion of the weld metal zone, a ratio between a carbon content of the weld metal zone and a carbon content of the steel substrate of the first or second sheet having a higher carbon content Cmax, is between 1.27 and 1.59; a composition of the steel substrate of at least the first or the second sheet, comprises the following elements, expressed in per cent by weight: 0.10%≦C≦0.5% 0.5%≦Mn≦3% 0.1%≦Si≦1% 0.01%≦Cr≦1% Ti≦0.2% Al≦0.1% S≦0.05% P≦0.1% 0.0002%≦B≦0.010%,
the balance being iron and unavoidable impurities from processing. 31. The steel part as recited in claim 30, wherein the ratio between the hardness of the welded metal zone and the hardness of the substrate of one of the first or second sheets having a higher carbon content is greater than 1.029+(0.36 Cmax), whereby Cmax is expressed in per cent by weight. 32. The steel part as recited in claim 30, wherein the composition of the steel substrate of at least the first or second sheet includes the following elements, expressed in per cent by weight:
0.15%≦C≦0.4% 0.8%≦Mn≦2.3% 0.1%≦Si≦0.35% 0.01%≦Cr≦1% Ti≦0.1% Al≦0.1% S≦0.03% P≦0.05% 0.0005%≦B≦0.010%,
the balance being iron and unavoidable impurities from processing. 33. The steel part as recited in claim 30, wherein the composition of the steel substrate of at least the first or second sheet includes the following elements, expressed in per cent by weight:
0.15%≦C≦0.25% 0.8%≦Mn≦1.8% 0.1%≦Si≦0.35% 0.01%≦Cr≦0.5% Ti≦0.1% Al≦0.1% S≦0.05% P≦0.1% 0.0002%≦B≦0.005%,
the balance being iron and unavoidable impurities from processing. 34. The steel part as recited in claim 30, wherein the carbon content of the weld metal zone is less than or equal to 0.35% by weight. 35. The steel part as recited in claim 30, wherein the metal alloy layer of the pre-coating includes, expressed in per cent by weight, between 8 and 11% silicon and between 2 and 4% iron, the remainder of the metal alloy layer composition consisting of aluminum and unavoidable impurities. 36. The steel part as recited claim 30, wherein a microstructure of the weld metal zone includes no ferrite. 37. The steel part as recited in claim 30, wherein a microstructure of the weld metal zone is martensitic. 38. The steel part as recited in claim 30, wherein hot forming of the welded blank is performed by a hot stamping operation. 39. The steel part as recited in claim 30, wherein the aluminum or aluminum alloy of the metal alloy layer is removed from respective cut edges (of peripheral edges of the first and second sheets destined to undergo the welding operation. 40. A method for the fabrication of a welded steel part as recited in claim 30, comprising the steps of:
providing at least the first and the second steel sheet; removing the metal alloy layer from at least one surface of a portion of the peripheral edges of each of the first and second steel sheets; butt welding the first and the second steel sheets at a level of the respective edges of the first and second steel sheets from which the metal alloy layer has been removed with a laser source and using a filler metal wire over at least a portion of the welded metal zone, the filler metal wire having a carbon content higher than that of the steel substrates of at least one of the first or second sheets to obtain a welded blank; heating the welded blank to give the weld metal zone an austenitic structure; hot forming and heating the welded blank to obtain a steel part; and cooling the steel part at a controlled rate to obtain specified mechanical strength characteristics. 41. The method as recited in claim 40, wherein the metal alloy layer has been removed from each of the facing surfaces of the respective peripheral edges of each of the first and second steel sheets leaving the intermetallic alloy layer in place. 42. The method as recited in claim 40, wherein a width of a zone from which the metal alloy layer has been removed at the level of the peripheral edge of the first and second sheets destined to undergo the welding operation is between 0.2 and 2.2 mm. 43. The method as recited in claim 40, wherein a composition of the steel substrate of at least the first or second sheet includes the following elements, expressed in per cent by weight
0.15%≦C≦0.4% 0.8%≦Mn≦2.3% 0.1%≦Si≦0.35% 0.01%≦Cr≦1% Ti≦0.1% Al≦0.1% S≦0.03% P≦0.05% 0.0005%≦B≦0.010%,
the balance being iron and unavoidable impurities from processing. 44. The method as recited in claim 40, wherein the composition of the steel substrate of at least the first or the second sheet includes the following elements, expressed in per cent by weight:
0.15%≦C≦0.25% 0.8%≦Mn≦1.8% 0.1%≦Si≦0.35% 0.01%≦Cr≦0.5% Ti≦0.1% Al≦0.1% S≦0.05% P≦0.1% 0.0002%≦B≦0.005%,
the balance being iron and unavoidable impurities from processing. 45. The method as recited in claim 40, wherein during the step of butt welding, the peripheral edges of the first and second steel sheets to be welded are located at a distance of 0.1 mm or less from each other. 46. The method as recited in claim 40, wherein a linear welding energy of the laser source during the welding operation is greater than 0.3 kJ/cm. 47. The method as recited in claim 46, wherein the laser source is a CO2 gas laser type, which delivers a linear welding energy greater than 1.4 kJ/cm, or a solid-state laser type which delivers a linear welding energy greater than 0.3 kJ/cm. 48. The method as recited in claim 47, wherein a welding speed is between 3 meters/minute and 8 meters/minute, and a power of the CO2 gas laser is greater than or equal to 7 kW and a power of the solid state laser is greater than or equal to 4 kW. 49. The method as recited in claim 40, wherein the butt welding step is performed under a helium or argon cover gas. 50. The method as recited in claim 49, wherein a flow rate of helium or argon during the butt welding step is greater than or equal to 15 liters per minute. 51. The method as recited in claim 40, wherein the filler metal wire comprises the following elements, expressed in per cent by weight:
0.6%≦C≦1.5% 1%≦Mn≦4% 0.1%≦Si≦0.6% Cr≦2% Ti≦0.2%
the balance being iron and unavoidable impurities from processing. 52. The method as recited in claim 51, wherein the filler metal wire includes the following elements, expressed in per cent by weight:
0.65%≦C≦0.75% 1.95%≦Mn≦2.05% 0.35%≦Si≦0.45% 0.95%≦Cr≦1.05% 0.15%≦Ti≦0.25%
the balance being iron and unavoidable impurities from processing. 53. The method as recited in claim 52, wherein a proportion of filler metal relative to a volume of the weld metal zone is between 12% and 26% and the welding speed is between 3 and 7 meters/minute. 54. The method as recited in claim 53, wherein filler metal relative to the volume of the weld metal zone and the welding speed are within a range (50) illustrated in FIG. 8. 55. The method as recited in claim 54, wherein a proportion of filler metal relative to the volume of the weld metal zone is between 12% and 26%, the welding speed is between 3 and 7 meters per minute and when the welding speed is greater than 3.5 meters per minute, the proportion of filler metal relative to the volume of the weld metal zone and the welding speed is such that Y≦−3.86X+39.5, whereby Y designates the proportion of filler metal expressed as a volume per cent and X designates the welding speed expressed in meters per minute. 56. The method as recited in claim 53, wherein the proportion of filler metal relative to the volume of the weld metal zone is between 14 and 16%, a helium or argon flow rate is between 13 and 17 liters per minute, a diameter at a point of impact on the sheet of the laser beam is between 500 and 700 μm, and an extremity of the filler wire is at a distance from the point of impact of the laser beam on the sheet of between 2 and 3 mm. 57. The method as recited in claim 40, wherein a cooling rate of the weld metal zone during the hot forming step is greater than or equal to a critical martensitic hardening rate of the weld metal zone. 58. A structural or safety part for an automotive vehicle comprising:
a welded steel part as recited in claim 30. 59. The method as recited in claim 40, wherein the steps are performed successively. 60. The method as recited in claim 40, wherein the structure of the weld metal zone is completely austenitic. 61. The method as recited in claim 40, wherein on respective cut edges of the peripheral edges of the first and second sheets destined to be welded, the metal alloy layer is removed during a previous cutting operation of each of the first and second sheets. 62. The steel part as recited in claim 30, wherein the welded steel part includes a mechanical strength greater than 1230 MPa. | 1,700 |
3,448 | 14,136,660 | 1,772 | Quaternary phosphonium haloaluminate compounds according to Formula (I):
are provided herein, wherein
R 1 -R 3 are the same or different and each is chosen from a hydrocarbyl; R 4 is different than R 1 -R 3 and is chosen from a hydrocarbyl; and X is a halogen. | 1. A quaternary phosphonium haloaluminate compound according to Formula (I):
wherein
R1-R3 are the same or different and each is chosen from a C1-C8 hydrocarbyl;
R4 is different than R1-R3 and is chosen from a C1-C15 hydrocarbyl; and
X is a halogen. 2. A compound according to Formula (I) of claim 1, wherein R1-R3 are the same. 3. A compound according to Formula (I) of claim 2, wherein R4 comprises at least one more carbon atom than each of R1-R3. 4. A compound according to Formula (I) of claim 1, wherein R4 is a C4-C12 hydrocarbyl. 5. A compound according to Formula (I) of claim 2, wherein each of R1-R3 is a C3-C6 alkyl. 6. A compound according to Formula (I) of claim 5, wherein each of R1-R3 is butyl. 7. A compound according to Formula (I) of claim 1, wherein R4 is a C5-C8 alkyl. 8. A compound according to Formula (I) of claim 7, wherein R4 is pentyl or hexyl. 9. A compound according to Formula (I) of claim 1, wherein the quaternary phosphonium haloaluminate is selected from the group consisting of tripropylhexylphosphonium-Al2X7; tributylmethylphosphonium-Al2X7; tributylpentylphosphonium-Al2X7; tributylhexylphosphonium-Al2X7; tributylheptylphosphonium-Al2X7; tributyloctylphosphonium-Al2X7; tributylnonylphosphonium-Al2X7; tributyldecylphosphonium-Al2X7; tributylundecylphosphonium-Al2X7; tributyldodecylphosphonium-Al2X7; and tributyltetradecylphosphonium-Al2X7. 10. A compound according to Formula (I) of claim 9, wherein the quaternary phosphonium haloaluminate is tributylpentylphosphonium-Al2X7. 11. A compound according to Formula (I) of claim 9, wherein the quaternary phosphonium haloaluminate is tributylhexylphosphonium-Al2X7. 12. A compound according to Formula (I) of claim 11, wherein the quaternary phosphonium haloaluminate is tri-n-butyl-hexylphosphonium-Al2X7. 13. A compound according to Formula (I) of claim 9, wherein the quaternary phosphonium haloaluminate is tributylheptylphosphonium-Al2X7. 14. A compound according to Formula (I) of claim 9, wherein the quaternary phosphonium haloaluminate is tributyloctylphosphonium-Al2X7. 15. A compound according to Formula (I) of claim 9, wherein the quaternary phosphonium haloaluminate is tributyldodecylphosphonium-Al2X7. 16. A compound according to Formula (I) of claim 1, wherein X is selected from the group consisting of F, Cl, Br, and I. 17. A compound according to Formula (I) of claim 16, wherein X is Cl. 18. An ionic liquid composition comprising one or more quaternary phosphonium haloaluminate compounds as defined in claim 1. 19. An ionic liquid composition according to claim 18, wherein the one or more quaternary phosphonium haloaluminate is selected from the group consisting of tripropylhexylphosphonium-Al2X7; tributylmethylphosphonium-Al2X7; tributylpentylphosphonium-Al2X7; tributylhexylphosphonium-Al2X7; tributylheptylphosphonium-Al2X7; tributyloctylphosphonium-Al2X7; tributylnonylphosphonium-Al2X7; tributyldecylphosphonium-Al2X7; tributylundecylphosphonium-Al2X7; tributyldodecylphosphonium-Al2X7; and tributyltetradecylphosphonium-Al2X7. 20. An ionic liquid catalyst for reacting olefins and isoparaffins to generate an alkylate, said catalyst comprising a quaternary phosphonium haloaluminate compound as defined in claim 1. 21. An ionic liquid catalyst according to claim 20, wherein the catalyst has an initial kinematic viscosity of at least 50 cSt at a temperature of 20° C. 22. An ionic liquid catalyst according to claim 20, wherein the catalyst has an initial kinematic viscosity of at least 20 cSt at a temperature of 50° C. 23. An ionic liquid catalyst according to claim 20, wherein the boiling point at atmospheric pressure of HR4 of the phosphonium haloaluminate compound is at least 30° C. greater than the boiling point at atmospheric pressure of HR1. 24. An ionic liquid catalyst according to claim 20 further comprising a co-catalyst, wherein said ionic liquid catalyst is coupled with the co-catalyst. 25. An ionic liquid catalyst according to claim 24, wherein the co-catalyst is a Brønsted acid selected from the group consisting of HCl, HBr, HI, and mixtures thereof. 26. An ionic liquid catalyst according to claim 25, wherein said Brønsted acid co-catalyst is HCl. | Quaternary phosphonium haloaluminate compounds according to Formula (I):
are provided herein, wherein
R 1 -R 3 are the same or different and each is chosen from a hydrocarbyl; R 4 is different than R 1 -R 3 and is chosen from a hydrocarbyl; and X is a halogen.1. A quaternary phosphonium haloaluminate compound according to Formula (I):
wherein
R1-R3 are the same or different and each is chosen from a C1-C8 hydrocarbyl;
R4 is different than R1-R3 and is chosen from a C1-C15 hydrocarbyl; and
X is a halogen. 2. A compound according to Formula (I) of claim 1, wherein R1-R3 are the same. 3. A compound according to Formula (I) of claim 2, wherein R4 comprises at least one more carbon atom than each of R1-R3. 4. A compound according to Formula (I) of claim 1, wherein R4 is a C4-C12 hydrocarbyl. 5. A compound according to Formula (I) of claim 2, wherein each of R1-R3 is a C3-C6 alkyl. 6. A compound according to Formula (I) of claim 5, wherein each of R1-R3 is butyl. 7. A compound according to Formula (I) of claim 1, wherein R4 is a C5-C8 alkyl. 8. A compound according to Formula (I) of claim 7, wherein R4 is pentyl or hexyl. 9. A compound according to Formula (I) of claim 1, wherein the quaternary phosphonium haloaluminate is selected from the group consisting of tripropylhexylphosphonium-Al2X7; tributylmethylphosphonium-Al2X7; tributylpentylphosphonium-Al2X7; tributylhexylphosphonium-Al2X7; tributylheptylphosphonium-Al2X7; tributyloctylphosphonium-Al2X7; tributylnonylphosphonium-Al2X7; tributyldecylphosphonium-Al2X7; tributylundecylphosphonium-Al2X7; tributyldodecylphosphonium-Al2X7; and tributyltetradecylphosphonium-Al2X7. 10. A compound according to Formula (I) of claim 9, wherein the quaternary phosphonium haloaluminate is tributylpentylphosphonium-Al2X7. 11. A compound according to Formula (I) of claim 9, wherein the quaternary phosphonium haloaluminate is tributylhexylphosphonium-Al2X7. 12. A compound according to Formula (I) of claim 11, wherein the quaternary phosphonium haloaluminate is tri-n-butyl-hexylphosphonium-Al2X7. 13. A compound according to Formula (I) of claim 9, wherein the quaternary phosphonium haloaluminate is tributylheptylphosphonium-Al2X7. 14. A compound according to Formula (I) of claim 9, wherein the quaternary phosphonium haloaluminate is tributyloctylphosphonium-Al2X7. 15. A compound according to Formula (I) of claim 9, wherein the quaternary phosphonium haloaluminate is tributyldodecylphosphonium-Al2X7. 16. A compound according to Formula (I) of claim 1, wherein X is selected from the group consisting of F, Cl, Br, and I. 17. A compound according to Formula (I) of claim 16, wherein X is Cl. 18. An ionic liquid composition comprising one or more quaternary phosphonium haloaluminate compounds as defined in claim 1. 19. An ionic liquid composition according to claim 18, wherein the one or more quaternary phosphonium haloaluminate is selected from the group consisting of tripropylhexylphosphonium-Al2X7; tributylmethylphosphonium-Al2X7; tributylpentylphosphonium-Al2X7; tributylhexylphosphonium-Al2X7; tributylheptylphosphonium-Al2X7; tributyloctylphosphonium-Al2X7; tributylnonylphosphonium-Al2X7; tributyldecylphosphonium-Al2X7; tributylundecylphosphonium-Al2X7; tributyldodecylphosphonium-Al2X7; and tributyltetradecylphosphonium-Al2X7. 20. An ionic liquid catalyst for reacting olefins and isoparaffins to generate an alkylate, said catalyst comprising a quaternary phosphonium haloaluminate compound as defined in claim 1. 21. An ionic liquid catalyst according to claim 20, wherein the catalyst has an initial kinematic viscosity of at least 50 cSt at a temperature of 20° C. 22. An ionic liquid catalyst according to claim 20, wherein the catalyst has an initial kinematic viscosity of at least 20 cSt at a temperature of 50° C. 23. An ionic liquid catalyst according to claim 20, wherein the boiling point at atmospheric pressure of HR4 of the phosphonium haloaluminate compound is at least 30° C. greater than the boiling point at atmospheric pressure of HR1. 24. An ionic liquid catalyst according to claim 20 further comprising a co-catalyst, wherein said ionic liquid catalyst is coupled with the co-catalyst. 25. An ionic liquid catalyst according to claim 24, wherein the co-catalyst is a Brønsted acid selected from the group consisting of HCl, HBr, HI, and mixtures thereof. 26. An ionic liquid catalyst according to claim 25, wherein said Brønsted acid co-catalyst is HCl. | 1,700 |
3,449 | 15,160,287 | 1,723 | The present invention relates to a method for forming and transferring an unbonded fibrous structure to a carrier, the method comprising the steps of: receiving fibrous material on a shell travelling at a first speed through a receiving zone to form a fibrous patch; transferring the shell from the receiving zone to an application zone; applying the fibrous patch to the carrier travelling at a second speed through the application zone; and controlling the speed of the shell by a motor, the motor comprising a stator and at least one mover; wherein the shell is driven by at least one mover, wherein the mover maintains the shell at the first speed in the receiving zone and the second speed in the application zone, and wherein the mover is mounted on a stationary track. | 1. A method for forming and transferring an unbonded fibrous structure to a carrier, the method comprising the steps of:
receiving fibrous material on a shell travelling at a first speed through a receiving zone to form a fibrous patch; transferring the shell from the receiving zone to an application zone; applying the fibrous patch to the carrier travelling at a second speed through the application zone; and controlling the speed of the shell by a motor, the motor comprising a stator and at least one mover; and wherein the shell is driven by at least one mover, wherein the mover maintains the shell at the first speed in the receiving zone and the second speed in the application zone, and wherein the mover is mounted on a stationary track. 2. The method of claim 1, wherein the stator comprises a plurality of stationary electromagnets. 3. The method of claim 2, wherein the movers comprise permanent magnets and wherein the variable speed of the movers along the stationary track is controlled by varying the current supplied to the stationary electromagnets. 4. The method of claim 1, wherein the stationary track follows a continuous, closed path. 5. The method of claim 4, wherein the closed, continuous path is a circular path. 6. The method of claim 1, wherein the fibrous material is held against the shell, at least in the receiving zone by vacuum. 7. The method of claim 1, wherein a plurality of shells travel at the first speed through the receiving zone and at a second speed through the application zone, and wherein the speed of each shell is independently controlled by at least one mover. | The present invention relates to a method for forming and transferring an unbonded fibrous structure to a carrier, the method comprising the steps of: receiving fibrous material on a shell travelling at a first speed through a receiving zone to form a fibrous patch; transferring the shell from the receiving zone to an application zone; applying the fibrous patch to the carrier travelling at a second speed through the application zone; and controlling the speed of the shell by a motor, the motor comprising a stator and at least one mover; wherein the shell is driven by at least one mover, wherein the mover maintains the shell at the first speed in the receiving zone and the second speed in the application zone, and wherein the mover is mounted on a stationary track.1. A method for forming and transferring an unbonded fibrous structure to a carrier, the method comprising the steps of:
receiving fibrous material on a shell travelling at a first speed through a receiving zone to form a fibrous patch; transferring the shell from the receiving zone to an application zone; applying the fibrous patch to the carrier travelling at a second speed through the application zone; and controlling the speed of the shell by a motor, the motor comprising a stator and at least one mover; and wherein the shell is driven by at least one mover, wherein the mover maintains the shell at the first speed in the receiving zone and the second speed in the application zone, and wherein the mover is mounted on a stationary track. 2. The method of claim 1, wherein the stator comprises a plurality of stationary electromagnets. 3. The method of claim 2, wherein the movers comprise permanent magnets and wherein the variable speed of the movers along the stationary track is controlled by varying the current supplied to the stationary electromagnets. 4. The method of claim 1, wherein the stationary track follows a continuous, closed path. 5. The method of claim 4, wherein the closed, continuous path is a circular path. 6. The method of claim 1, wherein the fibrous material is held against the shell, at least in the receiving zone by vacuum. 7. The method of claim 1, wherein a plurality of shells travel at the first speed through the receiving zone and at a second speed through the application zone, and wherein the speed of each shell is independently controlled by at least one mover. | 1,700 |
3,450 | 15,448,267 | 1,735 | A method of forming an engine component according to an exemplary aspect of the present disclosure includes, among other things, introducing molten metal into a cavity between a shell and a casting article in the shell. The casting article includes a ceramic portion and a plurality of fibers. The method further includes separately removing the ceramic portion and the fibers from an interior of the component. | 1. A method of forming an engine component, comprising:
introducing molten metal into a cavity between a shell and a casting article in the shell, the casting article including a ceramic portion and a plurality of fibers; and separately removing the ceramic portion and the fibers from an interior of the component. 2. The method as recited in claim 1, further comprising:
cooling the molten metal, wherein the plurality of fibers and the ceramic portion are removed after the molten metal cools. 3. The method as recited in claim 2, wherein the ceramic portion is removed from the component using a leaching fluid, and the fibers are mechanically removed from the component. 4. The method as recited in claim 3, wherein the fibers are blown out of the component using a pressurized fluid. 5. The method as recited in claim 4, wherein the pressurized fluid is pressurized air. 6. The method as recited in claim 4, wherein a maximum length of the fibers is less than a smallest orifice formed in the engine component. 7. The method as recited in claim 1, wherein the fibers dissolve during the introducing step. 8. The method as recited in claim 7, wherein the fibers fully dissolve during the introducing step. 9. The method as recited in claim 7, wherein, after the molten metal cools, the remainder of the casting article is removed from the component using a leaching fluid. 10. The method as recited in claim 7, wherein the size and chemical composition of the fibers is selected such that the fibers will intentionally dissolve during the introducing step. 11. The method as recited in claim 1, wherein the fibers are randomly oriented within the ceramic portion. 12. The method as recited in claim 11, wherein the ceramic portion includes alumina (Al2O3). 13. The method as recited in claim 1, wherein the fibers are provided by one of (1) silicon (Si) fibers, (2) carbon (C) fibers, and (3) metal fibers. 14. A method of forming an engine component, comprising:
introducing molten metal into a cavity between a shell and a casting article, the casting article including a ceramic portion and a plurality of fibers; dissolving the fibers during the introducing step; and removing the remainder of the casting article from the interior of the component using a leaching fluid. 15. The method as recited in claim 14, wherein the size and material of the fibers is selected such that the fibers will intentionally dissolve during the introducing step. 16. The method as recited in claim 14, wherein the fibers completely dissolve during the introducing step. 17. The method as recited in claim 14, wherein the ceramic portion includes alumina (Al2O3). 18. The method as recited in claim 14, wherein the fibers are provided by one of (1) silicon (Si) fibers, (2) carbon (C) fibers, and (3) metal fibers. 19. A method of forming an engine component, comprising:
providing a ceramic shell and a casting article, the casting article including a ceramic portion and a plurality of fibers; sintering the ceramic shell and the casting article, wherein the plurality of fibers are dissolved by the sintering step; introducing a molten metal between the shell and the casting article; and removing the remainder of the casting article from the interior of the component. | A method of forming an engine component according to an exemplary aspect of the present disclosure includes, among other things, introducing molten metal into a cavity between a shell and a casting article in the shell. The casting article includes a ceramic portion and a plurality of fibers. The method further includes separately removing the ceramic portion and the fibers from an interior of the component.1. A method of forming an engine component, comprising:
introducing molten metal into a cavity between a shell and a casting article in the shell, the casting article including a ceramic portion and a plurality of fibers; and separately removing the ceramic portion and the fibers from an interior of the component. 2. The method as recited in claim 1, further comprising:
cooling the molten metal, wherein the plurality of fibers and the ceramic portion are removed after the molten metal cools. 3. The method as recited in claim 2, wherein the ceramic portion is removed from the component using a leaching fluid, and the fibers are mechanically removed from the component. 4. The method as recited in claim 3, wherein the fibers are blown out of the component using a pressurized fluid. 5. The method as recited in claim 4, wherein the pressurized fluid is pressurized air. 6. The method as recited in claim 4, wherein a maximum length of the fibers is less than a smallest orifice formed in the engine component. 7. The method as recited in claim 1, wherein the fibers dissolve during the introducing step. 8. The method as recited in claim 7, wherein the fibers fully dissolve during the introducing step. 9. The method as recited in claim 7, wherein, after the molten metal cools, the remainder of the casting article is removed from the component using a leaching fluid. 10. The method as recited in claim 7, wherein the size and chemical composition of the fibers is selected such that the fibers will intentionally dissolve during the introducing step. 11. The method as recited in claim 1, wherein the fibers are randomly oriented within the ceramic portion. 12. The method as recited in claim 11, wherein the ceramic portion includes alumina (Al2O3). 13. The method as recited in claim 1, wherein the fibers are provided by one of (1) silicon (Si) fibers, (2) carbon (C) fibers, and (3) metal fibers. 14. A method of forming an engine component, comprising:
introducing molten metal into a cavity between a shell and a casting article, the casting article including a ceramic portion and a plurality of fibers; dissolving the fibers during the introducing step; and removing the remainder of the casting article from the interior of the component using a leaching fluid. 15. The method as recited in claim 14, wherein the size and material of the fibers is selected such that the fibers will intentionally dissolve during the introducing step. 16. The method as recited in claim 14, wherein the fibers completely dissolve during the introducing step. 17. The method as recited in claim 14, wherein the ceramic portion includes alumina (Al2O3). 18. The method as recited in claim 14, wherein the fibers are provided by one of (1) silicon (Si) fibers, (2) carbon (C) fibers, and (3) metal fibers. 19. A method of forming an engine component, comprising:
providing a ceramic shell and a casting article, the casting article including a ceramic portion and a plurality of fibers; sintering the ceramic shell and the casting article, wherein the plurality of fibers are dissolved by the sintering step; introducing a molten metal between the shell and the casting article; and removing the remainder of the casting article from the interior of the component. | 1,700 |
3,451 | 15,585,920 | 1,777 | The invention relates to a method and apparatus for treatment of produced or process water from hydrocarbon production to reduce the volume of the produced or process water while simultaneously reducing the salinity of a highly saline stream, for example, the brine from a seawater desalination plant. The method includes causing a feed stream comprising produced or process water to flow through the lumen of a hollow fiber osmotic membrane 4 which is immersed in an open channel 2 or tank of flowing draw solution 6 which has high salinity. In this way, water from the feed stream is drawn through the osmotic membrane 4 by an osmotic pressure differential caused by the difference in salinity between the feed stream and the draw solution 6. | 1. A method for the treatment of produced or process water from hydrocarbon production to reduce the volume of the produced or process water, the method comprising:
a) causing a feed stream comprising produced or process water to flow through a lumen of a hollow fiber osmotic membrane; b) causing a draw solution comprising saline water of higher salinity than the produced or process water to flow past the outside of the hollow fiber osmotic membrane; c) whereby water from the feed stream is drawn through the osmotic membrane by osmotic pressure differential caused by a difference in salinity between the feed stream and the draw solution; wherein d) the saline water flows in an open channel or tank and the hollow fiber osmotic membrane is arranged in an immersed membrane configuration in the open channel or tank. 2. The method claimed in claim 1 wherein the feed stream is passed through between 1,000 and 10,000,000 hollow fiber membranes, preferably between 50,000 and 1,000,000, in a combination of series and parallel arrangements. 3. The method claimed in claim 2 wherein the feed stream is passed through more than 2 hollow fiber membranes connected sequentially in series, such as between 2 and 40 fiber membranes in series. 4. The method claimed in claim 1 wherein the membrane is part of a membrane module, the module comprising a plurality, such as between 250 and 5,000, fiber membranes mounted therein with respective ends of the fiber membranes mounted in an inlet header and an outlet header of the module. 5. The method of claim 4, wherein two or more said membrane modules are arranged in a frame. 6. The method of claim 5, wherein the lumens of two or more fiber membranes in respective modules and/or respective frames communicate in series. 7. The method claimed in claim 1 wherein the volume of the produced or process water is reduced by more than 25%, optionally more than 50%. 8. The method claimed in claim 1 wherein the volume of the produced or process water is reduced by between 25% and 90%, for example between 50% and 75%. 9. The method claimed in claim 1 wherein the draw solution is seawater, saline effluent from a water desalination plant or hypersaline groundwater. 10. The method claimed in claim 1, further comprising taking the feed stream downstream of the osmotic membranes and injecting it into a disposal well. 11. The method claimed in claim 1, further comprising taking the feed stream downstream of the osmotic membranes and treating it further prior to disposal. 12. The method claimed in claim 1, further comprising taking the draw solution downstream of the osmotic membranes and passing it into a desalination process or into the sea. 13. The method as claimed in claim 1, wherein the osmotic pressure differential is in the range 5 to 250 bar, optionally 10 to 60 bar. 14. The method as claimed in claim 1, wherein the produced or process water is subject to pre-treatment processes including suspended solids removal and oil removal. 15. The method of claim 1, wherein the interior diameter of the lumens of the hollow fiber membranes is between 0.1mm and 2.0 mm and the length of each hollow fiber membrane is between 0.25 m and 2.0 m. 16. The method of claim 1 wherein the feed water passes along the lumen of a continuous fiber membrane or series of sequentially connected fiber membranes of total length between 0.25 m and 80 m, optionally between 1 m and 40 m, such as between 5 m and 20 m, more particularly between 2 m and 10 m, and wherein the internal diameter of the fiber lumen is between 0.1 mm and 2.0 mm, optionally between 0.6 mm and 1.6 mm. 17. Apparatus for the treatment of produced or process water from hydrocarbon production to reduce the volume of the produced or process water, the apparatus comprising a plurality of hollow fiber osmotic membranes mounted in modules adapted for immersion in an open channel or tank, wherein at least two of said fiber membranes communicate in series. 18. The apparatus as claimed in claim 17, wherein two or more said membrane modules are provided, and wherein the lumen of at least one fiber membrane in one of said modules communicates in series with the lumen of at least one fiber membrane in a second one of said modules. 19. The apparatus as claimed in claim 17, wherein two or more said membrane modules are arranged in a frame adapted for immersion in said open channel or tank. 20. The apparatus as claimed in claim 19, wherein at least two said frames with modules mounted therein are connected such that the lumen of at least one fiber membrane in one of said frames communicates in series with the lumen of at least one fiber membrane in a second one of said frames. 21. The apparatus of claim 17, wherein the fiber membrane lumens have an internal diameter between 0.1 mm and 2.0 mm and said at least two series connected fiber membranes have total combined length of lumen between 0.25 m and 80 m, optionally between 1 m and 40 m, such as between 5 m and 20 m, more particularly between 2 m and 10 m. 22. A system comprising the apparatus as claimed in claim 17 together with an open channel or tank containing flowing draw solution in which the said apparatus is immersed, and a pumped supply of produced or process water communicating with the lumens of the fiber membranes, the draw solution having a higher salinity than the produced or process water. | The invention relates to a method and apparatus for treatment of produced or process water from hydrocarbon production to reduce the volume of the produced or process water while simultaneously reducing the salinity of a highly saline stream, for example, the brine from a seawater desalination plant. The method includes causing a feed stream comprising produced or process water to flow through the lumen of a hollow fiber osmotic membrane 4 which is immersed in an open channel 2 or tank of flowing draw solution 6 which has high salinity. In this way, water from the feed stream is drawn through the osmotic membrane 4 by an osmotic pressure differential caused by the difference in salinity between the feed stream and the draw solution 6.1. A method for the treatment of produced or process water from hydrocarbon production to reduce the volume of the produced or process water, the method comprising:
a) causing a feed stream comprising produced or process water to flow through a lumen of a hollow fiber osmotic membrane; b) causing a draw solution comprising saline water of higher salinity than the produced or process water to flow past the outside of the hollow fiber osmotic membrane; c) whereby water from the feed stream is drawn through the osmotic membrane by osmotic pressure differential caused by a difference in salinity between the feed stream and the draw solution; wherein d) the saline water flows in an open channel or tank and the hollow fiber osmotic membrane is arranged in an immersed membrane configuration in the open channel or tank. 2. The method claimed in claim 1 wherein the feed stream is passed through between 1,000 and 10,000,000 hollow fiber membranes, preferably between 50,000 and 1,000,000, in a combination of series and parallel arrangements. 3. The method claimed in claim 2 wherein the feed stream is passed through more than 2 hollow fiber membranes connected sequentially in series, such as between 2 and 40 fiber membranes in series. 4. The method claimed in claim 1 wherein the membrane is part of a membrane module, the module comprising a plurality, such as between 250 and 5,000, fiber membranes mounted therein with respective ends of the fiber membranes mounted in an inlet header and an outlet header of the module. 5. The method of claim 4, wherein two or more said membrane modules are arranged in a frame. 6. The method of claim 5, wherein the lumens of two or more fiber membranes in respective modules and/or respective frames communicate in series. 7. The method claimed in claim 1 wherein the volume of the produced or process water is reduced by more than 25%, optionally more than 50%. 8. The method claimed in claim 1 wherein the volume of the produced or process water is reduced by between 25% and 90%, for example between 50% and 75%. 9. The method claimed in claim 1 wherein the draw solution is seawater, saline effluent from a water desalination plant or hypersaline groundwater. 10. The method claimed in claim 1, further comprising taking the feed stream downstream of the osmotic membranes and injecting it into a disposal well. 11. The method claimed in claim 1, further comprising taking the feed stream downstream of the osmotic membranes and treating it further prior to disposal. 12. The method claimed in claim 1, further comprising taking the draw solution downstream of the osmotic membranes and passing it into a desalination process or into the sea. 13. The method as claimed in claim 1, wherein the osmotic pressure differential is in the range 5 to 250 bar, optionally 10 to 60 bar. 14. The method as claimed in claim 1, wherein the produced or process water is subject to pre-treatment processes including suspended solids removal and oil removal. 15. The method of claim 1, wherein the interior diameter of the lumens of the hollow fiber membranes is between 0.1mm and 2.0 mm and the length of each hollow fiber membrane is between 0.25 m and 2.0 m. 16. The method of claim 1 wherein the feed water passes along the lumen of a continuous fiber membrane or series of sequentially connected fiber membranes of total length between 0.25 m and 80 m, optionally between 1 m and 40 m, such as between 5 m and 20 m, more particularly between 2 m and 10 m, and wherein the internal diameter of the fiber lumen is between 0.1 mm and 2.0 mm, optionally between 0.6 mm and 1.6 mm. 17. Apparatus for the treatment of produced or process water from hydrocarbon production to reduce the volume of the produced or process water, the apparatus comprising a plurality of hollow fiber osmotic membranes mounted in modules adapted for immersion in an open channel or tank, wherein at least two of said fiber membranes communicate in series. 18. The apparatus as claimed in claim 17, wherein two or more said membrane modules are provided, and wherein the lumen of at least one fiber membrane in one of said modules communicates in series with the lumen of at least one fiber membrane in a second one of said modules. 19. The apparatus as claimed in claim 17, wherein two or more said membrane modules are arranged in a frame adapted for immersion in said open channel or tank. 20. The apparatus as claimed in claim 19, wherein at least two said frames with modules mounted therein are connected such that the lumen of at least one fiber membrane in one of said frames communicates in series with the lumen of at least one fiber membrane in a second one of said frames. 21. The apparatus of claim 17, wherein the fiber membrane lumens have an internal diameter between 0.1 mm and 2.0 mm and said at least two series connected fiber membranes have total combined length of lumen between 0.25 m and 80 m, optionally between 1 m and 40 m, such as between 5 m and 20 m, more particularly between 2 m and 10 m. 22. A system comprising the apparatus as claimed in claim 17 together with an open channel or tank containing flowing draw solution in which the said apparatus is immersed, and a pumped supply of produced or process water communicating with the lumens of the fiber membranes, the draw solution having a higher salinity than the produced or process water. | 1,700 |
3,452 | 14,833,378 | 1,796 | The invention is related to a method for producing silicone hydrogel contact lenses with having a stable coating thereon. A method of the invention comprises a water-based coating process (step) for forming a relatively-stable base coating of a homo- or copolymer of acrylic acid or C 1 -C 3 alkylacrylic acid onto a silicone hydrogel contact lens made from a lens formulation comprising from about 35% to about 60% by weight of N-vinylpyrrolidone. | 1. A method for producing coated silicone hydrogel contact lenses each having a crosslinked hydrophilic coating thereon, comprising the steps of:
(a) obtaining a silicone hydrogel contact lens from a polymerizable composition comprising at least one silicone-containing vinylic monomer or macromer and from about 30% to about 60% by weight of N-vinylpyrrolidone relative to the total amount of polymerizable components; and (b) contacting the silicone hydrogel contact lens with an aqueous solution of a homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid to form a base coating on the silicone hydrogel contact lens, wherein the base coating exhibits a water-break-up-time (WBUT) of about 20 seconds or more after the silicone hydrogel contact lens has been autoclaved at 115° C. to 125° C. in a phosphate buffered saline having a pH from about 6.5 to about 7.5 for about 30 minutes. 2. The method of claim 1, wherein the polymerizable composition comprises from about 35% to about 56% by weight of N-vinylpyrrolidone relative to the total amount of polymerizable components. 3. The method of claim 1, wherein the polymerizable composition comprises from about 40% to about 52% by weight of N-vinylpyrrolidone relative to the total amount of polymerizable components. 4. The method of claim 1, wherein the homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid is polyacrylic acid, polymethacrylic acid, polyethylacrylic acid, polypropylacrlic acid, poly(acrylic acid-co-methacrylic acid), poly[(meth)acrylic acid-co-ethylacrylic acid], poly[(meth)acrylic acid-co-propylacrylic acid], poly[(meth)acrylic acid-co-acrylamide], poly[(meth)acrylic acid-co-vinyl pyrrolidone], poly[ethylacrylic acid-co-acrylamide], poly[ethylacrylic acid-co-vinylpyrrolidone], poly[propylacrylic acid-co-acrylamide], poly[propylacrylic acid-co-vinyl pyrrolidone], hydrolyzed poly[(meth)acrylic acid-co-vinylacetate], hydrolyzed poly[ethylacrylic acid-co-vinylacetate], hydrolyzed poly[propylacrylic acid-co-vinylacetate], or combinations thereof. 5. The method of claim 4, wherein the weight average molecular weight Mw of a homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid for forming a base coating on silicone hydrogel contact lenses is at least about 10,000 Daltons. 6. The method of claim 5, wherein the homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid is polyacrylic acid, polymethacrylic acid, polyethylacrylic acid, polypropylacrlic acid, poly(acrylic acid-co-methacrylic acid), poly[(meth)acrylic acid-co-ethylacrylic acid], poly[(meth)acrylic acid-co-propylacrylic acid], or combinations thereof. 7. The method of claim 4, wherein the aqueous solution of the homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid has a pH of from about 2.5 to about 5.5. 8. The method of claim 4, further comprising a step of covalently attaching and crosslinking a water-soluble and thermally-crosslinkable hydrophilic polymeric material having azetidinium groups onto the base coating to form a non-silicone hydrogel coating on the silicone hydrogel contact lens. 9. The method of claim 8, wherein the step of covalently attaching and crosslinking is carried out directly in a sealed lens package containing a packaging solution including the water-soluble, thermally crosslinkable hydrophilic polymeric material during sterilization by autoclave at a temperature from about 115° C. to about 125° C. for at least about 20 minutes. 10. The method of claim 8, further comprising the steps of: contacting at room temperature the silicone hydrogel contact lens having the base coating thereon with an aqueous solution of a water-soluble thermally-crosslinkable hydrophilic polymeric material having azetidinium groups to form a top layer of the thermally-crosslinkable hydrophilic polymeric material on the surface of the silicone hydrogel contact lens; immersing the silicone hydrogel contact lens with the top layer of the thermally-crosslinkable hydrophilic polymeric material and the base coating thereon in a packaging solution in a lens package; sealing the lens package; and autoclaving at a temperature from about 115° C. to about 125° C. for at least about 20 minutes the lens package with the silicone hydrogel contact lens therein to form the non-silicone hydrogel coating on the silicone hydrogel contact lens. 11. The method of claim 2, wherein the homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid is polyacrylic acid, polymethacrylic acid, polyethylacrylic acid, polypropylacrlic acid, poly(acrylic acid-co-methacrylic acid), poly[(meth)acrylic acid-co-ethylacrylic acid], poly[(meth)acrylic acid-co-propylacrylic acid], poly[(meth)acrylic acid-co-acrylamide], poly[(meth)acrylic acid-co-vinyl pyrrolidone], poly[ethylacrylic acid-co-acrylamide], poly[ethylacrylic acid-co-vinylpyrrolidone], poly[propylacrylic acid-co-acrylamide], poly[propylacrylic acid-co-vinyl pyrrolidone], hydrolyzed poly[(meth)acrylic acid-co-vinylacetate], hydrolyzed poly[ethylacrylic acid-co-vinylacetate], hydrolyzed poly[propylacrylic acid-co-vinylacetate], or combinations thereof. 12. The method of claim 11, wherein the weight average molecular weight Mw of a homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid for forming a base coating on silicone hydrogel contact lenses is at least about 10,000 Daltons. 13. The method of claim 12, wherein the homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid is polyacrylic acid, polymethacrylic acid, polyethylacrylic acid, polypropylacrlic acid, poly(acrylic acid-co-methacrylic acid), poly[(meth)acrylic acid-co-ethylacrylic acid], poly[(meth)acrylic acid-co-propylacrylic acid], or combinations thereof. 14. The method of claim 11, wherein the aqueous solution of the homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid has a pH of from about 2.5 to about 5.5. 15. The method of claim 11, further comprising a step of covalently attaching and crosslinking a water-soluble and thermally-crosslinkable hydrophilic polymeric material having azetidinium groups onto the base coating to form a non-silicone hydrogel coating on the silicone hydrogel contact lens. 16. The method of claim 15, wherein the step of covalently attaching and crosslinking is carried out directly in a sealed lens package containing a packaging solution including the water-soluble, thermally crosslinkable hydrophilic polymeric material during sterilization by autoclave at a temperature from about 115° C. to about 125° C. for at least about 20 minutes. 17. The method of claim 15, further comprising the steps of: contacting at room temperature the silicone hydrogel contact lens having the base coating thereon with an aqueous solution of a water-soluble thermally-crosslinkable hydrophilic polymeric material having azetidinium groups to form a top layer of the thermally-crosslinkable hydrophilic polymeric material on the surface of the silicone hydrogel contact lens; immersing the silicone hydrogel contact lens with the top layer of the thermally-crosslinkable hydrophilic polymeric material and the base coating thereon in a packaging solution in a lens package; sealing the lens package; and autoclaving at a temperature from about 115° C. to about 125° C. for at least about 20 minutes the lens package with the silicone hydrogel contact lens therein to form the non-silicone hydrogel coating on the silicone hydrogel contact lens. 18. The method of claim 3, wherein the homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid has a weight average molecular weight Mw of at least about 10,000 Daltons and is polyacrylic acid, polymethacrylic acid, polyethylacrylic acid, polypropylacrlic acid, poly(acrylic acid-co-methacrylic acid), poly[(meth)acrylic acid-co-ethylacrylic acid], poly[(meth)acrylic acid-co-propylacrylic acid], or combinations thereof. 19. The method of claim 18, wherein the aqueous solution of the homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid has a pH of from about 2.5 to about 5.5. 20. The method of claim 19, further comprising a step of covalently attaching and crosslinking a water-soluble and thermally-crosslinkable hydrophilic polymeric material having azetidinium groups onto the base coating to form a non-silicone hydrogel coating on the silicone hydrogel contact lens. | The invention is related to a method for producing silicone hydrogel contact lenses with having a stable coating thereon. A method of the invention comprises a water-based coating process (step) for forming a relatively-stable base coating of a homo- or copolymer of acrylic acid or C 1 -C 3 alkylacrylic acid onto a silicone hydrogel contact lens made from a lens formulation comprising from about 35% to about 60% by weight of N-vinylpyrrolidone.1. A method for producing coated silicone hydrogel contact lenses each having a crosslinked hydrophilic coating thereon, comprising the steps of:
(a) obtaining a silicone hydrogel contact lens from a polymerizable composition comprising at least one silicone-containing vinylic monomer or macromer and from about 30% to about 60% by weight of N-vinylpyrrolidone relative to the total amount of polymerizable components; and (b) contacting the silicone hydrogel contact lens with an aqueous solution of a homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid to form a base coating on the silicone hydrogel contact lens, wherein the base coating exhibits a water-break-up-time (WBUT) of about 20 seconds or more after the silicone hydrogel contact lens has been autoclaved at 115° C. to 125° C. in a phosphate buffered saline having a pH from about 6.5 to about 7.5 for about 30 minutes. 2. The method of claim 1, wherein the polymerizable composition comprises from about 35% to about 56% by weight of N-vinylpyrrolidone relative to the total amount of polymerizable components. 3. The method of claim 1, wherein the polymerizable composition comprises from about 40% to about 52% by weight of N-vinylpyrrolidone relative to the total amount of polymerizable components. 4. The method of claim 1, wherein the homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid is polyacrylic acid, polymethacrylic acid, polyethylacrylic acid, polypropylacrlic acid, poly(acrylic acid-co-methacrylic acid), poly[(meth)acrylic acid-co-ethylacrylic acid], poly[(meth)acrylic acid-co-propylacrylic acid], poly[(meth)acrylic acid-co-acrylamide], poly[(meth)acrylic acid-co-vinyl pyrrolidone], poly[ethylacrylic acid-co-acrylamide], poly[ethylacrylic acid-co-vinylpyrrolidone], poly[propylacrylic acid-co-acrylamide], poly[propylacrylic acid-co-vinyl pyrrolidone], hydrolyzed poly[(meth)acrylic acid-co-vinylacetate], hydrolyzed poly[ethylacrylic acid-co-vinylacetate], hydrolyzed poly[propylacrylic acid-co-vinylacetate], or combinations thereof. 5. The method of claim 4, wherein the weight average molecular weight Mw of a homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid for forming a base coating on silicone hydrogel contact lenses is at least about 10,000 Daltons. 6. The method of claim 5, wherein the homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid is polyacrylic acid, polymethacrylic acid, polyethylacrylic acid, polypropylacrlic acid, poly(acrylic acid-co-methacrylic acid), poly[(meth)acrylic acid-co-ethylacrylic acid], poly[(meth)acrylic acid-co-propylacrylic acid], or combinations thereof. 7. The method of claim 4, wherein the aqueous solution of the homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid has a pH of from about 2.5 to about 5.5. 8. The method of claim 4, further comprising a step of covalently attaching and crosslinking a water-soluble and thermally-crosslinkable hydrophilic polymeric material having azetidinium groups onto the base coating to form a non-silicone hydrogel coating on the silicone hydrogel contact lens. 9. The method of claim 8, wherein the step of covalently attaching and crosslinking is carried out directly in a sealed lens package containing a packaging solution including the water-soluble, thermally crosslinkable hydrophilic polymeric material during sterilization by autoclave at a temperature from about 115° C. to about 125° C. for at least about 20 minutes. 10. The method of claim 8, further comprising the steps of: contacting at room temperature the silicone hydrogel contact lens having the base coating thereon with an aqueous solution of a water-soluble thermally-crosslinkable hydrophilic polymeric material having azetidinium groups to form a top layer of the thermally-crosslinkable hydrophilic polymeric material on the surface of the silicone hydrogel contact lens; immersing the silicone hydrogel contact lens with the top layer of the thermally-crosslinkable hydrophilic polymeric material and the base coating thereon in a packaging solution in a lens package; sealing the lens package; and autoclaving at a temperature from about 115° C. to about 125° C. for at least about 20 minutes the lens package with the silicone hydrogel contact lens therein to form the non-silicone hydrogel coating on the silicone hydrogel contact lens. 11. The method of claim 2, wherein the homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid is polyacrylic acid, polymethacrylic acid, polyethylacrylic acid, polypropylacrlic acid, poly(acrylic acid-co-methacrylic acid), poly[(meth)acrylic acid-co-ethylacrylic acid], poly[(meth)acrylic acid-co-propylacrylic acid], poly[(meth)acrylic acid-co-acrylamide], poly[(meth)acrylic acid-co-vinyl pyrrolidone], poly[ethylacrylic acid-co-acrylamide], poly[ethylacrylic acid-co-vinylpyrrolidone], poly[propylacrylic acid-co-acrylamide], poly[propylacrylic acid-co-vinyl pyrrolidone], hydrolyzed poly[(meth)acrylic acid-co-vinylacetate], hydrolyzed poly[ethylacrylic acid-co-vinylacetate], hydrolyzed poly[propylacrylic acid-co-vinylacetate], or combinations thereof. 12. The method of claim 11, wherein the weight average molecular weight Mw of a homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid for forming a base coating on silicone hydrogel contact lenses is at least about 10,000 Daltons. 13. The method of claim 12, wherein the homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid is polyacrylic acid, polymethacrylic acid, polyethylacrylic acid, polypropylacrlic acid, poly(acrylic acid-co-methacrylic acid), poly[(meth)acrylic acid-co-ethylacrylic acid], poly[(meth)acrylic acid-co-propylacrylic acid], or combinations thereof. 14. The method of claim 11, wherein the aqueous solution of the homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid has a pH of from about 2.5 to about 5.5. 15. The method of claim 11, further comprising a step of covalently attaching and crosslinking a water-soluble and thermally-crosslinkable hydrophilic polymeric material having azetidinium groups onto the base coating to form a non-silicone hydrogel coating on the silicone hydrogel contact lens. 16. The method of claim 15, wherein the step of covalently attaching and crosslinking is carried out directly in a sealed lens package containing a packaging solution including the water-soluble, thermally crosslinkable hydrophilic polymeric material during sterilization by autoclave at a temperature from about 115° C. to about 125° C. for at least about 20 minutes. 17. The method of claim 15, further comprising the steps of: contacting at room temperature the silicone hydrogel contact lens having the base coating thereon with an aqueous solution of a water-soluble thermally-crosslinkable hydrophilic polymeric material having azetidinium groups to form a top layer of the thermally-crosslinkable hydrophilic polymeric material on the surface of the silicone hydrogel contact lens; immersing the silicone hydrogel contact lens with the top layer of the thermally-crosslinkable hydrophilic polymeric material and the base coating thereon in a packaging solution in a lens package; sealing the lens package; and autoclaving at a temperature from about 115° C. to about 125° C. for at least about 20 minutes the lens package with the silicone hydrogel contact lens therein to form the non-silicone hydrogel coating on the silicone hydrogel contact lens. 18. The method of claim 3, wherein the homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid has a weight average molecular weight Mw of at least about 10,000 Daltons and is polyacrylic acid, polymethacrylic acid, polyethylacrylic acid, polypropylacrlic acid, poly(acrylic acid-co-methacrylic acid), poly[(meth)acrylic acid-co-ethylacrylic acid], poly[(meth)acrylic acid-co-propylacrylic acid], or combinations thereof. 19. The method of claim 18, wherein the aqueous solution of the homo- or copolymer of acrylic acid or C1-C3 alkylacrylic acid has a pH of from about 2.5 to about 5.5. 20. The method of claim 19, further comprising a step of covalently attaching and crosslinking a water-soluble and thermally-crosslinkable hydrophilic polymeric material having azetidinium groups onto the base coating to form a non-silicone hydrogel coating on the silicone hydrogel contact lens. | 1,700 |
3,453 | 14,392,012 | 1,712 | A method of depositing a coating utilizing a coating apparatus includes providing a coating apparatus above a glass substrate and forming a coating on a surface of the glass substrate while flowing a fluorine-containing compound into the coating apparatus. The fluorine-containing compound inhibits the formation of the coating on one or more portions of the coating apparatus. | 1-21. (canceled) 22. A method of depositing a coating utilizing a coating apparatus, comprising:
providing a coating apparatus above a glass substrate; and forming a coating on a surface of the glass substrate while flowing a fluorine-containing compound into the coating apparatus, wherein the fluorine-containing compound inhibits the formation of the coating on one or more portions of the coating apparatus. 23. The method as claimed in claim 22, wherein the coating comprises an oxide of silicon. 24. The method as claimed in claim 22, wherein the glass substrate is moving. 25. The method as claimed in claim 22, further comprising positioning the coating apparatus within a deposition chamber. 26. The method as claimed in claim 22, wherein the coating is formed on the surface of the glass substrate by chemical vapor deposition. 27. The method as claimed in claim 22, wherein the glass substrate is at a temperature of between about 1050° F. (566° C.) and 1400° F. (760° C.). 28. The method as claimed in claim 22, wherein the coating contains no fluorine or only trace amounts thereof. 29. The method as claimed in claim 22, wherein the coating apparatus comprises one or more exhaust gas passages and the fluorine-containing compound is introduced into an exhaust gas passage. 30. The method as claimed in claim 22, wherein the fluorine-containing compound is anhydrous HF. 31. The method as claimed in claim 22, wherein the fluorine-containing compound inhibits the formation of the coating within one or more exhaust gas passages. 32. The method as claimed in claim 22, wherein the fluorine-containing compound inhibits the formation of the coating on a surface of the coating apparatus. 33. The method as claimed in claim 22, further comprising forming a gaseous mixture comprising a silicon-containing compound, an oxygen-containing compound and a radical scavenger, flowing the gaseous mixture into the coating apparatus and directing the gaseous mixture through the coating apparatus to the surface of the glass substrate. 34. The method as claimed in claim 22, wherein the fluorine-containing compound flows into the coating apparatus prior to forming the coating on the surface of the glass substrate. 35. The method as claimed in claim 22, wherein the coating is a silica coating. 36. The method as claimed in claim 29, wherein the fluorine-containing compound is introduced into each exhaust gas passage via separate gas distribution tubes. 37. The method as claimed in claim 22, wherein the ratio of fluorine-containing compound to silicon-containing compound flowing into the coating apparatus is equal to or greater than 2:1. 38. The method as claimed in claim 37, wherein the ratio of fluorine-containing compound to silicon-containing compound flowing into the coating apparatus is equal to or greater than 4:1. 39. A method of depositing a coating utilizing a coating apparatus, comprising:
providing a coating apparatus which comprises one or more exhaust gas passages above a moving glass substrate; and forming a silica coating on a surface of the glass substrate which contains no fluorine or only trace amounts thereof while flowing a fluorine-containing compound into the coating apparatus, wherein the fluorine-containing compound inhibits the formation of the silica coating in the one or more exhaust gas passages. 40. The method as claimed in claim 39, wherein the glass substrate is at a temperature of between about 1050° F. (566° C.) and 1400° F. (760° C.). 41. The method as claimed in claim 39, further comprising forming a gaseous mixture comprising a silicon-containing compound, an oxygen-containing compound and a radical scavenger, flowing the gaseous mixture into the coating apparatus and directing the gaseous mixture through the coating apparatus to the surface of the glass substrate and wherein the ratio of fluorine-containing compound to silicon-containing compound flowing into the coating apparatus is equal to or greater than 4:1. 42. A coated glass substrate comprising a coating, the coating being deposited by utilizing a coating apparatus, comprising:
providing a coating apparatus above a glass substrate; and forming a coating on a surface of the glass substrate while flowing a fluorine-containing compound into the coating apparatus, wherein the fluorine-containing compound inhibits the formation of the coating on one or more portions of the coating apparatus. | A method of depositing a coating utilizing a coating apparatus includes providing a coating apparatus above a glass substrate and forming a coating on a surface of the glass substrate while flowing a fluorine-containing compound into the coating apparatus. The fluorine-containing compound inhibits the formation of the coating on one or more portions of the coating apparatus.1-21. (canceled) 22. A method of depositing a coating utilizing a coating apparatus, comprising:
providing a coating apparatus above a glass substrate; and forming a coating on a surface of the glass substrate while flowing a fluorine-containing compound into the coating apparatus, wherein the fluorine-containing compound inhibits the formation of the coating on one or more portions of the coating apparatus. 23. The method as claimed in claim 22, wherein the coating comprises an oxide of silicon. 24. The method as claimed in claim 22, wherein the glass substrate is moving. 25. The method as claimed in claim 22, further comprising positioning the coating apparatus within a deposition chamber. 26. The method as claimed in claim 22, wherein the coating is formed on the surface of the glass substrate by chemical vapor deposition. 27. The method as claimed in claim 22, wherein the glass substrate is at a temperature of between about 1050° F. (566° C.) and 1400° F. (760° C.). 28. The method as claimed in claim 22, wherein the coating contains no fluorine or only trace amounts thereof. 29. The method as claimed in claim 22, wherein the coating apparatus comprises one or more exhaust gas passages and the fluorine-containing compound is introduced into an exhaust gas passage. 30. The method as claimed in claim 22, wherein the fluorine-containing compound is anhydrous HF. 31. The method as claimed in claim 22, wherein the fluorine-containing compound inhibits the formation of the coating within one or more exhaust gas passages. 32. The method as claimed in claim 22, wherein the fluorine-containing compound inhibits the formation of the coating on a surface of the coating apparatus. 33. The method as claimed in claim 22, further comprising forming a gaseous mixture comprising a silicon-containing compound, an oxygen-containing compound and a radical scavenger, flowing the gaseous mixture into the coating apparatus and directing the gaseous mixture through the coating apparatus to the surface of the glass substrate. 34. The method as claimed in claim 22, wherein the fluorine-containing compound flows into the coating apparatus prior to forming the coating on the surface of the glass substrate. 35. The method as claimed in claim 22, wherein the coating is a silica coating. 36. The method as claimed in claim 29, wherein the fluorine-containing compound is introduced into each exhaust gas passage via separate gas distribution tubes. 37. The method as claimed in claim 22, wherein the ratio of fluorine-containing compound to silicon-containing compound flowing into the coating apparatus is equal to or greater than 2:1. 38. The method as claimed in claim 37, wherein the ratio of fluorine-containing compound to silicon-containing compound flowing into the coating apparatus is equal to or greater than 4:1. 39. A method of depositing a coating utilizing a coating apparatus, comprising:
providing a coating apparatus which comprises one or more exhaust gas passages above a moving glass substrate; and forming a silica coating on a surface of the glass substrate which contains no fluorine or only trace amounts thereof while flowing a fluorine-containing compound into the coating apparatus, wherein the fluorine-containing compound inhibits the formation of the silica coating in the one or more exhaust gas passages. 40. The method as claimed in claim 39, wherein the glass substrate is at a temperature of between about 1050° F. (566° C.) and 1400° F. (760° C.). 41. The method as claimed in claim 39, further comprising forming a gaseous mixture comprising a silicon-containing compound, an oxygen-containing compound and a radical scavenger, flowing the gaseous mixture into the coating apparatus and directing the gaseous mixture through the coating apparatus to the surface of the glass substrate and wherein the ratio of fluorine-containing compound to silicon-containing compound flowing into the coating apparatus is equal to or greater than 4:1. 42. A coated glass substrate comprising a coating, the coating being deposited by utilizing a coating apparatus, comprising:
providing a coating apparatus above a glass substrate; and forming a coating on a surface of the glass substrate while flowing a fluorine-containing compound into the coating apparatus, wherein the fluorine-containing compound inhibits the formation of the coating on one or more portions of the coating apparatus. | 1,700 |
3,454 | 14,611,580 | 1,733 | An additive manufacturing process includes simultaneously constructing a component and a non-contacting thermal support for the component. The non-contacting thermal support includes a three dimensional negative of the component. The non-contacting thermal support transfers heat from the component into a heat sink. | 1. An additive manufacturing process comprising:
simultaneously constructing a component and a non-contacting thermal support for said component, wherein the non-contacting thermal support includes a three dimensional negative of the component; and dissipating heat from said component through said non-contacting thermal support to a heat sink. 2. The additive manufacturing process of claim 1, wherein dissipating heat from said component through said non-contacting thermal support to a heat sink comprises providing a thermal passage across a gap defined between said non-contacting thermal support and said component. 3. The additive manufacturing process of claim 1, further comprising constructing said thermal support as a solid component. 4. The additive manufacturing process of claim 1, further comprising constructing said thermal support as a thermally conductive wall supported by a structural support. 5. The additive manufacturing process of claim 1, wherein simultaneously constructing a component and a non-contacting thermal support for said component comprises defining a gap between said component and said non-contacting surface. 6. The additive manufacturing process of claim 5, wherein said gap is in the range of about three to five times an average particle size of a powder particle utilized in said additive manufacturing process. 7. The additive manufacturing process of claim 6, wherein simultaneously constructing a component and a non-contacting thermal support for said component comprises constructing at least one downward facing surface of said component and at least one upward facing surface of said non-contacting thermal support, and wherein said at least one downward facing surface is opposite said at least one upward facing surface across said gap. 8. The additive manufacturing process of claim 1, further comprising removing said component from said non-contacting thermal support without mechanically altering said non-contacting thermal support and without chemically altering said non-contacting thermal support. 9. The additive manufacturing process of claim 1, wherein simultaneously constructing a component and a non-contacting thermal support for said component comprises constructing each of said component and said non-contacting thermal support using a direct metal laser sintering process. 10. An additive manufacturing process comprising:
dissipating heat from at least one inaccessible downward facing surface of a component being assembled through a corresponding upward facing surface of a non-contacting thermal support. 11. The method of claim 10, wherein said at least one inaccessible downward facing surface includes a finish absent heat artifacts. 12. The additive manufacturing process of claim 10, wherein said non-contacting thermal support defines an at least partial three dimensional negative image of the component being assembled and wherein said component being assembled is positioned at least partially within said at least partial three dimensional negative image. 13. The additive manufacturing process of claim 12, further comprising defining a gap between said non-contacting thermal support and at least one surface of said component, the gap being in the range of about three to five times an average particle size of a powder used in the additive manufacturing process. 14. The additive manufacturing process of claim 13, wherein dissipating heat from at least one inaccessible downward facing surface of a component being assembled through a corresponding upward facing surface of a non-contacting thermal support comprises dissipating heat across said gap into said non-contacting thermal support. 15. The additive manufacturing process of claim 14, further comprising determining dimensions of said non-contacting thermal support based on received dimensions of said component using a controller. 16. A non-contacting thermal support for an additively manufactured component comprising:
an interior surface defining an at least partial three dimensional negative image of a component; and the at least partial three dimensional negative image including at least one upwards facing surface configured to provide a thermal path from a corresponding inaccessible downward facing surface to a heat sink. 17. The non-contacting thermal support of claim 16, wherein the at least partial three dimension negative image is configured to define a gap between said non-contacting thermal support and a component. 18. The non-contacting thermal support of claim 17, wherein the gap has a width in the range of about three to five times an average particle size of an additive manufacturing powder particle. 19. The non-contacting thermal support of claim 16, wherein the non-contacting thermal support is a direct metal laser sintered thermal support. 20. The non-contacting thermal support of claim 16, wherein said at least partial three dimensional negative image is defined by a wall, and wherein said wall is structurally supported by an integral structural and thermal support. | An additive manufacturing process includes simultaneously constructing a component and a non-contacting thermal support for the component. The non-contacting thermal support includes a three dimensional negative of the component. The non-contacting thermal support transfers heat from the component into a heat sink.1. An additive manufacturing process comprising:
simultaneously constructing a component and a non-contacting thermal support for said component, wherein the non-contacting thermal support includes a three dimensional negative of the component; and dissipating heat from said component through said non-contacting thermal support to a heat sink. 2. The additive manufacturing process of claim 1, wherein dissipating heat from said component through said non-contacting thermal support to a heat sink comprises providing a thermal passage across a gap defined between said non-contacting thermal support and said component. 3. The additive manufacturing process of claim 1, further comprising constructing said thermal support as a solid component. 4. The additive manufacturing process of claim 1, further comprising constructing said thermal support as a thermally conductive wall supported by a structural support. 5. The additive manufacturing process of claim 1, wherein simultaneously constructing a component and a non-contacting thermal support for said component comprises defining a gap between said component and said non-contacting surface. 6. The additive manufacturing process of claim 5, wherein said gap is in the range of about three to five times an average particle size of a powder particle utilized in said additive manufacturing process. 7. The additive manufacturing process of claim 6, wherein simultaneously constructing a component and a non-contacting thermal support for said component comprises constructing at least one downward facing surface of said component and at least one upward facing surface of said non-contacting thermal support, and wherein said at least one downward facing surface is opposite said at least one upward facing surface across said gap. 8. The additive manufacturing process of claim 1, further comprising removing said component from said non-contacting thermal support without mechanically altering said non-contacting thermal support and without chemically altering said non-contacting thermal support. 9. The additive manufacturing process of claim 1, wherein simultaneously constructing a component and a non-contacting thermal support for said component comprises constructing each of said component and said non-contacting thermal support using a direct metal laser sintering process. 10. An additive manufacturing process comprising:
dissipating heat from at least one inaccessible downward facing surface of a component being assembled through a corresponding upward facing surface of a non-contacting thermal support. 11. The method of claim 10, wherein said at least one inaccessible downward facing surface includes a finish absent heat artifacts. 12. The additive manufacturing process of claim 10, wherein said non-contacting thermal support defines an at least partial three dimensional negative image of the component being assembled and wherein said component being assembled is positioned at least partially within said at least partial three dimensional negative image. 13. The additive manufacturing process of claim 12, further comprising defining a gap between said non-contacting thermal support and at least one surface of said component, the gap being in the range of about three to five times an average particle size of a powder used in the additive manufacturing process. 14. The additive manufacturing process of claim 13, wherein dissipating heat from at least one inaccessible downward facing surface of a component being assembled through a corresponding upward facing surface of a non-contacting thermal support comprises dissipating heat across said gap into said non-contacting thermal support. 15. The additive manufacturing process of claim 14, further comprising determining dimensions of said non-contacting thermal support based on received dimensions of said component using a controller. 16. A non-contacting thermal support for an additively manufactured component comprising:
an interior surface defining an at least partial three dimensional negative image of a component; and the at least partial three dimensional negative image including at least one upwards facing surface configured to provide a thermal path from a corresponding inaccessible downward facing surface to a heat sink. 17. The non-contacting thermal support of claim 16, wherein the at least partial three dimension negative image is configured to define a gap between said non-contacting thermal support and a component. 18. The non-contacting thermal support of claim 17, wherein the gap has a width in the range of about three to five times an average particle size of an additive manufacturing powder particle. 19. The non-contacting thermal support of claim 16, wherein the non-contacting thermal support is a direct metal laser sintered thermal support. 20. The non-contacting thermal support of claim 16, wherein said at least partial three dimensional negative image is defined by a wall, and wherein said wall is structurally supported by an integral structural and thermal support. | 1,700 |
3,455 | 15,278,750 | 1,796 | To provide a light-emitting element with high emission efficiency and low driving voltage. The light-emitting element includes a guest material and a host material. A LUMO level of the guest material is lower than a LUMO level of the host material. An energy difference between the LUMO level and a HOMO level of the guest material is larger than an energy difference between the LUMO level and a HOMO level of the host material. The guest material has a function of converting triplet excitation energy into light emission. An energy difference between the LUMO level of the guest material and the HOMO level of the host material is larger than or equal to energy of light emission of the guest material. | 1. A light-emitting element comprising:
a guest material; and a host material, wherein a LUMO level of the guest material is lower than a LUMO level of the host material, wherein an energy difference between the LUMO level of the guest material and a HOMO level of the guest material is larger than an energy difference between the LUMO level of the host material and a HOMO level of the host material, and wherein the guest material is configured to convert triplet excitation energy into light emission. 2. A light-emitting element comprising:
a guest material; and a host material, wherein a LUMO level of the guest material is lower than a LUMO level of the host material, wherein an energy difference between the LUMO level of the guest material and a HOMO level of the guest material is larger than an energy difference between the LUMO level of the host material and a HOMO level of the host material, wherein the guest material is configured to convert triplet excitation energy into light emission, and wherein an energy difference between the LUMO level of the guest material and the HOMO level of the host material is larger than or equal to transition energy calculated from an absorption edge of an absorption spectrum of the guest material. 3. A light-emitting element comprising:
a guest material; and a host material, wherein a LUMO level of the guest material is lower than a LUMO level of the host material, wherein an energy difference between the LUMO level of the guest material and a HOMO level of the guest material is larger than an energy difference between the LUMO level of the host material and a HOMO level of the host material, wherein the guest material is configured to convert triplet excitation energy into light emission, and wherein an energy difference between the LUMO level of the guest material and the HOMO level of the host material is larger than or equal to light emission energy of the guest material. 4. The light-emitting element according to any one of claims 1 to 3,
wherein the energy difference between the LUMO level of the guest material and the HOMO level of the guest material is larger than the transition energy calculated from the absorption edge of the absorption spectrum of the guest material by 0.4 eV or more. 5. The light-emitting element according to any one of claims 1 to 3,
wherein the energy difference between the LUMO level of the guest material and the HOMO level of the guest material is larger than the light emission energy of the guest material by 0.4 eV or more. 6. The light-emitting element according to any one of claims 1 to 3,
wherein the host material has a difference between a singlet excitation energy level and a triplet excitation energy level of larger than 0 eV and smaller than or equal to 0.2 eV. 7. The light-emitting element according to any one of claims 1 to 3,
wherein the host material is configured to exhibit thermally activated delayed fluorescence at room temperature. 8. The light-emitting element according to any one of claims 1 to 3,
wherein the host material is configured to supply excitation energy to the guest material. 9. The light-emitting element according to any one of claims 1 to 3,
wherein a light emission spectrum of the host material comprises a wavelength region overlapping with an absorption band on the lowest energy side in the absorption spectrum of the guest material. 10. The light-emitting element according to any one of claims 1 to 3,
wherein the guest material comprises iridium. 11. The light-emitting element according to any one of claims 1 to 3,
wherein the guest material is configured to emit light. 12. The light-emitting element according to any one of claims 1 to 3,
wherein the host material is configured to transport an electron, and
wherein the host material is configured to transport a hole. 13. The light-emitting element according to any one of claims 1 to 3,
wherein the host material comprises a π-electron deficient heteroaromatic ring skeleton, and
wherein the host material comprises at least one of a π-electron rich heteroaromatic ring skeleton and an aromatic amine skeleton. 14. The light-emitting element according to claim 13,
wherein the π-electron deficient heteroaromatic ring skeleton comprises at least one of a diazine skeleton and a triazine skeleton, and wherein the π-electron rich heteroaromatic ring skeleton comprises at least one of an acridine skeleton, a phenoxazine skeleton, a phenothiazine skeleton, a furan skeleton, a thiophene skeleton, and a pyrrole skeleton. 15. The light-emitting element according to any one of claims 1 to 3,
wherein the host material is a compound represented by any one of Structural Formulae (500) to (503) below: 16. A display device comprising the light-emitting element according to any one of claims 1 to 3,
wherein the display device comprises at least one of a color filter and a transistor. 17. An electronic device comprising the display device according to claim 16,
wherein the electronic device comprises at least one of a housing and a touch sensor. 18. A lighting device comprising the light-emitting element according to any one of claims 1 to 3,
wherein the lighting device comprises at least one of a housing and a touch sensor. 19. A compound represented by any one of Structural Formulae (500) to (503) below: | To provide a light-emitting element with high emission efficiency and low driving voltage. The light-emitting element includes a guest material and a host material. A LUMO level of the guest material is lower than a LUMO level of the host material. An energy difference between the LUMO level and a HOMO level of the guest material is larger than an energy difference between the LUMO level and a HOMO level of the host material. The guest material has a function of converting triplet excitation energy into light emission. An energy difference between the LUMO level of the guest material and the HOMO level of the host material is larger than or equal to energy of light emission of the guest material.1. A light-emitting element comprising:
a guest material; and a host material, wherein a LUMO level of the guest material is lower than a LUMO level of the host material, wherein an energy difference between the LUMO level of the guest material and a HOMO level of the guest material is larger than an energy difference between the LUMO level of the host material and a HOMO level of the host material, and wherein the guest material is configured to convert triplet excitation energy into light emission. 2. A light-emitting element comprising:
a guest material; and a host material, wherein a LUMO level of the guest material is lower than a LUMO level of the host material, wherein an energy difference between the LUMO level of the guest material and a HOMO level of the guest material is larger than an energy difference between the LUMO level of the host material and a HOMO level of the host material, wherein the guest material is configured to convert triplet excitation energy into light emission, and wherein an energy difference between the LUMO level of the guest material and the HOMO level of the host material is larger than or equal to transition energy calculated from an absorption edge of an absorption spectrum of the guest material. 3. A light-emitting element comprising:
a guest material; and a host material, wherein a LUMO level of the guest material is lower than a LUMO level of the host material, wherein an energy difference between the LUMO level of the guest material and a HOMO level of the guest material is larger than an energy difference between the LUMO level of the host material and a HOMO level of the host material, wherein the guest material is configured to convert triplet excitation energy into light emission, and wherein an energy difference between the LUMO level of the guest material and the HOMO level of the host material is larger than or equal to light emission energy of the guest material. 4. The light-emitting element according to any one of claims 1 to 3,
wherein the energy difference between the LUMO level of the guest material and the HOMO level of the guest material is larger than the transition energy calculated from the absorption edge of the absorption spectrum of the guest material by 0.4 eV or more. 5. The light-emitting element according to any one of claims 1 to 3,
wherein the energy difference between the LUMO level of the guest material and the HOMO level of the guest material is larger than the light emission energy of the guest material by 0.4 eV or more. 6. The light-emitting element according to any one of claims 1 to 3,
wherein the host material has a difference between a singlet excitation energy level and a triplet excitation energy level of larger than 0 eV and smaller than or equal to 0.2 eV. 7. The light-emitting element according to any one of claims 1 to 3,
wherein the host material is configured to exhibit thermally activated delayed fluorescence at room temperature. 8. The light-emitting element according to any one of claims 1 to 3,
wherein the host material is configured to supply excitation energy to the guest material. 9. The light-emitting element according to any one of claims 1 to 3,
wherein a light emission spectrum of the host material comprises a wavelength region overlapping with an absorption band on the lowest energy side in the absorption spectrum of the guest material. 10. The light-emitting element according to any one of claims 1 to 3,
wherein the guest material comprises iridium. 11. The light-emitting element according to any one of claims 1 to 3,
wherein the guest material is configured to emit light. 12. The light-emitting element according to any one of claims 1 to 3,
wherein the host material is configured to transport an electron, and
wherein the host material is configured to transport a hole. 13. The light-emitting element according to any one of claims 1 to 3,
wherein the host material comprises a π-electron deficient heteroaromatic ring skeleton, and
wherein the host material comprises at least one of a π-electron rich heteroaromatic ring skeleton and an aromatic amine skeleton. 14. The light-emitting element according to claim 13,
wherein the π-electron deficient heteroaromatic ring skeleton comprises at least one of a diazine skeleton and a triazine skeleton, and wherein the π-electron rich heteroaromatic ring skeleton comprises at least one of an acridine skeleton, a phenoxazine skeleton, a phenothiazine skeleton, a furan skeleton, a thiophene skeleton, and a pyrrole skeleton. 15. The light-emitting element according to any one of claims 1 to 3,
wherein the host material is a compound represented by any one of Structural Formulae (500) to (503) below: 16. A display device comprising the light-emitting element according to any one of claims 1 to 3,
wherein the display device comprises at least one of a color filter and a transistor. 17. An electronic device comprising the display device according to claim 16,
wherein the electronic device comprises at least one of a housing and a touch sensor. 18. A lighting device comprising the light-emitting element according to any one of claims 1 to 3,
wherein the lighting device comprises at least one of a housing and a touch sensor. 19. A compound represented by any one of Structural Formulae (500) to (503) below: | 1,700 |
3,456 | 15,218,729 | 1,783 | The invention comprises a product. The product comprises a foam insulating panel having a first primary surface and an opposite second primary surface and a laminated fabric attached to the first primary surface of the foam insulating panel. The laminated fabric is impregnated with an air-resistant, water-resistant, vapor permeable, elastomeric polymeric material, wherein the air-resistant, water-resistant, vapor permeable elastomeric polymeric material has an elongation factor of greater than 100%, a water vapor transmission rating of at least 0.1 perm and an air permeance of less than 0.004 cfm/sq. ft. under a pressure differential of 0.3 inches of water, whereby the air-resistant, water-resistant, vapor permeable elastomeric polymeric material provides a water-resistant, vapor permeable air barrier. The laminated fabric comprises a woven or nonwoven carrier portion and a woven or nonwoven reinforcing portion attached to the carrier portion. A method of making a composite sheathing panel is also disclosed. | 1. A product comprising:
a foam insulating panel having a first primary surface and an opposite second primary surface; a laminated fabric attached to the first primary surface of the foam insulating panel, wherein the laminated fabric is impregnated with an air-resistant, water-resistant, vapor permeable, elastomeric polymeric material, wherein the air-resistant, water-resistant, vapor permeable elastomeric polymeric material has an elongation factor of greater than 100%, a water vapor transmission rating of at least 0.1 perm and an air permeance of less than 0.004 cfm/sq. ft. under a pressure differential of 0.3 inches of water, whereby the air-resistant, water-resistant, vapor permeable elastomeric polymeric material provides a water-resistant, vapor permeable air barrier; and wherein the laminated fabric comprises a woven or nonwoven carrier portion and a woven or nonwoven reinforcing portion attached to the carrier portion. 2. The product of claim 1, wherein the woven or nonwoven reinforcing portion comprises a laid scrim. 3. The product of claim 2, wherein the laid scrim is made from polypropylene; polyethylene; polyethylene terephthalate; vinyl; polyvinyl chloride; polyester acrylic; nylon; thermoplastic polyethylene having a molecular weight of approximately 2 to 6 million units; (poly(p-phenylene-2,6-benzobisoxazole); an aromatic polyester produced by the polycondensation of 4-hydroxybenzoic acid and 6-hydroxynaphthalene-2-carboxylic acid; p-phenylene terephthalamide; para polyaramide; the reaction product of 1,4-phenylene-diamine (para-phenylenediamine) and terephthaloyl chloride); the condensation product of monomers m-phenylenediamine and isophthaloyl chloride; highly oriented polypropylene, fiberglass, carbon fiber or mixtures or combinations thereof. 4. The product of claim 2, wherein the carrier portion is a nonwoven material made from a polypropylene, polyethylene, polyethylene terephthalate, vinyl, polystyrene, polyvinyl chloride, polyester, acrylic, nylon, rayon, acetate, spandex, lastex, aramid fibers or mixtures or combinations thereof. 5. The product of claim 2, wherein the carrier portion is made from a nonwoven fiberglass material. 6. The product of claim 2, wherein the laid scrim has a side-by-side, over/under, tri-directional or quad-directional configuration. 7. The product of claim 1, wherein the foam insulating panel is made from polystyrene, polyisocyanurate or polyurethane. 8. A method comprising:
applying an uncured thermal insulating polymer foam to a first primary surface of laminated fabric, wherein the laminated fabric is impregnated with an air-resistant, water-resistant, vapor permeable, elastomeric polymeric material, wherein the air-resistant, water-resistant, vapor permeable elastomeric polymeric material has an elongation factor of greater than 100%, a water vapor transmission rating of at least 0.1 perm and an air permeance of less than 0.004 cfm/sq. ft. under a pressure differential of 0.3 inches of water, whereby the air-resistant, water-resistant, vapor permeable elastomeric polymeric material provides a water-resistant, vapor permeable air barrier, and wherein the laminated fabric comprises a woven or nonwoven carrier portion and a woven or nonwoven reinforcing portion attached to the carrier portion; and at least partially curing the thermal insulating polymer foam. 9. The method of claim 8, wherein the woven or nonwoven reinforcing portion comprises a laid scrim. 10. The method of claim 9, wherein the laid scrim is made from polypropylene; polyethylene; polyethylene terephthalate; vinyl; polyvinyl chloride; polyester acrylic; nylon; thermoplastic polyethylene having a molecular weight of approximately 2 to 6 million units; (poly(p-phenylene-2,6-benzobisoxazole); an aromatic polyester produced by the polycondensation of 4-hydroxybenzoic acid and 6-hydroxynaphthalene-2-carboxylic acid; p-phenylene terephthalamide; para polyaramide; the reaction product of 1,4-phenylene-diamine (para-phenylenediamine) and terephthaloyl chloride); the condensation product of monomers m-phenylenediamine and isophthaloyl chloride; highly oriented polypropylene, carbon fiber, fiberglass or mixtures or combinations thereof. 11. The method of claim 9, wherein the carrier portion is made from a nonwoven polypropylene, polyethylene, polyethylene terephthalate, vinyl, polystyrene, polyvinyl chloride, polyester, acrylic, nylon, rayon, acetate, spandex, lastex, aramid fibers, fiberglass or mixtures or combinations thereof. 12. The method of claim 9, wherein the carrier portion is made from a nonwoven fiberglass material. 13. The product of claim 9, wherein the laid scrim has a side-by-side, over/under, tri-directional or quad-directional configuration. 14. The product of claim 9, wherein the foam insulating panel is made from polystyrene, polyisocyanurate or polyurethane. 15. A product comprising:
a polyisocyanurate or polyurethane foam panel having a first primary surface and an opposite second primary surface, wherein the foam panel has a thickness of greater than or equal to 1 inch; a laminated fabric attached to the first primary surface of the polyisocyanurate foam insulating panel, wherein the laminated fabric is impregnated with an air-resistant, water-resistant, vapor permeable, elastomeric polymeric material, wherein the air-resistant, water-resistant, vapor permeable elastomeric polymeric material has an elongation factor of greater than 100%, a water vapor transmission rating of at least 0.1 perm and an air permeance of less than 0.004 cfm/sq. ft. under a pressure differential of 0.3 inches of water, whereby the air-resistant, water-resistant, vapor permeable elastomeric polymeric material provides a water-resistant, vapor permeable air barrier; and wherein the laminated fabric comprises a first nonwoven carrier layer having a primary surface, a laid scrim attached to the primary surface of the carrier layer and a second carrier layer attached to the laid scrim so that the laid scrim is disposed between the first and second nonwoven carrier layers. 16. The product of claim 15, wherein the first and second carrier layers are made from nonwoven fiberglass. 17. The product of claim 16, wherein the laid scrim has a side-by-side, over/under, tri-directional or quad-directional configuration. 18. The product of claim 17, wherein the laid scrim is made from polypropylene; polyethylene; polyethylene terephthalate; vinyl; polyvinyl chloride; polyester acrylic; nylon; thermoplastic polyethylene having a molecular weight of approximately 2 to 6 million units; (poly(p-phenylene-2,6-benzobisoxazole); an aromatic polyester produced by the polycondensation of 4-hydroxybenzoic acid and 6-hydroxynaphthalene-2-carboxylic acid; p-phenylene terephthalamide; para polyaramide; the reaction product of 1,4-phenylene-diamine (para-phenylenediamine) and terephthaloyl chloride); the condensation product of monomers m-phenylenediamine and isophthaloyl chloride; highly oriented polypropylene, carbon fiber, fiberglass or mixtures or combinations thereof. 19. The product of claim 18, wherein the laminated fabric is attached to the foam panel with a vapor permeable adhesive. | The invention comprises a product. The product comprises a foam insulating panel having a first primary surface and an opposite second primary surface and a laminated fabric attached to the first primary surface of the foam insulating panel. The laminated fabric is impregnated with an air-resistant, water-resistant, vapor permeable, elastomeric polymeric material, wherein the air-resistant, water-resistant, vapor permeable elastomeric polymeric material has an elongation factor of greater than 100%, a water vapor transmission rating of at least 0.1 perm and an air permeance of less than 0.004 cfm/sq. ft. under a pressure differential of 0.3 inches of water, whereby the air-resistant, water-resistant, vapor permeable elastomeric polymeric material provides a water-resistant, vapor permeable air barrier. The laminated fabric comprises a woven or nonwoven carrier portion and a woven or nonwoven reinforcing portion attached to the carrier portion. A method of making a composite sheathing panel is also disclosed.1. A product comprising:
a foam insulating panel having a first primary surface and an opposite second primary surface; a laminated fabric attached to the first primary surface of the foam insulating panel, wherein the laminated fabric is impregnated with an air-resistant, water-resistant, vapor permeable, elastomeric polymeric material, wherein the air-resistant, water-resistant, vapor permeable elastomeric polymeric material has an elongation factor of greater than 100%, a water vapor transmission rating of at least 0.1 perm and an air permeance of less than 0.004 cfm/sq. ft. under a pressure differential of 0.3 inches of water, whereby the air-resistant, water-resistant, vapor permeable elastomeric polymeric material provides a water-resistant, vapor permeable air barrier; and wherein the laminated fabric comprises a woven or nonwoven carrier portion and a woven or nonwoven reinforcing portion attached to the carrier portion. 2. The product of claim 1, wherein the woven or nonwoven reinforcing portion comprises a laid scrim. 3. The product of claim 2, wherein the laid scrim is made from polypropylene; polyethylene; polyethylene terephthalate; vinyl; polyvinyl chloride; polyester acrylic; nylon; thermoplastic polyethylene having a molecular weight of approximately 2 to 6 million units; (poly(p-phenylene-2,6-benzobisoxazole); an aromatic polyester produced by the polycondensation of 4-hydroxybenzoic acid and 6-hydroxynaphthalene-2-carboxylic acid; p-phenylene terephthalamide; para polyaramide; the reaction product of 1,4-phenylene-diamine (para-phenylenediamine) and terephthaloyl chloride); the condensation product of monomers m-phenylenediamine and isophthaloyl chloride; highly oriented polypropylene, fiberglass, carbon fiber or mixtures or combinations thereof. 4. The product of claim 2, wherein the carrier portion is a nonwoven material made from a polypropylene, polyethylene, polyethylene terephthalate, vinyl, polystyrene, polyvinyl chloride, polyester, acrylic, nylon, rayon, acetate, spandex, lastex, aramid fibers or mixtures or combinations thereof. 5. The product of claim 2, wherein the carrier portion is made from a nonwoven fiberglass material. 6. The product of claim 2, wherein the laid scrim has a side-by-side, over/under, tri-directional or quad-directional configuration. 7. The product of claim 1, wherein the foam insulating panel is made from polystyrene, polyisocyanurate or polyurethane. 8. A method comprising:
applying an uncured thermal insulating polymer foam to a first primary surface of laminated fabric, wherein the laminated fabric is impregnated with an air-resistant, water-resistant, vapor permeable, elastomeric polymeric material, wherein the air-resistant, water-resistant, vapor permeable elastomeric polymeric material has an elongation factor of greater than 100%, a water vapor transmission rating of at least 0.1 perm and an air permeance of less than 0.004 cfm/sq. ft. under a pressure differential of 0.3 inches of water, whereby the air-resistant, water-resistant, vapor permeable elastomeric polymeric material provides a water-resistant, vapor permeable air barrier, and wherein the laminated fabric comprises a woven or nonwoven carrier portion and a woven or nonwoven reinforcing portion attached to the carrier portion; and at least partially curing the thermal insulating polymer foam. 9. The method of claim 8, wherein the woven or nonwoven reinforcing portion comprises a laid scrim. 10. The method of claim 9, wherein the laid scrim is made from polypropylene; polyethylene; polyethylene terephthalate; vinyl; polyvinyl chloride; polyester acrylic; nylon; thermoplastic polyethylene having a molecular weight of approximately 2 to 6 million units; (poly(p-phenylene-2,6-benzobisoxazole); an aromatic polyester produced by the polycondensation of 4-hydroxybenzoic acid and 6-hydroxynaphthalene-2-carboxylic acid; p-phenylene terephthalamide; para polyaramide; the reaction product of 1,4-phenylene-diamine (para-phenylenediamine) and terephthaloyl chloride); the condensation product of monomers m-phenylenediamine and isophthaloyl chloride; highly oriented polypropylene, carbon fiber, fiberglass or mixtures or combinations thereof. 11. The method of claim 9, wherein the carrier portion is made from a nonwoven polypropylene, polyethylene, polyethylene terephthalate, vinyl, polystyrene, polyvinyl chloride, polyester, acrylic, nylon, rayon, acetate, spandex, lastex, aramid fibers, fiberglass or mixtures or combinations thereof. 12. The method of claim 9, wherein the carrier portion is made from a nonwoven fiberglass material. 13. The product of claim 9, wherein the laid scrim has a side-by-side, over/under, tri-directional or quad-directional configuration. 14. The product of claim 9, wherein the foam insulating panel is made from polystyrene, polyisocyanurate or polyurethane. 15. A product comprising:
a polyisocyanurate or polyurethane foam panel having a first primary surface and an opposite second primary surface, wherein the foam panel has a thickness of greater than or equal to 1 inch; a laminated fabric attached to the first primary surface of the polyisocyanurate foam insulating panel, wherein the laminated fabric is impregnated with an air-resistant, water-resistant, vapor permeable, elastomeric polymeric material, wherein the air-resistant, water-resistant, vapor permeable elastomeric polymeric material has an elongation factor of greater than 100%, a water vapor transmission rating of at least 0.1 perm and an air permeance of less than 0.004 cfm/sq. ft. under a pressure differential of 0.3 inches of water, whereby the air-resistant, water-resistant, vapor permeable elastomeric polymeric material provides a water-resistant, vapor permeable air barrier; and wherein the laminated fabric comprises a first nonwoven carrier layer having a primary surface, a laid scrim attached to the primary surface of the carrier layer and a second carrier layer attached to the laid scrim so that the laid scrim is disposed between the first and second nonwoven carrier layers. 16. The product of claim 15, wherein the first and second carrier layers are made from nonwoven fiberglass. 17. The product of claim 16, wherein the laid scrim has a side-by-side, over/under, tri-directional or quad-directional configuration. 18. The product of claim 17, wherein the laid scrim is made from polypropylene; polyethylene; polyethylene terephthalate; vinyl; polyvinyl chloride; polyester acrylic; nylon; thermoplastic polyethylene having a molecular weight of approximately 2 to 6 million units; (poly(p-phenylene-2,6-benzobisoxazole); an aromatic polyester produced by the polycondensation of 4-hydroxybenzoic acid and 6-hydroxynaphthalene-2-carboxylic acid; p-phenylene terephthalamide; para polyaramide; the reaction product of 1,4-phenylene-diamine (para-phenylenediamine) and terephthaloyl chloride); the condensation product of monomers m-phenylenediamine and isophthaloyl chloride; highly oriented polypropylene, carbon fiber, fiberglass or mixtures or combinations thereof. 19. The product of claim 18, wherein the laminated fabric is attached to the foam panel with a vapor permeable adhesive. | 1,700 |
3,457 | 14,602,868 | 1,727 | An exemplary battery pack cover includes a polymer layer and a metallic layer grounded to a chassis of an electric vehicle. An exemplary method includes shielding battery cells of a battery pack against electromagnetic interference and thermal energy using a multilayer cover that is grounded to a chassis of an electrified vehicle. | 1. A battery pack cover, comprising:
a polymer layer; and a metallic layer grounded to a chassis of an electric vehicle. 2. The battery pack cover of claim 1, wherein the metallic layer is a foil layer. 3. The battery pack cover of claim 1, wherein the metallic layer comprises aluminum. 4. The battery pack cover of claim 1, wherein the polymer layer is coextensive with the metallic layer. 5. The battery pack cover of claim 1, including mechanical fasteners that secure the polymer layer and the metallic layer to a battery pack tray, the metallic layer grounded to the chassis through the mechanical fasteners. 6. The battery pack cover of claim 5, wherein the battery pack tray is metallic. 7. The battery pack cover of claim 1, wherein the metallic layer is an outer layer relative to the polymer layer. 8. The battery pack over of claim 1, wherein the metallic layer is from three to four millimeters thick. 9. An assembly, comprising:
at least one battery array housed within a cover and a tray, the cover including a metallic layer that is grounded to a chassis of an electrified vehicle. 10. The assembly of claim 9, wherein the cover is grounded to the chassis through fasteners attached to the chassis. 11. The assembly of claim 9, further comprising a motor to drive wheels of an electrified vehicle, the battery array powering the motor. 12. The assembly of claim 9, wherein the cover further comprises a polymer layer. 13. The assembly of claim 12, wherein the polymer layer is coextensive with the metallic layer. 14. The assembly of claim 12, wherein the polymer layer is polypropylene. 15. The assembly of claim 12, wherein the metallic layer is an outer layer relative to the polymer layer. 16. A method, comprising:
shielding battery cells of a battery pack against electromagnetic interference and thermal energy using a multilayer cover that is grounded to a chassis of an electrified vehicle. 17. The method of claim 16, wherein an aluminum foil layer provides the shielding. 18. The method of claim 16, further comprising adhering a metallic layer to a separate polymer layer to provide the multilayer cover. 19. The method of claim 18, wherein the metallic layer is coextensive with the polymer layer. 20. The method of claim 18, wherein the metallic layer is within a mold when the polymer layer is injected molded within the mold. | An exemplary battery pack cover includes a polymer layer and a metallic layer grounded to a chassis of an electric vehicle. An exemplary method includes shielding battery cells of a battery pack against electromagnetic interference and thermal energy using a multilayer cover that is grounded to a chassis of an electrified vehicle.1. A battery pack cover, comprising:
a polymer layer; and a metallic layer grounded to a chassis of an electric vehicle. 2. The battery pack cover of claim 1, wherein the metallic layer is a foil layer. 3. The battery pack cover of claim 1, wherein the metallic layer comprises aluminum. 4. The battery pack cover of claim 1, wherein the polymer layer is coextensive with the metallic layer. 5. The battery pack cover of claim 1, including mechanical fasteners that secure the polymer layer and the metallic layer to a battery pack tray, the metallic layer grounded to the chassis through the mechanical fasteners. 6. The battery pack cover of claim 5, wherein the battery pack tray is metallic. 7. The battery pack cover of claim 1, wherein the metallic layer is an outer layer relative to the polymer layer. 8. The battery pack over of claim 1, wherein the metallic layer is from three to four millimeters thick. 9. An assembly, comprising:
at least one battery array housed within a cover and a tray, the cover including a metallic layer that is grounded to a chassis of an electrified vehicle. 10. The assembly of claim 9, wherein the cover is grounded to the chassis through fasteners attached to the chassis. 11. The assembly of claim 9, further comprising a motor to drive wheels of an electrified vehicle, the battery array powering the motor. 12. The assembly of claim 9, wherein the cover further comprises a polymer layer. 13. The assembly of claim 12, wherein the polymer layer is coextensive with the metallic layer. 14. The assembly of claim 12, wherein the polymer layer is polypropylene. 15. The assembly of claim 12, wherein the metallic layer is an outer layer relative to the polymer layer. 16. A method, comprising:
shielding battery cells of a battery pack against electromagnetic interference and thermal energy using a multilayer cover that is grounded to a chassis of an electrified vehicle. 17. The method of claim 16, wherein an aluminum foil layer provides the shielding. 18. The method of claim 16, further comprising adhering a metallic layer to a separate polymer layer to provide the multilayer cover. 19. The method of claim 18, wherein the metallic layer is coextensive with the polymer layer. 20. The method of claim 18, wherein the metallic layer is within a mold when the polymer layer is injected molded within the mold. | 1,700 |
3,458 | 15,689,452 | 1,772 | A method of producing a purified mixed xylene comprising: introducing toluene and methanol to an alkylation reactor; reacting the toluene and the methanol in the alkylation reactor to form a hydrocarbon stream comprising a first mixed xylene, wherein the alkylation reactor comprises an alkylation catalyst; separating the hydrocarbon stream into a toluene stream and a separated C 8+ stream; introducing the toluene stream to a transalkylation reactor with a transalkylation catalyst to produce a transalkylated stream comprising a second mixed xylene; adding the transalkylated stream to the hydrocarbon stream; and separating a C 8 product stream comprising the purified mixed xylene from the separated C 8+ stream. | 1. A method of producing a purified mixed xylene comprising:
introducing toluene and methanol to an alkylation reactor; reacting the toluene and the methanol in the alkylation reactor to form a hydrocarbon stream comprising a first mixed xylene, wherein the alkylation reactor comprises an alkylation catalyst; separating the hydrocarbon stream into a toluene stream and a separated C8+ stream; introducing the toluene stream to a transalkylation reactor with a transalkylation catalyst to produce a transalkylated stream comprising a second mixed xylene; adding the transalkylated stream to the hydrocarbon stream; and separating a C8 product stream comprising the purified mixed xylene from the separated C8+ stream. 2. The method of claim 1, wherein the alkylation catalyst comprises a phosphorus containing, medium pore, pentasil zeolite having a silica/alumina ratio of greater than or equal to 200. 3. The method of claim 2, wherein the phosphorus is present in an amount of 0.01 to 0.15 g per gram of zeolite. 4. The method of claim 1, wherein greater than or equal to 0.05 g of C9+ aromatics per gram of toluene converted is produced in the alkylation reactor. 5. The method of claim 1, wherein the purified mixed xylene comprises greater than or equal to 85 wt % p-xylene based on the total amount of mixed xylene. 6. The method of claim 1, wherein the alkylation catalyst has a selectivity for para-xylene of greater than or equal to 80 mol %. 7. The method of claim 1, wherein the alkylation catalyst has a selectivity for para-xylene of less than or equal to 75 mol %. 8. The method of claim 1, further comprising separating the C8+ stream in a xylene column into the C8 product stream and a separated C9+ stream. 9. The method of claim 11, further comprising separating the separated C9+ stream in a C9 separation column into a C9 stream and a C10+ stream; and introducing the C9 stream to the transalkylation reactor. 10. The method of claim 1, further comprising introducing a C9+ stream to the transalkylation reactor. | A method of producing a purified mixed xylene comprising: introducing toluene and methanol to an alkylation reactor; reacting the toluene and the methanol in the alkylation reactor to form a hydrocarbon stream comprising a first mixed xylene, wherein the alkylation reactor comprises an alkylation catalyst; separating the hydrocarbon stream into a toluene stream and a separated C 8+ stream; introducing the toluene stream to a transalkylation reactor with a transalkylation catalyst to produce a transalkylated stream comprising a second mixed xylene; adding the transalkylated stream to the hydrocarbon stream; and separating a C 8 product stream comprising the purified mixed xylene from the separated C 8+ stream.1. A method of producing a purified mixed xylene comprising:
introducing toluene and methanol to an alkylation reactor; reacting the toluene and the methanol in the alkylation reactor to form a hydrocarbon stream comprising a first mixed xylene, wherein the alkylation reactor comprises an alkylation catalyst; separating the hydrocarbon stream into a toluene stream and a separated C8+ stream; introducing the toluene stream to a transalkylation reactor with a transalkylation catalyst to produce a transalkylated stream comprising a second mixed xylene; adding the transalkylated stream to the hydrocarbon stream; and separating a C8 product stream comprising the purified mixed xylene from the separated C8+ stream. 2. The method of claim 1, wherein the alkylation catalyst comprises a phosphorus containing, medium pore, pentasil zeolite having a silica/alumina ratio of greater than or equal to 200. 3. The method of claim 2, wherein the phosphorus is present in an amount of 0.01 to 0.15 g per gram of zeolite. 4. The method of claim 1, wherein greater than or equal to 0.05 g of C9+ aromatics per gram of toluene converted is produced in the alkylation reactor. 5. The method of claim 1, wherein the purified mixed xylene comprises greater than or equal to 85 wt % p-xylene based on the total amount of mixed xylene. 6. The method of claim 1, wherein the alkylation catalyst has a selectivity for para-xylene of greater than or equal to 80 mol %. 7. The method of claim 1, wherein the alkylation catalyst has a selectivity for para-xylene of less than or equal to 75 mol %. 8. The method of claim 1, further comprising separating the C8+ stream in a xylene column into the C8 product stream and a separated C9+ stream. 9. The method of claim 11, further comprising separating the separated C9+ stream in a C9 separation column into a C9 stream and a C10+ stream; and introducing the C9 stream to the transalkylation reactor. 10. The method of claim 1, further comprising introducing a C9+ stream to the transalkylation reactor. | 1,700 |
3,459 | 15,137,183 | 1,735 | A hollow metal article can be fabricated by casting a molten metal alloy around a core, solidifying the molten metal alloy to form a metal article, and chemically removing the core from the metal article to form a hollow cavity in the metal article. The core includes a ceramic core body and an x-ray radiopaque coating disposed on the ceramic core body. A method for testing the hollow metal article includes submitting the hollow metal article to x-ray imaging and determining based upon the x-ray imaging whether any of the x-ray radiopaque coating of the core remains in the hollow metal article. | 1. A method for testing a hollow metal article, the method comprising:
submitting a hollow metal article to x-ray imaging, wherein the hollow metal article was fabricated by casting a molten metal alloy around a core that had a ceramic core body and an x-ray radiopaque coating disposed on the ceramic core body, the core having been chemically removed; and determining based upon the x-ray imaging whether any of the x-ray radiopaque coating of the core remains in the hollow metal article. 2. The method as recited in claim 1, wherein the x-ray radiopaque coating has a greater x-ray attenuation than the hollow metal article. 3. The method as recited in claim 1, wherein the x-ray radiopaque coating includes at least one refractory metal chemical element. 4. The method as recited in claim 3, wherein the at least one refractory metal chemical element is selected from a group consisting of niobium, molybdenum, tantalum, tungsten, rhenium, and combinations thereof. 5. The method as recited in claim 3, wherein the at least one refractory metal chemical element is selected from a group consisting of titanium, vanadium, chromium, zirconium, hafnium, ruthenium, rhodium, osmium, iridium, and combinations thereof. 6. The method as recited in claim 1, further comprising submitting the hollow metal article to an additional removal process if any of the x-ray radiopaque coating of the core remains in the hollow metal article. 7. A method for testing a hollow metal article, the method comprising:
casting a molten metal alloy around a core and solidifying the molten metal alloy to form a metal article, wherein the core includes a ceramic core body and an x-ray radiopaque coating disposed on the ceramic core body; chemically removing the core from the metal article to form a hollow cavity in the metal article; and after chemically removing the core, submitting the metal article to x-ray imaging and determining based upon the x-ray imaging whether any of the x-ray radiopaque coating of the core remains in the hollow cavity. 8. The method as recited in claim 7, wherein x-ray radiopaque coating encloses the ceramic core body. 9. The method as recited in claim 7, wherein the x-ray radiopaque coating includes at least one refractory metal chemical element. 10. The method as recited in claim 9, wherein the at least one refractory metal chemical element is in metallic form. 11. The method as recited in claim 9, wherein the at least one refractory metal chemical element is in oxide form. 12. The method as recited in claim 9, wherein the x-ray radiopaque coating consists of the at least one refractory metal chemical element in metallic form, oxide form, or combinations thereof. 13. The method as recited in claim 7, further comprising fabricating the core by depositing the x-ray radiopaque coating on the ceramic core body. 14. The method as recited in claim 7, wherein x-ray radiopaque coating has a thickness of 13 micrometers or less. 15. The method as recited in claim 7, wherein the ceramic core body has a maximum thickness and the x-ray radiopaque coating has a thickness of 5% or less of the maximum thickness of the ceramic core body. 16. A casting core comprising:
a ceramic core body configured for forming a cavity in a metal article; and an x-ray radiopaque coating disposed on the ceramic core body. 17. The casting core as recited in claim 16, wherein the x-ray radiopaque coating encloses the ceramic core body. 18. The casting core as recited in claim 16, wherein the x-ray radiopaque coating includes at least one refractory metal chemical element. 19. The casting core as recited in claim 16, wherein the x-ray radiopaque coating includes at least one refractory metal chemical element selected from a group consisting of niobium, molybdenum, tantalum, tungsten, rhenium, titanium, vanadium, chromium, zirconium, hafnium, ruthenium, rhodium, osmium, iridium, and combinations thereof. 20. The casting core as recited in claim 16, wherein the ceramic core body has a maximum thickness and the x-ray radiopaque coating has a thickness of 5% or less of the maximum thickness of the ceramic core body. | A hollow metal article can be fabricated by casting a molten metal alloy around a core, solidifying the molten metal alloy to form a metal article, and chemically removing the core from the metal article to form a hollow cavity in the metal article. The core includes a ceramic core body and an x-ray radiopaque coating disposed on the ceramic core body. A method for testing the hollow metal article includes submitting the hollow metal article to x-ray imaging and determining based upon the x-ray imaging whether any of the x-ray radiopaque coating of the core remains in the hollow metal article.1. A method for testing a hollow metal article, the method comprising:
submitting a hollow metal article to x-ray imaging, wherein the hollow metal article was fabricated by casting a molten metal alloy around a core that had a ceramic core body and an x-ray radiopaque coating disposed on the ceramic core body, the core having been chemically removed; and determining based upon the x-ray imaging whether any of the x-ray radiopaque coating of the core remains in the hollow metal article. 2. The method as recited in claim 1, wherein the x-ray radiopaque coating has a greater x-ray attenuation than the hollow metal article. 3. The method as recited in claim 1, wherein the x-ray radiopaque coating includes at least one refractory metal chemical element. 4. The method as recited in claim 3, wherein the at least one refractory metal chemical element is selected from a group consisting of niobium, molybdenum, tantalum, tungsten, rhenium, and combinations thereof. 5. The method as recited in claim 3, wherein the at least one refractory metal chemical element is selected from a group consisting of titanium, vanadium, chromium, zirconium, hafnium, ruthenium, rhodium, osmium, iridium, and combinations thereof. 6. The method as recited in claim 1, further comprising submitting the hollow metal article to an additional removal process if any of the x-ray radiopaque coating of the core remains in the hollow metal article. 7. A method for testing a hollow metal article, the method comprising:
casting a molten metal alloy around a core and solidifying the molten metal alloy to form a metal article, wherein the core includes a ceramic core body and an x-ray radiopaque coating disposed on the ceramic core body; chemically removing the core from the metal article to form a hollow cavity in the metal article; and after chemically removing the core, submitting the metal article to x-ray imaging and determining based upon the x-ray imaging whether any of the x-ray radiopaque coating of the core remains in the hollow cavity. 8. The method as recited in claim 7, wherein x-ray radiopaque coating encloses the ceramic core body. 9. The method as recited in claim 7, wherein the x-ray radiopaque coating includes at least one refractory metal chemical element. 10. The method as recited in claim 9, wherein the at least one refractory metal chemical element is in metallic form. 11. The method as recited in claim 9, wherein the at least one refractory metal chemical element is in oxide form. 12. The method as recited in claim 9, wherein the x-ray radiopaque coating consists of the at least one refractory metal chemical element in metallic form, oxide form, or combinations thereof. 13. The method as recited in claim 7, further comprising fabricating the core by depositing the x-ray radiopaque coating on the ceramic core body. 14. The method as recited in claim 7, wherein x-ray radiopaque coating has a thickness of 13 micrometers or less. 15. The method as recited in claim 7, wherein the ceramic core body has a maximum thickness and the x-ray radiopaque coating has a thickness of 5% or less of the maximum thickness of the ceramic core body. 16. A casting core comprising:
a ceramic core body configured for forming a cavity in a metal article; and an x-ray radiopaque coating disposed on the ceramic core body. 17. The casting core as recited in claim 16, wherein the x-ray radiopaque coating encloses the ceramic core body. 18. The casting core as recited in claim 16, wherein the x-ray radiopaque coating includes at least one refractory metal chemical element. 19. The casting core as recited in claim 16, wherein the x-ray radiopaque coating includes at least one refractory metal chemical element selected from a group consisting of niobium, molybdenum, tantalum, tungsten, rhenium, titanium, vanadium, chromium, zirconium, hafnium, ruthenium, rhodium, osmium, iridium, and combinations thereof. 20. The casting core as recited in claim 16, wherein the ceramic core body has a maximum thickness and the x-ray radiopaque coating has a thickness of 5% or less of the maximum thickness of the ceramic core body. | 1,700 |
3,460 | 15,316,614 | 1,732 | Provided herein is a highly pure carbohydrate composition, and a method of making a highly pure carbohydrate composition. The method includes passing an aqueous carbohydrate solution through an anion exchange chromatography column including a polyethyleneimine (PEI) chromatographic media to obtain a purified solution, and isolating a highly pure carbohydrate composition from the purified solution. | 1. A method of making a highly pure carbohydrate composition comprising:
i) passing an aqueous carbohydrate solution through an anion exchange chromatography column to obtain a purified solution; and ii) isolating a highly pure carbohydrate composition from said purified solution. 2. The method according to claim 1 wherein said anion exchange resins is made of polyethyleneimine (PEI). 3. The method of making a highly pure carbohydrate composition according to claim 1 wherein said isolating step includes at least one of the steps of: crystallization with an alcohol, or spray drying said purified solution. 4. The method of making a highly pure carbohydrate composition according to claim 3 wherein said crystallization step is performed with ethanol. 5. The method of making a highly pure carbohydrate composition according to claim 1 further comprising a filtration step of said aqueous carbohydrate solution before passing said aqueous carbohydrate solution through an anion exchange chromatography column to obtain a purified solution. 6. The method of making a highly pure carbohydrate composition according to claim 1 wherein said resultant composition is a colorless material free of plant derived material. 7. The method according to claim 5 wherein said filtration step comprises passing said aqueous carbohydrate solution through a filter with a pore size of about 0.4 microns to about 0.5 microns. 8. The method according to claim 1 wherein said highly pure carbohydrate composition is selected from the group of carbohydrates including sucrose, galactose, and trehalose. 9. The method according to claim 1 wherein said highly pure carbohydrate composition has endotoxin levels of less than 2.5 Endotoxin Unit per gram. 10. The method according to claim 1 wherein said highly pure carbohydrate composition has less than 5 ppb of elemental impurities such as lead. 11. The method according to claim 1 wherein said highly pure carbohydrate composition has less than 100 ppm of related carbohydrate species, preferably less than 10 ppm. 12. A highly pure carbohydrate composition comprising an aqueous carbohydrate solution having an endotoxin value of less than 1 Endotoxin Units per gram, said highly pure composition made by the method of
i) passing an aqueous carbohydrate solution through an anion exchange chromatography column to obtain a purified solution; and ii) isolating a highly pure carbohydrate composition from said purified solution. 13. The highly pure carbohydrate composition of claim 12 wherein said aqueous carbohydrate solution has an endotoxin value of less than 0.4 Endotoxin Units per gram. 14. The highly pure carbohydrate composition of claim 12 wherein said aqueous carbohydrate solution has an endotoxin value of less than 0.3 Endotoxin Units per gram. 15. The highly pure carbohydrate composition of claim 12 wherein said aqueous carbohydrate solution has an endotoxin value of about 0.1 Endotoxin Units per gram. 16. The highly pure carbohydrate composition of claim 12 wherein said aqueous carbohydrate solution has been passed through an anion exchange chromatography column including a polyethyleneimine (PEI) chromatographic media. 17. The highly pure carbohydrate composition of claim 15 wherein said aqueous carbohydrate solution is further isolated by at least one of the steps of:
i) crystallization with an alcohol, or
ii) spray drying said purified solution. 18. The highly pure carbohydrate composition of claim 12, wherein said highly pure carbohydrate composition is selected from the group of sucrose, galactose, and trehalose. 19. The highly pure carbohydrate composition of claim 12 wherein said highly pure carbohydrate composition has less than 5 ppb of elemental impurities such as lead. 20. A formulation ingredient for a pharmaceutical composition comprising a highly pure carbohydrate composition having an endotoxin value of less than 1 Endotoxin Units per gram, said highly pure composition made by the method of
i) passing an aqueous carbohydrate solution through an anion exchange chromatography column to obtain a purified solution; and ii) isolating a highly pure carbohydrate composition from said purified solution. | Provided herein is a highly pure carbohydrate composition, and a method of making a highly pure carbohydrate composition. The method includes passing an aqueous carbohydrate solution through an anion exchange chromatography column including a polyethyleneimine (PEI) chromatographic media to obtain a purified solution, and isolating a highly pure carbohydrate composition from the purified solution.1. A method of making a highly pure carbohydrate composition comprising:
i) passing an aqueous carbohydrate solution through an anion exchange chromatography column to obtain a purified solution; and ii) isolating a highly pure carbohydrate composition from said purified solution. 2. The method according to claim 1 wherein said anion exchange resins is made of polyethyleneimine (PEI). 3. The method of making a highly pure carbohydrate composition according to claim 1 wherein said isolating step includes at least one of the steps of: crystallization with an alcohol, or spray drying said purified solution. 4. The method of making a highly pure carbohydrate composition according to claim 3 wherein said crystallization step is performed with ethanol. 5. The method of making a highly pure carbohydrate composition according to claim 1 further comprising a filtration step of said aqueous carbohydrate solution before passing said aqueous carbohydrate solution through an anion exchange chromatography column to obtain a purified solution. 6. The method of making a highly pure carbohydrate composition according to claim 1 wherein said resultant composition is a colorless material free of plant derived material. 7. The method according to claim 5 wherein said filtration step comprises passing said aqueous carbohydrate solution through a filter with a pore size of about 0.4 microns to about 0.5 microns. 8. The method according to claim 1 wherein said highly pure carbohydrate composition is selected from the group of carbohydrates including sucrose, galactose, and trehalose. 9. The method according to claim 1 wherein said highly pure carbohydrate composition has endotoxin levels of less than 2.5 Endotoxin Unit per gram. 10. The method according to claim 1 wherein said highly pure carbohydrate composition has less than 5 ppb of elemental impurities such as lead. 11. The method according to claim 1 wherein said highly pure carbohydrate composition has less than 100 ppm of related carbohydrate species, preferably less than 10 ppm. 12. A highly pure carbohydrate composition comprising an aqueous carbohydrate solution having an endotoxin value of less than 1 Endotoxin Units per gram, said highly pure composition made by the method of
i) passing an aqueous carbohydrate solution through an anion exchange chromatography column to obtain a purified solution; and ii) isolating a highly pure carbohydrate composition from said purified solution. 13. The highly pure carbohydrate composition of claim 12 wherein said aqueous carbohydrate solution has an endotoxin value of less than 0.4 Endotoxin Units per gram. 14. The highly pure carbohydrate composition of claim 12 wherein said aqueous carbohydrate solution has an endotoxin value of less than 0.3 Endotoxin Units per gram. 15. The highly pure carbohydrate composition of claim 12 wherein said aqueous carbohydrate solution has an endotoxin value of about 0.1 Endotoxin Units per gram. 16. The highly pure carbohydrate composition of claim 12 wherein said aqueous carbohydrate solution has been passed through an anion exchange chromatography column including a polyethyleneimine (PEI) chromatographic media. 17. The highly pure carbohydrate composition of claim 15 wherein said aqueous carbohydrate solution is further isolated by at least one of the steps of:
i) crystallization with an alcohol, or
ii) spray drying said purified solution. 18. The highly pure carbohydrate composition of claim 12, wherein said highly pure carbohydrate composition is selected from the group of sucrose, galactose, and trehalose. 19. The highly pure carbohydrate composition of claim 12 wherein said highly pure carbohydrate composition has less than 5 ppb of elemental impurities such as lead. 20. A formulation ingredient for a pharmaceutical composition comprising a highly pure carbohydrate composition having an endotoxin value of less than 1 Endotoxin Units per gram, said highly pure composition made by the method of
i) passing an aqueous carbohydrate solution through an anion exchange chromatography column to obtain a purified solution; and ii) isolating a highly pure carbohydrate composition from said purified solution. | 1,700 |
3,461 | 14,571,826 | 1,714 | Described herein is a method for growing InN, GaN, and AlN materials, the method comprising alternate growth of GaN and either InN or AlN to obtain a film of In x Ga 1−x N, Al x Ga 1−x N, Al x In 1−x N, or Al x In y Ga 1−(x+y) N | 1. A method for growing InN, GaN, and AlN materials, the method comprising alternate growth of GaN and either InN or AlN to obtain a film of InxGa1−xN, AlxGa1−xN, AlxIn1−xN, or AlxInyGa1−(x+y)N. 2. The method of claim 1, using N2 plasma as a nitrogen precursor. 3. The method of claim 1, using trimethylindium as an indium precursor. 4. The method of claim 1, using trimethylaluminum as an aluminum precursor. 5. The method of claim 1, using trimethylgallium as gallium precursor? 6. The method of claim 1, wherein InN is grown at a temperature of no greater than 300° C. 7. The method of claim 1, wherein GaN is grown at a temperature of no greater than 500° C. 8. The method of claim 1, wherein AlN is grown at a temperature of no greater than 650° C. 9. The method of claim 1, wherein the growth is conducted using atomic layer epitaxy. 10. A method for growing InN, GaN, and AlN materials, the method comprising alternate growth of GaN and either InN or AlN to obtain a film of InxGa1−xN, AlxGa1−xN, or AlxIn1−xN. 11. The method of claim 10, using N2 plasma as a nitrogen precursor. 12. The method of claim 10, using trimethylindium as an indium precursor. 13. The method of claim 10, using trimethylaluminum as an aluminum precursor. 14. The method of claim 10, using trimethylgallium as gallium precursor? 15. The method of claim 10, wherein InN is grown at a temperature of no greater than 300° C. 16. The method of claim 10, wherein GaN is grown at a temperature of no greater than 500° C. 17. The method of claim 10, wherein AlN is grown at a temperature of no greater than 650° C. 18. The method of claim 10, wherein the growth is conducted using atomic layer epitaxy. | Described herein is a method for growing InN, GaN, and AlN materials, the method comprising alternate growth of GaN and either InN or AlN to obtain a film of In x Ga 1−x N, Al x Ga 1−x N, Al x In 1−x N, or Al x In y Ga 1−(x+y) N1. A method for growing InN, GaN, and AlN materials, the method comprising alternate growth of GaN and either InN or AlN to obtain a film of InxGa1−xN, AlxGa1−xN, AlxIn1−xN, or AlxInyGa1−(x+y)N. 2. The method of claim 1, using N2 plasma as a nitrogen precursor. 3. The method of claim 1, using trimethylindium as an indium precursor. 4. The method of claim 1, using trimethylaluminum as an aluminum precursor. 5. The method of claim 1, using trimethylgallium as gallium precursor? 6. The method of claim 1, wherein InN is grown at a temperature of no greater than 300° C. 7. The method of claim 1, wherein GaN is grown at a temperature of no greater than 500° C. 8. The method of claim 1, wherein AlN is grown at a temperature of no greater than 650° C. 9. The method of claim 1, wherein the growth is conducted using atomic layer epitaxy. 10. A method for growing InN, GaN, and AlN materials, the method comprising alternate growth of GaN and either InN or AlN to obtain a film of InxGa1−xN, AlxGa1−xN, or AlxIn1−xN. 11. The method of claim 10, using N2 plasma as a nitrogen precursor. 12. The method of claim 10, using trimethylindium as an indium precursor. 13. The method of claim 10, using trimethylaluminum as an aluminum precursor. 14. The method of claim 10, using trimethylgallium as gallium precursor? 15. The method of claim 10, wherein InN is grown at a temperature of no greater than 300° C. 16. The method of claim 10, wherein GaN is grown at a temperature of no greater than 500° C. 17. The method of claim 10, wherein AlN is grown at a temperature of no greater than 650° C. 18. The method of claim 10, wherein the growth is conducted using atomic layer epitaxy. | 1,700 |
3,462 | 14,357,944 | 1,764 | A process for manufacturing eggshell powder for use in the production of bio-based products is provided. The process involves exposing a quantity of eggshell to high air speed at room temperatures to pulverize the eggshell and separate the eggshell component from the inner membrane component. Thus, the process avoids the use of high temperatures and other harsh chemical treatments to remove the inner membrane from the eggshell thereby resulting in an eggshell material that retains the original lipid-protein structure of the native eggshell from which the powder derives. Accordingly, an eggshell powder composition is provided that is substantially free of inner membrane material and possesses a lipid-protein structure substantially similar to that of the eggshell from which the powder is derived. A polymer composite composition comprising an eggshell component and a polymer component is also provided. | 1. A polymer composite composition comprising:
an eggshell component, wherein the eggshell component possesses a lipid-protein structure substantially similar to that of the eggshell from which the eggshell component is derived, and wherein the eggshell component is substantially free of eggshell inner membrane material; and a polymer component. 2. The composition of claim 1, wherein the polymer component is a thermoplastic polymer. 3. The composition of claim 1, wherein the polymer component is a thermoset polymer. 4. (canceled) 5. The composition of claim 1, wherein the eggshell component constitutes 50% of the polymer composite composition. 6.-9. (canceled) 10. The composition of claim 1 further comprising an additive component selected from the group consisting of heat stabilizers, antioxidants, UV/light stabilizers, antistatic agents, antifogging agents, lubricants, processing aids, anti-blocking agents, slipping agents, mold-releasing agents, flame-retardant agents, chemical-blowing agents, crosslink agents, nucleating agents, antimicrobial agents, coupling agents, gas scavengers, acid and base scavengers, water scavengers, odor controlling agents, and food flavoring agents. 11. The composition of claim 1 further comprising a filler component selected from the group consisting of calcium carbonate, dolomite, magnesium carbonate, calcium sulfate, barium sulfate, silica, silicate, zeolite, carbon black, talc, mica, kaolin, clay, graphite, wollastonite, whiskers, glass fiber, carbon fiber, conductive filler, nano-filler, wood flour, wood fiber, cellulose fiber, distilled drained grain, pigment, dye, and fluorescent whitening agent. 12. The composition of claim 1 wherein the eggshell component has a particle size from about 10 μm to about 100 μm. 13. (canceled) 14. The composition of claim 1 wherein the eggshell component is hydrophobic. 15. A biobased product comprising:
an eggshell powder, wherein the eggshell powder retains the lipid-protein structure of the eggshell from which the eggshell powder is derived; and a polymer. 16. The product of claim 15, wherein the polymer is a thermoplastic polymer. 17. The product of claim 15, wherein the polymer is a thermoset polymer. 18. (canceled) 19. The product of claim 15, wherein the eggshell powder constitutes 25% by weight of the total weight of the product. 20.-25. (canceled) 26. The product of claim 15, wherein the eggshell powder has a particle size from about 20 μm to about 50 μm. 27. (canceled) 28. The product of claim 15, wherein the eggshell powder is hydrophobic. 29. A process for producing an eggshell powder comprising the steps of:
exposing a quantity of eggshell to air flow at a speed sufficient to pulverize the eggshell thereby rendering a bulk pulverized material comprising an eggshell component and a separated inner membrane component; applying the bulk pulverized material to a first screen comprising a mesh size sufficient to retain the separated inner membrane component on the surface of the first screen while permitting passage of the eggshell component through the first screen; and collecting the eggshell component following passage through the first screen, wherein the eggshell component collected forms the eggshell powder of a first particle size, wherein the first particle size is less than or equal to that permitted to pass through the first screen. 30. The process of claim 29, wherein the first particle size is less than or equal to 100 μm. 31. The process of claim 29, further comprising the step of applying the eggshell powder to a second screen comprising a mesh size sufficient to permit passage of a second particle size, wherein the second particle size is less than the first particle size; and
collecting the eggshell powder that passes through the second screen, wherein the eggshell powder that passes through the second screen has a particle size less than or equal to the second particle size. 32. The process of claim 31, wherein the second particle size is less than or equal to 50 μm. 33. The process of claim 31, wherein the second particle size is less than or equal to 20 μm. 34. (canceled) 35. The process of claim 31, further comprising the steps of:
collecting the eggshell powder that is retained on the second screen, wherein the eggshell powder retained on the second screen has a particle size greater than the second particle size; re-exposing the eggshell powder retained on the second screen to air flow at a speed sufficient to further reduce the particle size; and re-applying the eggshell powder to the second screen. 36. The process of claim 35 wherein the re-exposure of air flow is at a speed of 5,700 rpm for 10 seconds. 37. The process of claim 35 wherein the eggshell powder is exposed to air flow for a third time at a speed of 10,000 for 10 seconds. 38. The process of claim 29, further comprising the step of sterilizing the eggshell prior to pulverizing. 39. The process of claim 29, wherein the eggshell is not heated during the entire process. 40. The process of claim 29, wherein the air flow is at a speed of 3,500 rpm for 10 seconds. 41. The process of claim 29, wherein the step of exposing the eggshell to air flow is performed in a vortex dryer. 42. The process of claim 29, wherein the step of exposing the eggshell to air flow is performed in a cyclone wind tunnel. 43. A composition comprising an eggshell powder, wherein the eggshell powder possesses the lipid-protein structure of the eggshell from which the eggshell powder is derived, and wherein the eggshell powder is substantially free of eggshell inner membrane material. 44.-58. (canceled) 59. The composition of claim 43, wherein the eggshell powder has a particle size from about 10 μm to about 100 μm. 60.-82. (canceled) 83. The composition of claim 43, wherein the eggshell component is hydrophobic. 84.-87. (canceled) | A process for manufacturing eggshell powder for use in the production of bio-based products is provided. The process involves exposing a quantity of eggshell to high air speed at room temperatures to pulverize the eggshell and separate the eggshell component from the inner membrane component. Thus, the process avoids the use of high temperatures and other harsh chemical treatments to remove the inner membrane from the eggshell thereby resulting in an eggshell material that retains the original lipid-protein structure of the native eggshell from which the powder derives. Accordingly, an eggshell powder composition is provided that is substantially free of inner membrane material and possesses a lipid-protein structure substantially similar to that of the eggshell from which the powder is derived. A polymer composite composition comprising an eggshell component and a polymer component is also provided.1. A polymer composite composition comprising:
an eggshell component, wherein the eggshell component possesses a lipid-protein structure substantially similar to that of the eggshell from which the eggshell component is derived, and wherein the eggshell component is substantially free of eggshell inner membrane material; and a polymer component. 2. The composition of claim 1, wherein the polymer component is a thermoplastic polymer. 3. The composition of claim 1, wherein the polymer component is a thermoset polymer. 4. (canceled) 5. The composition of claim 1, wherein the eggshell component constitutes 50% of the polymer composite composition. 6.-9. (canceled) 10. The composition of claim 1 further comprising an additive component selected from the group consisting of heat stabilizers, antioxidants, UV/light stabilizers, antistatic agents, antifogging agents, lubricants, processing aids, anti-blocking agents, slipping agents, mold-releasing agents, flame-retardant agents, chemical-blowing agents, crosslink agents, nucleating agents, antimicrobial agents, coupling agents, gas scavengers, acid and base scavengers, water scavengers, odor controlling agents, and food flavoring agents. 11. The composition of claim 1 further comprising a filler component selected from the group consisting of calcium carbonate, dolomite, magnesium carbonate, calcium sulfate, barium sulfate, silica, silicate, zeolite, carbon black, talc, mica, kaolin, clay, graphite, wollastonite, whiskers, glass fiber, carbon fiber, conductive filler, nano-filler, wood flour, wood fiber, cellulose fiber, distilled drained grain, pigment, dye, and fluorescent whitening agent. 12. The composition of claim 1 wherein the eggshell component has a particle size from about 10 μm to about 100 μm. 13. (canceled) 14. The composition of claim 1 wherein the eggshell component is hydrophobic. 15. A biobased product comprising:
an eggshell powder, wherein the eggshell powder retains the lipid-protein structure of the eggshell from which the eggshell powder is derived; and a polymer. 16. The product of claim 15, wherein the polymer is a thermoplastic polymer. 17. The product of claim 15, wherein the polymer is a thermoset polymer. 18. (canceled) 19. The product of claim 15, wherein the eggshell powder constitutes 25% by weight of the total weight of the product. 20.-25. (canceled) 26. The product of claim 15, wherein the eggshell powder has a particle size from about 20 μm to about 50 μm. 27. (canceled) 28. The product of claim 15, wherein the eggshell powder is hydrophobic. 29. A process for producing an eggshell powder comprising the steps of:
exposing a quantity of eggshell to air flow at a speed sufficient to pulverize the eggshell thereby rendering a bulk pulverized material comprising an eggshell component and a separated inner membrane component; applying the bulk pulverized material to a first screen comprising a mesh size sufficient to retain the separated inner membrane component on the surface of the first screen while permitting passage of the eggshell component through the first screen; and collecting the eggshell component following passage through the first screen, wherein the eggshell component collected forms the eggshell powder of a first particle size, wherein the first particle size is less than or equal to that permitted to pass through the first screen. 30. The process of claim 29, wherein the first particle size is less than or equal to 100 μm. 31. The process of claim 29, further comprising the step of applying the eggshell powder to a second screen comprising a mesh size sufficient to permit passage of a second particle size, wherein the second particle size is less than the first particle size; and
collecting the eggshell powder that passes through the second screen, wherein the eggshell powder that passes through the second screen has a particle size less than or equal to the second particle size. 32. The process of claim 31, wherein the second particle size is less than or equal to 50 μm. 33. The process of claim 31, wherein the second particle size is less than or equal to 20 μm. 34. (canceled) 35. The process of claim 31, further comprising the steps of:
collecting the eggshell powder that is retained on the second screen, wherein the eggshell powder retained on the second screen has a particle size greater than the second particle size; re-exposing the eggshell powder retained on the second screen to air flow at a speed sufficient to further reduce the particle size; and re-applying the eggshell powder to the second screen. 36. The process of claim 35 wherein the re-exposure of air flow is at a speed of 5,700 rpm for 10 seconds. 37. The process of claim 35 wherein the eggshell powder is exposed to air flow for a third time at a speed of 10,000 for 10 seconds. 38. The process of claim 29, further comprising the step of sterilizing the eggshell prior to pulverizing. 39. The process of claim 29, wherein the eggshell is not heated during the entire process. 40. The process of claim 29, wherein the air flow is at a speed of 3,500 rpm for 10 seconds. 41. The process of claim 29, wherein the step of exposing the eggshell to air flow is performed in a vortex dryer. 42. The process of claim 29, wherein the step of exposing the eggshell to air flow is performed in a cyclone wind tunnel. 43. A composition comprising an eggshell powder, wherein the eggshell powder possesses the lipid-protein structure of the eggshell from which the eggshell powder is derived, and wherein the eggshell powder is substantially free of eggshell inner membrane material. 44.-58. (canceled) 59. The composition of claim 43, wherein the eggshell powder has a particle size from about 10 μm to about 100 μm. 60.-82. (canceled) 83. The composition of claim 43, wherein the eggshell component is hydrophobic. 84.-87. (canceled) | 1,700 |
3,463 | 14,252,711 | 1,777 | A sample dispatcher is disclosed and is configured for individually introducing a plurality of portions of one or more sample fluids into a flow of a mobile phase of a liquid separation system. The liquid separation system is configured for separating compounds of the sample fluids and comprises a mobile phase drive configured for driving the mobile phase through a separation unit configured for separating compounds of the sample fluids in the mobile phase. The sample dispatcher comprises one or more sample reservoirs, each configured for receiving and temporarily storing a respective sample fluid portion or at least a part thereof, and a bypass channel. | 1. A sample dispatcher configured for individually introducing a plurality of portions of one or more sample fluids into a flow of a mobile phase of a separation system configured for separating compounds of the sample fluids, wherein the separation system comprises a mobile phase drive configured for driving the mobile phase through a separation unit configured for separating compounds of the sample fluids in the mobile phase; the sample dispatcher comprising:
one or more sample reservoirs, each configured for receiving and temporarily storing a respective sample fluid portion or at least a part thereof, and a bypass channel, wherein the sample dispatcher is configured for selectively coupling at least one of the one or more sample reservoirs between the mobile phase drive and the separation unit, and for coupling the bypass channel in parallel to the at least one of the one or more sample reservoirs and between the mobile phase drive and the separation unit during a dilution state of the sample dispatcher in order to dilute the respective sample fluid portion with the mobile phase. 2. The sample dispatcher of claim 1, wherein
the sample dispatcher is configured for coupling the bypass channel between the mobile phase drive and the separation unit at least during an intermediate state of the sample dispatcher wherein neither of the at least one of the one or more sample reservoirs is coupled between mobile phase drive and the separation unit. 3. A sample dispatcher configured for individually introducing a plurality of portions of one or more sample fluids into a flow of a mobile phase of a liquid separation system configured for separating compounds of the sample fluids, wherein the liquid separation system comprises a mobile phase drive configured for driving the mobile phase through a separation unit configured for separating compounds of the sample fluids in the mobile phase; the sample dispatcher comprising:
one or more sample reservoirs, each configured for receiving and temporarily storing a respective sample fluid portion or at least a part thereof, and a bypass channel, wherein the sample dispatcher is configured for selectively coupling the at least one of the one or more sample reservoirs between the mobile phase drive and the separation unit, and for coupling the bypass channel between the mobile phase drive and the separation unit at least during an intermediate state of the sample dispatcher wherein neither of the at least one of the one or more sample reservoirs is coupled between mobile phase drive and the separation unit. 4. The sample dispatcher of the preceding claim, wherein
the sample dispatcher is configured for coupling the bypass channel in parallel to either one of the at least one of the one or more sample reservoirs and between mobile phase drive and the separation unit during a dilution state of the sample dispatcher in order to dilute the respective sample fluid within the mobile phase. 5. The sample dispatcher of claim 1, being configured for having a sample reservoir state, wherein
at least one of the one or more sample reservoirs is coupled between the mobile phase drive and the separation unit while the bypass channel is not coupled between the mobile phase drive and the separation unit. 6. The sample dispatcher of claim 1, comprising at least one of:
the bypass channel is configured to have significantly smaller volume than each of the one or more sample reservoirs; the bypass channel is configured to be exchangeable or adjustable in its flow restrictivity, so that a flow ratio between a flow through the respective one of the at least one of the one or more sample reservoirs and a flow through the bypass channel and thus a dilution ratio in parallel connection can be adjusted; wherein the sample dispatcher is configured so that at any point in the time at least one of the one or more sample reservoirs and the bypass channel, either alone or in a parallel combination, is coupled between the mobile phase drive and the separation unit; the at least one of the one or more sample reservoirs comprise a first sample reservoir configured for receiving and temporarily storing a first sample fluid portion or at least a part thereof, and a second sample reservoir configured for receiving and temporarily storing a second sample fluid portion or at least a part thereof. 7. The sample dispatcher of claim 1, wherein
the sample dispatcher receives the plurality of portions of one or more sample fluids and is configured for loading a respective sample fluid portion into at least one of the one or more sample reservoirs. 8. A liquid separation system for separating sample fluid compounds, the liquid separation system comprising:
a first mobile phase drive, preferably a pumping system, adapted to drive a first mobile phase through the liquid separation system, a sample providing apparatus being configured to provide a plurality of portions of one or more sample fluids, a sample dispatcher of claim 1 being coupled to the first mobile phase drive and to the sample providing apparatus, and being configured to introduce the provided sample fluid portions into a flow of the first mobile phase, and a first separation unit, preferably a chromatographic column, adapted for separating compounds of the sample fluid in the first mobile phase, wherein the sample dispatcher is configured to load a respective sample fluid portion into at least one of the one or more sample reservoirs. 9. The liquid separation system of the preceding claim, further comprising at least one of:
a detector adapted to detect separated compounds of the sample fluid; a collection unit adapted to collect separated compounds of the sample fluid; a data processing unit adapted to process data received from the liquid separation system; a degasser for degassing the mobile phase. 10. The liquid separation system of claim 8, wherein the sample providing apparatus comprises:
a second mobile phase drive, preferably a pumping system, adapted to drive a second mobile phase through a separation subsystem; a second separation unit, preferably a chromatographic column, adapted for separating compounds of the sample fluid in the second mobile phase, wherein at least a portion of the separated compounds are provided to the sample dispatcher as the plurality of portions of one or more sample fluids. 11. A method of individually introducing a plurality of portions of one or more sample fluids into a flow of a mobile phase of a liquid separation system configured for separating compounds of the sample fluids, wherein the liquid separation system comprises: a mobile phase drive configured for driving the mobile phase through a separation unit configured for separating compounds of the sample fluids in the mobile phase, and a sample dispatcher having one or more sample reservoirs, each configured for receiving and temporarily storing a respective sample fluid portion or at least a part thereof, and a bypass channel; the method comprising:
selectively coupling at least one of the one or more sample reservoirs between the mobile phase drive and the separation unit, and coupling the bypass channel in parallel to the at least one of the one or more sample reservoirs and between the mobile phase drive and the separation unit during a dilution state of the sample dispatcher in order to dilute the respective sample fluid portion within the mobile phase. 12. The method of the preceding claim, further comprising:
coupling the bypass channel between the mobile phase drive and the separation unit at least during an intermediate state of the sample dispatcher wherein neither of the at least one of the one or more sample reservoirs is coupled between mobile phase drive and the separation unit. 13. A method of individually introducing a plurality of portions of one or more sample fluids into a flow of a mobile phase of a liquid separation system configured for separating compounds of the sample fluids, wherein the liquid separation system comprises: a mobile phase drive configured for driving the mobile phase through a separation unit configured for separating compounds of the sample fluids in the mobile phase, and a sample dispatcher having one or more sample reservoirs, each configured for receiving and temporarily storing a respective sample fluid portion or at least a part thereof, and a bypass channel; the method comprising:
selectively coupling at least one of the one or more sample reservoirs between the mobile phase drive and the separation unit, and coupling the bypass channel between the mobile phase drive and the separation unit at least during an intermediate state of the sample dispatcher wherein neither of the at least one of the one or more sample reservoirs is coupled between mobile phase drive and the separation unit. 14. A software program or product, preferably stored on a data carrier, for controlling or executing the method of claim 11 or any of the above claims, when run on a data processing system such as a computer. | A sample dispatcher is disclosed and is configured for individually introducing a plurality of portions of one or more sample fluids into a flow of a mobile phase of a liquid separation system. The liquid separation system is configured for separating compounds of the sample fluids and comprises a mobile phase drive configured for driving the mobile phase through a separation unit configured for separating compounds of the sample fluids in the mobile phase. The sample dispatcher comprises one or more sample reservoirs, each configured for receiving and temporarily storing a respective sample fluid portion or at least a part thereof, and a bypass channel.1. A sample dispatcher configured for individually introducing a plurality of portions of one or more sample fluids into a flow of a mobile phase of a separation system configured for separating compounds of the sample fluids, wherein the separation system comprises a mobile phase drive configured for driving the mobile phase through a separation unit configured for separating compounds of the sample fluids in the mobile phase; the sample dispatcher comprising:
one or more sample reservoirs, each configured for receiving and temporarily storing a respective sample fluid portion or at least a part thereof, and a bypass channel, wherein the sample dispatcher is configured for selectively coupling at least one of the one or more sample reservoirs between the mobile phase drive and the separation unit, and for coupling the bypass channel in parallel to the at least one of the one or more sample reservoirs and between the mobile phase drive and the separation unit during a dilution state of the sample dispatcher in order to dilute the respective sample fluid portion with the mobile phase. 2. The sample dispatcher of claim 1, wherein
the sample dispatcher is configured for coupling the bypass channel between the mobile phase drive and the separation unit at least during an intermediate state of the sample dispatcher wherein neither of the at least one of the one or more sample reservoirs is coupled between mobile phase drive and the separation unit. 3. A sample dispatcher configured for individually introducing a plurality of portions of one or more sample fluids into a flow of a mobile phase of a liquid separation system configured for separating compounds of the sample fluids, wherein the liquid separation system comprises a mobile phase drive configured for driving the mobile phase through a separation unit configured for separating compounds of the sample fluids in the mobile phase; the sample dispatcher comprising:
one or more sample reservoirs, each configured for receiving and temporarily storing a respective sample fluid portion or at least a part thereof, and a bypass channel, wherein the sample dispatcher is configured for selectively coupling the at least one of the one or more sample reservoirs between the mobile phase drive and the separation unit, and for coupling the bypass channel between the mobile phase drive and the separation unit at least during an intermediate state of the sample dispatcher wherein neither of the at least one of the one or more sample reservoirs is coupled between mobile phase drive and the separation unit. 4. The sample dispatcher of the preceding claim, wherein
the sample dispatcher is configured for coupling the bypass channel in parallel to either one of the at least one of the one or more sample reservoirs and between mobile phase drive and the separation unit during a dilution state of the sample dispatcher in order to dilute the respective sample fluid within the mobile phase. 5. The sample dispatcher of claim 1, being configured for having a sample reservoir state, wherein
at least one of the one or more sample reservoirs is coupled between the mobile phase drive and the separation unit while the bypass channel is not coupled between the mobile phase drive and the separation unit. 6. The sample dispatcher of claim 1, comprising at least one of:
the bypass channel is configured to have significantly smaller volume than each of the one or more sample reservoirs; the bypass channel is configured to be exchangeable or adjustable in its flow restrictivity, so that a flow ratio between a flow through the respective one of the at least one of the one or more sample reservoirs and a flow through the bypass channel and thus a dilution ratio in parallel connection can be adjusted; wherein the sample dispatcher is configured so that at any point in the time at least one of the one or more sample reservoirs and the bypass channel, either alone or in a parallel combination, is coupled between the mobile phase drive and the separation unit; the at least one of the one or more sample reservoirs comprise a first sample reservoir configured for receiving and temporarily storing a first sample fluid portion or at least a part thereof, and a second sample reservoir configured for receiving and temporarily storing a second sample fluid portion or at least a part thereof. 7. The sample dispatcher of claim 1, wherein
the sample dispatcher receives the plurality of portions of one or more sample fluids and is configured for loading a respective sample fluid portion into at least one of the one or more sample reservoirs. 8. A liquid separation system for separating sample fluid compounds, the liquid separation system comprising:
a first mobile phase drive, preferably a pumping system, adapted to drive a first mobile phase through the liquid separation system, a sample providing apparatus being configured to provide a plurality of portions of one or more sample fluids, a sample dispatcher of claim 1 being coupled to the first mobile phase drive and to the sample providing apparatus, and being configured to introduce the provided sample fluid portions into a flow of the first mobile phase, and a first separation unit, preferably a chromatographic column, adapted for separating compounds of the sample fluid in the first mobile phase, wherein the sample dispatcher is configured to load a respective sample fluid portion into at least one of the one or more sample reservoirs. 9. The liquid separation system of the preceding claim, further comprising at least one of:
a detector adapted to detect separated compounds of the sample fluid; a collection unit adapted to collect separated compounds of the sample fluid; a data processing unit adapted to process data received from the liquid separation system; a degasser for degassing the mobile phase. 10. The liquid separation system of claim 8, wherein the sample providing apparatus comprises:
a second mobile phase drive, preferably a pumping system, adapted to drive a second mobile phase through a separation subsystem; a second separation unit, preferably a chromatographic column, adapted for separating compounds of the sample fluid in the second mobile phase, wherein at least a portion of the separated compounds are provided to the sample dispatcher as the plurality of portions of one or more sample fluids. 11. A method of individually introducing a plurality of portions of one or more sample fluids into a flow of a mobile phase of a liquid separation system configured for separating compounds of the sample fluids, wherein the liquid separation system comprises: a mobile phase drive configured for driving the mobile phase through a separation unit configured for separating compounds of the sample fluids in the mobile phase, and a sample dispatcher having one or more sample reservoirs, each configured for receiving and temporarily storing a respective sample fluid portion or at least a part thereof, and a bypass channel; the method comprising:
selectively coupling at least one of the one or more sample reservoirs between the mobile phase drive and the separation unit, and coupling the bypass channel in parallel to the at least one of the one or more sample reservoirs and between the mobile phase drive and the separation unit during a dilution state of the sample dispatcher in order to dilute the respective sample fluid portion within the mobile phase. 12. The method of the preceding claim, further comprising:
coupling the bypass channel between the mobile phase drive and the separation unit at least during an intermediate state of the sample dispatcher wherein neither of the at least one of the one or more sample reservoirs is coupled between mobile phase drive and the separation unit. 13. A method of individually introducing a plurality of portions of one or more sample fluids into a flow of a mobile phase of a liquid separation system configured for separating compounds of the sample fluids, wherein the liquid separation system comprises: a mobile phase drive configured for driving the mobile phase through a separation unit configured for separating compounds of the sample fluids in the mobile phase, and a sample dispatcher having one or more sample reservoirs, each configured for receiving and temporarily storing a respective sample fluid portion or at least a part thereof, and a bypass channel; the method comprising:
selectively coupling at least one of the one or more sample reservoirs between the mobile phase drive and the separation unit, and coupling the bypass channel between the mobile phase drive and the separation unit at least during an intermediate state of the sample dispatcher wherein neither of the at least one of the one or more sample reservoirs is coupled between mobile phase drive and the separation unit. 14. A software program or product, preferably stored on a data carrier, for controlling or executing the method of claim 11 or any of the above claims, when run on a data processing system such as a computer. | 1,700 |
3,464 | 14,230,895 | 1,794 | The present invention describes a composition and method to control dimensional growth during an anodizing process. Potassium permanganate has been discovered, when added to an anodizing solution containing at least one acid, to minimize dimensional change. This novel composition and method were found to be safer, quicker and less expensive than the conventional method of anodizing aluminum. In addition, the novel composition and method were found to have superior properties to aluminum anodized by the conventional method with respect to durability and corrosion resistance. In addition to anodizing, the novel solution described herein is capable of several other uses including the removal of organic and metal contaminants from solution, producing black electroless nickel on a substrate, producing a bright nickel coating on a substrate such as aluminum, and cleaning and activating aluminum for plating. | 1. An anodizing solution comprising:
deionized water; at least one acid selected from the group consisting of sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, citric acid, boric acid, carboxylic acid, carbonic acid and combinations thereof; and at least one oxidizing agent selected from the group consisting of potassium permanganate, sodium permanganate, hydrogen permanganate, lithium permanganate, sodium persulfate, potassium persulfate, ammonium persulfate, sodium orthovanadate and combinations thereof. 2. The solution of claim 1, wherein the acid is present in the solution at a concentration of between about 1% w/v to about 40% w/v. 3. The solution of claim 1, wherein the acid is sulfuric acid. 4. The solution of claim 3, wherein the acid is present in the solution at a concentration of between about 10% w/v to about 20% w/v. 5. The composition of claim 1, wherein the oxidizing agent is present in the solution at a concentration of between about 0.01% w/v to about 10% w/v. 6. The composition of claim 1, wherein the oxidizing agent is potassium permanganate. 7. The composition of claim 6, wherein the oxidizing agent is present in the solution at a concentration of between about 0.01% w/v to about 10% w/v. 8. A method of controlling dimensional growth in an anodizing process comprising:
adding at least one acid to a container of deionized water to form a solution wherein the acid is selected from the group consisting of sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, citric acid, boric acid, carboxylic acid, carbonic acid and combinations thereof; adding at least one oxidizing agent to the solution wherein the oxidizing agent is selected from the group consisting of potassium permanganate, sodium permanganate, hydrogen permanganate, lithium permanganate, sodium persulfate, potassium persulfate, ammonium persulfate, sodium orthovanadate and combinations thereof; placing the solution in a test plating cell; cooling the solution; placing a metal substrate into the cooled solution; anodizing the metal substrate for a specified amount of time; and removing the anodized metal substrate from the test plating cell. 9. The method of claim 8, further comprising cleaning the metal specimen prior to placement in the cooled solution. 10. The method of claim 8, further comprising cooling the solution to room temperature prior to adding the oxidizing agent. 11. The method of claim 8, wherein the acid is sulfuric acid. 12. The method of claim 11, wherein the concentration of sulfuric acid in the solution is between about 10% w/v to about 20% w/v. 13. The method of claim 8, wherein the oxidizing agent is potassium permanganate. 14. The method of claim 13, wherein the concentration of potassium permanganate is about 0.01% w/v to about 10% w/v. 15. The method of claim 8, wherein the anodizing step occurs at a temperature of between about 60° F. to about 75° F. 16. The method of claim 8, wherein the anodizing step uses direct current (DC) voltage. 17. The method of claim 16, wherein the anodizing step uses DC voltage at about 15 V. 18. The method of claim 8, wherein the metal specimen is anodized for between about 20 to about 30 minutes. 19. A method of forming a bright nickel coating on a substrate comprising:
plating a substrate with an electrolytic nickel coating; plating an electrolytic zinc coating over the nickel coating; and immersing the substrate into a solution comprising
deionized water;
at least one acid selected from the group consisting of sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, citric acid, boric acid, carboxylic acid, carbonic acid and combinations thereof; and
at least one oxidizing agent selected from the group consisting of potassium permanganate, sodium permanganate, hydrogen permanganate, lithium permanganate, sodium persulfate, potassium persulfate, ammonium persulfate, sodium orthovanadate and combinations thereof;
removing the substrate from the solution; wherein after immersion, the substrate exhibits a bright nickel coating. 20. The method of claim 19, wherein the substrate is selected from the group consisting of zinc, copper, brass, steel and aluminum. 21. The method of claim 19, wherein the at least one acid in the solution is sulfuric acid. 22. The method of claim 21, wherein the concentration of sulfuric acid in the solution is between about 10% w/v to about 20% w/v. 23. The method of claim 19, wherein the oxidizing agent is potassium permanganate. 24. The method of claim 23, wherein the concentration of potassium permanganate in the solution is about 0.01% w/v to about 10% w/v. 25. A method of forming a black electroless nickel coating on a substrate comprising:
plating a substrate with a phosphorous electroless nickel coating wherein coating is between about 5% to about 10% phosphorous; immersing the substrate in a solution comprising
deionized water;
at least one acid selected from the group consisting of sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, citric acid, boric acid, carboxylic acid carbonic acid and combinations thereof; and
at least one oxidizing agent selected from the group consisting of potassium permanganate, sodium permanganate, hydrogen permanganate, lithium permanganate, sodium persulfate, potassium persulfate, ammonium persulfate, sodium orthovanadate and combinations thereof;
removing the substrate from the solution; wherein after immersion, the substrate exhibits a hard black electroless nickel coating. 26. The method of claim 25, wherein the phosphorous electroless nickel coating is selected from the group consisting of mid-phosphorous electroless nickel coating and high-phosphorous electroless nickel coating. 27. The method of claim 25, wherein the substrate is selected from the group consisting of aluminum, steel, copper and brass. 28. The method of claim 25, wherein the at least one acid in the solution is sulfuric acid. 29. The method of claim 28, wherein the concentration of sulfuric acid in the solution is between about 10% w/v to about 20% w/v. 30. The method of claim 25, wherein the oxidizing agent is potassium permanganate. 31. The method of claim 30, wherein the concentration of potassium permanganate in the solution is about 0.01% w/v to about 10% w/v. 32. A method of cleaning and activating aluminum for plating comprising:
immersing an aluminum substrate in a solution comprising
deionized water;
at least one acid selected from the group consisting of sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, citric acid, boric acid, carboxylic acid, carbonic acid and combinations thereof; and
at least one oxidizing agent selected from the group consisting of potassium permanganate, sodium permanganate, hydrogen permanganate, lithium permanganate, sodium persulfate, potassium persulfate, ammonium persulfate, sodium orthovanadate and combinations thereof;
removing the substrate from the solution; immersing the substrate in an electroless nickel plating solution for about 15 minutes; removing the substrate from the electroless nickel plating solution; wherein after removal from the electroless nickel plating solution the substrate exhibits excellent adhesion properties and is activated for plating. 33. The method of claim 32, wherein the at least one acid in the solution is sulfuric acid. 34. The method of claim 33, wherein the concentration of sulfuric acid in the solution is between about 10% w/v to about 20% w/v. 35. The method of claim 32, wherein the oxidizing agent is potassium permanganate. 36. The method of claim 35, wherein the concentration of potassium permanganate in the solution is about 0.01% w/v to about 10% w/v. | The present invention describes a composition and method to control dimensional growth during an anodizing process. Potassium permanganate has been discovered, when added to an anodizing solution containing at least one acid, to minimize dimensional change. This novel composition and method were found to be safer, quicker and less expensive than the conventional method of anodizing aluminum. In addition, the novel composition and method were found to have superior properties to aluminum anodized by the conventional method with respect to durability and corrosion resistance. In addition to anodizing, the novel solution described herein is capable of several other uses including the removal of organic and metal contaminants from solution, producing black electroless nickel on a substrate, producing a bright nickel coating on a substrate such as aluminum, and cleaning and activating aluminum for plating.1. An anodizing solution comprising:
deionized water; at least one acid selected from the group consisting of sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, citric acid, boric acid, carboxylic acid, carbonic acid and combinations thereof; and at least one oxidizing agent selected from the group consisting of potassium permanganate, sodium permanganate, hydrogen permanganate, lithium permanganate, sodium persulfate, potassium persulfate, ammonium persulfate, sodium orthovanadate and combinations thereof. 2. The solution of claim 1, wherein the acid is present in the solution at a concentration of between about 1% w/v to about 40% w/v. 3. The solution of claim 1, wherein the acid is sulfuric acid. 4. The solution of claim 3, wherein the acid is present in the solution at a concentration of between about 10% w/v to about 20% w/v. 5. The composition of claim 1, wherein the oxidizing agent is present in the solution at a concentration of between about 0.01% w/v to about 10% w/v. 6. The composition of claim 1, wherein the oxidizing agent is potassium permanganate. 7. The composition of claim 6, wherein the oxidizing agent is present in the solution at a concentration of between about 0.01% w/v to about 10% w/v. 8. A method of controlling dimensional growth in an anodizing process comprising:
adding at least one acid to a container of deionized water to form a solution wherein the acid is selected from the group consisting of sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, citric acid, boric acid, carboxylic acid, carbonic acid and combinations thereof; adding at least one oxidizing agent to the solution wherein the oxidizing agent is selected from the group consisting of potassium permanganate, sodium permanganate, hydrogen permanganate, lithium permanganate, sodium persulfate, potassium persulfate, ammonium persulfate, sodium orthovanadate and combinations thereof; placing the solution in a test plating cell; cooling the solution; placing a metal substrate into the cooled solution; anodizing the metal substrate for a specified amount of time; and removing the anodized metal substrate from the test plating cell. 9. The method of claim 8, further comprising cleaning the metal specimen prior to placement in the cooled solution. 10. The method of claim 8, further comprising cooling the solution to room temperature prior to adding the oxidizing agent. 11. The method of claim 8, wherein the acid is sulfuric acid. 12. The method of claim 11, wherein the concentration of sulfuric acid in the solution is between about 10% w/v to about 20% w/v. 13. The method of claim 8, wherein the oxidizing agent is potassium permanganate. 14. The method of claim 13, wherein the concentration of potassium permanganate is about 0.01% w/v to about 10% w/v. 15. The method of claim 8, wherein the anodizing step occurs at a temperature of between about 60° F. to about 75° F. 16. The method of claim 8, wherein the anodizing step uses direct current (DC) voltage. 17. The method of claim 16, wherein the anodizing step uses DC voltage at about 15 V. 18. The method of claim 8, wherein the metal specimen is anodized for between about 20 to about 30 minutes. 19. A method of forming a bright nickel coating on a substrate comprising:
plating a substrate with an electrolytic nickel coating; plating an electrolytic zinc coating over the nickel coating; and immersing the substrate into a solution comprising
deionized water;
at least one acid selected from the group consisting of sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, citric acid, boric acid, carboxylic acid, carbonic acid and combinations thereof; and
at least one oxidizing agent selected from the group consisting of potassium permanganate, sodium permanganate, hydrogen permanganate, lithium permanganate, sodium persulfate, potassium persulfate, ammonium persulfate, sodium orthovanadate and combinations thereof;
removing the substrate from the solution; wherein after immersion, the substrate exhibits a bright nickel coating. 20. The method of claim 19, wherein the substrate is selected from the group consisting of zinc, copper, brass, steel and aluminum. 21. The method of claim 19, wherein the at least one acid in the solution is sulfuric acid. 22. The method of claim 21, wherein the concentration of sulfuric acid in the solution is between about 10% w/v to about 20% w/v. 23. The method of claim 19, wherein the oxidizing agent is potassium permanganate. 24. The method of claim 23, wherein the concentration of potassium permanganate in the solution is about 0.01% w/v to about 10% w/v. 25. A method of forming a black electroless nickel coating on a substrate comprising:
plating a substrate with a phosphorous electroless nickel coating wherein coating is between about 5% to about 10% phosphorous; immersing the substrate in a solution comprising
deionized water;
at least one acid selected from the group consisting of sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, citric acid, boric acid, carboxylic acid carbonic acid and combinations thereof; and
at least one oxidizing agent selected from the group consisting of potassium permanganate, sodium permanganate, hydrogen permanganate, lithium permanganate, sodium persulfate, potassium persulfate, ammonium persulfate, sodium orthovanadate and combinations thereof;
removing the substrate from the solution; wherein after immersion, the substrate exhibits a hard black electroless nickel coating. 26. The method of claim 25, wherein the phosphorous electroless nickel coating is selected from the group consisting of mid-phosphorous electroless nickel coating and high-phosphorous electroless nickel coating. 27. The method of claim 25, wherein the substrate is selected from the group consisting of aluminum, steel, copper and brass. 28. The method of claim 25, wherein the at least one acid in the solution is sulfuric acid. 29. The method of claim 28, wherein the concentration of sulfuric acid in the solution is between about 10% w/v to about 20% w/v. 30. The method of claim 25, wherein the oxidizing agent is potassium permanganate. 31. The method of claim 30, wherein the concentration of potassium permanganate in the solution is about 0.01% w/v to about 10% w/v. 32. A method of cleaning and activating aluminum for plating comprising:
immersing an aluminum substrate in a solution comprising
deionized water;
at least one acid selected from the group consisting of sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, citric acid, boric acid, carboxylic acid, carbonic acid and combinations thereof; and
at least one oxidizing agent selected from the group consisting of potassium permanganate, sodium permanganate, hydrogen permanganate, lithium permanganate, sodium persulfate, potassium persulfate, ammonium persulfate, sodium orthovanadate and combinations thereof;
removing the substrate from the solution; immersing the substrate in an electroless nickel plating solution for about 15 minutes; removing the substrate from the electroless nickel plating solution; wherein after removal from the electroless nickel plating solution the substrate exhibits excellent adhesion properties and is activated for plating. 33. The method of claim 32, wherein the at least one acid in the solution is sulfuric acid. 34. The method of claim 33, wherein the concentration of sulfuric acid in the solution is between about 10% w/v to about 20% w/v. 35. The method of claim 32, wherein the oxidizing agent is potassium permanganate. 36. The method of claim 35, wherein the concentration of potassium permanganate in the solution is about 0.01% w/v to about 10% w/v. | 1,700 |
3,465 | 14,974,926 | 1,792 | The rate of degradation of a cooked food product that is maintained at an elevated temperature can be reduced by the use of an encapsulated environment food holder. The encapsulated environment is a small, airtight or semi-airtight containment vessel that retains compositions that escape from a cooked food product over time. The volume of an encapsulated environment is greater than one hundred percent but less than one-thousand percent of the cooked food product volume. By holding single servings or portions of a cooked food product in a small, encapsulated environment palatability or taste of a cooked food product can be extended. | 1-8. (canceled) 9. An apparatus for preserving the palatability of a cooked food product having a predetermined volume, the apparatus comprising:
a food holding cabinet having a plurality of food holding compartments, at least one of the food holding compartments including a heating element that maintains a temperature of the food holding compartment at an elevated, food holding temperature of 140° F. or greater; a food holding tray disposed within one of the food holding compartments; and an encapsulated environment device disposed within the food holding tray, the encapsulated environment device being made from a material impermeable to liquids and gases emitted from a cooked food product that is disposed within the encapsulated environment device, the cooked food product displacing a first volume, wherein an interior volume of the encapsulated environment device encloses the cooked food product within a predetermined headspace volume, the headspace volume being greater than one hundred percent of the first volume but less than one-thousand percent of the first volume. 10. The apparatus of claim 9, wherein the encapsulated environment is comprised of at least one vent. 11. The apparatus of claim 9, wherein the encapsulated environment is configured to maintain a cooked food product in contact with compositions from the cooked food product. 12. The apparatus of claim 9, wherein the encapsulated environment is configured to maintain a cooked food product separated from compositions from the cooked food product. 13. (canceled) 14. The apparatus of claim 9, wherein the heating device comprises the food holding tray. 15. The apparatus of claim 9, wherein the heating device is a grill surface. 16. The apparatus of claim 9, wherein the heating device is comprised of a source of infrared energy configured to direct infrared energy downwardly. 17. The apparatus of claim 9, wherein the heating device is comprised of a solar oven. 18. The apparatus of claim 9, wherein the encapsulated environment device has an interior shape that is substantially cylindrical. 19. The apparatus of claim 9, wherein the encapsulated environment device has an interior shape that is substantially a parallelepiped. 20. The apparatus of claim 9, further comprising a timer configured to measure a time period, prior to the expiration of which the cooked food product is served, after the expiration of which the food product is discarded. 21. The apparatus of claim 9, wherein the cooked food product comprises a cooked patty and wherein the encapsulated environment device comprises a substantially cylindrical base portion having a closed bottom and an open top, the encapsulated environment device further comprising a top, which is configured to fit over and close the open top of the base portion such that when the base portion and the top are assembled, they provide an enclosed volume. 22. A method of preserving the palatability of a cooked food product, the method comprising:
cooking a food product, the food product displacing a first volume; placing the food product into an encapsulated environment device, the encapsulated environment device being made from a material impermeable to liquids and gases emitted from the food product, an interior volume of the encapsulated environment device enclosing the cooked food product within a predetermined headspace volume, the headspace volume being greater than one hundred percent of the first volume but less than one-thousand percent of the first volume; and maintaining the food product at an elevated temperature of at least 140° F. within the encapsulated environment device. 23. The method of claim 22, further comprising:
venting some, but not all, of the compositions released from the food product out of the encapsulated environment device. 24. The method of claim 22, further comprising:
starting a timer after placing the food product into the encapsulated environment device; and discarding the food product if the timer reaches a predetermined maximum holding time. 25. The method of claim 22, wherein the predetermined maximum holding time is greater than 15 minutes, but less than 1.5 hours. 26. The method of claim 22, further comprising:
placing the encapsulated environment device into a food holding cabinet, the food holding cabinet including a plurality of food holding compartments. 27. The method of claim 22, further comprising:
placing the encapsulated environment device into a food holding tray. 28. The method of claim 22, further comprising:
placing the encapsulated environment device onto a grill. 29. The method of claim 22, further comprising:
placing the encapsulated environment device under a heat lamp. | The rate of degradation of a cooked food product that is maintained at an elevated temperature can be reduced by the use of an encapsulated environment food holder. The encapsulated environment is a small, airtight or semi-airtight containment vessel that retains compositions that escape from a cooked food product over time. The volume of an encapsulated environment is greater than one hundred percent but less than one-thousand percent of the cooked food product volume. By holding single servings or portions of a cooked food product in a small, encapsulated environment palatability or taste of a cooked food product can be extended.1-8. (canceled) 9. An apparatus for preserving the palatability of a cooked food product having a predetermined volume, the apparatus comprising:
a food holding cabinet having a plurality of food holding compartments, at least one of the food holding compartments including a heating element that maintains a temperature of the food holding compartment at an elevated, food holding temperature of 140° F. or greater; a food holding tray disposed within one of the food holding compartments; and an encapsulated environment device disposed within the food holding tray, the encapsulated environment device being made from a material impermeable to liquids and gases emitted from a cooked food product that is disposed within the encapsulated environment device, the cooked food product displacing a first volume, wherein an interior volume of the encapsulated environment device encloses the cooked food product within a predetermined headspace volume, the headspace volume being greater than one hundred percent of the first volume but less than one-thousand percent of the first volume. 10. The apparatus of claim 9, wherein the encapsulated environment is comprised of at least one vent. 11. The apparatus of claim 9, wherein the encapsulated environment is configured to maintain a cooked food product in contact with compositions from the cooked food product. 12. The apparatus of claim 9, wherein the encapsulated environment is configured to maintain a cooked food product separated from compositions from the cooked food product. 13. (canceled) 14. The apparatus of claim 9, wherein the heating device comprises the food holding tray. 15. The apparatus of claim 9, wherein the heating device is a grill surface. 16. The apparatus of claim 9, wherein the heating device is comprised of a source of infrared energy configured to direct infrared energy downwardly. 17. The apparatus of claim 9, wherein the heating device is comprised of a solar oven. 18. The apparatus of claim 9, wherein the encapsulated environment device has an interior shape that is substantially cylindrical. 19. The apparatus of claim 9, wherein the encapsulated environment device has an interior shape that is substantially a parallelepiped. 20. The apparatus of claim 9, further comprising a timer configured to measure a time period, prior to the expiration of which the cooked food product is served, after the expiration of which the food product is discarded. 21. The apparatus of claim 9, wherein the cooked food product comprises a cooked patty and wherein the encapsulated environment device comprises a substantially cylindrical base portion having a closed bottom and an open top, the encapsulated environment device further comprising a top, which is configured to fit over and close the open top of the base portion such that when the base portion and the top are assembled, they provide an enclosed volume. 22. A method of preserving the palatability of a cooked food product, the method comprising:
cooking a food product, the food product displacing a first volume; placing the food product into an encapsulated environment device, the encapsulated environment device being made from a material impermeable to liquids and gases emitted from the food product, an interior volume of the encapsulated environment device enclosing the cooked food product within a predetermined headspace volume, the headspace volume being greater than one hundred percent of the first volume but less than one-thousand percent of the first volume; and maintaining the food product at an elevated temperature of at least 140° F. within the encapsulated environment device. 23. The method of claim 22, further comprising:
venting some, but not all, of the compositions released from the food product out of the encapsulated environment device. 24. The method of claim 22, further comprising:
starting a timer after placing the food product into the encapsulated environment device; and discarding the food product if the timer reaches a predetermined maximum holding time. 25. The method of claim 22, wherein the predetermined maximum holding time is greater than 15 minutes, but less than 1.5 hours. 26. The method of claim 22, further comprising:
placing the encapsulated environment device into a food holding cabinet, the food holding cabinet including a plurality of food holding compartments. 27. The method of claim 22, further comprising:
placing the encapsulated environment device into a food holding tray. 28. The method of claim 22, further comprising:
placing the encapsulated environment device onto a grill. 29. The method of claim 22, further comprising:
placing the encapsulated environment device under a heat lamp. | 1,700 |
3,466 | 14,726,947 | 1,781 | A coated component with a coating applied by Electron Beam Physical Vapor Deposition (EB-PVD) includes at least one Non Line of Sight (NLOS) area and at least one Line of Sight (LOS) area, a coating on the workpiece defines a ratio greater than about 10% NLOS/LOS. | 1. A coated component with a coating applied by Electron Beam Physical Vapor Deposition (EB-PVD), comprising:
at least one Non Line of Sight (NLOS) area and at least one Line of Sight (LOS) area, a coating on the workpiece defines a ratio greater than about 10% NLOS/LOS. 2. The component as recited in claim 1, wherein the coating applied to the workpiece is at a ratio of between about 10%-50% NLOS/LOS. 3. The component as recited in claim 1, wherein the coating applied to the workpiece is at about 5-15 mil thick in the LOS area. 4. The component as recited in claim 1, wherein the coating applied to the workpiece is at about 4-11 mil thick in the NLOS area. 5. The component as recited in claim 1, wherein the coating applied to the workpiece is at about 5-15 mil thick at the LOS area and about 4-11 mil thick NLOS area. 6. The component as recited in claim 1, wherein the coating applied to the workpiece is at a ratio of about 10 mil thick at the LOS area to about 4 mil thick at the NLOS area. 7. The component as recited in claim 1, wherein the LOS area includes a leading edge of an airfoil. 8. The component as recited in claim 1, wherein the NLOS area includes an area between two airfoils. 9. A coated component, comprising:
at least one Non Line of Sight (NLOS) area including an area adjacent to an airfoil and at least one Line of Sight (LOS) area including a leading edge of the airfoil, a coating on the workpiece defines a ratio greater than about 10% NLOS/LOS. 10. The component as recited in claim 9, wherein the coating applied to the workpiece is at a ratio of between about 10%-50% NLOS/LOS. 11. The component as recited in claim 9, wherein the coating applied to the workpiece is at about 5-15 mil thick in the LOS area. 12. The component as recited in claim 9, wherein the coating applied to the workpiece is at about 4-11 mil thick in the NLOS area. 13. The component as recited in claim 9, wherein the coating applied to the workpiece is at about 5-15 mil thick at the LOS area and about 4-11 mil thick NLOS area. 14. The component as recited in claim 9, wherein the coating applied to the workpiece is at a ratio of about 10 mil thick at the LOS area to about 4 mil thick at the NLOS area. 15. A method of Electron Beam Physical Vapor Deposition, comprising:
maintaining a deposition chamber at a pressure between about 4-20 Pa; and positioning a workpiece with a part manipulator to position a workpiece within the deposition chamber and respect to an ingot to define at least one Non Line of Sight (NLOS) area and at least one Line of Sight (LOS) area, wherein the coating applied to the workpiece is at a ratio greater than about 10% NLOS/LOS. 16. The method as recited in claim 15, wherein the coating applied to the workpiece is at about 5-15 mil thick at the LOS area. 17. The method as recited in claim 15, wherein the coating applied to the workpiece is at about 4-11 mil thick at the NLOS area. 18. The method as recited in claim 15, wherein the LOS area includes a leading edge of an airfoil. 19. The method as recited in claim 15, wherein the NLOS area includes an area between two airfoils. 20. The method as recited in claim 15, wherein the coating applied to the workpiece is at a ratio of between about 10%-50% NLOS/LOS. | A coated component with a coating applied by Electron Beam Physical Vapor Deposition (EB-PVD) includes at least one Non Line of Sight (NLOS) area and at least one Line of Sight (LOS) area, a coating on the workpiece defines a ratio greater than about 10% NLOS/LOS.1. A coated component with a coating applied by Electron Beam Physical Vapor Deposition (EB-PVD), comprising:
at least one Non Line of Sight (NLOS) area and at least one Line of Sight (LOS) area, a coating on the workpiece defines a ratio greater than about 10% NLOS/LOS. 2. The component as recited in claim 1, wherein the coating applied to the workpiece is at a ratio of between about 10%-50% NLOS/LOS. 3. The component as recited in claim 1, wherein the coating applied to the workpiece is at about 5-15 mil thick in the LOS area. 4. The component as recited in claim 1, wherein the coating applied to the workpiece is at about 4-11 mil thick in the NLOS area. 5. The component as recited in claim 1, wherein the coating applied to the workpiece is at about 5-15 mil thick at the LOS area and about 4-11 mil thick NLOS area. 6. The component as recited in claim 1, wherein the coating applied to the workpiece is at a ratio of about 10 mil thick at the LOS area to about 4 mil thick at the NLOS area. 7. The component as recited in claim 1, wherein the LOS area includes a leading edge of an airfoil. 8. The component as recited in claim 1, wherein the NLOS area includes an area between two airfoils. 9. A coated component, comprising:
at least one Non Line of Sight (NLOS) area including an area adjacent to an airfoil and at least one Line of Sight (LOS) area including a leading edge of the airfoil, a coating on the workpiece defines a ratio greater than about 10% NLOS/LOS. 10. The component as recited in claim 9, wherein the coating applied to the workpiece is at a ratio of between about 10%-50% NLOS/LOS. 11. The component as recited in claim 9, wherein the coating applied to the workpiece is at about 5-15 mil thick in the LOS area. 12. The component as recited in claim 9, wherein the coating applied to the workpiece is at about 4-11 mil thick in the NLOS area. 13. The component as recited in claim 9, wherein the coating applied to the workpiece is at about 5-15 mil thick at the LOS area and about 4-11 mil thick NLOS area. 14. The component as recited in claim 9, wherein the coating applied to the workpiece is at a ratio of about 10 mil thick at the LOS area to about 4 mil thick at the NLOS area. 15. A method of Electron Beam Physical Vapor Deposition, comprising:
maintaining a deposition chamber at a pressure between about 4-20 Pa; and positioning a workpiece with a part manipulator to position a workpiece within the deposition chamber and respect to an ingot to define at least one Non Line of Sight (NLOS) area and at least one Line of Sight (LOS) area, wherein the coating applied to the workpiece is at a ratio greater than about 10% NLOS/LOS. 16. The method as recited in claim 15, wherein the coating applied to the workpiece is at about 5-15 mil thick at the LOS area. 17. The method as recited in claim 15, wherein the coating applied to the workpiece is at about 4-11 mil thick at the NLOS area. 18. The method as recited in claim 15, wherein the LOS area includes a leading edge of an airfoil. 19. The method as recited in claim 15, wherein the NLOS area includes an area between two airfoils. 20. The method as recited in claim 15, wherein the coating applied to the workpiece is at a ratio of between about 10%-50% NLOS/LOS. | 1,700 |
3,467 | 14,269,905 | 1,796 | Alumina binder obtained from aluminum sulfate, the process of preparing the binder and the process of using the binder to prepare catalyst compositions are disclosed. Catalytic cracking catalyst compositions, in particularly, fluid catalytic cracking catalyst composition comprising zeolites, optionally clay and matrix materials bound by an alumina binder obtained from aluminum sulfate are disclosed. | 1-22. (canceled) 23. A method of forming a particulate composition of matter having a Davison Index of less than 30, said method comprising
a) forming an aqueous slurry comprising a plurality of inorganic metal oxide particles and aluminum sulfate in an amount sufficient to provide at least 5 wt % alumina in a final particulate inorganic metal oxide composition; b) optionally, milling the slurry; c) spray drying the slurry to form inorganic metal oxide particles bound by aluminum sulfate; d) optionally, calcining the aluminum sulfate bound metal oxide particles; e) re-slurrying the aluminum sulfate bound inorganic metal oxide particles in an aqueous base solution at a pH of about 7 to about 13 for a time and at a temperature sufficient to remove all or substantially all sulfate ions; and; f) recovering and drying the resulting inorganic metal oxide composition to obtain a final inorganic metal oxide composition bound with alumina obtained from aluminum sulfate. 24. The method of claim 23 wherein aluminum sulfate is present in the slurry in an amount sufficient to provide about 5 to about 25 wt % of the alumina in the final inorganic metal oxide composition. 25. The method of claim 23 wherein the aluminum sulfate bound particles are calcined at temperatures ranging from about 150° C. to about 600° C. for about 2 hours to about 10 minutes. 26. The method of claim 23 wherein the temperature during the re-slurry step ranges from about 1° C. to about 100° C. for about 1 minute to about 3 hours. 27. A method of forming a catalytic cracking catalyst composition having a Davison Index of less than 30, said method comprising
a) forming an aqueous slurry comprising at least one zeolite particle having catalytic cracking activity under catalytic cracking conditions and aluminum sulfate in an amount sufficient to provide at least 5 wt % alumina in a final catalyst composition; b) milling the slurry; c) spray drying the milled slurry to form particles; d) calcining the spray-dried particles at a temperature and for a time sufficient to remove volatiles; e) re-slurrying the calcined particles in an aqueous base solution at a pH of about 7 to about 13 for a time and at a temperature sufficient to remove all or substantially all sulfate ions; and f) recovering and drying the resulting particles to obtain a final catalyst composition comprising at least 5 wt % alumina obtained from aluminum sulfate. 28. The method of claim 27 wherein aluminum sulfate is present in the slurry in an amount significant to provide about 5 to about 25 wt % alumina obtained from aluminum sulfate in the final catalyst composition. 29. The method of claim 27 wherein the spray-dried particles are calcined at temperatures ranging from about 150° C. to about 600° C. for about 2 hours to about 10 minutes. 30. The method of claim 27 wherein the temperature during the re-slurry step ranges from about 1° C. to about 100° C. for about 1 minute to about 3 hours. 31. The method of claim 27 wherein the at least one zeolite comprise faujasite zeolite. 32. The method of claim 31 wherein the faujasite zeolite is selected from the group consisting of Y-type zeolite, USY zeolite, REUSY zeolite, or a mixture thereof. 33. The method of claim 32 wherein the zeolite is partially exchanged with ions selected from the group consisting of rare earth metals ions, alkaline earth metal ions, ammonium ions, acid ions and mixtures thereof. 34. The method of claim 27 wherein the slurry further comprises clay. 35. The method of claim 27 wherein the slurry further comprises at least one matrix material selected from the group consisting of alumina, silcica, silica-alumina, oxides of transition metals selected from Groups 3, 4, 5, 6, 7, 8, 9, 10, 11, 12 of the New Notations of the Periodic Table, oxides of rare earth metals, oxides of alkaline earth metals and mixtures thereof. 36-38. (canceled) 39. The method of claim 34 wherein the slurry further comprises at least one matrix material selected from the group consisting of alumina, silcica, silica-alumina, oxides of transition metals selected from Groups 3, 4, 5, 6, 7, 8, 9, 10, 11, 12 of the New Notations of the Periodic Table, oxides of rare earth metals, oxides of alkaline earth metals and mixtures thereof. | Alumina binder obtained from aluminum sulfate, the process of preparing the binder and the process of using the binder to prepare catalyst compositions are disclosed. Catalytic cracking catalyst compositions, in particularly, fluid catalytic cracking catalyst composition comprising zeolites, optionally clay and matrix materials bound by an alumina binder obtained from aluminum sulfate are disclosed.1-22. (canceled) 23. A method of forming a particulate composition of matter having a Davison Index of less than 30, said method comprising
a) forming an aqueous slurry comprising a plurality of inorganic metal oxide particles and aluminum sulfate in an amount sufficient to provide at least 5 wt % alumina in a final particulate inorganic metal oxide composition; b) optionally, milling the slurry; c) spray drying the slurry to form inorganic metal oxide particles bound by aluminum sulfate; d) optionally, calcining the aluminum sulfate bound metal oxide particles; e) re-slurrying the aluminum sulfate bound inorganic metal oxide particles in an aqueous base solution at a pH of about 7 to about 13 for a time and at a temperature sufficient to remove all or substantially all sulfate ions; and; f) recovering and drying the resulting inorganic metal oxide composition to obtain a final inorganic metal oxide composition bound with alumina obtained from aluminum sulfate. 24. The method of claim 23 wherein aluminum sulfate is present in the slurry in an amount sufficient to provide about 5 to about 25 wt % of the alumina in the final inorganic metal oxide composition. 25. The method of claim 23 wherein the aluminum sulfate bound particles are calcined at temperatures ranging from about 150° C. to about 600° C. for about 2 hours to about 10 minutes. 26. The method of claim 23 wherein the temperature during the re-slurry step ranges from about 1° C. to about 100° C. for about 1 minute to about 3 hours. 27. A method of forming a catalytic cracking catalyst composition having a Davison Index of less than 30, said method comprising
a) forming an aqueous slurry comprising at least one zeolite particle having catalytic cracking activity under catalytic cracking conditions and aluminum sulfate in an amount sufficient to provide at least 5 wt % alumina in a final catalyst composition; b) milling the slurry; c) spray drying the milled slurry to form particles; d) calcining the spray-dried particles at a temperature and for a time sufficient to remove volatiles; e) re-slurrying the calcined particles in an aqueous base solution at a pH of about 7 to about 13 for a time and at a temperature sufficient to remove all or substantially all sulfate ions; and f) recovering and drying the resulting particles to obtain a final catalyst composition comprising at least 5 wt % alumina obtained from aluminum sulfate. 28. The method of claim 27 wherein aluminum sulfate is present in the slurry in an amount significant to provide about 5 to about 25 wt % alumina obtained from aluminum sulfate in the final catalyst composition. 29. The method of claim 27 wherein the spray-dried particles are calcined at temperatures ranging from about 150° C. to about 600° C. for about 2 hours to about 10 minutes. 30. The method of claim 27 wherein the temperature during the re-slurry step ranges from about 1° C. to about 100° C. for about 1 minute to about 3 hours. 31. The method of claim 27 wherein the at least one zeolite comprise faujasite zeolite. 32. The method of claim 31 wherein the faujasite zeolite is selected from the group consisting of Y-type zeolite, USY zeolite, REUSY zeolite, or a mixture thereof. 33. The method of claim 32 wherein the zeolite is partially exchanged with ions selected from the group consisting of rare earth metals ions, alkaline earth metal ions, ammonium ions, acid ions and mixtures thereof. 34. The method of claim 27 wherein the slurry further comprises clay. 35. The method of claim 27 wherein the slurry further comprises at least one matrix material selected from the group consisting of alumina, silcica, silica-alumina, oxides of transition metals selected from Groups 3, 4, 5, 6, 7, 8, 9, 10, 11, 12 of the New Notations of the Periodic Table, oxides of rare earth metals, oxides of alkaline earth metals and mixtures thereof. 36-38. (canceled) 39. The method of claim 34 wherein the slurry further comprises at least one matrix material selected from the group consisting of alumina, silcica, silica-alumina, oxides of transition metals selected from Groups 3, 4, 5, 6, 7, 8, 9, 10, 11, 12 of the New Notations of the Periodic Table, oxides of rare earth metals, oxides of alkaline earth metals and mixtures thereof. | 1,700 |
3,468 | 14,596,092 | 1,768 | Compositions for treating high-molecular-weight components of a petroleum fluid are generally disclosed. In some embodiments, such compositions include olefinic ester compounds, such as alkyl esters of C 10-18 unsaturated fatty acids. In some embodiments, such compositions are added to a petroleum fluid to improve the rheological properties, e.g., breaking up or inhibiting the precipitation of high-molecular-weight components of petroleum fluids. In some other embodiments, such compositions are used for removing deposits of such high-molecular-weight components from the surfaces of equipment used for extracting or transporting petroleum or natural gas. | 1. A composition for dissolving petroleum wax or asphaltenes, the composition comprising olefinic ester compounds, wherein the olefinic ester compounds are C1-6 alkanol esters of C10-18 carboxylic acids having one or more carbon-carbon double bonds. 2. The composition of claim 1, wherein the olefinic ester compounds make up at least 50 percent by weight, or at least 60 percent by weight, or at least 70 percent by weight, or at least 80 percent by weight, or at least 90 percent by weight, or at least 95 percent by weight of the composition, based on the total weight of the composition. 3-5. (canceled) 6. The composition of claim 2, further comprising a surfactant. 7. (canceled) 8. (canceled) 9. The composition of claim 6, wherein the surfactant is a non-ionic surfactant. 10. The composition of claim 9, wherein the non-ionic surfactant comprises one or more alkoxylated fatty acids, such as non-ionic surfactants having a hydrophilic-lipophilic balance (HLB) ranging from 4 to 10, or from 5 to 9, or from 6 to 8, where HLB is determined by Griffin's Method. 11. The composition of claim 9, wherein the surfactant has a molecular weight ranging from 200 amu to 800 amu, or from 250 amu to 700 amu, or from 300 amu to 600 amu. 12-15. (canceled) 16. The composition of claim 1, wherein the composition is substantially free of water. 17-20. (canceled) 21. The composition of claim 1, wherein at least 50 percent by weight, or at least 60 percent by weight, or at least 70 percent by weight, or at least 80 percent by weight of the olefinic ester compounds in the composition are methyl esters of C10-12 carboxylic acids having one carbon-carbon double bond. 22. The composition of claim 21, wherein at least 50 percent by weight, or at least 60 percent by weight, or at least 70 percent by weight, or at least 80 percent by weight of the olefinic ester compounds in the composition are methyl esters of 9-decenoic acid, 9-undecenoid acid, or 9-dodecenoic acid. 23. The composition of claim 22, wherein at least 50 percent by weight, or at least 60 percent by weight, or at least 70 percent by weight, or at least 80 percent by weight of the olefinic ester compounds in the composition are methyl 9-dodecenoate. 24. (canceled) 25. (canceled) 26. The composition of claim 1, wherein the olefinic ester compounds are compounds of formula (I):
wherein:
R1 is C9-17 alkenyl; and
R2 is C1-6 alkyl. 27. The composition of claim 26, wherein R1 is C9-11 alkenyl. 28-30. (canceled) 31. The composition of claim 26, wherein R1 is —(CH2)7—CH═CH—CH2—CH3. 32. (canceled) 33. (canceled) 34. The composition of claim 26, wherein R2 is methyl. 35-37. (canceled) 38. The composition of claim 1, wherein the composition is a cleaning composition, useful for cleaning petroleum wax or asphaltene deposits. 39. The composition of claim 1, wherein the composition is a petroleum additive composition. 40. A petroleum composition comprising:
a petroleum fluid; and a petroleum additive composition of claim 39. 41-51. (canceled) 52. A method of reducing agglomerates in a petroleum fluid, comprising:
providing a petroleum fluid comprising one or more agglomerating materials, the agglomerating materials comprising asphaltenes, petroleum waxes, or a combination thereof; and introducing to the petroleum fluid the petroleum additive composition of claim 39 to form a treated petroleum fluid. 53. The method of claim 52, wherein the introducing comprises adding the petroleum additive composition to the petroleum fluid in an amount such that the petroleum additive composition makes up no more than 5 percent by weight, or no more than 3 percent by weight, or no more than 2 percent by weight, or no more than 1 percent by weight, of the treated petroleum composition, based on the total weight of the treated petroleum composition. 54-56. (canceled) 57. The method of claim 52, wherein the one or more agglomerating materials comprise macrocrystalline waxes, microcrystalline waxes, or combinations thereof. 58-63. (canceled) | Compositions for treating high-molecular-weight components of a petroleum fluid are generally disclosed. In some embodiments, such compositions include olefinic ester compounds, such as alkyl esters of C 10-18 unsaturated fatty acids. In some embodiments, such compositions are added to a petroleum fluid to improve the rheological properties, e.g., breaking up or inhibiting the precipitation of high-molecular-weight components of petroleum fluids. In some other embodiments, such compositions are used for removing deposits of such high-molecular-weight components from the surfaces of equipment used for extracting or transporting petroleum or natural gas.1. A composition for dissolving petroleum wax or asphaltenes, the composition comprising olefinic ester compounds, wherein the olefinic ester compounds are C1-6 alkanol esters of C10-18 carboxylic acids having one or more carbon-carbon double bonds. 2. The composition of claim 1, wherein the olefinic ester compounds make up at least 50 percent by weight, or at least 60 percent by weight, or at least 70 percent by weight, or at least 80 percent by weight, or at least 90 percent by weight, or at least 95 percent by weight of the composition, based on the total weight of the composition. 3-5. (canceled) 6. The composition of claim 2, further comprising a surfactant. 7. (canceled) 8. (canceled) 9. The composition of claim 6, wherein the surfactant is a non-ionic surfactant. 10. The composition of claim 9, wherein the non-ionic surfactant comprises one or more alkoxylated fatty acids, such as non-ionic surfactants having a hydrophilic-lipophilic balance (HLB) ranging from 4 to 10, or from 5 to 9, or from 6 to 8, where HLB is determined by Griffin's Method. 11. The composition of claim 9, wherein the surfactant has a molecular weight ranging from 200 amu to 800 amu, or from 250 amu to 700 amu, or from 300 amu to 600 amu. 12-15. (canceled) 16. The composition of claim 1, wherein the composition is substantially free of water. 17-20. (canceled) 21. The composition of claim 1, wherein at least 50 percent by weight, or at least 60 percent by weight, or at least 70 percent by weight, or at least 80 percent by weight of the olefinic ester compounds in the composition are methyl esters of C10-12 carboxylic acids having one carbon-carbon double bond. 22. The composition of claim 21, wherein at least 50 percent by weight, or at least 60 percent by weight, or at least 70 percent by weight, or at least 80 percent by weight of the olefinic ester compounds in the composition are methyl esters of 9-decenoic acid, 9-undecenoid acid, or 9-dodecenoic acid. 23. The composition of claim 22, wherein at least 50 percent by weight, or at least 60 percent by weight, or at least 70 percent by weight, or at least 80 percent by weight of the olefinic ester compounds in the composition are methyl 9-dodecenoate. 24. (canceled) 25. (canceled) 26. The composition of claim 1, wherein the olefinic ester compounds are compounds of formula (I):
wherein:
R1 is C9-17 alkenyl; and
R2 is C1-6 alkyl. 27. The composition of claim 26, wherein R1 is C9-11 alkenyl. 28-30. (canceled) 31. The composition of claim 26, wherein R1 is —(CH2)7—CH═CH—CH2—CH3. 32. (canceled) 33. (canceled) 34. The composition of claim 26, wherein R2 is methyl. 35-37. (canceled) 38. The composition of claim 1, wherein the composition is a cleaning composition, useful for cleaning petroleum wax or asphaltene deposits. 39. The composition of claim 1, wherein the composition is a petroleum additive composition. 40. A petroleum composition comprising:
a petroleum fluid; and a petroleum additive composition of claim 39. 41-51. (canceled) 52. A method of reducing agglomerates in a petroleum fluid, comprising:
providing a petroleum fluid comprising one or more agglomerating materials, the agglomerating materials comprising asphaltenes, petroleum waxes, or a combination thereof; and introducing to the petroleum fluid the petroleum additive composition of claim 39 to form a treated petroleum fluid. 53. The method of claim 52, wherein the introducing comprises adding the petroleum additive composition to the petroleum fluid in an amount such that the petroleum additive composition makes up no more than 5 percent by weight, or no more than 3 percent by weight, or no more than 2 percent by weight, or no more than 1 percent by weight, of the treated petroleum composition, based on the total weight of the treated petroleum composition. 54-56. (canceled) 57. The method of claim 52, wherein the one or more agglomerating materials comprise macrocrystalline waxes, microcrystalline waxes, or combinations thereof. 58-63. (canceled) | 1,700 |
3,469 | 14,701,857 | 1,726 | A microstructured ZnO coating that improves the performance of Cu(In,Ga)Se 2 (CIGS) photovoltaic (PV) devices via two mechanisms; it acts an antireflective layer with superior non-normal performance to thin film anti-reflective (AR) coatings, and it scatters a large fraction of incoming light at a large angle, resulting in absorption that is on average closer to the p-n junction. | 1. A photovoltaic device, comprising:
a thin film of copper indium gallium selenide (CIGS) on a substrate; a layer of CdS on the CIGS; a layer of ZnO on the CdS; a layer of aluminum-doped ZnO (AZO) on the ZnO; and a microstructured ZnO coating on the AZO, wherein the microstructured ZnO coating forms antireflective surface structures on the AZO layer. 2. The photovoltaic device of claim 1, wherein the substrate comprises glass with a Mo bottom contact. 3. A photovoltaic device, made by the method comprising:
coating a substrate with a thin film of copper indium gallium selenide (CIGS); depositing a layer of CdS on the CIGS; depositing a layer of ZnO on the CdS; depositing a layer of aluminum-doped ZnO (AZO) on the ZnO; and depositing a top layer of ZnO on the AZO and etching the top ZnO layer to form a textured ZnO top layer, wherein the textured ZnO top layer forms antireflective surface structures on the AZO layer. 4. The photovoltaic device of claim 3, wherein the substrate comprises glass with a Mo bottom contact. 5. The photovoltaic device of claim 3, wherein the thin film of CIGS is about 2 μm. 6. The photovoltaic device of claim 3, wherein the CdS layer is about 50 nm. 7. The photovoltaic device of claim 3, wherein the ZnO layer on the CdS is about 60 nm. 8. The photovoltaic device of claim 3, wherein the AZO layer is about 200 nm. 9. The photovoltaic device of claim 3, wherein the ZnO layer, the AZO layer, and the ZnO top layer are deposited at a substrate temperature of 200° C. 10. The photovoltaic device of claim 3, wherein the top ZnO layer is etched for up to 30 seconds. 11. A method of making a photovoltaic device, comprising:
coating a substrate with a thin film of copper indium gallium selenide (CIGS); depositing a layer of CdS on the CIGS; depositing a layer of ZnO on the CdS; depositing a layer of aluminum-doped ZnO (AZO) on the ZnO; and depositing a top layer of ZnO on the AZO and etching the top ZnO layer to form a textured ZnO top layer, wherein the textured ZnO top layer forms antireflective surface structures on the AZO layer. 12. The method of claim 11, wherein the substrate comprises glass with a Mo bottom contact. 13. The method of claim 11, wherein the thin film of CIGS is about 2 μm. 14. The method of claim 11, wherein the CdS layer is about 50 nm. 15. The method of claim 11, wherein the ZnO layer on the CdS is about 60 nm. 16. The method of claim 11, wherein the AZO layer is about 200 nm. 17. The method of claim 11, wherein the ZnO layer, the AZO layer, and the ZnO top layer are deposited at a substrate temperature of 200° C. 18. The method of claim 11, wherein the top ZnO layer is etched for up to 30 seconds. | A microstructured ZnO coating that improves the performance of Cu(In,Ga)Se 2 (CIGS) photovoltaic (PV) devices via two mechanisms; it acts an antireflective layer with superior non-normal performance to thin film anti-reflective (AR) coatings, and it scatters a large fraction of incoming light at a large angle, resulting in absorption that is on average closer to the p-n junction.1. A photovoltaic device, comprising:
a thin film of copper indium gallium selenide (CIGS) on a substrate; a layer of CdS on the CIGS; a layer of ZnO on the CdS; a layer of aluminum-doped ZnO (AZO) on the ZnO; and a microstructured ZnO coating on the AZO, wherein the microstructured ZnO coating forms antireflective surface structures on the AZO layer. 2. The photovoltaic device of claim 1, wherein the substrate comprises glass with a Mo bottom contact. 3. A photovoltaic device, made by the method comprising:
coating a substrate with a thin film of copper indium gallium selenide (CIGS); depositing a layer of CdS on the CIGS; depositing a layer of ZnO on the CdS; depositing a layer of aluminum-doped ZnO (AZO) on the ZnO; and depositing a top layer of ZnO on the AZO and etching the top ZnO layer to form a textured ZnO top layer, wherein the textured ZnO top layer forms antireflective surface structures on the AZO layer. 4. The photovoltaic device of claim 3, wherein the substrate comprises glass with a Mo bottom contact. 5. The photovoltaic device of claim 3, wherein the thin film of CIGS is about 2 μm. 6. The photovoltaic device of claim 3, wherein the CdS layer is about 50 nm. 7. The photovoltaic device of claim 3, wherein the ZnO layer on the CdS is about 60 nm. 8. The photovoltaic device of claim 3, wherein the AZO layer is about 200 nm. 9. The photovoltaic device of claim 3, wherein the ZnO layer, the AZO layer, and the ZnO top layer are deposited at a substrate temperature of 200° C. 10. The photovoltaic device of claim 3, wherein the top ZnO layer is etched for up to 30 seconds. 11. A method of making a photovoltaic device, comprising:
coating a substrate with a thin film of copper indium gallium selenide (CIGS); depositing a layer of CdS on the CIGS; depositing a layer of ZnO on the CdS; depositing a layer of aluminum-doped ZnO (AZO) on the ZnO; and depositing a top layer of ZnO on the AZO and etching the top ZnO layer to form a textured ZnO top layer, wherein the textured ZnO top layer forms antireflective surface structures on the AZO layer. 12. The method of claim 11, wherein the substrate comprises glass with a Mo bottom contact. 13. The method of claim 11, wherein the thin film of CIGS is about 2 μm. 14. The method of claim 11, wherein the CdS layer is about 50 nm. 15. The method of claim 11, wherein the ZnO layer on the CdS is about 60 nm. 16. The method of claim 11, wherein the AZO layer is about 200 nm. 17. The method of claim 11, wherein the ZnO layer, the AZO layer, and the ZnO top layer are deposited at a substrate temperature of 200° C. 18. The method of claim 11, wherein the top ZnO layer is etched for up to 30 seconds. | 1,700 |
3,470 | 12,859,976 | 1,727 | Methods and systems provide for the creation of power, water, and heat utilizing a fuel cell. According to embodiments described herein, fuel is provided to a fuel cell for the creation of power and a fuel byproduct. The fuel byproduct is routed to a byproduct separation phase of a power and water generation system, where water is separated from the fuel byproduct. The remaining mixture is reacted in a burner phase of the system to create additional heat that may be converted to mechanical energy and/or utilized with other processes within the system or outside of the system. According to other aspects, the separated water may be utilized within a biofuel production subsystem for the creation of biofuel to be used by the fuel cell. | 1. A method for generating water and power within a fuel cell system, the method comprising:
receiving fuel; utilizing the fuel within a fuel cell to generate power and a fuel byproduct; separating water from the fuel byproduct to create a conditioned fuel byproduct and water; burning the conditioned fuel byproduct to create heat; and providing the power, the water, and the heat for use. 2. The method of claim 1, further comprising conditioning the fuel prior to utilization in the fuel cell to create conditioned fuel for the fuel cell. 3. The method of claim 2, wherein conditioning the fuel prior to utilization comprises reforming the fuel and removing sulfur from the fuel. 4. The method of claim 1, wherein the fuel cell comprises a solid oxide fuel cell (SOFC). 5. The method of claim 1, wherein separating the water from the fuel byproduct comprises routing the fuel byproduct to a separator and separating the water vapor from the fuel byproduct. 6. The method of claim 1, wherein burning the conditioned fuel byproduct comprises providing the conditioned fuel byproduct to an afterburner and combusting the conditioned fuel byproduct to create an exhaust flow. 7. The method of claim 6, further comprising routing the exhaust flow through a turbo-compressor to transform heat energy to mechanical energy. 8. The method of claim 6, further comprising routing the exhaust flow to a fuel conditioner phase of the fuel cell system and provide heat to an endothermic reformation process of the fuel conditioner phase. 9. The method of claim 1, wherein the fuel is a biofuel and wherein the method further comprises producing the biofuel in a biofuel creation subsystem. 10. The method of claim 9, wherein providing the water for use comprises providing the water to the biofuel creation subsystem for use in production of the biofuel. 11. A power and water generation system, comprising:
a fuel cell configured to convert fuel into power and a fuel byproduct; a byproduct separation phase positioned downstream of the fuel cell and configured to separate water from the fuel byproduct to create water and a conditioned fuel byproduct; and a burner phase positioned downstream of the byproduct separation phase and configured to burn the conditioned fuel byproduct to create heat. 12. The power and water generation system of claim 11, wherein the fuel cell comprises a SOFC. 13. The power and water generation system of claim 11, wherein the byproduct separation phase comprises a separator configured to separate water from the fuel byproduct to create the water. 14. The power and water generation system of claim 13, wherein the byproduct separation phase further comprises water processing equipment configured to produce potable water from the water. 15. The power and water generation system of claim 11, wherein the burner phase comprises an afterburner configured to combust the conditioned fuel byproduct with air to create an exhaust flow comprising the heat. 16. The power and water generation system of claim 15, wherein the burner phase comprises a turbo-compressor configured to transform the exhaust flow to mechanical energy. 17. The power and water generation system of claim 15, wherein the burner phase is thermally coupled to a fuel conditioner phase comprising a reformer configured to condition the fuel for the fuel cell. 18. The power and water generation system of claim 11, wherein the fuel is a biofuel and wherein the power and water generation system further comprises a biofuel production subsystem configured to receive the water and to create the biofuel for use by the fuel cell. 19. A power and water generation system, comprising:
a biofuel production subsystem configured to receive water and biofuel ingredients and to create a biofuel; a fuel conditioner phase configured to receive the biofuel and create conditioned fuel; a fuel cell positioned downstream from the fuel conditioner phase and configured to convert the conditioned fuel into power and a fuel byproduct; a byproduct separation phase positioned downstream of the fuel cell and configured to separate water from the fuel byproduct to create the water and a conditioned fuel byproduct and to provide the water to the biofuel production subsystem; and a burner phase positioned downstream of the byproduct separation phase and configured to react the conditioned fuel byproduct to create a heated exhaust stream. 20. The power and water generation system of claim 19, wherein the fuel cell comprises a SOFC, wherein the burner phase comprises a turbo-compressor configured to transform the heat to mechanical energy, and wherein the burner phase is thermally coupled to the fuel conditioner phase to provide heat to the fuel conditioner phase during creation of the conditioned fuel. | Methods and systems provide for the creation of power, water, and heat utilizing a fuel cell. According to embodiments described herein, fuel is provided to a fuel cell for the creation of power and a fuel byproduct. The fuel byproduct is routed to a byproduct separation phase of a power and water generation system, where water is separated from the fuel byproduct. The remaining mixture is reacted in a burner phase of the system to create additional heat that may be converted to mechanical energy and/or utilized with other processes within the system or outside of the system. According to other aspects, the separated water may be utilized within a biofuel production subsystem for the creation of biofuel to be used by the fuel cell.1. A method for generating water and power within a fuel cell system, the method comprising:
receiving fuel; utilizing the fuel within a fuel cell to generate power and a fuel byproduct; separating water from the fuel byproduct to create a conditioned fuel byproduct and water; burning the conditioned fuel byproduct to create heat; and providing the power, the water, and the heat for use. 2. The method of claim 1, further comprising conditioning the fuel prior to utilization in the fuel cell to create conditioned fuel for the fuel cell. 3. The method of claim 2, wherein conditioning the fuel prior to utilization comprises reforming the fuel and removing sulfur from the fuel. 4. The method of claim 1, wherein the fuel cell comprises a solid oxide fuel cell (SOFC). 5. The method of claim 1, wherein separating the water from the fuel byproduct comprises routing the fuel byproduct to a separator and separating the water vapor from the fuel byproduct. 6. The method of claim 1, wherein burning the conditioned fuel byproduct comprises providing the conditioned fuel byproduct to an afterburner and combusting the conditioned fuel byproduct to create an exhaust flow. 7. The method of claim 6, further comprising routing the exhaust flow through a turbo-compressor to transform heat energy to mechanical energy. 8. The method of claim 6, further comprising routing the exhaust flow to a fuel conditioner phase of the fuel cell system and provide heat to an endothermic reformation process of the fuel conditioner phase. 9. The method of claim 1, wherein the fuel is a biofuel and wherein the method further comprises producing the biofuel in a biofuel creation subsystem. 10. The method of claim 9, wherein providing the water for use comprises providing the water to the biofuel creation subsystem for use in production of the biofuel. 11. A power and water generation system, comprising:
a fuel cell configured to convert fuel into power and a fuel byproduct; a byproduct separation phase positioned downstream of the fuel cell and configured to separate water from the fuel byproduct to create water and a conditioned fuel byproduct; and a burner phase positioned downstream of the byproduct separation phase and configured to burn the conditioned fuel byproduct to create heat. 12. The power and water generation system of claim 11, wherein the fuel cell comprises a SOFC. 13. The power and water generation system of claim 11, wherein the byproduct separation phase comprises a separator configured to separate water from the fuel byproduct to create the water. 14. The power and water generation system of claim 13, wherein the byproduct separation phase further comprises water processing equipment configured to produce potable water from the water. 15. The power and water generation system of claim 11, wherein the burner phase comprises an afterburner configured to combust the conditioned fuel byproduct with air to create an exhaust flow comprising the heat. 16. The power and water generation system of claim 15, wherein the burner phase comprises a turbo-compressor configured to transform the exhaust flow to mechanical energy. 17. The power and water generation system of claim 15, wherein the burner phase is thermally coupled to a fuel conditioner phase comprising a reformer configured to condition the fuel for the fuel cell. 18. The power and water generation system of claim 11, wherein the fuel is a biofuel and wherein the power and water generation system further comprises a biofuel production subsystem configured to receive the water and to create the biofuel for use by the fuel cell. 19. A power and water generation system, comprising:
a biofuel production subsystem configured to receive water and biofuel ingredients and to create a biofuel; a fuel conditioner phase configured to receive the biofuel and create conditioned fuel; a fuel cell positioned downstream from the fuel conditioner phase and configured to convert the conditioned fuel into power and a fuel byproduct; a byproduct separation phase positioned downstream of the fuel cell and configured to separate water from the fuel byproduct to create the water and a conditioned fuel byproduct and to provide the water to the biofuel production subsystem; and a burner phase positioned downstream of the byproduct separation phase and configured to react the conditioned fuel byproduct to create a heated exhaust stream. 20. The power and water generation system of claim 19, wherein the fuel cell comprises a SOFC, wherein the burner phase comprises a turbo-compressor configured to transform the heat to mechanical energy, and wherein the burner phase is thermally coupled to the fuel conditioner phase to provide heat to the fuel conditioner phase during creation of the conditioned fuel. | 1,700 |
3,471 | 15,191,961 | 1,784 | Embodiments of alkali aluminosilicate glass articles that may be chemically strengthened to achieve a maximum surface compressive stress that exceeds compressive stresses that have been achieved in similar glasses are disclosed. In one or more embodiments, the fictive temperature of these glass articles may be equal to the 10 11 poise (P) viscosity temperature of the glass article. In some embodiments, the strengthened alkali aluminosilicate glass articles described herein may exhibit a maximum compressive stress of at least about 400 MPa, 800 MPa, 930 MPa or 1050 MPa. In some embodiments, the strengthened alkali aluminosilicate glass articles described herein may exhibit a compressive stress layer extending to a depth of layer of at least about 40 μm (in samples having a thickness of 1 mm). In still other embodiments, these strengthened alkali aluminosilicate glass articles exhibit a parabolic or near-parabolic tensile stress profile in the central region of the glass articles. | 1. An alkali aluminosilicate glass article comprising: a compressive stress layer extending from a surface of the alkali aluminosilicate glass to a depth of layer (DOL), the compressive stress layer having a maximum compressive stress of at least 400 MPa at the surface, wherein the alkali aluminosilicate glass article comprises at least about 58 mol % SiO2, from about 0.5 mol % to about 3 mol % P2O5, at least about 11 mol % Al2O3, Na2O and Li2O, wherein the ratio of the amount of Li2O (mol %) to Na2O (mol %) (Li2O/Na2O) is less than 1.0, and wherein the alkali aluminosilicate glass article is free of B2O3. 2. The alkali aluminosilicate glass article of claim 1, wherein the alkali aluminosilicate glass article comprises a fictive temperature Tf that is equal to a temperature at which the alkali aluminosilicate glass article has a viscosity of 1011 Poise. 3. The alkali aluminosilicate glass article of claim 1, wherein the alkali aluminosilicate glass article comprises a zircon breakdown temperature of less than about 35 kPoise. 4. The alkali aluminosilicate glass article of claim 1, wherein the alkali aluminosilicate glass article comprises a liquidus viscosity of at least 200 kPoise. 5. The alkali aluminosilicate glass article of claim 1, wherein the alkali aluminosilicate glass article comprises a ratio R2O (mol %)/Al2O3 (mol %) that is less than 2, where R2O=Li2O+Na2O. 6. The alkali aluminosilicate glass article of claim 1, wherein the alkali aluminosilicate glass article comprises a total amount of SiO2 and P2O5 that is greater than 65 mol % and less than 67 mol % (65 mol %<SiO2 (mol %)+P2O5 (mol %)<67 mol %). 7. The alkali aluminosilicate glass article of claim 1, wherein the alkali aluminosilicate glass article comprises a relationship R2O (mol %)+R′O (mol %)−Al2O3 (mol %)+P2O5 (mol %) that is greater than about −3 mol %, wherein R2O=the total amount of Li2O and Na2O present in the alkali aluminosilicate glass article and R′O is a total amount of divalent metal oxides present in the alkali aluminosilicate glass article. 8. The alkali aluminosilicate glass article of claim 1, wherein the alkali aluminosilicate glass article comprises from about 58 mol % to about 65 mol % SiO2; from about 11 mol % to about 20 mol % Al2O3; from about 6 mol % to about 18 mol % Na2O; from 0 mol % to about 6 mol % MgO; and from 0 mol % to about 6 mol % ZnO. 9. The alkali aluminosilicate glass article of claim 1, wherein the alkali aluminosilicate glass article comprises P2O5 in an amount in a range from about 0.5 mol % to about 2.8 mol %. 10. The alkali aluminosilicate glass article of claim 1, wherein the alkali aluminosilicate glass article comprises Li2O in an amount up to about 10 mol %. 11. The alkali aluminosilicate glass article of claim 1, further comprising a thickness in a range from about 0.05 mm to about 1.5 mm. 12. The alkali aluminosilicate glass article of claim 1, further comprising a thickness of at least 1 mm, wherein the maximum compressive stress is at least about 1050 MPa at the surface. 13. The alkali aluminosilicate glass article of claim 1, further comprising a thickness of at least 1 mm, wherein the maximum compressive stress is at least about 930 MPa at the surface. 14. The alkali aluminosilicate glass article of claim 1, wherein the glass is chemically strengthened. 15. The alkali aluminosilicate glass article of claim 1, further comprising a thickness and a central region extending from the DOL to a depth equal to 0.5 times the thickness, and wherein the central region is free of K2O. 16. A consumer electronic device comprising: a housing; electrical components provided at least partially internal to the housing, the electrical components including at least a controller, a memory, and a display, the display being provided at or adjacent to a front surface of the housing; and a cover article disposed at or over the front surface of the housing and over the display, wherein the cover article comprises the alkali aluminosilicate glass article of claim 1. 17. An alkali aluminosilicate glass article comprising: a thickness t, a compressive stress layer extending from a surface of the alkali aluminosilicate glass to a depth of layer (DOL), and a central region comprising a maximum tensile stress,
wherein the central region extends from the DOL, and wherein the alkali aluminosilicate glass is free of B2O3 and comprises at least about 58 mol % SiO2, from about 0.5 mol % to about 3 mol % P2O5, at least about 11 mol % Al2O3, Na2O and, Li2O, wherein the ratio of the amount of Li2O (mol %) to Na2O (mol %) (Li2O/Na2O) is less than 1.0, wherein the DOL is less than or equal to 0.25*t, and wherein the maximum tensile stress is about 35 MPa or greater. 18. The alkali aluminosilicate glass article of claim 17, wherein the alkali aluminosilicate glass article comprises a fictive temperature Tf that is equal to a temperature at which the alkali aluminosilicate glass article has a viscosity of 1011 Poise. 19. The alkali aluminosilicate glass of claim 17, wherein the alkali aluminosilicate glass article comprises a zircon breakdown temperature of less than about 35 kPoise. 20. The alkali aluminosilicate glass of claim 17, wherein the alkali aluminosilicate glass article comprises a liquidus viscosity of at least 200 kPoise. 21. The alkali aluminosilicate glass of claim 17, wherein the alkali aluminosilicate glass article comprises a ratio R2O (mol %)/Al2O3 (mol %) that is less than 2, where R2O=Li2O+Na2O. 22. The alkali aluminosilicate glass claim 17, wherein the alkali aluminosilicate glass article comprises a total amount of SiO2 and P2O5 that is greater than 65 mol % and less than 67 mol % (65 mol %<SiO2 (mol %)+P2O5 (mol %)<67 mol %). 23. The alkali aluminosilicate glass of claim 17, wherein the alkali aluminosilicate glass article comprises a relationship R2O (mol %)+R′O (mol %)−Al2O3 (mol %)+P2O5 (mol %) that is greater than about −3 mol %, wherein R2O=the total amount of Li2O and Na2O present in the alkali aluminosilicate glass article and R′O is a total amount of divalent metal oxides present in the alkali aluminosilicate glass article. 24. The alkali aluminosilicate glass of claim 17, wherein the alkali aluminosilicate glass article comprises from about 58 mol % to about 65 mol % SiO2; from about 11 mol % to about 20 mol % Al2O3; from about 6 mol % to about 18 mol % Na2O; from 0 mol % to about 6 mol % MgO; and from 0 mol % to about 6 mol % ZnO. 25. A device comprising:
a housing having front, back, and side surfaces; electrical components that are at least partially inside the housing; a display at or adjacent to the front surface of the housing; and a strengthened alkali aluminosilicate glass article disposed over the display, wherein the strengthened alkali aluminosilicate glass article comprises a compressive stress layer extending from a surface of the alkali aluminosilicate glass article to a depth of layer (DOL), the compressive layer having a maximum compressive stress of at least 400 MPa at the surface, wherein the alkali aluminosilicate article comprises at least about 58 mol % SiO2, from about 0.5 mol % to about 3 mol % P2O5, at least about 11 mol % Al2O3, Na2O and Li2O, wherein the ratio of the amount of Li2O (mol %) to Na2O (mol %) (Li2O/Na2O) is less than 1.0, and wherein the alkali aluminosilicate glass article is free of B2O3. 26. The device of claim 25, wherein the device comprises a mobile electronic communication and entertainment device selected from the group consisting of a mobile phone, a smart phone, a tablet, a video player, an information terminal (IT) device, a music player, and a laptop computer. 27. An alkali aluminosilicate glass article comprising: at least about 58 mol % SiO2, from about 0.5 mol % to about 3 mol % P2O5, at least about 11 mol % Al2O3, Na2O and Li2O, wherein the alkali aluminosilicate glass article is free of B2O3 and K2O, and wherein the ratio of the amount of Li2O (mol %) to Na2O (mol %) (Li2O/Na2O) is less than 1.0. 28. The alkali aluminosilicate glass article of claim 27, wherein the alkali aluminosilicate glass article comprises P2O5 in an amount in a range from about 0.5 mol % to about 2.8 mol %. 29. The alkali aluminosilicate glass article of claim 27, wherein the alkali aluminosilicate glass article comprises Li2O in an amount up to about 10 mol % Li2O. 30. The alkali aluminosilicate glass article or claim 27, wherein the alkali aluminosilicate glass article comprises any one of
a ratio R2O (mol %)/Al2O3 (mol %) that is less than 2, where R2O=Li2O+Na2O; a total amount of SiO2 and P2O5 that is greater than 65 mol % and less than 67 mol % (65 mol %<SiO2 (mol %)+P2O5 (mol %)<67 mol %); and a relationship R2O (mol %)+R′O (mol %)−Al2O3 (mol %)+P2O5 (mol %) that is greater than about −3 mol %, wherein R2O=the total amount of Li2O and Na2O present in the alkali aluminosilicate glass article and R′O is a total amount of divalent metal oxides present in the alkali aluminosilicate glass article. | Embodiments of alkali aluminosilicate glass articles that may be chemically strengthened to achieve a maximum surface compressive stress that exceeds compressive stresses that have been achieved in similar glasses are disclosed. In one or more embodiments, the fictive temperature of these glass articles may be equal to the 10 11 poise (P) viscosity temperature of the glass article. In some embodiments, the strengthened alkali aluminosilicate glass articles described herein may exhibit a maximum compressive stress of at least about 400 MPa, 800 MPa, 930 MPa or 1050 MPa. In some embodiments, the strengthened alkali aluminosilicate glass articles described herein may exhibit a compressive stress layer extending to a depth of layer of at least about 40 μm (in samples having a thickness of 1 mm). In still other embodiments, these strengthened alkali aluminosilicate glass articles exhibit a parabolic or near-parabolic tensile stress profile in the central region of the glass articles.1. An alkali aluminosilicate glass article comprising: a compressive stress layer extending from a surface of the alkali aluminosilicate glass to a depth of layer (DOL), the compressive stress layer having a maximum compressive stress of at least 400 MPa at the surface, wherein the alkali aluminosilicate glass article comprises at least about 58 mol % SiO2, from about 0.5 mol % to about 3 mol % P2O5, at least about 11 mol % Al2O3, Na2O and Li2O, wherein the ratio of the amount of Li2O (mol %) to Na2O (mol %) (Li2O/Na2O) is less than 1.0, and wherein the alkali aluminosilicate glass article is free of B2O3. 2. The alkali aluminosilicate glass article of claim 1, wherein the alkali aluminosilicate glass article comprises a fictive temperature Tf that is equal to a temperature at which the alkali aluminosilicate glass article has a viscosity of 1011 Poise. 3. The alkali aluminosilicate glass article of claim 1, wherein the alkali aluminosilicate glass article comprises a zircon breakdown temperature of less than about 35 kPoise. 4. The alkali aluminosilicate glass article of claim 1, wherein the alkali aluminosilicate glass article comprises a liquidus viscosity of at least 200 kPoise. 5. The alkali aluminosilicate glass article of claim 1, wherein the alkali aluminosilicate glass article comprises a ratio R2O (mol %)/Al2O3 (mol %) that is less than 2, where R2O=Li2O+Na2O. 6. The alkali aluminosilicate glass article of claim 1, wherein the alkali aluminosilicate glass article comprises a total amount of SiO2 and P2O5 that is greater than 65 mol % and less than 67 mol % (65 mol %<SiO2 (mol %)+P2O5 (mol %)<67 mol %). 7. The alkali aluminosilicate glass article of claim 1, wherein the alkali aluminosilicate glass article comprises a relationship R2O (mol %)+R′O (mol %)−Al2O3 (mol %)+P2O5 (mol %) that is greater than about −3 mol %, wherein R2O=the total amount of Li2O and Na2O present in the alkali aluminosilicate glass article and R′O is a total amount of divalent metal oxides present in the alkali aluminosilicate glass article. 8. The alkali aluminosilicate glass article of claim 1, wherein the alkali aluminosilicate glass article comprises from about 58 mol % to about 65 mol % SiO2; from about 11 mol % to about 20 mol % Al2O3; from about 6 mol % to about 18 mol % Na2O; from 0 mol % to about 6 mol % MgO; and from 0 mol % to about 6 mol % ZnO. 9. The alkali aluminosilicate glass article of claim 1, wherein the alkali aluminosilicate glass article comprises P2O5 in an amount in a range from about 0.5 mol % to about 2.8 mol %. 10. The alkali aluminosilicate glass article of claim 1, wherein the alkali aluminosilicate glass article comprises Li2O in an amount up to about 10 mol %. 11. The alkali aluminosilicate glass article of claim 1, further comprising a thickness in a range from about 0.05 mm to about 1.5 mm. 12. The alkali aluminosilicate glass article of claim 1, further comprising a thickness of at least 1 mm, wherein the maximum compressive stress is at least about 1050 MPa at the surface. 13. The alkali aluminosilicate glass article of claim 1, further comprising a thickness of at least 1 mm, wherein the maximum compressive stress is at least about 930 MPa at the surface. 14. The alkali aluminosilicate glass article of claim 1, wherein the glass is chemically strengthened. 15. The alkali aluminosilicate glass article of claim 1, further comprising a thickness and a central region extending from the DOL to a depth equal to 0.5 times the thickness, and wherein the central region is free of K2O. 16. A consumer electronic device comprising: a housing; electrical components provided at least partially internal to the housing, the electrical components including at least a controller, a memory, and a display, the display being provided at or adjacent to a front surface of the housing; and a cover article disposed at or over the front surface of the housing and over the display, wherein the cover article comprises the alkali aluminosilicate glass article of claim 1. 17. An alkali aluminosilicate glass article comprising: a thickness t, a compressive stress layer extending from a surface of the alkali aluminosilicate glass to a depth of layer (DOL), and a central region comprising a maximum tensile stress,
wherein the central region extends from the DOL, and wherein the alkali aluminosilicate glass is free of B2O3 and comprises at least about 58 mol % SiO2, from about 0.5 mol % to about 3 mol % P2O5, at least about 11 mol % Al2O3, Na2O and, Li2O, wherein the ratio of the amount of Li2O (mol %) to Na2O (mol %) (Li2O/Na2O) is less than 1.0, wherein the DOL is less than or equal to 0.25*t, and wherein the maximum tensile stress is about 35 MPa or greater. 18. The alkali aluminosilicate glass article of claim 17, wherein the alkali aluminosilicate glass article comprises a fictive temperature Tf that is equal to a temperature at which the alkali aluminosilicate glass article has a viscosity of 1011 Poise. 19. The alkali aluminosilicate glass of claim 17, wherein the alkali aluminosilicate glass article comprises a zircon breakdown temperature of less than about 35 kPoise. 20. The alkali aluminosilicate glass of claim 17, wherein the alkali aluminosilicate glass article comprises a liquidus viscosity of at least 200 kPoise. 21. The alkali aluminosilicate glass of claim 17, wherein the alkali aluminosilicate glass article comprises a ratio R2O (mol %)/Al2O3 (mol %) that is less than 2, where R2O=Li2O+Na2O. 22. The alkali aluminosilicate glass claim 17, wherein the alkali aluminosilicate glass article comprises a total amount of SiO2 and P2O5 that is greater than 65 mol % and less than 67 mol % (65 mol %<SiO2 (mol %)+P2O5 (mol %)<67 mol %). 23. The alkali aluminosilicate glass of claim 17, wherein the alkali aluminosilicate glass article comprises a relationship R2O (mol %)+R′O (mol %)−Al2O3 (mol %)+P2O5 (mol %) that is greater than about −3 mol %, wherein R2O=the total amount of Li2O and Na2O present in the alkali aluminosilicate glass article and R′O is a total amount of divalent metal oxides present in the alkali aluminosilicate glass article. 24. The alkali aluminosilicate glass of claim 17, wherein the alkali aluminosilicate glass article comprises from about 58 mol % to about 65 mol % SiO2; from about 11 mol % to about 20 mol % Al2O3; from about 6 mol % to about 18 mol % Na2O; from 0 mol % to about 6 mol % MgO; and from 0 mol % to about 6 mol % ZnO. 25. A device comprising:
a housing having front, back, and side surfaces; electrical components that are at least partially inside the housing; a display at or adjacent to the front surface of the housing; and a strengthened alkali aluminosilicate glass article disposed over the display, wherein the strengthened alkali aluminosilicate glass article comprises a compressive stress layer extending from a surface of the alkali aluminosilicate glass article to a depth of layer (DOL), the compressive layer having a maximum compressive stress of at least 400 MPa at the surface, wherein the alkali aluminosilicate article comprises at least about 58 mol % SiO2, from about 0.5 mol % to about 3 mol % P2O5, at least about 11 mol % Al2O3, Na2O and Li2O, wherein the ratio of the amount of Li2O (mol %) to Na2O (mol %) (Li2O/Na2O) is less than 1.0, and wherein the alkali aluminosilicate glass article is free of B2O3. 26. The device of claim 25, wherein the device comprises a mobile electronic communication and entertainment device selected from the group consisting of a mobile phone, a smart phone, a tablet, a video player, an information terminal (IT) device, a music player, and a laptop computer. 27. An alkali aluminosilicate glass article comprising: at least about 58 mol % SiO2, from about 0.5 mol % to about 3 mol % P2O5, at least about 11 mol % Al2O3, Na2O and Li2O, wherein the alkali aluminosilicate glass article is free of B2O3 and K2O, and wherein the ratio of the amount of Li2O (mol %) to Na2O (mol %) (Li2O/Na2O) is less than 1.0. 28. The alkali aluminosilicate glass article of claim 27, wherein the alkali aluminosilicate glass article comprises P2O5 in an amount in a range from about 0.5 mol % to about 2.8 mol %. 29. The alkali aluminosilicate glass article of claim 27, wherein the alkali aluminosilicate glass article comprises Li2O in an amount up to about 10 mol % Li2O. 30. The alkali aluminosilicate glass article or claim 27, wherein the alkali aluminosilicate glass article comprises any one of
a ratio R2O (mol %)/Al2O3 (mol %) that is less than 2, where R2O=Li2O+Na2O; a total amount of SiO2 and P2O5 that is greater than 65 mol % and less than 67 mol % (65 mol %<SiO2 (mol %)+P2O5 (mol %)<67 mol %); and a relationship R2O (mol %)+R′O (mol %)−Al2O3 (mol %)+P2O5 (mol %) that is greater than about −3 mol %, wherein R2O=the total amount of Li2O and Na2O present in the alkali aluminosilicate glass article and R′O is a total amount of divalent metal oxides present in the alkali aluminosilicate glass article. | 1,700 |
3,472 | 12,734,356 | 1,791 | A process for obtaining a minimum concentration of 20.10 −6 kg/L of iso-α-acids in a liquid composition, said process being characterized by mixing in water: a natural source of α-acids; and at least one metal oxide. | 1. A process for obtaining minimum concentration of 20.10−6 kg/L of iso-α-acids in a liquid composition, said process being characterized by mixing in water:
a natural source of α-acids; and
at least one metal oxide. 2. A process according to claim 1 wherein said liquid composition is prepared in situ prior to its addition to a wort or to a fermented beverage. 3. A process according to claim 1, wherein said metal oxide is chosen in the group consisting of alkaline earth metal oxide or ferrous metal oxide. 4. A process according to claim 3, wherein said metal oxide is MgO. 5. A process according to claim 1 wherein the metal oxide is present in an amount comprised between 0.05 kg and 0.8 kg of metal oxide per kg of α-acids. 6. A process according to claim 1, characterized in that the water is heated at a temperature between 60 and 110° C. 7. A process for preparing a fermented beverage comprising the following steps:
producing a mash; filtering said mash and recovering the wort; boiling said wort; fermenting said wort to produce a fermented beverage, characterized in that, a liquid composition comprising iso-α-acids is added to said wort or to said fermented beverage and in that said liquid composition is prepared in situ prior to its addition—to the wort or fermented beverage—by mixing in water at least one metal oxide with a source of α-acids. 8. A process as identified in claim 7 wherein said liquid composition is prepared in situ prior to its addition said wort or to said fermented beverage. 9. A process according to claim 7, wherein said metal oxide is chosen in the group consisting of alkaline earth metal oxide or ferrous metal oxide. 10. A process according to claim 9, wherein said metal oxide is MgO. 11. A process for brewing a fermented beverage according to claim 7, characterized in that the final conversion yield of α-acids into iso-α-acids is at least 40%. 12. A liquid composition comprising iso-α-acids prepared by mixing in water at least one metal oxide with a natural source of α-acids, characterized in that it comprises a minimum concentration of 20.10−6 kg/L. 13. A liquid composition according to claim 12, comprising between 0.05 kg and 0.8 kg of metal oxide per kg of α-acids. 14. Apparatus for the preparation of a fermented beverage containing a mashing unit, means for separating wort there from and for boiling said wort, and a fermentation unit, characterized in that it further comprises a vessel, said vessel containing a liquid composition with a minimum concentration of 20.10−6 kg/L of iso-α-acids by mixing in water a natural source of α-acids and at least one metal oxide. 15. A process according to claim 4 wherein the metal oxide is present in an amount comprised between 0.05 kg and 0.8 kg of metal oxide per kg of α-acids. 16. A process according to claim 5 characterized in that the water is heated at a temperature between 60 and 110° C. | A process for obtaining a minimum concentration of 20.10 −6 kg/L of iso-α-acids in a liquid composition, said process being characterized by mixing in water: a natural source of α-acids; and at least one metal oxide.1. A process for obtaining minimum concentration of 20.10−6 kg/L of iso-α-acids in a liquid composition, said process being characterized by mixing in water:
a natural source of α-acids; and
at least one metal oxide. 2. A process according to claim 1 wherein said liquid composition is prepared in situ prior to its addition to a wort or to a fermented beverage. 3. A process according to claim 1, wherein said metal oxide is chosen in the group consisting of alkaline earth metal oxide or ferrous metal oxide. 4. A process according to claim 3, wherein said metal oxide is MgO. 5. A process according to claim 1 wherein the metal oxide is present in an amount comprised between 0.05 kg and 0.8 kg of metal oxide per kg of α-acids. 6. A process according to claim 1, characterized in that the water is heated at a temperature between 60 and 110° C. 7. A process for preparing a fermented beverage comprising the following steps:
producing a mash; filtering said mash and recovering the wort; boiling said wort; fermenting said wort to produce a fermented beverage, characterized in that, a liquid composition comprising iso-α-acids is added to said wort or to said fermented beverage and in that said liquid composition is prepared in situ prior to its addition—to the wort or fermented beverage—by mixing in water at least one metal oxide with a source of α-acids. 8. A process as identified in claim 7 wherein said liquid composition is prepared in situ prior to its addition said wort or to said fermented beverage. 9. A process according to claim 7, wherein said metal oxide is chosen in the group consisting of alkaline earth metal oxide or ferrous metal oxide. 10. A process according to claim 9, wherein said metal oxide is MgO. 11. A process for brewing a fermented beverage according to claim 7, characterized in that the final conversion yield of α-acids into iso-α-acids is at least 40%. 12. A liquid composition comprising iso-α-acids prepared by mixing in water at least one metal oxide with a natural source of α-acids, characterized in that it comprises a minimum concentration of 20.10−6 kg/L. 13. A liquid composition according to claim 12, comprising between 0.05 kg and 0.8 kg of metal oxide per kg of α-acids. 14. Apparatus for the preparation of a fermented beverage containing a mashing unit, means for separating wort there from and for boiling said wort, and a fermentation unit, characterized in that it further comprises a vessel, said vessel containing a liquid composition with a minimum concentration of 20.10−6 kg/L of iso-α-acids by mixing in water a natural source of α-acids and at least one metal oxide. 15. A process according to claim 4 wherein the metal oxide is present in an amount comprised between 0.05 kg and 0.8 kg of metal oxide per kg of α-acids. 16. A process according to claim 5 characterized in that the water is heated at a temperature between 60 and 110° C. | 1,700 |
3,473 | 13,723,544 | 1,796 | The present invention relates to a catalyst for the dehydrogenation of hydrocarbons which is based on iron oxide and additionally comprises at least one potassium compound, at least one cerium compound, from 0.7 to 10% by weight of at least one manganese compound, calculated as MnO 2 , and from 10 to 200 ppm of at least one titanium compound, calculated as TiO 2 , and also to a process for the production thereof. Furthermore, the present invention relates to a process for the catalytic dehydrogenation of hydrocarbons using the catalyst of the invention. | 1. A dehydrogenation catalyst comprising at least one iron compound, at least one potassium compound, at least one cerium compound, from 0.7 to 10% by weight of at least one manganese compound, calculated as MnO2, and from 10 to 200 ppm of at least one titanium compound, calculated as TiO2. 2. The dehydrogenation catalyst according to claim 1, wherein the catalyst comprises from 0.7 to 3% by weight of at least one manganese compound, calculated as MnO2. 3. The dehydrogenation catalyst according to claim 1, wherein the catalyst comprises from 30 to 150 ppm of at least one titanium compound, calculated as TiO2. 4. The dehydrogenation catalyst according to claim 1, wherein the catalyst comprises
from 50 to 90% by weight of at least one iron compound, calculated as Fe2O3; from 1 to 30% by weight of at least one potassium compound, calculated as K2O; from 0.7 to 10% by weight of at least one manganese compound, calculated as MnO2; from 10 to 200 ppm of at least one titanium compound, calculated as TiO2; from 2 to 20% by weight of at least one cerium compound, calculated as CeO2; and optionally from 0 to 30% by weight of at least one further component. 5. The dehydrogenation catalyst according to claim 1, wherein the catalyst comprises from 0.1 to 10% by weight of at least one compound selected from the group consisting of molybdenum, tungsten and vanadium, calculated as oxide in the respective highest oxidation state, as further component. 6. The dehydrogenation catalyst according to claim 1, wherein the catalyst comprises from 0.1 to 10% by weight of at least one alkaline earth metal compound, calculated as oxide, as further component. 7. The dehydrogenation catalyst according to claim 1, wherein the catalyst comprises
from 50 to 90% by weight of at least one iron compound, calculated as Fe2O3; from 1 to 30% by weight of at least one potassium compound, calculated as K2O; from 0.7 to 10% by weight of at least one manganese compound, calculated as MnO2; from 10 to 200 ppm of at least one titanium compound, calculated as TiO2; from 2 to 20% by weight of at least one cerium compound, calculated as CeO2; from 0.1 to 10% by weight of at least one magnesium compound, calculated as MgO; from 0.1 to 10% by weight of at least one calcium compound, calculated as CaO; from 0.1 to 10% by weight of at least one molybdenum compound, calculated as MoO3; from 0 to 10% by weight of at least one vanadium compound, calculated as V2O5, and from 0 to 10% by weight of at least one further component. 8. A process for producing a dehydrogenation catalyst according to claim 1, which comprises the following steps
i) production of a catalyst premix by mixing at least one iron compound, at least one potassium compound, at least one cerium compound, from 0.7 to 10% by weight, based on the finished catalyst, of at least one manganese compound, calculated as MnO2, from 10 to 200 ppm, based on the finished catalyst, of at least one titanium compound, calculated as TiO2, optionally further metal compounds, optionally further components and optionally at least one binder with a solvent; ii) production of shaped catalyst bodies from the catalyst premix obtained in step i); iii) drying of the shaped catalyst bodies and calcination of the shaped catalyst bodies. 9. The process for producing a dehydrogenation catalyst according to claim 8, wherein the shaped catalyst bodies are calcined at temperatures in the range from 500 to 1200° C. in step iii). 10. A process for the catalytic dehydrogenation of a hydrocarbon, wherein a mixture of steam and at least one hydrocarbon is brought into contact with a dehydrogenation catalyst according to claim 1. 11. The process for the catalytic dehydrogenation of a hydrocarbon according to claim 10, wherein a mixture of steam and at least one hydrocarbon having a molar steam/hydrocarbon ratio in the range from 3 to 7.35 is used. 12. A process for the catalytic dehydrogenation of a hydrocarbon, wherein a mixture of steam and at least one hydrocarbon having a molar steam/hydrocarbon ratio in the range from 3 to 7.35 is brought into contact with a dehydrogenation catalyst comprising
at least one iron compound, at least one potassium compound, at least one cerium compound and from 0.7 to 10% by weight of at least one manganese compound, calculated as MnO2. 13. The catalytic dehydrogenation process according to claim 10, wherein a mixture of steam and at least one hydrocarbon having a molar steam/hydrocarbon ratio in the range from 4 to 7 is used. 14. The catalytic dehydrogenation process according to claim 12, wherein a mixture of steam and at least one hydrocarbon having a molar steam/hydrocarbon ratio in the range from 4 to 7 is used. 15. The catalytic dehydrogenation process according to claim 10, wherein the hydrocarbon is ethylbenzene. 16. The catalytic dehydrogenation process according to claim 12 wherein the hydrocarbon is ethylbenzene. | The present invention relates to a catalyst for the dehydrogenation of hydrocarbons which is based on iron oxide and additionally comprises at least one potassium compound, at least one cerium compound, from 0.7 to 10% by weight of at least one manganese compound, calculated as MnO 2 , and from 10 to 200 ppm of at least one titanium compound, calculated as TiO 2 , and also to a process for the production thereof. Furthermore, the present invention relates to a process for the catalytic dehydrogenation of hydrocarbons using the catalyst of the invention.1. A dehydrogenation catalyst comprising at least one iron compound, at least one potassium compound, at least one cerium compound, from 0.7 to 10% by weight of at least one manganese compound, calculated as MnO2, and from 10 to 200 ppm of at least one titanium compound, calculated as TiO2. 2. The dehydrogenation catalyst according to claim 1, wherein the catalyst comprises from 0.7 to 3% by weight of at least one manganese compound, calculated as MnO2. 3. The dehydrogenation catalyst according to claim 1, wherein the catalyst comprises from 30 to 150 ppm of at least one titanium compound, calculated as TiO2. 4. The dehydrogenation catalyst according to claim 1, wherein the catalyst comprises
from 50 to 90% by weight of at least one iron compound, calculated as Fe2O3; from 1 to 30% by weight of at least one potassium compound, calculated as K2O; from 0.7 to 10% by weight of at least one manganese compound, calculated as MnO2; from 10 to 200 ppm of at least one titanium compound, calculated as TiO2; from 2 to 20% by weight of at least one cerium compound, calculated as CeO2; and optionally from 0 to 30% by weight of at least one further component. 5. The dehydrogenation catalyst according to claim 1, wherein the catalyst comprises from 0.1 to 10% by weight of at least one compound selected from the group consisting of molybdenum, tungsten and vanadium, calculated as oxide in the respective highest oxidation state, as further component. 6. The dehydrogenation catalyst according to claim 1, wherein the catalyst comprises from 0.1 to 10% by weight of at least one alkaline earth metal compound, calculated as oxide, as further component. 7. The dehydrogenation catalyst according to claim 1, wherein the catalyst comprises
from 50 to 90% by weight of at least one iron compound, calculated as Fe2O3; from 1 to 30% by weight of at least one potassium compound, calculated as K2O; from 0.7 to 10% by weight of at least one manganese compound, calculated as MnO2; from 10 to 200 ppm of at least one titanium compound, calculated as TiO2; from 2 to 20% by weight of at least one cerium compound, calculated as CeO2; from 0.1 to 10% by weight of at least one magnesium compound, calculated as MgO; from 0.1 to 10% by weight of at least one calcium compound, calculated as CaO; from 0.1 to 10% by weight of at least one molybdenum compound, calculated as MoO3; from 0 to 10% by weight of at least one vanadium compound, calculated as V2O5, and from 0 to 10% by weight of at least one further component. 8. A process for producing a dehydrogenation catalyst according to claim 1, which comprises the following steps
i) production of a catalyst premix by mixing at least one iron compound, at least one potassium compound, at least one cerium compound, from 0.7 to 10% by weight, based on the finished catalyst, of at least one manganese compound, calculated as MnO2, from 10 to 200 ppm, based on the finished catalyst, of at least one titanium compound, calculated as TiO2, optionally further metal compounds, optionally further components and optionally at least one binder with a solvent; ii) production of shaped catalyst bodies from the catalyst premix obtained in step i); iii) drying of the shaped catalyst bodies and calcination of the shaped catalyst bodies. 9. The process for producing a dehydrogenation catalyst according to claim 8, wherein the shaped catalyst bodies are calcined at temperatures in the range from 500 to 1200° C. in step iii). 10. A process for the catalytic dehydrogenation of a hydrocarbon, wherein a mixture of steam and at least one hydrocarbon is brought into contact with a dehydrogenation catalyst according to claim 1. 11. The process for the catalytic dehydrogenation of a hydrocarbon according to claim 10, wherein a mixture of steam and at least one hydrocarbon having a molar steam/hydrocarbon ratio in the range from 3 to 7.35 is used. 12. A process for the catalytic dehydrogenation of a hydrocarbon, wherein a mixture of steam and at least one hydrocarbon having a molar steam/hydrocarbon ratio in the range from 3 to 7.35 is brought into contact with a dehydrogenation catalyst comprising
at least one iron compound, at least one potassium compound, at least one cerium compound and from 0.7 to 10% by weight of at least one manganese compound, calculated as MnO2. 13. The catalytic dehydrogenation process according to claim 10, wherein a mixture of steam and at least one hydrocarbon having a molar steam/hydrocarbon ratio in the range from 4 to 7 is used. 14. The catalytic dehydrogenation process according to claim 12, wherein a mixture of steam and at least one hydrocarbon having a molar steam/hydrocarbon ratio in the range from 4 to 7 is used. 15. The catalytic dehydrogenation process according to claim 10, wherein the hydrocarbon is ethylbenzene. 16. The catalytic dehydrogenation process according to claim 12 wherein the hydrocarbon is ethylbenzene. | 1,700 |
3,474 | 15,569,540 | 1,785 | The present disclosure is drawn to primer compositions, which can include a polyvinyl alcohol, a cationic salt, and water. The polyvinyl alcohol can be present in an amount of at least 8 wt % of all dry components of the primer composition. The cationic salt can be present in an amount of at least 15 wt % of all dry components of the primer composition. The polyvinyl alcohol and cationic salt together can make up at least 30 wt % of all dry components of the primer composition. | 1. A primer composition, comprising:
a polyvinyl alcohol present in an amount of at least 8 wt % of all dry components of the primer composition; and a cationic salt present in an amount of at least 15 wt % of all dry components of the primer composition, wherein the polyvinyl alcohol and cationic salt together make up at least 30 wt % of all dry components of the primer composition. 2. The primer composition of claim 1, further comprising a latex polymer, wherein the polyvinyl alcohol, cationic salt, and latex polymer make up at least 80 wt % of all dry components of the primer composition. 3. The primer composition of claim 2, wherein the latex polymer is a cationic latex polymer. 4. The primer composition of claim 1, wherein the polyvinyl alcohol is present at from 10 wt % to 30 wt % of all dry components of the primer composition. 5. The primer composition of claim 1, wherein the cationic salt is present at from 15 wt % to 70 wt % of all dry components of the primer composition. 6. The primer composition of claim 1, wherein the cationic salt comprises a cation of a metal selected from sodium, calcium, copper, nickel, magnesium, zinc, barium, iron, aluminum, or chromium. 7. The primer composition of claim 1, wherein the composition is substantially devoid of water-soluble polymers other than polyvinyl alcohol. 8. The primer composition of claim 1, further comprising a wax. 9. The primer composition of claim 1, wherein the polyvinyl alcohol has a weight-average molecular weight from about 20,000 Mw to about 300,000 Mw and a degree of hydrolysis from about 78 mol % to about 100 mol %. 10. The primer composition of claim 1, wherein the primer composition comprises an inorganic pigment in an amount of about 5 wt % or less of all dry components of the primer composition. 11. A method of coating a media substrate, comprising applying a primer composition to a media substrate, wherein the primer composition comprises a polyvinyl alcohol present in an amount of at least 8 wt % of all dry components of the primer composition, a cationic salt present in an amount of at least 15 wt % of all dry components of the primer composition, and water, wherein the polyvinyl alcohol and cationic salt make up at least 30 wt % of all dry components of the primer composition. 12. The method of claim 11, wherein the primer composition further comprises a latex polymer, wherein the polyvinyl alcohol, cationic salt, and latex polymer make up at least 80 wt % of all dry components of the primer composition. 13. The method of claim 11, wherein the polyvinyl alcohol is present at from 10 wt % to 30 wt % of all dry components of the primer composition and the cationic salt is present at from 30 wt % to 70 wt % of all dry components of the primer composition. 14. The method of claim 11, wherein the primer composition comprises an inorganic pigment in an amount of about 5 wt % or less of all dry components of the primer composition. 15. A coated media substrate, comprising:
a media substrate; and an ink-receiving primer layer coated on a surface of the media substrate, the ink-receiving primer layer comprising:
a polyvinyl alcohol present in an amount of at least 8 wt % of all dry components of the primer layer; and
a cationic salt present in an amount of at least 15 wt % of all dry components of the primer layer,
wherein the polyvinyl alcohol and cationic salt together make up at least 30 wt % of all dry components of the primer layer. | The present disclosure is drawn to primer compositions, which can include a polyvinyl alcohol, a cationic salt, and water. The polyvinyl alcohol can be present in an amount of at least 8 wt % of all dry components of the primer composition. The cationic salt can be present in an amount of at least 15 wt % of all dry components of the primer composition. The polyvinyl alcohol and cationic salt together can make up at least 30 wt % of all dry components of the primer composition.1. A primer composition, comprising:
a polyvinyl alcohol present in an amount of at least 8 wt % of all dry components of the primer composition; and a cationic salt present in an amount of at least 15 wt % of all dry components of the primer composition, wherein the polyvinyl alcohol and cationic salt together make up at least 30 wt % of all dry components of the primer composition. 2. The primer composition of claim 1, further comprising a latex polymer, wherein the polyvinyl alcohol, cationic salt, and latex polymer make up at least 80 wt % of all dry components of the primer composition. 3. The primer composition of claim 2, wherein the latex polymer is a cationic latex polymer. 4. The primer composition of claim 1, wherein the polyvinyl alcohol is present at from 10 wt % to 30 wt % of all dry components of the primer composition. 5. The primer composition of claim 1, wherein the cationic salt is present at from 15 wt % to 70 wt % of all dry components of the primer composition. 6. The primer composition of claim 1, wherein the cationic salt comprises a cation of a metal selected from sodium, calcium, copper, nickel, magnesium, zinc, barium, iron, aluminum, or chromium. 7. The primer composition of claim 1, wherein the composition is substantially devoid of water-soluble polymers other than polyvinyl alcohol. 8. The primer composition of claim 1, further comprising a wax. 9. The primer composition of claim 1, wherein the polyvinyl alcohol has a weight-average molecular weight from about 20,000 Mw to about 300,000 Mw and a degree of hydrolysis from about 78 mol % to about 100 mol %. 10. The primer composition of claim 1, wherein the primer composition comprises an inorganic pigment in an amount of about 5 wt % or less of all dry components of the primer composition. 11. A method of coating a media substrate, comprising applying a primer composition to a media substrate, wherein the primer composition comprises a polyvinyl alcohol present in an amount of at least 8 wt % of all dry components of the primer composition, a cationic salt present in an amount of at least 15 wt % of all dry components of the primer composition, and water, wherein the polyvinyl alcohol and cationic salt make up at least 30 wt % of all dry components of the primer composition. 12. The method of claim 11, wherein the primer composition further comprises a latex polymer, wherein the polyvinyl alcohol, cationic salt, and latex polymer make up at least 80 wt % of all dry components of the primer composition. 13. The method of claim 11, wherein the polyvinyl alcohol is present at from 10 wt % to 30 wt % of all dry components of the primer composition and the cationic salt is present at from 30 wt % to 70 wt % of all dry components of the primer composition. 14. The method of claim 11, wherein the primer composition comprises an inorganic pigment in an amount of about 5 wt % or less of all dry components of the primer composition. 15. A coated media substrate, comprising:
a media substrate; and an ink-receiving primer layer coated on a surface of the media substrate, the ink-receiving primer layer comprising:
a polyvinyl alcohol present in an amount of at least 8 wt % of all dry components of the primer layer; and
a cationic salt present in an amount of at least 15 wt % of all dry components of the primer layer,
wherein the polyvinyl alcohol and cationic salt together make up at least 30 wt % of all dry components of the primer layer. | 1,700 |
3,475 | 14,441,207 | 1,782 | A coated tube can comprise: a tube and a coating composition on the tube. The coating composition can comprise a polyester and an impact modifier, and wherein the impact modifier comprises at least one pendent group selected from epoxy groups and maleic anhydride groups and/or a polyester and an impact modifier, and wherein the polyester comprises poly(butylene terephthalate). | 1. A coated tube comprising:
a tube; and a coating composition on the tube, wherein the coating composition comprises a polyester and an impact modifier, and wherein the impact modifier comprises at least one pendent group selected from epoxy groups and maleic anhydride groups. 2. The coated tube of claim 1, wherein the polyester comprises 50 to 100 wt % poly(butylene terephthalate), based on the total amount of the polyester. 3. (canceled) 4. The coated tube of claim 1, wherein impact modifier is present in an amount of 1 to 35 wt %, based upon a total weight of the coating composition. 5. The coated tube of claim 1, wherein the coating composition comprises 65 to 95 wt % of polyester and 5 to 35 wt % of the impact modifier, based upon a total weight of the coating composition. 6. The coated tube of claim 1, wherein the coating composition further comprises a polycarbonate, a polyarylate, a polyester-carbonate resin, or a combination comprising one or more of the foregoing. 7. The coated tube of claim 1, wherein the coating composition is free of carbonate units. 8. The coated tube of claim 1, wherein the impact modifier is at least one of acrylic rubber and polyolefin copolymers. 9. The coated tube of claim 1, wherein the impact modifier comprises a polyolefin copolymer comprising a unit derived from at least one of acrylic, vinyl ester, and vinyl ether. 10. The coated tube of claim 1, wherein the impact modifier comprises methacrylate butadiene rubber. 11. The coated tube of claim 1, wherein the pendent group comprises the epoxy group. 12. The coated tube of claim 1, wherein impact modifier is an epoxy containing acrylic impact modifier. 13. The coated tube of claim 1, wherein impact modifier comprises one or more of acrylonitrile-butadiene-styrene, methyl methacrylate-butadiene-styrene, polyethylene, and styrene-ethylene-butadiene-styrene. 14. The coated tube of claim 1, wherein the impact modifier has an epoxide equivalent molecular weight of 100 to 20,000 g/mol. 15. The coated tube of claim 1, wherein a 4 mm thick tensile bar (ISO 527) made from the coating composition soaked in a solvent comprising one or more of battery acid, biodiesel, brake fluid, calcium chloride, diesel #2, E-22, E-85 low pHe, engine coolant, oxidized gasoline, sodium chloride, TF-2, water, zinc chloride, CE-10, and CM-15 results in a change in percent elongation relative to an unsoaked test bar of less than or equal to 400 times after exposure to a solvent for 500 hours at 23° C. as determined by GMW3013. 16. The coated tube of claim 1, wherein a 0.254 mm nominal gauge film of the coating composition has an average peel strength from a 1 inch wide metal strip of greater than or equal to 0.5 N/mm when peeled at a 90° angle and/or wherein a 0.508 mm nominal gauge film of the coating composition has an average peel strength from a 1 inch wide metal strip of greater than or equal to 0.5 N/mm when peeled at a 90° angle, wherein the 1 inch wide metal strip comprises steel and a metal coating, wherein the metal coating comprises 95 wt % zinc and 5 wt % aluminum based upon a total weight of the metal coating. 17. The coated tube of claim 1, wherein the tube comprises steel. 18. The coated tube of claim 1, further comprising a metal coating between the coating composition and the tube, wherein the metal coating comprises greater than or equal to 70 wt % zinc, based upon a total weight of the metal coating. 19. The coated tube of claim 1, wherein the coating composition comprises 20-100 wt % poly(butylene terephthalate);
0-30 wt % polycarbonate; and 0-50 wt % poly(ethylene terephthalate); wherein the weight percentages are based upon a total weight of resin in the coating composition. 20. The coated tube of claim 1, wherein the polyester comprises poly(butylene terephthalate). 21. A method of coating a tube comprising:
applying a coating composition to a tube; wherein the coating composition comprises a polyester and an impact modifier, and wherein the impact modifier comprises at least one pendent group selected from epoxy groups and maleic anhydride groups; or the coating composition comprises a polyester and an impact modifier, and wherein the polyester comprises poly(butylene terephthalate); or the coating composition comprises a polyester and an impact modifier, and wherein the polyester comprises poly(butylene terephthalate) and the impact modifier comprises at least one pendent group selected from epoxy groups and maleic anhydride groups. | A coated tube can comprise: a tube and a coating composition on the tube. The coating composition can comprise a polyester and an impact modifier, and wherein the impact modifier comprises at least one pendent group selected from epoxy groups and maleic anhydride groups and/or a polyester and an impact modifier, and wherein the polyester comprises poly(butylene terephthalate).1. A coated tube comprising:
a tube; and a coating composition on the tube, wherein the coating composition comprises a polyester and an impact modifier, and wherein the impact modifier comprises at least one pendent group selected from epoxy groups and maleic anhydride groups. 2. The coated tube of claim 1, wherein the polyester comprises 50 to 100 wt % poly(butylene terephthalate), based on the total amount of the polyester. 3. (canceled) 4. The coated tube of claim 1, wherein impact modifier is present in an amount of 1 to 35 wt %, based upon a total weight of the coating composition. 5. The coated tube of claim 1, wherein the coating composition comprises 65 to 95 wt % of polyester and 5 to 35 wt % of the impact modifier, based upon a total weight of the coating composition. 6. The coated tube of claim 1, wherein the coating composition further comprises a polycarbonate, a polyarylate, a polyester-carbonate resin, or a combination comprising one or more of the foregoing. 7. The coated tube of claim 1, wherein the coating composition is free of carbonate units. 8. The coated tube of claim 1, wherein the impact modifier is at least one of acrylic rubber and polyolefin copolymers. 9. The coated tube of claim 1, wherein the impact modifier comprises a polyolefin copolymer comprising a unit derived from at least one of acrylic, vinyl ester, and vinyl ether. 10. The coated tube of claim 1, wherein the impact modifier comprises methacrylate butadiene rubber. 11. The coated tube of claim 1, wherein the pendent group comprises the epoxy group. 12. The coated tube of claim 1, wherein impact modifier is an epoxy containing acrylic impact modifier. 13. The coated tube of claim 1, wherein impact modifier comprises one or more of acrylonitrile-butadiene-styrene, methyl methacrylate-butadiene-styrene, polyethylene, and styrene-ethylene-butadiene-styrene. 14. The coated tube of claim 1, wherein the impact modifier has an epoxide equivalent molecular weight of 100 to 20,000 g/mol. 15. The coated tube of claim 1, wherein a 4 mm thick tensile bar (ISO 527) made from the coating composition soaked in a solvent comprising one or more of battery acid, biodiesel, brake fluid, calcium chloride, diesel #2, E-22, E-85 low pHe, engine coolant, oxidized gasoline, sodium chloride, TF-2, water, zinc chloride, CE-10, and CM-15 results in a change in percent elongation relative to an unsoaked test bar of less than or equal to 400 times after exposure to a solvent for 500 hours at 23° C. as determined by GMW3013. 16. The coated tube of claim 1, wherein a 0.254 mm nominal gauge film of the coating composition has an average peel strength from a 1 inch wide metal strip of greater than or equal to 0.5 N/mm when peeled at a 90° angle and/or wherein a 0.508 mm nominal gauge film of the coating composition has an average peel strength from a 1 inch wide metal strip of greater than or equal to 0.5 N/mm when peeled at a 90° angle, wherein the 1 inch wide metal strip comprises steel and a metal coating, wherein the metal coating comprises 95 wt % zinc and 5 wt % aluminum based upon a total weight of the metal coating. 17. The coated tube of claim 1, wherein the tube comprises steel. 18. The coated tube of claim 1, further comprising a metal coating between the coating composition and the tube, wherein the metal coating comprises greater than or equal to 70 wt % zinc, based upon a total weight of the metal coating. 19. The coated tube of claim 1, wherein the coating composition comprises 20-100 wt % poly(butylene terephthalate);
0-30 wt % polycarbonate; and 0-50 wt % poly(ethylene terephthalate); wherein the weight percentages are based upon a total weight of resin in the coating composition. 20. The coated tube of claim 1, wherein the polyester comprises poly(butylene terephthalate). 21. A method of coating a tube comprising:
applying a coating composition to a tube; wherein the coating composition comprises a polyester and an impact modifier, and wherein the impact modifier comprises at least one pendent group selected from epoxy groups and maleic anhydride groups; or the coating composition comprises a polyester and an impact modifier, and wherein the polyester comprises poly(butylene terephthalate); or the coating composition comprises a polyester and an impact modifier, and wherein the polyester comprises poly(butylene terephthalate) and the impact modifier comprises at least one pendent group selected from epoxy groups and maleic anhydride groups. | 1,700 |
3,476 | 15,876,426 | 1,771 | Methods of making a diesel fuel blend having enhanced cold properties; methods of lowering the cloud point of a mineral middle distillate fuel; and diesel fuel blends having a blend of a renewable fuel and a mineral middle distillate fuel. | 1. A diesel fuel blend comprising:
a blend of a renewable fuel component and a mineral middle distillate fuel component in which the renewable fuel component and mineral middle distillate fuel component are present in a ratio of amounts by volume of from 10:90 to 90:10; and the diesel fuel blend contains 10-25 wt % n-paraffins in a C14-C20 range and an amount of isoparaffins in the C14-C20 range, such that a ratio of a sum of wt % amounts of isoparaffins in the C14-C20 range to a sum of wt % amounts of n-paraffins in the C14-C20 range is less than 2.2. 2. A diesel fuel blend according to claim 1, wherein the renewable fuel component and mineral middle distillate fuel component have cloud points that differ by no more than 17° C. 3. A diesel fuel blend according to claim 1, wherein the ratio of the sum of wt % amounts of isoparaffins in the C14-C20 range to the sum of wt % amounts of n-paraffins in the C14-C20 range is from 1.1 to 2.2. 4. A diesel fuel blend according to claim 1, wherein the diesel fuel blend has from 22 wt % to 55 wt % isoparaffins in the C14-C20 range. 5. A diesel fuel blend according to claim 1, wherein the mineral middle distillate fuel component is derived from sources selected from a group consisting of crude petroleum oil, shale oil, and combinations thereof. 6. A diesel fuel blend according to claim 1, wherein the mineral middle distillate fuel component is a diesel fuel. 7. A diesel fuel blend according to claim 1, wherein a fresh feed for the renewable fuel component is selected from a group consisting of plant oils/fats, animal fats/oils, fish fats/oils, fats contained in plants bred by gene manipulation, recycled fats of food industry and combinations thereof. 8. A diesel fuel blend according to claim 1, wherein the renewable fuel component and mineral middle distillate fuel component are present in a ratio of amounts by volume of from 20:80 to 80:20. 9. A diesel fuel blend according to claim 1, wherein a isomerization ratio of the renewable fuel component is at least 50%. 10. A method of making a diesel fuel blend having enhanced cold properties, the method comprising:
(a) selecting a renewable fuel component and a mineral middle distillate fuel component having cloud points that differ by no more than 17° C.; and (b) blending the renewable fuel component and mineral middle distillate fuel component in a ratio of amounts by volume of from 10:90 to 90:10 to form a diesel fuel blend, wherein the diesel fuel blend contains 10-25 wt % n-paraffins in a C14-C20 range and an amount of isoparaffins in a C14-C20 range such that a ratio of a sum of wt % amounts of isoparaffins in the C14-C20 range to a sum of wt % amounts of n-paraffins in the C14-C20 range is less than 2.2; and wherein the diesel fuel blend has a cloud point that is lower than a weighted mean of the cloud points of the mineral middle distillate component and the renewable fuel component. 11. A method according to claim 10, wherein the diesel fuel blend has a ratio of the sum of wt % amounts of isoparaffins in the C14-C20 range to the sum of wt % amounts of n-paraffins in the C14-C20 range that is from 1.1 to 2.2. 12. A method according to claim 11, wherein the diesel fuel blend has from 22 wt % to 55 wt % isoparaffins in the C14-C20 range. 13. A method according to claim 12, wherein a fresh feed of renewable fuel is selected from a group consisting of plant oils/fats, animal fats/oils, fish fats/oils, fats contained in plants bred by means of gene manipulation, recycled fats of food industry and combinations thereof. 14. A method according to claim 13, wherein the isomerization ratio of the renewable fuel component is at least 50%. 15. A method according to claim 10, wherein the diesel fuel blend has a cloud point that is lower than the cloud point of the mineral middle distillate fuel component. 16. A method according to claim 10, wherein the diesel fuel blend has a cloud point that is lower than the cloud point of the renewable fuel component. 17. A method for lowering a cloud point of a mineral middle distillate fuel using a renewable fuel, the method comprising:
(a) determining a cloud point of a mineral middle distillate fuel; (b) selecting a renewable fuel having properties as follows:
(i) a cloud point that differs by no more than 17° C. from the cloud point of the mineral middle distillate fuel;
(ii) an amount of n-paraffins sufficient to provide a diesel fuel blend containing 10-25 wt % n-paraffins in a C14-C20 range when the renewable fuel is blended with the mineral middle distillate fuel; and
(iii) an amount of isoparaffins in the C14-C20 range sufficient to provide a diesel fuel blend having a ratio of a sum of wt % amounts of isoparaffins in the C14-C20 range to a sum of wt % amounts of n-paraffins in the C14-C20 range of from 1.1 to 2.2 when the renewable fuel is blended with the mineral middle distillate fuel; and
(c) blending the renewable fuel with the mineral middle distillate fuel in a ratio of amounts by volume of from 10:90 to 90:10 to form a diesel fuel blend having a cloud point that is lower than the cloud point of the mineral middle distillate fuel. 18. A method for lowering the cloud point of a renewable fuel using a mineral middle distillate, the method comprising:
(a) determining a cloud point of a renewable fuel; (b) selecting a mineral middle distillate having properties as follows:
(i) a cloud point that differs by no more than 17° C. from the cloud point of the renewable fuel;
(ii) an amount of n-paraffins sufficient to provide a diesel fuel blend containing 10-25 wt % n-paraffins in a C14-C20 range when the renewable fuel is blended with the mineral middle distillate fuel; and
(iii) an amount of isoparaffins in the C14-C20 range sufficient to provide a diesel fuel blend having a ratio of a sum of wt % amounts of isoparaffins in the C14-C20 range to a sum of wt % amounts of n-paraffins in the C14-C20 range of from 1.1 to 2.2 when the renewable fuel is blended with the mineral middle distillate fuel; and
(c) blending the renewable fuel with the mineral middle distillate fuel in a ratio of amounts by volume of from 10:90 to 90:10 to form a diesel fuel blend having a cloud point that is lower than the cloud point of the renewable fuel. 19. A diesel fuel blend having enhanced cold properties obtained by a method according to claim 10. 20. A diesel fuel blend according to claim 1, wherein the renewable fuel component and mineral middle distillate fuel component have cloud points that differ by no more than 13° C. 21. A diesel fuel blend according to claim 2, wherein the ratio of the sum of wt % amounts of isoparaffins in the C14-C20 range to the sum of wt % amounts of n-paraffins in the C14-C20 range is from 1.1 to 2.2. 22. A diesel fuel blend according to claim 21, wherein the diesel fuel blend has from 22 wt % to 55 wt % isoparaffins in the C14-C20 range. 23. A diesel fuel blend according to claim 22, wherein the renewable fuel component and mineral middle distillate fuel component are present in a ratio of amounts by volume of from 20:80 to 80:20. 24. A diesel fuel blend according to claim 1, wherein a isomerization ratio of the renewable fuel component is at least 60%. 25. A method according to claim 10, wherein the cloud points of the renewable fuel component and the mineral middle distillate fuel component differ by no more than 13° C. 26. A method according to claim 13, wherein the isomerization ratio of the renewable fuel component is at least 60%. 27. A diesel fuel blend having enhanced cold properties obtained by a method according to claim 17. 28. A diesel fuel blend having enhanced cold properties obtained by a method according to claim 18. | Methods of making a diesel fuel blend having enhanced cold properties; methods of lowering the cloud point of a mineral middle distillate fuel; and diesel fuel blends having a blend of a renewable fuel and a mineral middle distillate fuel.1. A diesel fuel blend comprising:
a blend of a renewable fuel component and a mineral middle distillate fuel component in which the renewable fuel component and mineral middle distillate fuel component are present in a ratio of amounts by volume of from 10:90 to 90:10; and the diesel fuel blend contains 10-25 wt % n-paraffins in a C14-C20 range and an amount of isoparaffins in the C14-C20 range, such that a ratio of a sum of wt % amounts of isoparaffins in the C14-C20 range to a sum of wt % amounts of n-paraffins in the C14-C20 range is less than 2.2. 2. A diesel fuel blend according to claim 1, wherein the renewable fuel component and mineral middle distillate fuel component have cloud points that differ by no more than 17° C. 3. A diesel fuel blend according to claim 1, wherein the ratio of the sum of wt % amounts of isoparaffins in the C14-C20 range to the sum of wt % amounts of n-paraffins in the C14-C20 range is from 1.1 to 2.2. 4. A diesel fuel blend according to claim 1, wherein the diesel fuel blend has from 22 wt % to 55 wt % isoparaffins in the C14-C20 range. 5. A diesel fuel blend according to claim 1, wherein the mineral middle distillate fuel component is derived from sources selected from a group consisting of crude petroleum oil, shale oil, and combinations thereof. 6. A diesel fuel blend according to claim 1, wherein the mineral middle distillate fuel component is a diesel fuel. 7. A diesel fuel blend according to claim 1, wherein a fresh feed for the renewable fuel component is selected from a group consisting of plant oils/fats, animal fats/oils, fish fats/oils, fats contained in plants bred by gene manipulation, recycled fats of food industry and combinations thereof. 8. A diesel fuel blend according to claim 1, wherein the renewable fuel component and mineral middle distillate fuel component are present in a ratio of amounts by volume of from 20:80 to 80:20. 9. A diesel fuel blend according to claim 1, wherein a isomerization ratio of the renewable fuel component is at least 50%. 10. A method of making a diesel fuel blend having enhanced cold properties, the method comprising:
(a) selecting a renewable fuel component and a mineral middle distillate fuel component having cloud points that differ by no more than 17° C.; and (b) blending the renewable fuel component and mineral middle distillate fuel component in a ratio of amounts by volume of from 10:90 to 90:10 to form a diesel fuel blend, wherein the diesel fuel blend contains 10-25 wt % n-paraffins in a C14-C20 range and an amount of isoparaffins in a C14-C20 range such that a ratio of a sum of wt % amounts of isoparaffins in the C14-C20 range to a sum of wt % amounts of n-paraffins in the C14-C20 range is less than 2.2; and wherein the diesel fuel blend has a cloud point that is lower than a weighted mean of the cloud points of the mineral middle distillate component and the renewable fuel component. 11. A method according to claim 10, wherein the diesel fuel blend has a ratio of the sum of wt % amounts of isoparaffins in the C14-C20 range to the sum of wt % amounts of n-paraffins in the C14-C20 range that is from 1.1 to 2.2. 12. A method according to claim 11, wherein the diesel fuel blend has from 22 wt % to 55 wt % isoparaffins in the C14-C20 range. 13. A method according to claim 12, wherein a fresh feed of renewable fuel is selected from a group consisting of plant oils/fats, animal fats/oils, fish fats/oils, fats contained in plants bred by means of gene manipulation, recycled fats of food industry and combinations thereof. 14. A method according to claim 13, wherein the isomerization ratio of the renewable fuel component is at least 50%. 15. A method according to claim 10, wherein the diesel fuel blend has a cloud point that is lower than the cloud point of the mineral middle distillate fuel component. 16. A method according to claim 10, wherein the diesel fuel blend has a cloud point that is lower than the cloud point of the renewable fuel component. 17. A method for lowering a cloud point of a mineral middle distillate fuel using a renewable fuel, the method comprising:
(a) determining a cloud point of a mineral middle distillate fuel; (b) selecting a renewable fuel having properties as follows:
(i) a cloud point that differs by no more than 17° C. from the cloud point of the mineral middle distillate fuel;
(ii) an amount of n-paraffins sufficient to provide a diesel fuel blend containing 10-25 wt % n-paraffins in a C14-C20 range when the renewable fuel is blended with the mineral middle distillate fuel; and
(iii) an amount of isoparaffins in the C14-C20 range sufficient to provide a diesel fuel blend having a ratio of a sum of wt % amounts of isoparaffins in the C14-C20 range to a sum of wt % amounts of n-paraffins in the C14-C20 range of from 1.1 to 2.2 when the renewable fuel is blended with the mineral middle distillate fuel; and
(c) blending the renewable fuel with the mineral middle distillate fuel in a ratio of amounts by volume of from 10:90 to 90:10 to form a diesel fuel blend having a cloud point that is lower than the cloud point of the mineral middle distillate fuel. 18. A method for lowering the cloud point of a renewable fuel using a mineral middle distillate, the method comprising:
(a) determining a cloud point of a renewable fuel; (b) selecting a mineral middle distillate having properties as follows:
(i) a cloud point that differs by no more than 17° C. from the cloud point of the renewable fuel;
(ii) an amount of n-paraffins sufficient to provide a diesel fuel blend containing 10-25 wt % n-paraffins in a C14-C20 range when the renewable fuel is blended with the mineral middle distillate fuel; and
(iii) an amount of isoparaffins in the C14-C20 range sufficient to provide a diesel fuel blend having a ratio of a sum of wt % amounts of isoparaffins in the C14-C20 range to a sum of wt % amounts of n-paraffins in the C14-C20 range of from 1.1 to 2.2 when the renewable fuel is blended with the mineral middle distillate fuel; and
(c) blending the renewable fuel with the mineral middle distillate fuel in a ratio of amounts by volume of from 10:90 to 90:10 to form a diesel fuel blend having a cloud point that is lower than the cloud point of the renewable fuel. 19. A diesel fuel blend having enhanced cold properties obtained by a method according to claim 10. 20. A diesel fuel blend according to claim 1, wherein the renewable fuel component and mineral middle distillate fuel component have cloud points that differ by no more than 13° C. 21. A diesel fuel blend according to claim 2, wherein the ratio of the sum of wt % amounts of isoparaffins in the C14-C20 range to the sum of wt % amounts of n-paraffins in the C14-C20 range is from 1.1 to 2.2. 22. A diesel fuel blend according to claim 21, wherein the diesel fuel blend has from 22 wt % to 55 wt % isoparaffins in the C14-C20 range. 23. A diesel fuel blend according to claim 22, wherein the renewable fuel component and mineral middle distillate fuel component are present in a ratio of amounts by volume of from 20:80 to 80:20. 24. A diesel fuel blend according to claim 1, wherein a isomerization ratio of the renewable fuel component is at least 60%. 25. A method according to claim 10, wherein the cloud points of the renewable fuel component and the mineral middle distillate fuel component differ by no more than 13° C. 26. A method according to claim 13, wherein the isomerization ratio of the renewable fuel component is at least 60%. 27. A diesel fuel blend having enhanced cold properties obtained by a method according to claim 17. 28. A diesel fuel blend having enhanced cold properties obtained by a method according to claim 18. | 1,700 |
3,477 | 15,258,685 | 1,766 | The method of making a compressed biocomposite body includes compressing a mass of biocomposite material comprised of discrete particles and a network of interconnected glucan-containing mycelia cells in the presence of heat and moisture into a compressed body having a density in excess of 18 pcf. Compression may take place batch wise in a press or continuously in a path of narrowing cross-section defined by a series of heated rollers. | 1. A method of making a composite body comprising the steps of
obtaining a mass of biocomposite material comprised of discrete particles, a network of interconnected glucan-containing mycelia cells extending around the discrete particles and a moisture content of greater than 10% by weight; molding said mass into a plurality of tiles of rectangular shape; stacking said tiles in alternating manner with a plurality of wooden veneers and with a plate of porous plastic on an underside thereof to from a stack; compressing said stack to compress said tiles to approximately three times density while drying the compressed tiles to obtain a pre-compressed biocomposite body; thereafter compressing said pre-compressed biocomposite body at a force of 20 tons and at a temperature of 600° F. for a time of two minutes while reducing the moisture content to less than 10% to obtain a compressed composite body. 2. A method as set forth in claim 1 wherein said compressed composite body has a density of 20 lbs/ft3, a modulus of elasticity around 80 ksi, a modulus of rupture around 800 psi, and a screw hold strength around 100 lbf. 3. A method of making a composite body comprising the steps of
obtaining a mass of biocomposite material comprised of discrete particles, a network of interconnected glucan-containing mycelia cells extending around the discrete particles and a moisture content of greater than 10% by weight; and thereafter compressing said mass at a pressure between 25 psi and 5000 psi and at a temperature of 600° F. for a time of four minutes while reducing the moisture content to less than 10% to obtain a compressed composite body. 4. A method as set forth in claim 3 wherein said compressed composite body has a density of 34 lbs/ft3, a modulus of elasticity around 132 ksi, a modulus of rupture around 1698 psi, and a screw hold strength around 24 lbf at half an inch thickness. 5. A method as set forth in claim 3 wherein said compressed composite body has a density of 29 lbs/ft3, a modulus of elasticity around 120 ksi, a modulus of rupture around 819 psi, and a screw hold strength around 132 lbf at an inch thickness. 6. A method of making a composite body comprising the steps of
obtaining a mass of biocomposite material comprised of discrete particles, a network of interconnected glucan-containing mycelia cells extending around the discrete particles and a moisture content of greater than 10% by weight; and thereafter compressing said mass at a pressure between 25 psi and 5000 psi and at a temperature of 300° F. for a time of one minute while reducing the moisture content to less than 10% to obtain a compressed composite body. 7. A method as set forth in claim 6 wherein said mass is molded into a sheet prior to said step of compressing and pressed into a deformed geometric shape. 8. A method as set forth in claim 7 wherein said sheet has dimensions of 18 inches by 18 inches by 1 inch and said deformed geometric shape is a semi-cylindrical shape. 9. A method of making a composite body comprising the steps of
obtaining a mass of biocomposite material comprised of discrete particles, a network of interconnected glucan-containing mycelia cells extending around the discrete particles and a moisture content of greater than 10% by weight; forming said mass of biocomposite material into a flat blank board of 1.25″ thickness with a 0.25″ hemp nonwoven matt grown into at least one face of said flat blank board; thereafter compressing said flat blank board into the predetermined curved shape under a compressive force of 3000 psi and at a temperature of 340° F. for a time of 10 minutes while reducing the moisture content to less than 10% to obtain a compressed composite body of curved shape. 10. A method as set forth in claim 9 wherein said step of forming said mass of biocomposite material into a flat blank board includes embossing said at least one face with a predetermined sculptured feature. 11. A method of making a composite body comprising the steps of
cultivating mycelium into a sheet; freeze drying said sheet; thereafter milling said dried sheet to form a first mass of particles; milling Kenaf pith to form a second mass of particles; blending said first mass of particles and said second mass of particles into a mixture; thereafter heating and compressing said mixture in a mold cavity for a time sufficient to form a cohesive product; and removing said product from the mold as a self-supporting composite body. 12. A method as set forth in claim 11 wherein said step of cultivating mycelium into a sheet includes cultivating the mycelium on malt extract at a rate of 32 g per liter for 7 days at ambient conditions of 75° F., 20% relative humidity and 2000 ppm CO2 until said sheet of mycelium is formed. 13. A method as set forth in claim 11 wherein said step of milling said dried sheet includes hammer milling through a 0.0625″ screen. 14. A method as set forth in claim 11 wherein said step of milling Kenaf pith includes hammer milling through a 22 mesh and over a 38 mesh screen. 15. A method as set forth in claim 11 wherein said step of blending blends said Kenaf pith and said mycelium together at a 9:1 ratio. 16. A method as set forth in claim 11 wherein said step of heating and compressing said mixture includes heating the mold cavity to 380° F. and compressing said mixture under 30 tons of force for four minutes to form the cohesive product. 17. A self-supporting composite body comprising a substrate of discrete particles and a network of interconnected mycelia cells extending through and around the discrete particles and bonding the discrete particles together, said composite body being characterized in being stiff and in having a density between 18 and 60 pounds per cubic foot (pcf), a modulus of elasticity of up to 250 ksi and a modulus of rupture of up to 2500 psi. 18. A self-supporting composite body comprising a substrate of discrete fibers and a network of interconnected mycelia cells extending through and around the discrete fibers and bonding the discrete fibers together, said composite body being characterized in being stiff and in having a density between 18 and 60 pounds per cubic foot (pcf), a modulus of elasticity greater than 250 ksi and a modulus of rupture of up to 2500 psi. | The method of making a compressed biocomposite body includes compressing a mass of biocomposite material comprised of discrete particles and a network of interconnected glucan-containing mycelia cells in the presence of heat and moisture into a compressed body having a density in excess of 18 pcf. Compression may take place batch wise in a press or continuously in a path of narrowing cross-section defined by a series of heated rollers.1. A method of making a composite body comprising the steps of
obtaining a mass of biocomposite material comprised of discrete particles, a network of interconnected glucan-containing mycelia cells extending around the discrete particles and a moisture content of greater than 10% by weight; molding said mass into a plurality of tiles of rectangular shape; stacking said tiles in alternating manner with a plurality of wooden veneers and with a plate of porous plastic on an underside thereof to from a stack; compressing said stack to compress said tiles to approximately three times density while drying the compressed tiles to obtain a pre-compressed biocomposite body; thereafter compressing said pre-compressed biocomposite body at a force of 20 tons and at a temperature of 600° F. for a time of two minutes while reducing the moisture content to less than 10% to obtain a compressed composite body. 2. A method as set forth in claim 1 wherein said compressed composite body has a density of 20 lbs/ft3, a modulus of elasticity around 80 ksi, a modulus of rupture around 800 psi, and a screw hold strength around 100 lbf. 3. A method of making a composite body comprising the steps of
obtaining a mass of biocomposite material comprised of discrete particles, a network of interconnected glucan-containing mycelia cells extending around the discrete particles and a moisture content of greater than 10% by weight; and thereafter compressing said mass at a pressure between 25 psi and 5000 psi and at a temperature of 600° F. for a time of four minutes while reducing the moisture content to less than 10% to obtain a compressed composite body. 4. A method as set forth in claim 3 wherein said compressed composite body has a density of 34 lbs/ft3, a modulus of elasticity around 132 ksi, a modulus of rupture around 1698 psi, and a screw hold strength around 24 lbf at half an inch thickness. 5. A method as set forth in claim 3 wherein said compressed composite body has a density of 29 lbs/ft3, a modulus of elasticity around 120 ksi, a modulus of rupture around 819 psi, and a screw hold strength around 132 lbf at an inch thickness. 6. A method of making a composite body comprising the steps of
obtaining a mass of biocomposite material comprised of discrete particles, a network of interconnected glucan-containing mycelia cells extending around the discrete particles and a moisture content of greater than 10% by weight; and thereafter compressing said mass at a pressure between 25 psi and 5000 psi and at a temperature of 300° F. for a time of one minute while reducing the moisture content to less than 10% to obtain a compressed composite body. 7. A method as set forth in claim 6 wherein said mass is molded into a sheet prior to said step of compressing and pressed into a deformed geometric shape. 8. A method as set forth in claim 7 wherein said sheet has dimensions of 18 inches by 18 inches by 1 inch and said deformed geometric shape is a semi-cylindrical shape. 9. A method of making a composite body comprising the steps of
obtaining a mass of biocomposite material comprised of discrete particles, a network of interconnected glucan-containing mycelia cells extending around the discrete particles and a moisture content of greater than 10% by weight; forming said mass of biocomposite material into a flat blank board of 1.25″ thickness with a 0.25″ hemp nonwoven matt grown into at least one face of said flat blank board; thereafter compressing said flat blank board into the predetermined curved shape under a compressive force of 3000 psi and at a temperature of 340° F. for a time of 10 minutes while reducing the moisture content to less than 10% to obtain a compressed composite body of curved shape. 10. A method as set forth in claim 9 wherein said step of forming said mass of biocomposite material into a flat blank board includes embossing said at least one face with a predetermined sculptured feature. 11. A method of making a composite body comprising the steps of
cultivating mycelium into a sheet; freeze drying said sheet; thereafter milling said dried sheet to form a first mass of particles; milling Kenaf pith to form a second mass of particles; blending said first mass of particles and said second mass of particles into a mixture; thereafter heating and compressing said mixture in a mold cavity for a time sufficient to form a cohesive product; and removing said product from the mold as a self-supporting composite body. 12. A method as set forth in claim 11 wherein said step of cultivating mycelium into a sheet includes cultivating the mycelium on malt extract at a rate of 32 g per liter for 7 days at ambient conditions of 75° F., 20% relative humidity and 2000 ppm CO2 until said sheet of mycelium is formed. 13. A method as set forth in claim 11 wherein said step of milling said dried sheet includes hammer milling through a 0.0625″ screen. 14. A method as set forth in claim 11 wherein said step of milling Kenaf pith includes hammer milling through a 22 mesh and over a 38 mesh screen. 15. A method as set forth in claim 11 wherein said step of blending blends said Kenaf pith and said mycelium together at a 9:1 ratio. 16. A method as set forth in claim 11 wherein said step of heating and compressing said mixture includes heating the mold cavity to 380° F. and compressing said mixture under 30 tons of force for four minutes to form the cohesive product. 17. A self-supporting composite body comprising a substrate of discrete particles and a network of interconnected mycelia cells extending through and around the discrete particles and bonding the discrete particles together, said composite body being characterized in being stiff and in having a density between 18 and 60 pounds per cubic foot (pcf), a modulus of elasticity of up to 250 ksi and a modulus of rupture of up to 2500 psi. 18. A self-supporting composite body comprising a substrate of discrete fibers and a network of interconnected mycelia cells extending through and around the discrete fibers and bonding the discrete fibers together, said composite body being characterized in being stiff and in having a density between 18 and 60 pounds per cubic foot (pcf), a modulus of elasticity greater than 250 ksi and a modulus of rupture of up to 2500 psi. | 1,700 |
3,478 | 15,346,190 | 1,786 | A composite material including an organic compound and an inorganic compound and having a high carrier-transport property is provided. A composite material having a high carrier-injection property to an organic compound is provided. A composite material in which light absorption due to charge transfer interaction is unlikely to occur is provided. A light-emitting element having high emission efficiency is provided by including the composite material. A light-emitting element having a low drive voltage is provided. A light-emitting element having a long lifetime is provided. A composite material including a heterocyclic compound having a dibenzothiophene skeleton or a dibenzofuran skeleton and an inorganic compound exhibiting an electron-accepting property with respect to the heterocyclic compound is provided. | 1. A composite material comprising:
a heterocyclic compound comprising one of a dibenzothiophene skeleton and a dibenzofuran skeleton; and an inorganic compound exhibiting an electron-accepting property with respect to the heterocyclic compound. | A composite material including an organic compound and an inorganic compound and having a high carrier-transport property is provided. A composite material having a high carrier-injection property to an organic compound is provided. A composite material in which light absorption due to charge transfer interaction is unlikely to occur is provided. A light-emitting element having high emission efficiency is provided by including the composite material. A light-emitting element having a low drive voltage is provided. A light-emitting element having a long lifetime is provided. A composite material including a heterocyclic compound having a dibenzothiophene skeleton or a dibenzofuran skeleton and an inorganic compound exhibiting an electron-accepting property with respect to the heterocyclic compound is provided.1. A composite material comprising:
a heterocyclic compound comprising one of a dibenzothiophene skeleton and a dibenzofuran skeleton; and an inorganic compound exhibiting an electron-accepting property with respect to the heterocyclic compound. | 1,700 |
3,479 | 14,959,941 | 1,791 | A composition comprising a whole grain with hydrolyzed starch. Although the starch can shift from relatively higher molecular weight moieties to relatively lower molecular weight moieties during hydrolysis, the relative proportions of the principal anatomical components of the caryopses of the grain—the starchy endosperm, germ and bran—remain approximately the same as evinced, for example, by the weight percentages and relative mass ratios of starch, fat, protein, dietary fiber, beta-glucan, and sugar in the composition. Additionally, the whole grain composition can be a powder, for example, a flour, and the whole grain composition can be granulated to a desired size to provide a powder that is highly dispersible in liquid. When gelatinized, hydrated and dispersed in a liquid, the whole grain with hydrolyzed starch can have a lower viscosity, grittiness, and graininess compared to the same variety of whole grain with unhydrolyzed starch. | 1. A composition comprising:
a whole grain; wherein the whole grain comprises hydrolyzed starch. 2. The composition of claim 1, wherein the hydrolyzed starch is a gelatinized, hydrolyzed starch. 3. The composition of claim 1, further comprising:
deactivated α-amylase enzyme. 4. The composition of claim 1, wherein the whole grain is extruded. 5. The composition of claim 1, wherein the whole grain is selected from the group consisting of whole oat and whole barley. 6. The composition of claim 1, wherein the whole grain comprises whole grain flour. 7. The composition of claim 1, wherein the whole grain is made from unhydrolyzed whole grain. 8. The composition of claim 1, wherein the whole grain is made from unprocessed whole grain. 9. The composition of claim 6, wherein the whole grain flour comprises hydrolyzed starch. 10. The composition of claim 6, wherein the hydrolyzed starch is a gelatinized, hydrolyzed starch. 11. The composition of claim 6, further comprising:
deactivated amylase enzyme. 12. The composition of claim 6, wherein the whole grain flour is extruded. 13. The composition of claim 1, further comprising a liquid. 14. The composition of claim 13, wherein the liquid comprises a water-containing component. 15. The composition of claim 14, wherein the liquid comprises water. 16. The composition of claim 14, wherein the liquid comprises milk. 17. The composition of claim 16, wherein the liquid comprises a non-dairy milk. 18. The composition of claim 14, wherein the composition comprises about 70-95 wt % water. 19. The composition of claim 1, wherein the composition comprises about 1.5 wt % to about 10 wt % water. 20. The composition of claim 1, wherein the composition is granulated to a Max 85% through a US 30 screen. | A composition comprising a whole grain with hydrolyzed starch. Although the starch can shift from relatively higher molecular weight moieties to relatively lower molecular weight moieties during hydrolysis, the relative proportions of the principal anatomical components of the caryopses of the grain—the starchy endosperm, germ and bran—remain approximately the same as evinced, for example, by the weight percentages and relative mass ratios of starch, fat, protein, dietary fiber, beta-glucan, and sugar in the composition. Additionally, the whole grain composition can be a powder, for example, a flour, and the whole grain composition can be granulated to a desired size to provide a powder that is highly dispersible in liquid. When gelatinized, hydrated and dispersed in a liquid, the whole grain with hydrolyzed starch can have a lower viscosity, grittiness, and graininess compared to the same variety of whole grain with unhydrolyzed starch.1. A composition comprising:
a whole grain; wherein the whole grain comprises hydrolyzed starch. 2. The composition of claim 1, wherein the hydrolyzed starch is a gelatinized, hydrolyzed starch. 3. The composition of claim 1, further comprising:
deactivated α-amylase enzyme. 4. The composition of claim 1, wherein the whole grain is extruded. 5. The composition of claim 1, wherein the whole grain is selected from the group consisting of whole oat and whole barley. 6. The composition of claim 1, wherein the whole grain comprises whole grain flour. 7. The composition of claim 1, wherein the whole grain is made from unhydrolyzed whole grain. 8. The composition of claim 1, wherein the whole grain is made from unprocessed whole grain. 9. The composition of claim 6, wherein the whole grain flour comprises hydrolyzed starch. 10. The composition of claim 6, wherein the hydrolyzed starch is a gelatinized, hydrolyzed starch. 11. The composition of claim 6, further comprising:
deactivated amylase enzyme. 12. The composition of claim 6, wherein the whole grain flour is extruded. 13. The composition of claim 1, further comprising a liquid. 14. The composition of claim 13, wherein the liquid comprises a water-containing component. 15. The composition of claim 14, wherein the liquid comprises water. 16. The composition of claim 14, wherein the liquid comprises milk. 17. The composition of claim 16, wherein the liquid comprises a non-dairy milk. 18. The composition of claim 14, wherein the composition comprises about 70-95 wt % water. 19. The composition of claim 1, wherein the composition comprises about 1.5 wt % to about 10 wt % water. 20. The composition of claim 1, wherein the composition is granulated to a Max 85% through a US 30 screen. | 1,700 |
3,480 | 13,718,061 | 1,797 | An apparatus for receiving a chemical species is disclosed. The apparatus includes an emission block configured to receive a vapor phase chemical species that is excited by chemical reaction in the emission block to provide an excited species that emits hot. The emission block has an interior portion having a surface. A coating is disposed over the surface and the coating reduces adsorption of the excited species onto the surface. | 1. An apparatus for receiving a chemical species, the apparatus comprising:
an emission block configured to receive a vapor phase chemical species that is excited by chemical reaction in the emission block to provide an excited species that emits light, the emission block having an interior portion having a surface; and a coating disposed over the surface, wherein the coating reduces adsorption of the excited species onto the surface. 2. An apparatus as claimed in claim 1, wherein the excited species comprises sulfur. 3. An apparatus as claimed in claim 1, wherein the excited species comprises nitrogen. 4. An apparatus as claimed in claim 1, wherein the excited species comprises phosphorus. 5. An apparatus as claimed in claim 1, wherein the coating comprises silicon. 6. An apparatus as claimed in claim 5, wherein the coating further comprises chemically modified silicon. 7. An apparatus as claimed in claim 6, wherein the chemically modified silicon comprises an organic material. 8. An apparatus as claimed in claim 1, wherein the coating comprises hydrogenated amorphous silicon. 9. An apparatus as claimed in claim 8, wherein the hydrogenated amorphous silicon is modified with an organic material. 10. An apparatus as claimed in claim 1, wherein the coating comprises a fluoropolymer. 11. An apparatus as claimed in claim 1, wherein the vapor phase species is received from a gas chromatograph (GC). 12. An apparatus as claimed in claim 1, further comprising a transfer line comprising a first end and a second end opposing the first end, wherein the vapor phase is received at the emission block from the second end. 13. An apparatus as claimed in claim 12, further comprising:
a block heater disposed around a first portion of the transfer line, the block heater comprising a heater configured to maintain the first portion of the transfer line at a first temperature range; and a body tube substantially surrounding a second portion of the transfer line, the body tube mechanically and thermally coupled to the emission block, wherein the emission block and the body tube are maintained at a second temperature range that is lower than the first temperature range, and the second portion of the transfer line is maintained at the first temperature range. 14. An apparatus as claimed in claim 13, wherein the body tube is brazed to the transfer line and to the emission block. 15. An apparatus as claimed in claim 13, wherein the heater is a first heater and the emission block comprises a second heater configured to maintain the emission block at the second temperature range. 16. An apparatus as claimed in claim 15, further comprising a controller configured to maintain the second heater so that the emission block is maintained at the second temperature range. 17. An apparatus as claimed in claim 13, further comprising a jet housing disposed around the second portion of the transfer line, wherein the jet housing is brazed to the transfer line. 18. An apparatus as claimed in claim 17, wherein the body tube is brazed to the emission block at a first end of the body tube, and the body tube is brazed to the jet housing at a second end of the body tube. 19. An apparatus as claimed in claim 1, wherein the apparatus is a flame photometric detector. 20. An apparatus as claimed in claim 1, wherein the apparatus is a chemiluminescence detector. | An apparatus for receiving a chemical species is disclosed. The apparatus includes an emission block configured to receive a vapor phase chemical species that is excited by chemical reaction in the emission block to provide an excited species that emits hot. The emission block has an interior portion having a surface. A coating is disposed over the surface and the coating reduces adsorption of the excited species onto the surface.1. An apparatus for receiving a chemical species, the apparatus comprising:
an emission block configured to receive a vapor phase chemical species that is excited by chemical reaction in the emission block to provide an excited species that emits light, the emission block having an interior portion having a surface; and a coating disposed over the surface, wherein the coating reduces adsorption of the excited species onto the surface. 2. An apparatus as claimed in claim 1, wherein the excited species comprises sulfur. 3. An apparatus as claimed in claim 1, wherein the excited species comprises nitrogen. 4. An apparatus as claimed in claim 1, wherein the excited species comprises phosphorus. 5. An apparatus as claimed in claim 1, wherein the coating comprises silicon. 6. An apparatus as claimed in claim 5, wherein the coating further comprises chemically modified silicon. 7. An apparatus as claimed in claim 6, wherein the chemically modified silicon comprises an organic material. 8. An apparatus as claimed in claim 1, wherein the coating comprises hydrogenated amorphous silicon. 9. An apparatus as claimed in claim 8, wherein the hydrogenated amorphous silicon is modified with an organic material. 10. An apparatus as claimed in claim 1, wherein the coating comprises a fluoropolymer. 11. An apparatus as claimed in claim 1, wherein the vapor phase species is received from a gas chromatograph (GC). 12. An apparatus as claimed in claim 1, further comprising a transfer line comprising a first end and a second end opposing the first end, wherein the vapor phase is received at the emission block from the second end. 13. An apparatus as claimed in claim 12, further comprising:
a block heater disposed around a first portion of the transfer line, the block heater comprising a heater configured to maintain the first portion of the transfer line at a first temperature range; and a body tube substantially surrounding a second portion of the transfer line, the body tube mechanically and thermally coupled to the emission block, wherein the emission block and the body tube are maintained at a second temperature range that is lower than the first temperature range, and the second portion of the transfer line is maintained at the first temperature range. 14. An apparatus as claimed in claim 13, wherein the body tube is brazed to the transfer line and to the emission block. 15. An apparatus as claimed in claim 13, wherein the heater is a first heater and the emission block comprises a second heater configured to maintain the emission block at the second temperature range. 16. An apparatus as claimed in claim 15, further comprising a controller configured to maintain the second heater so that the emission block is maintained at the second temperature range. 17. An apparatus as claimed in claim 13, further comprising a jet housing disposed around the second portion of the transfer line, wherein the jet housing is brazed to the transfer line. 18. An apparatus as claimed in claim 17, wherein the body tube is brazed to the emission block at a first end of the body tube, and the body tube is brazed to the jet housing at a second end of the body tube. 19. An apparatus as claimed in claim 1, wherein the apparatus is a flame photometric detector. 20. An apparatus as claimed in claim 1, wherein the apparatus is a chemiluminescence detector. | 1,700 |
3,481 | 14,243,959 | 1,786 | The present disclosure is generally directed to a primer saturated carrier medium assembly including a carrier medium having a front face and an opposing rear face, a primer saturating the carrier medium between the front face and the opposing rear face, and removable film impenetrable to the primer covering opposite faces of the carrier medium. A method of applying primer to a surface includes applying a face of a primer saturated carrier medium to contact a surface, and curing the primer saturated carrier medium on the surface. A structure includes a primer saturated medium including a carrier medium having a front face and an opposing rear face, and a primer saturating the carrier medium between the front face and the opposing rear face. The structure further includes a surface adhered to the primer on one face of the primer saturated medium. | 1. A primer saturated carrier medium assembly comprising:
a carrier medium having a first face and an opposing second face; a primer substantially saturating the carrier medium between the first face and the opposing second face; and removable film substantially impenetrable to the primer covering both the first face and the opposing second face of the primer saturated carrier medium. 2. The primer saturated carrier medium assembly of claim 1, wherein the carrier medium comprises a non-woven mat including at least one of nylon, polyester or glass. 3. The primer saturated carrier medium assembly of claim 1, wherein the carrier medium further comprises carbon fibers. 4. The primer of claim 3, wherein the carbon fibers are metallized with at least one of Ni, Cu/Ni, Ag, Au or Ru. 5. The primer carrier saturated medium of claim 1, wherein the primer comprises a chromate-based corrosion resistant primer. 6. The primer carrier saturated medium of claim 1, wherein the removable film comprises one of nylon, polyester or glass. 7. A method of applying primer to a surface comprising:
removing a first film impenetrable to a primer on an opposing second face of a primer saturated carrier medium assembly including
a carrier medium having a first face and the opposing second face,
a primer saturating the carrier medium between the first face and the opposing second face, and
at least one film impenetrable to the primer covering the first face of the carrier medium;
applying the opposing second face of the primer saturated carrier medium assembly to contact a surface; and curing the primer saturated carrier medium on the surface. 8. The method of claim 7, wherein the primer saturated carrier medium comprises a non-woven mat comprising at least one of nylon, polyester or glass. 9. The method of claim 7, wherein the primer saturated carrier medium further comprises carbon fibers. 10. The method of claim 7, further comprising:
removing an opposing second removable film from the primer saturated carrier medium after curing the primer saturated carrier medium on the surface. 11. The method of claim 7, wherein curing comprises one of:
heating the primer saturated carrier medium to adhere the primer to the surface; treating the primer saturated carrier medium with infrared (IR) energy to adhere the primer to the surface; treating the primer saturated carrier medium with ultraviolet (UV) energy to adhere the primer to the surface; or exposing the primer saturated carrier medium to ambient temperature air to adhere the primer to the surface. 12. The method of claim 7, wherein the primer may be a chromate-based corrosion resistant primer. 13. A structure comprising:
a primer saturated medium including
a carrier medium having a first face and an opposing second face, and
a primer substantially saturating the carrier medium between the first face and the opposing second face,
the primer saturated medium capable of adhering to a surface at one face of the primer saturated medium. 14. The structure of claim 13, wherein the primer may be a chromate-based corrosion resistant primer. 15. The structure of claim 13, wherein the carrier medium comprises a non-woven mat including at least one of nylon, polyester, or glass. 16. The structure of claim 13, further comprising an adhesive adhered to the primer saturated medium on an opposing face, and a repair patch applied over the adhesive. 17. The structure of claim 13, wherein the surface further includes a carbon fiber structure. 18. The structure of claim 17, wherein the carrier medium further comprises carbon fibers. 19. The structure of claim 17, wherein the carrier medium further comprises carbon fibers metallized with at least one of Ni, Cu/Ni, Ag, Au or Ru. 20. An aircraft comprising the primer saturated carrier medium assembly of claim 1. | The present disclosure is generally directed to a primer saturated carrier medium assembly including a carrier medium having a front face and an opposing rear face, a primer saturating the carrier medium between the front face and the opposing rear face, and removable film impenetrable to the primer covering opposite faces of the carrier medium. A method of applying primer to a surface includes applying a face of a primer saturated carrier medium to contact a surface, and curing the primer saturated carrier medium on the surface. A structure includes a primer saturated medium including a carrier medium having a front face and an opposing rear face, and a primer saturating the carrier medium between the front face and the opposing rear face. The structure further includes a surface adhered to the primer on one face of the primer saturated medium.1. A primer saturated carrier medium assembly comprising:
a carrier medium having a first face and an opposing second face; a primer substantially saturating the carrier medium between the first face and the opposing second face; and removable film substantially impenetrable to the primer covering both the first face and the opposing second face of the primer saturated carrier medium. 2. The primer saturated carrier medium assembly of claim 1, wherein the carrier medium comprises a non-woven mat including at least one of nylon, polyester or glass. 3. The primer saturated carrier medium assembly of claim 1, wherein the carrier medium further comprises carbon fibers. 4. The primer of claim 3, wherein the carbon fibers are metallized with at least one of Ni, Cu/Ni, Ag, Au or Ru. 5. The primer carrier saturated medium of claim 1, wherein the primer comprises a chromate-based corrosion resistant primer. 6. The primer carrier saturated medium of claim 1, wherein the removable film comprises one of nylon, polyester or glass. 7. A method of applying primer to a surface comprising:
removing a first film impenetrable to a primer on an opposing second face of a primer saturated carrier medium assembly including
a carrier medium having a first face and the opposing second face,
a primer saturating the carrier medium between the first face and the opposing second face, and
at least one film impenetrable to the primer covering the first face of the carrier medium;
applying the opposing second face of the primer saturated carrier medium assembly to contact a surface; and curing the primer saturated carrier medium on the surface. 8. The method of claim 7, wherein the primer saturated carrier medium comprises a non-woven mat comprising at least one of nylon, polyester or glass. 9. The method of claim 7, wherein the primer saturated carrier medium further comprises carbon fibers. 10. The method of claim 7, further comprising:
removing an opposing second removable film from the primer saturated carrier medium after curing the primer saturated carrier medium on the surface. 11. The method of claim 7, wherein curing comprises one of:
heating the primer saturated carrier medium to adhere the primer to the surface; treating the primer saturated carrier medium with infrared (IR) energy to adhere the primer to the surface; treating the primer saturated carrier medium with ultraviolet (UV) energy to adhere the primer to the surface; or exposing the primer saturated carrier medium to ambient temperature air to adhere the primer to the surface. 12. The method of claim 7, wherein the primer may be a chromate-based corrosion resistant primer. 13. A structure comprising:
a primer saturated medium including
a carrier medium having a first face and an opposing second face, and
a primer substantially saturating the carrier medium between the first face and the opposing second face,
the primer saturated medium capable of adhering to a surface at one face of the primer saturated medium. 14. The structure of claim 13, wherein the primer may be a chromate-based corrosion resistant primer. 15. The structure of claim 13, wherein the carrier medium comprises a non-woven mat including at least one of nylon, polyester, or glass. 16. The structure of claim 13, further comprising an adhesive adhered to the primer saturated medium on an opposing face, and a repair patch applied over the adhesive. 17. The structure of claim 13, wherein the surface further includes a carbon fiber structure. 18. The structure of claim 17, wherein the carrier medium further comprises carbon fibers. 19. The structure of claim 17, wherein the carrier medium further comprises carbon fibers metallized with at least one of Ni, Cu/Ni, Ag, Au or Ru. 20. An aircraft comprising the primer saturated carrier medium assembly of claim 1. | 1,700 |
3,482 | 14,787,840 | 1,793 | A food composition comprises starch and sodium and enhances saltiness perception while maintaining good taste and texture. The sodium is added to the composition after a food polymer transition in which an insoluble starch gel is formed, and the food polymer has reduced affinity for sodium after the transition. As a result, the sodium is more in the aqueous phase of the composition rather than in the polymer phase. Distribution of the sodium more in the aqueous phase causes the sodium to be more available for saltiness perception when the composition is consumed relative to compositions in which the sodium is mainly in the polymer phase. Potassium chloride can be added before the food polymer transition and entrapped or bound by the food polymer to decrease the sodium affinity of the food polymer and also mask the off taste associated with high levels of potassium chloride. | 1. A method of producing a food composition, the method comprising the steps of:
cooling gelatinized starch to form an insoluble starch gel; and adding sodium chloride to at least one of the gelatinized starch or the insoluble starch gel to form the food composition. 2. A method of producing a food composition, the method comprising the steps of:
cooking starch to form a gelatinized starch; cooling the gelatinized starch to form an insoluble starch gel; and adding sodium chloride to at least one of the gelatinized starch or the insoluble starch gel to form the food composition. 3. The method according to claim 1 or 2, further comprising:
cooking starch to form the gelatinized starch; and
adding positively charged metal ions at a time selected from the group consisting of before the cooking, during the cooking, and a combination thereof. 4. The method according to claim 3, wherein the positively charged metal ions are non-sodium metal ions. 5. The method according to claim 3, wherein the positively charged metal ions are potassium chloride. 6. The method according to claim 1, wherein at least a portion of the sodium chloride is added after the cooking. 7. The method according to claim 1, wherein at least a portion of the sodium chloride is added during the cooling while the insoluble starch gel is forming. 8. The method according to claim 1, wherein at least a portion of the sodium chloride is added after the cooling when the insoluble starch gel has been completely formed. 9. The method according to claim 1, wherein the sodium chloride is added to the gelatinized starch with a sodium distribution enhancer selected from the group consisting of an acidifying component, an alkalinizing component, a gum component, a sugar and combinations thereof. 10. A food composition comprising a starch and sodium chloride, the starch is at least partially in a form of an insoluble starch gel, and a portion of the sodium chloride entrapped by or bound to the insoluble starch gel is less than a portion of the sodium chloride not entrapped by or bound to the insoluble starch gel. 11. The food composition according to claim 10, wherein the food composition is selected from the group consisting of a water-based sauce, a dairy-based sauce, a tomato-based sauce, and combinations thereof. 12. The food composition according to claim 10, comprising positively charged metal ions in a position selected from the group consisting of entrapped by the insoluble starch gel, bound to the insoluble starch gel, and a combination thereof. 13. A method for reducing sodium in a food product comprising:
cooling gelatinized starch to form an insoluble starch gel; and adding sodium chloride to at least one of the gelatinized starch or the insoluble starch gel to form the food composition, the food product comprising 0.30 wt % to 3.50 wt % of sodium chloride. 14. The method according to claim 13, wherein the insoluble starch gel at least partially blocks migration of the sodium chloride into the starch. 15. A method for increasing potassium in a food product comprising:
cooking starch in the presence of 0.25 wt % to 3.2 wt % of potassium chloride to form gelatinized starch; cooling the gelatinized starch to form an insoluble starch gel; and adding sodium chloride to at least one of the gelatinized starch or the insoluble starch gel to form the food product, the food product comprising 0.30 wt % to 2.50 wt % of sodium chloride. 16. The method according to claim 15, wherein the insoluble starch gel at least partially blocks migration of the potassium chloride from the starch. 17. A food composition obtainable from the method according to claim 1. 18. The method according to claim 2 comprising:
cooking starch to form the gelatinized starch; and
adding positively charged metal ions at a time selected from the group consisting of before the cooking, during the cooking, and a combination thereof. 19. The method according to claim 18, wherein the positively charged metal ions are non-sodium metal ions. 20. The method according to claim 18, wherein the positively charged metal ions are potassium chloride. 21. The method according to claim 2, wherein at least a portion of the sodium chloride is added after the cooking. 22. The method according to claim 2, wherein at least a portion of the sodium chloride is added during the cooling while the insoluble starch gel is forming. 23. The method according to claim 2, wherein at least a portion of the sodium chloride is added after the cooling when the insoluble starch gel has been completely formed. 24. The method according to claim 2, wherein the sodium chloride is added to the gelatinized starch with a sodium distribution enhancer selected from the group consisting of an acidifying component, an alkalinizing component, a gum component, a sugar and combinations thereof. 25. A food composition obtainable from the method according to claim 2. 26. A food composition obtainable from the method according to claim 13. 27. A food composition obtainable from the method according to claim 15. | A food composition comprises starch and sodium and enhances saltiness perception while maintaining good taste and texture. The sodium is added to the composition after a food polymer transition in which an insoluble starch gel is formed, and the food polymer has reduced affinity for sodium after the transition. As a result, the sodium is more in the aqueous phase of the composition rather than in the polymer phase. Distribution of the sodium more in the aqueous phase causes the sodium to be more available for saltiness perception when the composition is consumed relative to compositions in which the sodium is mainly in the polymer phase. Potassium chloride can be added before the food polymer transition and entrapped or bound by the food polymer to decrease the sodium affinity of the food polymer and also mask the off taste associated with high levels of potassium chloride.1. A method of producing a food composition, the method comprising the steps of:
cooling gelatinized starch to form an insoluble starch gel; and adding sodium chloride to at least one of the gelatinized starch or the insoluble starch gel to form the food composition. 2. A method of producing a food composition, the method comprising the steps of:
cooking starch to form a gelatinized starch; cooling the gelatinized starch to form an insoluble starch gel; and adding sodium chloride to at least one of the gelatinized starch or the insoluble starch gel to form the food composition. 3. The method according to claim 1 or 2, further comprising:
cooking starch to form the gelatinized starch; and
adding positively charged metal ions at a time selected from the group consisting of before the cooking, during the cooking, and a combination thereof. 4. The method according to claim 3, wherein the positively charged metal ions are non-sodium metal ions. 5. The method according to claim 3, wherein the positively charged metal ions are potassium chloride. 6. The method according to claim 1, wherein at least a portion of the sodium chloride is added after the cooking. 7. The method according to claim 1, wherein at least a portion of the sodium chloride is added during the cooling while the insoluble starch gel is forming. 8. The method according to claim 1, wherein at least a portion of the sodium chloride is added after the cooling when the insoluble starch gel has been completely formed. 9. The method according to claim 1, wherein the sodium chloride is added to the gelatinized starch with a sodium distribution enhancer selected from the group consisting of an acidifying component, an alkalinizing component, a gum component, a sugar and combinations thereof. 10. A food composition comprising a starch and sodium chloride, the starch is at least partially in a form of an insoluble starch gel, and a portion of the sodium chloride entrapped by or bound to the insoluble starch gel is less than a portion of the sodium chloride not entrapped by or bound to the insoluble starch gel. 11. The food composition according to claim 10, wherein the food composition is selected from the group consisting of a water-based sauce, a dairy-based sauce, a tomato-based sauce, and combinations thereof. 12. The food composition according to claim 10, comprising positively charged metal ions in a position selected from the group consisting of entrapped by the insoluble starch gel, bound to the insoluble starch gel, and a combination thereof. 13. A method for reducing sodium in a food product comprising:
cooling gelatinized starch to form an insoluble starch gel; and adding sodium chloride to at least one of the gelatinized starch or the insoluble starch gel to form the food composition, the food product comprising 0.30 wt % to 3.50 wt % of sodium chloride. 14. The method according to claim 13, wherein the insoluble starch gel at least partially blocks migration of the sodium chloride into the starch. 15. A method for increasing potassium in a food product comprising:
cooking starch in the presence of 0.25 wt % to 3.2 wt % of potassium chloride to form gelatinized starch; cooling the gelatinized starch to form an insoluble starch gel; and adding sodium chloride to at least one of the gelatinized starch or the insoluble starch gel to form the food product, the food product comprising 0.30 wt % to 2.50 wt % of sodium chloride. 16. The method according to claim 15, wherein the insoluble starch gel at least partially blocks migration of the potassium chloride from the starch. 17. A food composition obtainable from the method according to claim 1. 18. The method according to claim 2 comprising:
cooking starch to form the gelatinized starch; and
adding positively charged metal ions at a time selected from the group consisting of before the cooking, during the cooking, and a combination thereof. 19. The method according to claim 18, wherein the positively charged metal ions are non-sodium metal ions. 20. The method according to claim 18, wherein the positively charged metal ions are potassium chloride. 21. The method according to claim 2, wherein at least a portion of the sodium chloride is added after the cooking. 22. The method according to claim 2, wherein at least a portion of the sodium chloride is added during the cooling while the insoluble starch gel is forming. 23. The method according to claim 2, wherein at least a portion of the sodium chloride is added after the cooling when the insoluble starch gel has been completely formed. 24. The method according to claim 2, wherein the sodium chloride is added to the gelatinized starch with a sodium distribution enhancer selected from the group consisting of an acidifying component, an alkalinizing component, a gum component, a sugar and combinations thereof. 25. A food composition obtainable from the method according to claim 2. 26. A food composition obtainable from the method according to claim 13. 27. A food composition obtainable from the method according to claim 15. | 1,700 |
3,483 | 14,960,938 | 1,741 | In a method of forming a conical shape on a glass rod including an effective portion and an ineffective portion adjoining the effective portion to form a conical shape in the effective portion by simultaneously heating a boundary and the vicinity of the boundary between the effective portion and the ineffective portion and pulling an end of the ineffective portion, the temperature of a heater is raised and a heating target on the glass rod is simultaneously moved from the ineffective portion to the boundary. | 1. A method of forming a conical shape on a glass rod including an effective portion and an ineffective portion adjoining the effective portion, a conical shape being formed in the effective portion by simultaneously heating a boundary and a vicinity of the boundary between the effective portion and the ineffective portion and pulling an end of the ineffective portion, the method comprising:
simultaneously raising temperature of the heater and moving a heating target on the glass rod from the ineffective portion side to the boundary. 2. The method of forming a conical shape on a glass rod according to claim 1, wherein the simultaneous raj sing of the temperature of the heater and moving of the heating target start from a portion in the ineffective portion. 3. The method of forming a conical shape on a glass rod according to claim 1, wherein the moving starts after the temperature of the heater has been raised to a predetermined heating temperature. 4. The method of forming a conical shape on a glass rod according to claim 1, wherein the heating temperature of the heater is 1700° C. or above when the heating target has come to the boundary. 5. A glass rod including a conical shape formed by the method of forming a conical shape on a glass rod according to claim 1. | In a method of forming a conical shape on a glass rod including an effective portion and an ineffective portion adjoining the effective portion to form a conical shape in the effective portion by simultaneously heating a boundary and the vicinity of the boundary between the effective portion and the ineffective portion and pulling an end of the ineffective portion, the temperature of a heater is raised and a heating target on the glass rod is simultaneously moved from the ineffective portion to the boundary.1. A method of forming a conical shape on a glass rod including an effective portion and an ineffective portion adjoining the effective portion, a conical shape being formed in the effective portion by simultaneously heating a boundary and a vicinity of the boundary between the effective portion and the ineffective portion and pulling an end of the ineffective portion, the method comprising:
simultaneously raising temperature of the heater and moving a heating target on the glass rod from the ineffective portion side to the boundary. 2. The method of forming a conical shape on a glass rod according to claim 1, wherein the simultaneous raj sing of the temperature of the heater and moving of the heating target start from a portion in the ineffective portion. 3. The method of forming a conical shape on a glass rod according to claim 1, wherein the moving starts after the temperature of the heater has been raised to a predetermined heating temperature. 4. The method of forming a conical shape on a glass rod according to claim 1, wherein the heating temperature of the heater is 1700° C. or above when the heating target has come to the boundary. 5. A glass rod including a conical shape formed by the method of forming a conical shape on a glass rod according to claim 1. | 1,700 |
3,484 | 13,497,009 | 1,784 | A multi layered aluminum alloy brazing sheet including a core material, an intermediate layer on at least one side of the core material, the intermediate layer comprising an Al—Si braze alloy, and a thin covering layer on top of the intermediate layer, The core material and the covering layer have a higher melting temperature than the Al—Si braze alloy. The covering layer includes Bi 0.01 to 1.0 wt-%, Mg≦0.01 wt-%, Mn≦1.0 wt-%, Cu≦1.2 wt-%, Fe≦1.0 wt-%, Si≦4.0 wt-%, Ti≦0.1 wt-%, Zr, Cr, V and/or Sc in total ≦0.2%, and unavoidable impurities each in amounts less than 0.05 wt-%, and a total impurity content of less than 0.2 wt-%, the balance including aluminium. A heat exchanger including the alloy brazing sheet. | 1-11. (canceled) 12. A multi layered aluminum alloy brazing sheet, comprising:
a core material; an intermediate layer on at least one side of the core material, the intermediate layer comprising an Al—Si braze alloy; and a thin covering layer on top of the intermediate layer, wherein the core material and the covering layer has a higher melting temperature than the Al—Si braze alloy, wherein the covering layer comprising
Bi 0.01 to 1.0 wt-%,
Mg ≦0.05 wt-%,
Mn ≦1.0 wt-%,
Cu ≦1.2 wt-%,
Fe ≦1.0 wt-%,
Si ≦4.0 wt-%,
Ti ≦0.1 wt-%,
Zn ≦6 wt-%, Sn ≦0.1 wt-%, In ≦0.1 wt-%, and
unavoidable impurities each in amounts less than 0.05 wt-%, and
a total impurity content of less than 0.2 wt-%,
and a balance of aluminum. 13. The aluminum alloy brazing sheet according to claim 12, wherein the covering layer comprises Mg ≦0.01 wt-%. 14. The aluminum alloy brazing sheet according to claim 12, wherein the covering layer comprises Mg 0%. 15. The aluminum alloy brazing sheet according to claim 12, wherein the covering layer comprises Si ≦2.0-wt %. 16. The aluminum alloy brazing sheet according to claim 12, wherein the covering layer comprises Bi in an amount of 0.05 to 0.7 wt-%. 17. The aluminum alloy brazing sheet according to claim 12, wherein the covering layer comprises Bi in an amount of 0.07 to 0.5 wt-%. 18. The aluminum alloy brazing sheet according to claim 12, wherein the thin covering layer comprises Si in an amount of ≦1.9 wt-%. 19. The aluminum alloy brazing sheet according to claim 12, wherein the thin covering layer comprises Si in an amount of ≦1.65 wt %. 20. The aluminum alloy brazing sheet according to claim 12, wherein the thin covering layer comprises Si in an amount of ≦1.4 wt-%. 21. The aluminum alloy brazing sheet according to claim 12, wherein the thin covering layer comprises Si in an amount of ≦0.9 wt-%. 22. The aluminum alloy brazing sheet according to claim 12, wherein the Al—Si braze alloy does not contain Bi. 23. The aluminum alloy brazing sheet according to claim 12, wherein the intermediate layer and the covering layer are present on both sides of the core. 24. The aluminum brazing sheet according to claim 12, wherein the covering layer has a thickness between 0.4 and 160 μm. 25. The aluminum alloy brazing sheet according to claim 12, wherein a total thickness of the aluminum brazing sheet is between 0.04 and 4 mm. 26. The aluminum alloy brazing sheet according to claim 12, wherein a thickness of the thin covering layer relative to the intermediate layer is between 1% and 40%. 27. The aluminum alloy brazing sheet according to claim 12, wherein a thickness of the thin covering layer relative to the intermediate layer is between 1 and 30%. 28. The aluminum alloy brazing sheet according to claim 12, wherein a thickness of the thin covering layer relative to the intermediate layer is between 10 and 30%. 29. The aluminum alloy brazing sheet according to claim 12, wherein a thickness of the intermediate layer relative to a thickness of the aluminum alloy brazing sheet is 3 to 30%. 30. The aluminum alloy brazing sheet according to claim 12, wherein the Al—Si braze alloy comprises
Si 5 to 14%,
Mg 0.01 to 5%,
Bi ≦1.5%,
Fe ≦0.8%
Cu ≦0.3%,
Mn ≦0.15%,
Zn ≦4% Zn,
Sn ≦0.1 wt-%
In ≦0.1 wt-%
Sr ≦0.05 wt-%, and
unavoidable impurities each in amounts less than 0.05% and a total impurity content of less than 0.2%, and balance aluminium. 31. The aluminum alloy brazing sheet according to claim 30, wherein the Al—Si braze alloy comprises Si 7 to 13%. 32. The aluminum alloy brazing sheet according to claim 30, wherein the Al—Si braze alloy comprises Si 10-12.5%. 33. The aluminum alloy brazing sheet according to claim 30, wherein the Al—Si braze alloy comprises Mg 0.05 to 2.5%. 34. The aluminum alloy brazing sheet according to claim 30, wherein the Al—Si braze alloy comprises Mg 0.1 to 2.0%. 35. The aluminum alloy brazing sheet according to claim 30, wherein the Al—Si braze alloy comprises Bi 0.05 to 0.5%. 36. The aluminum alloy brazing sheet according to claim 30, wherein the Al—Si braze alloy comprises Bi 0.07 to 0.3%. 37. The aluminum alloy brazing sheet according to claim 12, wherein the core comprises
Mn 0.5-2.0%, Cu ≦1.2%, Fe ≦1.0%, Si ≦1.0%, Ti ≦0.2%, Mg ≦2.5%, Zr, Cr, V and/or Sc in total ≦0.2%, and unavoidable impurities each in amounts less than 0.05% and a total impurity content of less than 0.2%, and a balance of aluminum. 38. The aluminum alloy brazing sheet according to claim 37, wherein the core comprises Mg 0.03-2.0%. 39. A heat exchanger, comprising:
an aluminum alloy brazing sheet comprising
a core material;
an intermediate layer on at least one side of the core material, the intermediate layer comprising an Al—Si braze alloy; and
a thin covering layer on top of the intermediate layer,
wherein the said core material and the covering layer has a higher melting temperature than the Al—Si braze alloy,
wherein the covering layer comprising
Bi 0.01 to 1.0 wt-%, Mg ≦0.05 wt-%, Mn ≦1.0 wt-%, Cu ≦1.2 wt-%, Fe ≦1.0 wt-%, Si ≦4.0 wt-%, Ti ≦0.1 wt-%, Zn ≦6 wt-%, Sn ≦0.1 wt-%, In ≦0.1 wt-%, and unavoidable impurities each in amounts less than 0.05 wt-%, and a total impurity content of less than 0.2 wt-%, and a balance of aluminum. | A multi layered aluminum alloy brazing sheet including a core material, an intermediate layer on at least one side of the core material, the intermediate layer comprising an Al—Si braze alloy, and a thin covering layer on top of the intermediate layer, The core material and the covering layer have a higher melting temperature than the Al—Si braze alloy. The covering layer includes Bi 0.01 to 1.0 wt-%, Mg≦0.01 wt-%, Mn≦1.0 wt-%, Cu≦1.2 wt-%, Fe≦1.0 wt-%, Si≦4.0 wt-%, Ti≦0.1 wt-%, Zr, Cr, V and/or Sc in total ≦0.2%, and unavoidable impurities each in amounts less than 0.05 wt-%, and a total impurity content of less than 0.2 wt-%, the balance including aluminium. A heat exchanger including the alloy brazing sheet.1-11. (canceled) 12. A multi layered aluminum alloy brazing sheet, comprising:
a core material; an intermediate layer on at least one side of the core material, the intermediate layer comprising an Al—Si braze alloy; and a thin covering layer on top of the intermediate layer, wherein the core material and the covering layer has a higher melting temperature than the Al—Si braze alloy, wherein the covering layer comprising
Bi 0.01 to 1.0 wt-%,
Mg ≦0.05 wt-%,
Mn ≦1.0 wt-%,
Cu ≦1.2 wt-%,
Fe ≦1.0 wt-%,
Si ≦4.0 wt-%,
Ti ≦0.1 wt-%,
Zn ≦6 wt-%, Sn ≦0.1 wt-%, In ≦0.1 wt-%, and
unavoidable impurities each in amounts less than 0.05 wt-%, and
a total impurity content of less than 0.2 wt-%,
and a balance of aluminum. 13. The aluminum alloy brazing sheet according to claim 12, wherein the covering layer comprises Mg ≦0.01 wt-%. 14. The aluminum alloy brazing sheet according to claim 12, wherein the covering layer comprises Mg 0%. 15. The aluminum alloy brazing sheet according to claim 12, wherein the covering layer comprises Si ≦2.0-wt %. 16. The aluminum alloy brazing sheet according to claim 12, wherein the covering layer comprises Bi in an amount of 0.05 to 0.7 wt-%. 17. The aluminum alloy brazing sheet according to claim 12, wherein the covering layer comprises Bi in an amount of 0.07 to 0.5 wt-%. 18. The aluminum alloy brazing sheet according to claim 12, wherein the thin covering layer comprises Si in an amount of ≦1.9 wt-%. 19. The aluminum alloy brazing sheet according to claim 12, wherein the thin covering layer comprises Si in an amount of ≦1.65 wt %. 20. The aluminum alloy brazing sheet according to claim 12, wherein the thin covering layer comprises Si in an amount of ≦1.4 wt-%. 21. The aluminum alloy brazing sheet according to claim 12, wherein the thin covering layer comprises Si in an amount of ≦0.9 wt-%. 22. The aluminum alloy brazing sheet according to claim 12, wherein the Al—Si braze alloy does not contain Bi. 23. The aluminum alloy brazing sheet according to claim 12, wherein the intermediate layer and the covering layer are present on both sides of the core. 24. The aluminum brazing sheet according to claim 12, wherein the covering layer has a thickness between 0.4 and 160 μm. 25. The aluminum alloy brazing sheet according to claim 12, wherein a total thickness of the aluminum brazing sheet is between 0.04 and 4 mm. 26. The aluminum alloy brazing sheet according to claim 12, wherein a thickness of the thin covering layer relative to the intermediate layer is between 1% and 40%. 27. The aluminum alloy brazing sheet according to claim 12, wherein a thickness of the thin covering layer relative to the intermediate layer is between 1 and 30%. 28. The aluminum alloy brazing sheet according to claim 12, wherein a thickness of the thin covering layer relative to the intermediate layer is between 10 and 30%. 29. The aluminum alloy brazing sheet according to claim 12, wherein a thickness of the intermediate layer relative to a thickness of the aluminum alloy brazing sheet is 3 to 30%. 30. The aluminum alloy brazing sheet according to claim 12, wherein the Al—Si braze alloy comprises
Si 5 to 14%,
Mg 0.01 to 5%,
Bi ≦1.5%,
Fe ≦0.8%
Cu ≦0.3%,
Mn ≦0.15%,
Zn ≦4% Zn,
Sn ≦0.1 wt-%
In ≦0.1 wt-%
Sr ≦0.05 wt-%, and
unavoidable impurities each in amounts less than 0.05% and a total impurity content of less than 0.2%, and balance aluminium. 31. The aluminum alloy brazing sheet according to claim 30, wherein the Al—Si braze alloy comprises Si 7 to 13%. 32. The aluminum alloy brazing sheet according to claim 30, wherein the Al—Si braze alloy comprises Si 10-12.5%. 33. The aluminum alloy brazing sheet according to claim 30, wherein the Al—Si braze alloy comprises Mg 0.05 to 2.5%. 34. The aluminum alloy brazing sheet according to claim 30, wherein the Al—Si braze alloy comprises Mg 0.1 to 2.0%. 35. The aluminum alloy brazing sheet according to claim 30, wherein the Al—Si braze alloy comprises Bi 0.05 to 0.5%. 36. The aluminum alloy brazing sheet according to claim 30, wherein the Al—Si braze alloy comprises Bi 0.07 to 0.3%. 37. The aluminum alloy brazing sheet according to claim 12, wherein the core comprises
Mn 0.5-2.0%, Cu ≦1.2%, Fe ≦1.0%, Si ≦1.0%, Ti ≦0.2%, Mg ≦2.5%, Zr, Cr, V and/or Sc in total ≦0.2%, and unavoidable impurities each in amounts less than 0.05% and a total impurity content of less than 0.2%, and a balance of aluminum. 38. The aluminum alloy brazing sheet according to claim 37, wherein the core comprises Mg 0.03-2.0%. 39. A heat exchanger, comprising:
an aluminum alloy brazing sheet comprising
a core material;
an intermediate layer on at least one side of the core material, the intermediate layer comprising an Al—Si braze alloy; and
a thin covering layer on top of the intermediate layer,
wherein the said core material and the covering layer has a higher melting temperature than the Al—Si braze alloy,
wherein the covering layer comprising
Bi 0.01 to 1.0 wt-%, Mg ≦0.05 wt-%, Mn ≦1.0 wt-%, Cu ≦1.2 wt-%, Fe ≦1.0 wt-%, Si ≦4.0 wt-%, Ti ≦0.1 wt-%, Zn ≦6 wt-%, Sn ≦0.1 wt-%, In ≦0.1 wt-%, and unavoidable impurities each in amounts less than 0.05 wt-%, and a total impurity content of less than 0.2 wt-%, and a balance of aluminum. | 1,700 |
3,485 | 14,366,611 | 1,772 | A process for dehydrogenating alkane or alkylaromatic compounds comprising contacting the given compound and a dehydrogenation catalyst in a fluidized bed. The dehydrogenation catalyst is prepared from an at least partially deactivated platinum/gallium catalyst on an alumina-based support that is reconstituted by impregnating it with a platinum salt solution, then calcining it at a temperature from 400° C. to 1000° C., under conditions such that it has a platinum content ranging from 1 to 500 ppm, based on weight of catalyst; a gallium content ranging from 0.2 to 2.0 wt %; and a platinum to gallium ratio ranging from 1:20,000 to 1:4. It also has a Pt retention that is equal to or greater than that of a fresh catalyst being used in a same or similar catalytic process. | 1. A process for dehydrogenating alkane or alkylaromatic compounds comprising
contacting, in a fluidized bed, an alkane compound or an alkylaromatic compound and a reconstituted dehydrogenation catalyst, such reconstituted dehydrogenation catalyst having been prepared by (a) obtaining a dehydrogenation catalyst comprising platinum and gallium on an alumina-based support, the dehydrogenation catalyst having been previously fresh but having become at least partially deactivated; (b) impregnating the at least partially deactivated dehydrogenation catalyst with a platinum salt solution to form an impregnated dehydrogenation catalyst; and (c) calcining the impregnated dehydrogenation catalyst at a temperature ranging from 400° C. to 1000° C.; (b) and (c) being carried out under conditions suitable to form a reconstituted dehydrogenation catalyst having (i) a platinum content ranging from 1 part per million, based on weight of catalyst, to 500 parts per million, based on weight of catalyst; (ii) a gallium content ranging from 0.2 wt % to 2.0 wt %; and (iii) a ratio of platinum to gallium ranging from 1:20,000 to 1:4; wherein the reconstituted dehydrogenation catalyst further exhibits a platinum retention greater than or equal to the platinum retention of a fresh dehydrogenation catalyst when each is used in the same or another, otherwise identical dehydrogenation process. 2. The process of claim 1, wherein the platinum content of the reconstituted dehydrogenation catalyst ranges from 40 parts per million, based on weight of catalyst, to 400 parts per million, based on weight of catalyst, and the ratio of platinum to gallium content ranges from 1:500 to 1:5. 3. The process of claim 2, wherein the platinum content of the reconstituted dehydrogenation catalyst ranges from 150 parts per million, based on weight of catalyst, to 300 parts per million, based on weight of catalyst, and the ratio of platinum to gallium content ranges from 3:400 to 3:80. 4. The process of claim 1, wherein the reconstituted dehydrogenation catalyst exhibits a propane dehydrogenation activity that is at least 2% absolute propane conversion greater than that exhibited by the at least partially deactivated catalyst. 5. The process of claim 1, further comprising the step of drying the impregnated dehydrogenation catalyst at a temperature ranging from 50° C. to 150° C. prior to calcining it. 6. A dehydrogenation catalyst composition comprising
a reconstituted platinum/gallium catalyst on an alumina-based support, the reconstituted platinum/gallium catalyst having been prepared by a process comprising (a) obtaining a dehydrogenation catalyst comprising platinum and gallium on an alumina-based support, the dehydrogenation catalyst having been previously fresh but having become at least partially deactivated; (b) impregnating the at least partially deactivated dehydrogenation catalyst with a platinum salt solution to form an impregnated dehydrogenation catalyst; and (c) calcining the impregnated dehydrogenation catalyst at a temperature ranging from 400° C. to 1000° C.; (b) and (c) being carried out under conditions suitable to form a reconstituted dehydrogenation catalyst having (i) a platinum content ranging from 1 part per million, based on weight of catalyst, to 500 parts per million, based on weight of catalyst; (ii) a gallium content ranging from 0.2 wt % to 2.0 wt %; and (iii) a ratio of platinum to gallium ranging from 1:20,000 to 1:4; wherein the reconstituted dehydrogenation catalyst further exhibits having a platinum retention greater than or equal to the platinum retention of a fresh dehydrogenation catalyst when each is used in the same or another, otherwise identical dehydrogenation process. 7. A process to prepare a catalyst comprising
(a) obtaining a dehydrogenation catalyst comprising platinum and gallium on an alumina-based support, the dehydrogenation catalyst having been previously fresh but having become at least partially deactivated; (b) impregnating the at least partially deactivated dehydrogenation catalyst with a platinum salt solution to form an impregnated dehydrogenation catalyst; and (c) calcining the impregnated dehydrogenation catalyst at a temperature ranging from 400° C. to 1000° C.; (b) and (c) being carried out under conditions suitable to form a reconstituted dehydrogenation catalyst having (i) a platinum content ranging from 1 part per million, based on weight of catalyst, to 500 parts per million, based on weight of catalyst; (ii) a gallium content ranging from 0.2 wt % to 2.0 wt %; and (iii) a ratio of platinum to gallium ranging from 1:20,000 to 1:4; wherein the reconstituted dehydrogenation catalyst further exhibits a platinum retention greater than or equal to the platinum retention of a fresh dehydrogenation catalyst when each is used in the same or another, otherwise identical dehydrogenation process. 8. The process of claim 7, further comprising a step, between (b) and (c), of drying the impregnated dehydrogenation catalyst at a temperature ranging from 50° C. to 150° C. | A process for dehydrogenating alkane or alkylaromatic compounds comprising contacting the given compound and a dehydrogenation catalyst in a fluidized bed. The dehydrogenation catalyst is prepared from an at least partially deactivated platinum/gallium catalyst on an alumina-based support that is reconstituted by impregnating it with a platinum salt solution, then calcining it at a temperature from 400° C. to 1000° C., under conditions such that it has a platinum content ranging from 1 to 500 ppm, based on weight of catalyst; a gallium content ranging from 0.2 to 2.0 wt %; and a platinum to gallium ratio ranging from 1:20,000 to 1:4. It also has a Pt retention that is equal to or greater than that of a fresh catalyst being used in a same or similar catalytic process.1. A process for dehydrogenating alkane or alkylaromatic compounds comprising
contacting, in a fluidized bed, an alkane compound or an alkylaromatic compound and a reconstituted dehydrogenation catalyst, such reconstituted dehydrogenation catalyst having been prepared by (a) obtaining a dehydrogenation catalyst comprising platinum and gallium on an alumina-based support, the dehydrogenation catalyst having been previously fresh but having become at least partially deactivated; (b) impregnating the at least partially deactivated dehydrogenation catalyst with a platinum salt solution to form an impregnated dehydrogenation catalyst; and (c) calcining the impregnated dehydrogenation catalyst at a temperature ranging from 400° C. to 1000° C.; (b) and (c) being carried out under conditions suitable to form a reconstituted dehydrogenation catalyst having (i) a platinum content ranging from 1 part per million, based on weight of catalyst, to 500 parts per million, based on weight of catalyst; (ii) a gallium content ranging from 0.2 wt % to 2.0 wt %; and (iii) a ratio of platinum to gallium ranging from 1:20,000 to 1:4; wherein the reconstituted dehydrogenation catalyst further exhibits a platinum retention greater than or equal to the platinum retention of a fresh dehydrogenation catalyst when each is used in the same or another, otherwise identical dehydrogenation process. 2. The process of claim 1, wherein the platinum content of the reconstituted dehydrogenation catalyst ranges from 40 parts per million, based on weight of catalyst, to 400 parts per million, based on weight of catalyst, and the ratio of platinum to gallium content ranges from 1:500 to 1:5. 3. The process of claim 2, wherein the platinum content of the reconstituted dehydrogenation catalyst ranges from 150 parts per million, based on weight of catalyst, to 300 parts per million, based on weight of catalyst, and the ratio of platinum to gallium content ranges from 3:400 to 3:80. 4. The process of claim 1, wherein the reconstituted dehydrogenation catalyst exhibits a propane dehydrogenation activity that is at least 2% absolute propane conversion greater than that exhibited by the at least partially deactivated catalyst. 5. The process of claim 1, further comprising the step of drying the impregnated dehydrogenation catalyst at a temperature ranging from 50° C. to 150° C. prior to calcining it. 6. A dehydrogenation catalyst composition comprising
a reconstituted platinum/gallium catalyst on an alumina-based support, the reconstituted platinum/gallium catalyst having been prepared by a process comprising (a) obtaining a dehydrogenation catalyst comprising platinum and gallium on an alumina-based support, the dehydrogenation catalyst having been previously fresh but having become at least partially deactivated; (b) impregnating the at least partially deactivated dehydrogenation catalyst with a platinum salt solution to form an impregnated dehydrogenation catalyst; and (c) calcining the impregnated dehydrogenation catalyst at a temperature ranging from 400° C. to 1000° C.; (b) and (c) being carried out under conditions suitable to form a reconstituted dehydrogenation catalyst having (i) a platinum content ranging from 1 part per million, based on weight of catalyst, to 500 parts per million, based on weight of catalyst; (ii) a gallium content ranging from 0.2 wt % to 2.0 wt %; and (iii) a ratio of platinum to gallium ranging from 1:20,000 to 1:4; wherein the reconstituted dehydrogenation catalyst further exhibits having a platinum retention greater than or equal to the platinum retention of a fresh dehydrogenation catalyst when each is used in the same or another, otherwise identical dehydrogenation process. 7. A process to prepare a catalyst comprising
(a) obtaining a dehydrogenation catalyst comprising platinum and gallium on an alumina-based support, the dehydrogenation catalyst having been previously fresh but having become at least partially deactivated; (b) impregnating the at least partially deactivated dehydrogenation catalyst with a platinum salt solution to form an impregnated dehydrogenation catalyst; and (c) calcining the impregnated dehydrogenation catalyst at a temperature ranging from 400° C. to 1000° C.; (b) and (c) being carried out under conditions suitable to form a reconstituted dehydrogenation catalyst having (i) a platinum content ranging from 1 part per million, based on weight of catalyst, to 500 parts per million, based on weight of catalyst; (ii) a gallium content ranging from 0.2 wt % to 2.0 wt %; and (iii) a ratio of platinum to gallium ranging from 1:20,000 to 1:4; wherein the reconstituted dehydrogenation catalyst further exhibits a platinum retention greater than or equal to the platinum retention of a fresh dehydrogenation catalyst when each is used in the same or another, otherwise identical dehydrogenation process. 8. The process of claim 7, further comprising a step, between (b) and (c), of drying the impregnated dehydrogenation catalyst at a temperature ranging from 50° C. to 150° C. | 1,700 |
3,486 | 15,113,482 | 1,783 | A molding material for a multi-layered structure, includes a thermoplastic resin layer (X) including carbon fibers (A) having a weight-average fiber length of 0.01 mm to less than 3 mm; and a thermoplastic resin layer (Y) including carbon fibers (B) having a weight-average fiber length of 3 mm to 100 mm, in which a density parameter P Y of the thermoplastic resin layer (Y) expressed by the following Equation (1) is 1×10 2 to less than 1×10 4 , and in which a density parameter P X of the thermoplastic resin layer (X) expressed by the following Equation (1) is more than 1×10 1 :
P =( q×Ln 3 )/ h (1),
where q is the number of flow units of carbon fibers included in the thermoplastic resin layer per 1 mm 2 unit area, Ln is a number-average fiber length (mm) of the carbon fibers, and h is a thickness (mm) of the thermoplastic resin layer. | 1. A molding material for a multi-layered structure, comprising:
a thermoplastic resin layer (X) including carbon fibers (A) having a weight-average fiber length of 0.01 mm to less than 3 mm; and a thermoplastic resin layer (Y) including carbon fibers (B) having a weight-average fiber length of 3 mm to 100 mm, wherein a density parameter PY of the thermoplastic resin layer (Y) expressed by the following Equation (1) is 1×102 to less than 1×104, and wherein a density parameter PX of the thermoplastic resin layer (X) expressed by the following Equation (1) is more than 1×101:
P=(q×Ln 3)/h (1)
wherein q is the number of flow units of carbon fibers included in the thermoplastic resin layer per 1 mm2 unit area; Ln is a number-average fiber length (mm) of the carbon fibers; and h is a thickness (mm) of the thermoplastic resin layer. 2. The molding material for a multi-layered structure according to claim 1, wherein a ratio (PX/PY) of the density parameter PX of the thermoplastic resin layer (X) to the density parameter PY of the thermoplastic resin layer (Y) is 1.0×10−3 to 3.0. 3. The molding material for a multi-layered structure according to claim 1, wherein a weight proportion of the thermoplastic resin layer (X) to a total weight of the thermoplastic resin layer (X) and the thermoplastic resin layer (Y) is 5 wt % to 40 wt %. 4. The molding material for a multi-layered structure according to claim 1, wherein the thermoplastic resin layer (Y) is disposed in an outermost layer on at least one side of a multi-layered structure. 5. The molding material for a multi-layered structure according to claim 1, wherein the thermoplastic resin layer (X) is disposed at a center in at least a stacking direction. 6. The molding material for a multi-layered structure according to claim 5, wherein the thermoplastic resin layer (X) is a single layer, and the thermoplastic resin layer (Y) is of two layers. 7. The molding material for a multi-layered structure according to claim 1, wherein the carbon fibers (B) included in the thermoplastic resin layer (Y) are randomly oriented in two-dimensional directions. 8. The molding material for a multi-layered structure according to claim 1, wherein the carbon fibers (B) included in the thermoplastic resin layer (Y) include a carbon fiber bundle (Bb) constituted by single fibers of a critical number of single fiber or more, defined by the following Equation (2), a proportion of the carbon fiber bundle (Bb) to a total amount of the carbon fibers (B) is more than 0 Vol % and less than 99 Vol %, and an average number (NB) of fibers in the carbon fiber bundle (Bb) satisfies the following Expression (3):
Critical number of single fiber=600/D B (2)
0.7×104 /D B 2 <N B<6×105 /D B 2 (3)
wherein DB is an average fiber diameter (μm) of the carbon fibers (B). 9. A molded article of a multi-layered structure, molded by molding a molding material,
wherein the molding material is a molding material according to claim 1. 10. The molded article of a multi-layered structure according to claim 9, wherein the thermoplastic resin layer (Y) is present at an end of the molded article. 11. The molded article of a multi-layered structure according to claim 9, wherein the multi-layered structure is a structure having a molding layer of the thermoplastic resin layer (Y) located in an outermost layer on at least one side, and a molding layer of the thermoplastic resin layer (X) adjacent to the molding layer of the thermoplastic resin layer (Y), and
wherein a protrusion portion is provided on a surface of the molding layer of the thermoplastic resin layer (Y), and a part of the molding layer of the thermoplastic resin layer (X) pushes up the molding layer of the thermoplastic resin layer (Y) at the protrusion portion in a direction in which the protrusion portion protrudes. 12. The molded article of a multi-layered structure according to claim 9, wherein the multi-layered structure is a structure having a molding layer of the thermoplastic resin layer (Y) located in an outermost layer on at least one side, and a molding layer of the thermoplastic resin layer (X) adjacent to the molding layer of the thermoplastic resin layer (Y), and
wherein a protrusion portion is provided on a surface of the molding layer of the thermoplastic resin layer (Y), and a part of the molding layer of the thermoplastic resin layer (X) breaks through the molding layer of the thermoplastic resin layer (Y) at the protrusion portion in a direction in which the protrusion portion protrudes. | A molding material for a multi-layered structure, includes a thermoplastic resin layer (X) including carbon fibers (A) having a weight-average fiber length of 0.01 mm to less than 3 mm; and a thermoplastic resin layer (Y) including carbon fibers (B) having a weight-average fiber length of 3 mm to 100 mm, in which a density parameter P Y of the thermoplastic resin layer (Y) expressed by the following Equation (1) is 1×10 2 to less than 1×10 4 , and in which a density parameter P X of the thermoplastic resin layer (X) expressed by the following Equation (1) is more than 1×10 1 :
P =( q×Ln 3 )/ h (1),
where q is the number of flow units of carbon fibers included in the thermoplastic resin layer per 1 mm 2 unit area, Ln is a number-average fiber length (mm) of the carbon fibers, and h is a thickness (mm) of the thermoplastic resin layer.1. A molding material for a multi-layered structure, comprising:
a thermoplastic resin layer (X) including carbon fibers (A) having a weight-average fiber length of 0.01 mm to less than 3 mm; and a thermoplastic resin layer (Y) including carbon fibers (B) having a weight-average fiber length of 3 mm to 100 mm, wherein a density parameter PY of the thermoplastic resin layer (Y) expressed by the following Equation (1) is 1×102 to less than 1×104, and wherein a density parameter PX of the thermoplastic resin layer (X) expressed by the following Equation (1) is more than 1×101:
P=(q×Ln 3)/h (1)
wherein q is the number of flow units of carbon fibers included in the thermoplastic resin layer per 1 mm2 unit area; Ln is a number-average fiber length (mm) of the carbon fibers; and h is a thickness (mm) of the thermoplastic resin layer. 2. The molding material for a multi-layered structure according to claim 1, wherein a ratio (PX/PY) of the density parameter PX of the thermoplastic resin layer (X) to the density parameter PY of the thermoplastic resin layer (Y) is 1.0×10−3 to 3.0. 3. The molding material for a multi-layered structure according to claim 1, wherein a weight proportion of the thermoplastic resin layer (X) to a total weight of the thermoplastic resin layer (X) and the thermoplastic resin layer (Y) is 5 wt % to 40 wt %. 4. The molding material for a multi-layered structure according to claim 1, wherein the thermoplastic resin layer (Y) is disposed in an outermost layer on at least one side of a multi-layered structure. 5. The molding material for a multi-layered structure according to claim 1, wherein the thermoplastic resin layer (X) is disposed at a center in at least a stacking direction. 6. The molding material for a multi-layered structure according to claim 5, wherein the thermoplastic resin layer (X) is a single layer, and the thermoplastic resin layer (Y) is of two layers. 7. The molding material for a multi-layered structure according to claim 1, wherein the carbon fibers (B) included in the thermoplastic resin layer (Y) are randomly oriented in two-dimensional directions. 8. The molding material for a multi-layered structure according to claim 1, wherein the carbon fibers (B) included in the thermoplastic resin layer (Y) include a carbon fiber bundle (Bb) constituted by single fibers of a critical number of single fiber or more, defined by the following Equation (2), a proportion of the carbon fiber bundle (Bb) to a total amount of the carbon fibers (B) is more than 0 Vol % and less than 99 Vol %, and an average number (NB) of fibers in the carbon fiber bundle (Bb) satisfies the following Expression (3):
Critical number of single fiber=600/D B (2)
0.7×104 /D B 2 <N B<6×105 /D B 2 (3)
wherein DB is an average fiber diameter (μm) of the carbon fibers (B). 9. A molded article of a multi-layered structure, molded by molding a molding material,
wherein the molding material is a molding material according to claim 1. 10. The molded article of a multi-layered structure according to claim 9, wherein the thermoplastic resin layer (Y) is present at an end of the molded article. 11. The molded article of a multi-layered structure according to claim 9, wherein the multi-layered structure is a structure having a molding layer of the thermoplastic resin layer (Y) located in an outermost layer on at least one side, and a molding layer of the thermoplastic resin layer (X) adjacent to the molding layer of the thermoplastic resin layer (Y), and
wherein a protrusion portion is provided on a surface of the molding layer of the thermoplastic resin layer (Y), and a part of the molding layer of the thermoplastic resin layer (X) pushes up the molding layer of the thermoplastic resin layer (Y) at the protrusion portion in a direction in which the protrusion portion protrudes. 12. The molded article of a multi-layered structure according to claim 9, wherein the multi-layered structure is a structure having a molding layer of the thermoplastic resin layer (Y) located in an outermost layer on at least one side, and a molding layer of the thermoplastic resin layer (X) adjacent to the molding layer of the thermoplastic resin layer (Y), and
wherein a protrusion portion is provided on a surface of the molding layer of the thermoplastic resin layer (Y), and a part of the molding layer of the thermoplastic resin layer (X) breaks through the molding layer of the thermoplastic resin layer (Y) at the protrusion portion in a direction in which the protrusion portion protrudes. | 1,700 |
3,487 | 14,429,060 | 1,742 | The invention relates to a continuous method for producing, by using microparticles, thermoplastics provided with reinforcement fibres. The production methods relate to such composite materials, which contain the reinforcement fibres in a parallel (or predominantly parallel) arrangement in the thermoplastic matrix. | 1.-15. (canceled) 16. A process for producing polymer prepregs comprising at least the following steps:
applying microparticles to a woven fibre fabric, laid fibre scrim, fibre non-woven or the like, melting by introducing heat,
wherein at least 80% of the microparticles have a contour angle of >90°. 17. The process according to claim 16, wherein at least 90% of the microparticles have a contour angle of >90°. 18. The process according to claim 16, wherein at least 95% of the microparticles have a contour angle of >90°. 19. The process according to claim 16, wherein the contour angle of the microparticles is >105°. 20. The process according to claim 16, wherein the contour angle of the microparticles is >120°. 21. The process according to claim 16, wherein at least 80% of the microparticles have a maximum diameter smaller than or equal to 2000 μm. 22. The process according to claim 16, wherein at least 80% of the microparticles have a maximum diameter smaller than or equal to 1700 μm. 23. The process according to claim 16, wherein at least 80% of the microparticles have a maximum diameter smaller than or equal to 1300 μm. 24. The process according to claim 16, wherein at least 80% of the microparticles have a maximum diameter greater than or equal to 100 μm. 25. The process according to claim 16, wherein at least 80% of the microparticles have a maximum diameter greater than or equal to 200 μm. 26. The process according to claim 16, wherein at least 80% of the microparticles have a maximum diameter greater than or equal to 400 μm. 27. A polymer prepreg obtained by the process according to claim 16. 28. A method comprising utilizing the polymer prepreg according to claim 27 for producing composite materials. 29. A process for producing a composite material, wherein at least the following steps are performed:
preparing microparticles, where at least 80% of the microparticles have a contour angle of >90°, preparing a microparticle prepreg, and pressing the microparticle prepreg to give a composite material. 30. A composite material obtained by the process according to claim 29. | The invention relates to a continuous method for producing, by using microparticles, thermoplastics provided with reinforcement fibres. The production methods relate to such composite materials, which contain the reinforcement fibres in a parallel (or predominantly parallel) arrangement in the thermoplastic matrix.1.-15. (canceled) 16. A process for producing polymer prepregs comprising at least the following steps:
applying microparticles to a woven fibre fabric, laid fibre scrim, fibre non-woven or the like, melting by introducing heat,
wherein at least 80% of the microparticles have a contour angle of >90°. 17. The process according to claim 16, wherein at least 90% of the microparticles have a contour angle of >90°. 18. The process according to claim 16, wherein at least 95% of the microparticles have a contour angle of >90°. 19. The process according to claim 16, wherein the contour angle of the microparticles is >105°. 20. The process according to claim 16, wherein the contour angle of the microparticles is >120°. 21. The process according to claim 16, wherein at least 80% of the microparticles have a maximum diameter smaller than or equal to 2000 μm. 22. The process according to claim 16, wherein at least 80% of the microparticles have a maximum diameter smaller than or equal to 1700 μm. 23. The process according to claim 16, wherein at least 80% of the microparticles have a maximum diameter smaller than or equal to 1300 μm. 24. The process according to claim 16, wherein at least 80% of the microparticles have a maximum diameter greater than or equal to 100 μm. 25. The process according to claim 16, wherein at least 80% of the microparticles have a maximum diameter greater than or equal to 200 μm. 26. The process according to claim 16, wherein at least 80% of the microparticles have a maximum diameter greater than or equal to 400 μm. 27. A polymer prepreg obtained by the process according to claim 16. 28. A method comprising utilizing the polymer prepreg according to claim 27 for producing composite materials. 29. A process for producing a composite material, wherein at least the following steps are performed:
preparing microparticles, where at least 80% of the microparticles have a contour angle of >90°, preparing a microparticle prepreg, and pressing the microparticle prepreg to give a composite material. 30. A composite material obtained by the process according to claim 29. | 1,700 |
3,488 | 14,650,399 | 1,767 | The invention relates to a polymer comprising structural units of vinylidene fluoride, trifluoroethylene and chlorotrifluoroethylene, the molar ratio between the vinylidene fluoride and the trifluoroethylene in the polymer being between 55:45 and 65:35, and the molar proportion of the structural units of chlorotrifluoroethylene in the polymer being between 1.5 and 4.5%. The invention also relates to various items comprising said polymer, such as films, fibres, extruded plates and moulded items. | 1. A polymer comprising vinylidene fluoride, trifluoroethylene and chlorotrifluoroethylene structural units, wherein the vinylidene fluoride-to-trifluoroethylene molar ratio in the polymer is from 55:45 to 65:35, and the molar proportion of chlorotrifluoroethylene structural units in the polymer is from 1.5 to 4.5%. 2. The polymer of claim 1, wherein the polymer consists of vinylidene fluoride, trifluoroethylene and chlorotrifluoroethylene structural units. 3. The polymer of claim 1, having a weight average molecular weight of at least 100,000, preferably at least 200,000, and more preferably at least 300,000 or at least 400,000. 4. The polymer of claim 1, wherein the molar proportion of chlorotrifluoroethylene structural units in the polymer is from 3.2% to 4.5%, and preferably from 3.4% to 4.5%. 5. A polymer comprising vinylidene fluoride, trifluoroethylene and chlorotrifluoroethylene structural units, which is suitable for being formed into a film having an elastic modulus of at least 0.6 GPa. 6. The polymer of claim 5, wherein the vinylidene fluoride-to-trifluoroethylene molar ratio is from 55:45 to 75:25, preferably from 55:45 to 65:35 or from 62:38 to 72:28; and/or the molar proportion of chlorotrifluoroethylene structural units in the polymer is from 1.5 to 5.5%, advantageously from 1.5 to 4.5%, preferably from 1.8 to 5.5% or even from 1.8 to 4.5%, more preferably from 3.2% to 4.5%, and most preferably from 3.4% to 4.5%; and/or wherein the polymer consists of vinylidene fluoride, trifluoroethylene and chlorotrifluoroethylene structural units. 7. The polymer of claim 5, wherein the film:
has a dielectric constant of less than 40 at 1 kHz and 25° C.; and/or has an electrostrictive strain at 25° C. of at least 0.25%, preferably at least 0.4%, under an electric field gradient of 50 MV/m; or of at least 0.7%, preferably at least 1%, under an electric field gradient of 100 MV/m; and/or has a thickness of less than 30 μm, preferably a thickness of 1 to 5 μm, and more preferably a thickness of 1 to 3 μm. 8. The polymer of claim 5, wherein the film is produced by solvent casting, by extrusion or by hot melt pressing, then optionally stretched by a factor of 2 to 10, preferably 5 to 7, and annealed. 9. An article comprising the polymer of claim 1, selected from films, fibers, extruded plates and molded articles. 10. A film comprising the polymer of claim 1, or preferably consisting of the polymer. 11. The film of claim 10, having an elastic modulus of at least 0.6 GPa. 12. A film comprising a polymer which comprises vinylidene fluoride, trifluoroethylene and chlorotrifluoroethylene structural units, wherein the film has an elastic modulus of at least 0.6 GPa. 13. The film of claim 12, wherein the vinylidene fluoride-to-trifluoroethylene molar ratio in the polymer is from 55:45 to 75:25, preferably from 55:45 to 65:35 or from 62:38 to 72:28; and/or the molar proportion of chlorotrifluoroethylene structural units in the polymer is from 1.5 to 5.5%, advantageously from 1.5 to 4.5%, preferably from 1.8 to 5.5%, or even from 1.8 to 4.5%, more preferably from 3.2% to 4.5%, and most preferably from 3.4% to 4.5%; and/or the polymer consists of vinylidene fluoride, trifluoroethylene and chlorotrifluoroethylene structural units. 14. The film of claim 10, having a dielectric constant of less than 40 at 1 kHz and 25° C.; and/or having an electrostrictive strain at 25° C. of at least 0.25%, preferably at least 0.4%, under an electric field gradient of 50 MV/m; or of at least 0.7%, preferably at least 1%, under an electric field gradient of 100 MV/m. 15. The film of claim 10, having a thickness of less than 30 μm, preferably a thickness of 1 to 5 μm, and more preferably a thickness of 1 to 3 μm. 16. A method of making the polymer of claim 1, comprising polymerizing vinylidene fluoride monomers, trifluoroethylene monomers and chlorotrifluoroethylene monomers. 17. The method of claim 16, which is performed by suspension polymerization. 18. The method of claim 16, comprising the following successive steps:
(1) loading a reactor with an initial mixture of monomers; (2) adding a radical polymerization initiator to the reactor; (3) continuously adding a second mixture of monomers to the reactor to perform polymerization at a substantially constant pressure. 19. The method of claim 18, wherein the initial mixture comprises vinylidene fluoride and trifluoroethylene monomers, without chlorotrifluoroethylene monomers; and
the second mixture comprises vinylidene fluoride, trifluoroethylene and chlorotrifluoroethylene monomers. 20. The method of claim 16, wherein the pressure in the reactor in steps (2) and (3) is at least 80 bar; and the temperature in the reactor in steps (2) and (3) is from 40 to 60° C. 21. A method of manufacturing the film of claim 10, comprising a step of producing a film, optionally a step of stretching said film, and a step of annealing said film. 22. The method of claim 21, wherein the step of producing a film is performed by solvent casting, by extrusion or by hot melt pressing, preferably by solvent casting, and more preferably by solvent casting the composition. | The invention relates to a polymer comprising structural units of vinylidene fluoride, trifluoroethylene and chlorotrifluoroethylene, the molar ratio between the vinylidene fluoride and the trifluoroethylene in the polymer being between 55:45 and 65:35, and the molar proportion of the structural units of chlorotrifluoroethylene in the polymer being between 1.5 and 4.5%. The invention also relates to various items comprising said polymer, such as films, fibres, extruded plates and moulded items.1. A polymer comprising vinylidene fluoride, trifluoroethylene and chlorotrifluoroethylene structural units, wherein the vinylidene fluoride-to-trifluoroethylene molar ratio in the polymer is from 55:45 to 65:35, and the molar proportion of chlorotrifluoroethylene structural units in the polymer is from 1.5 to 4.5%. 2. The polymer of claim 1, wherein the polymer consists of vinylidene fluoride, trifluoroethylene and chlorotrifluoroethylene structural units. 3. The polymer of claim 1, having a weight average molecular weight of at least 100,000, preferably at least 200,000, and more preferably at least 300,000 or at least 400,000. 4. The polymer of claim 1, wherein the molar proportion of chlorotrifluoroethylene structural units in the polymer is from 3.2% to 4.5%, and preferably from 3.4% to 4.5%. 5. A polymer comprising vinylidene fluoride, trifluoroethylene and chlorotrifluoroethylene structural units, which is suitable for being formed into a film having an elastic modulus of at least 0.6 GPa. 6. The polymer of claim 5, wherein the vinylidene fluoride-to-trifluoroethylene molar ratio is from 55:45 to 75:25, preferably from 55:45 to 65:35 or from 62:38 to 72:28; and/or the molar proportion of chlorotrifluoroethylene structural units in the polymer is from 1.5 to 5.5%, advantageously from 1.5 to 4.5%, preferably from 1.8 to 5.5% or even from 1.8 to 4.5%, more preferably from 3.2% to 4.5%, and most preferably from 3.4% to 4.5%; and/or wherein the polymer consists of vinylidene fluoride, trifluoroethylene and chlorotrifluoroethylene structural units. 7. The polymer of claim 5, wherein the film:
has a dielectric constant of less than 40 at 1 kHz and 25° C.; and/or has an electrostrictive strain at 25° C. of at least 0.25%, preferably at least 0.4%, under an electric field gradient of 50 MV/m; or of at least 0.7%, preferably at least 1%, under an electric field gradient of 100 MV/m; and/or has a thickness of less than 30 μm, preferably a thickness of 1 to 5 μm, and more preferably a thickness of 1 to 3 μm. 8. The polymer of claim 5, wherein the film is produced by solvent casting, by extrusion or by hot melt pressing, then optionally stretched by a factor of 2 to 10, preferably 5 to 7, and annealed. 9. An article comprising the polymer of claim 1, selected from films, fibers, extruded plates and molded articles. 10. A film comprising the polymer of claim 1, or preferably consisting of the polymer. 11. The film of claim 10, having an elastic modulus of at least 0.6 GPa. 12. A film comprising a polymer which comprises vinylidene fluoride, trifluoroethylene and chlorotrifluoroethylene structural units, wherein the film has an elastic modulus of at least 0.6 GPa. 13. The film of claim 12, wherein the vinylidene fluoride-to-trifluoroethylene molar ratio in the polymer is from 55:45 to 75:25, preferably from 55:45 to 65:35 or from 62:38 to 72:28; and/or the molar proportion of chlorotrifluoroethylene structural units in the polymer is from 1.5 to 5.5%, advantageously from 1.5 to 4.5%, preferably from 1.8 to 5.5%, or even from 1.8 to 4.5%, more preferably from 3.2% to 4.5%, and most preferably from 3.4% to 4.5%; and/or the polymer consists of vinylidene fluoride, trifluoroethylene and chlorotrifluoroethylene structural units. 14. The film of claim 10, having a dielectric constant of less than 40 at 1 kHz and 25° C.; and/or having an electrostrictive strain at 25° C. of at least 0.25%, preferably at least 0.4%, under an electric field gradient of 50 MV/m; or of at least 0.7%, preferably at least 1%, under an electric field gradient of 100 MV/m. 15. The film of claim 10, having a thickness of less than 30 μm, preferably a thickness of 1 to 5 μm, and more preferably a thickness of 1 to 3 μm. 16. A method of making the polymer of claim 1, comprising polymerizing vinylidene fluoride monomers, trifluoroethylene monomers and chlorotrifluoroethylene monomers. 17. The method of claim 16, which is performed by suspension polymerization. 18. The method of claim 16, comprising the following successive steps:
(1) loading a reactor with an initial mixture of monomers; (2) adding a radical polymerization initiator to the reactor; (3) continuously adding a second mixture of monomers to the reactor to perform polymerization at a substantially constant pressure. 19. The method of claim 18, wherein the initial mixture comprises vinylidene fluoride and trifluoroethylene monomers, without chlorotrifluoroethylene monomers; and
the second mixture comprises vinylidene fluoride, trifluoroethylene and chlorotrifluoroethylene monomers. 20. The method of claim 16, wherein the pressure in the reactor in steps (2) and (3) is at least 80 bar; and the temperature in the reactor in steps (2) and (3) is from 40 to 60° C. 21. A method of manufacturing the film of claim 10, comprising a step of producing a film, optionally a step of stretching said film, and a step of annealing said film. 22. The method of claim 21, wherein the step of producing a film is performed by solvent casting, by extrusion or by hot melt pressing, preferably by solvent casting, and more preferably by solvent casting the composition. | 1,700 |
3,489 | 14,942,480 | 1,793 | In one embodiment, a method comprises adding a plurality of soybeans to an extractor, the soybeans having an average protein:oil ratio of greater than 2.3, heating the soybeans, removing hulls from the plurality of soybeans, and grinding the plurality of soybeans with water at a temperature between 180° F. and 190° F. to yield a soy extract having hexanal levels of less than 50 parts per billion (ppb). | 1. A method, comprising:
adding a plurality of soybeans to an extractor, the soybeans having an average protein:oil ratio of greater than 2.3; heating the soybeans; removing hulls from the plurality of soybeans; and grinding the plurality of soybeans with water at a temperature between 180° F. and 190° F. to yield a soy extract having hexanal levels of less than 50 parts per billion (ppb). 2. The method of claim 1, wherein the plurality of soybeans comprises:
a first set of soybeans having a protein:oil ratio of less than 2.3; and a second set of soybeans having a protein:oil ratio of greater than 2.5. 3. The method of claim 1, wherein the plurality of soybeans comprises:
a first set of soybeans having a protein:oil ratio of less than 2.2; and a second set of soybeans having a protein:oil ratio of greater than 2.6. 4. The method of claim 1, wherein the soybeans have an average protein:oil ratio of greater than 2.4 5. The method of claim 1, wherein the soybeans have an average protein:oil ratio of greater than 2.5 6. The method of claim 1, wherein the soy extract has hexanal levels of less than 30 ppb. 7. The method of claim 1, further comprising extruding the de-hulled soybeans to remove oil. 8. The method of claim 1, further comprising:
adding the soy extract to a mixer; adding ingredients to the mixer, the ingredients including at least one of the following: stabilizers, vitamins, minerals, flavors, functional ingredients, salts, antioxidants, or sugar; and mixing the ingredients, using the mixer, to yield a mixture having the soy extract and the ingredients dispersed substantially evenly throughout. 9. The method of claim 8, wherein the ingredients comprise at least one of calcium carbonate or ascorbic acid, and the method further comprises heating the mixture to a temperature that ranges from 285° F. to 300° F. for a period of 2 seconds to 6 seconds. 10. The method of claim 8, further comprising pasteurizing the mixture. 11. A composition made by the method comprising:
adding a plurality of soybeans to an extractor, the soybeans having an average protein:oil ratio of greater than 2.3; heating the soybeans; removing hulls from the plurality of soybeans; and grinding the plurality of soybeans with water at a temperature between 180° F. and 190° F. to yield a soy extract having hexanal levels of less than 50 parts per billion (ppb). 12. The composition of claim 11, wherein the plurality of soybeans comprises:
a first set of soybeans having a protein:oil ratio of less than 2.3; and a second set of soybeans having a protein:oil ratio of greater than 2.5. 13. The composition of claim 11, wherein the plurality of soybeans comprises:
a first set of soybeans having a protein:oil ratio of less than 2.2; and a second set of soybeans having a protein:oil ratio of greater than 2.6. 14. The composition of claim 11, wherein the soybeans have an average protein:oil ratio of greater than 2.4 15. The composition of claim 11, wherein the soybeans have an average protein:oil ratio of greater than 2.5 16. The composition of claim 11, wherein the method further comprises extruding the de-hulled soybeans to remove oil. 17. The composition of claim 11, wherein the method further comprises:
adding the soy extract to a mixer; adding ingredients to the mixer, the ingredients including at least one of the following: stabilizers, vitamins, minerals, flavors, functional ingredients, salts, antioxidants, or sugar; and mixing the ingredients, using the mixer, to yield a mixture having the soy extract and the ingredients dispersed substantially evenly throughout. 18. The method of claim 17, wherein the ingredients comprise at least one of calcium carbonate or ascorbic acid, and the method further comprises heating the mixture to a temperature that ranges from 285° F. to 300° F. for a period of 2 seconds to 6 seconds. 19. The method of claim 17, wherein the method further comprises pasteurizing the mixture. 20. A composition, comprising:
a soy extract having a protein:oil ratio of greater than 2.3, the soy extract comprising between 30% and 90% of the composition; one or more ingredients selected from the group consisting of stabilizers, vitamins, minerals, flavors, functional ingredients, salts, antioxidants, sugar, the one or more ingredients comprising between 0.4% and 7% of the composition; and water comprising the balance of the composition; wherein the composition comprises hexanal levels of less than 50 parts per billion (ppb). | In one embodiment, a method comprises adding a plurality of soybeans to an extractor, the soybeans having an average protein:oil ratio of greater than 2.3, heating the soybeans, removing hulls from the plurality of soybeans, and grinding the plurality of soybeans with water at a temperature between 180° F. and 190° F. to yield a soy extract having hexanal levels of less than 50 parts per billion (ppb).1. A method, comprising:
adding a plurality of soybeans to an extractor, the soybeans having an average protein:oil ratio of greater than 2.3; heating the soybeans; removing hulls from the plurality of soybeans; and grinding the plurality of soybeans with water at a temperature between 180° F. and 190° F. to yield a soy extract having hexanal levels of less than 50 parts per billion (ppb). 2. The method of claim 1, wherein the plurality of soybeans comprises:
a first set of soybeans having a protein:oil ratio of less than 2.3; and a second set of soybeans having a protein:oil ratio of greater than 2.5. 3. The method of claim 1, wherein the plurality of soybeans comprises:
a first set of soybeans having a protein:oil ratio of less than 2.2; and a second set of soybeans having a protein:oil ratio of greater than 2.6. 4. The method of claim 1, wherein the soybeans have an average protein:oil ratio of greater than 2.4 5. The method of claim 1, wherein the soybeans have an average protein:oil ratio of greater than 2.5 6. The method of claim 1, wherein the soy extract has hexanal levels of less than 30 ppb. 7. The method of claim 1, further comprising extruding the de-hulled soybeans to remove oil. 8. The method of claim 1, further comprising:
adding the soy extract to a mixer; adding ingredients to the mixer, the ingredients including at least one of the following: stabilizers, vitamins, minerals, flavors, functional ingredients, salts, antioxidants, or sugar; and mixing the ingredients, using the mixer, to yield a mixture having the soy extract and the ingredients dispersed substantially evenly throughout. 9. The method of claim 8, wherein the ingredients comprise at least one of calcium carbonate or ascorbic acid, and the method further comprises heating the mixture to a temperature that ranges from 285° F. to 300° F. for a period of 2 seconds to 6 seconds. 10. The method of claim 8, further comprising pasteurizing the mixture. 11. A composition made by the method comprising:
adding a plurality of soybeans to an extractor, the soybeans having an average protein:oil ratio of greater than 2.3; heating the soybeans; removing hulls from the plurality of soybeans; and grinding the plurality of soybeans with water at a temperature between 180° F. and 190° F. to yield a soy extract having hexanal levels of less than 50 parts per billion (ppb). 12. The composition of claim 11, wherein the plurality of soybeans comprises:
a first set of soybeans having a protein:oil ratio of less than 2.3; and a second set of soybeans having a protein:oil ratio of greater than 2.5. 13. The composition of claim 11, wherein the plurality of soybeans comprises:
a first set of soybeans having a protein:oil ratio of less than 2.2; and a second set of soybeans having a protein:oil ratio of greater than 2.6. 14. The composition of claim 11, wherein the soybeans have an average protein:oil ratio of greater than 2.4 15. The composition of claim 11, wherein the soybeans have an average protein:oil ratio of greater than 2.5 16. The composition of claim 11, wherein the method further comprises extruding the de-hulled soybeans to remove oil. 17. The composition of claim 11, wherein the method further comprises:
adding the soy extract to a mixer; adding ingredients to the mixer, the ingredients including at least one of the following: stabilizers, vitamins, minerals, flavors, functional ingredients, salts, antioxidants, or sugar; and mixing the ingredients, using the mixer, to yield a mixture having the soy extract and the ingredients dispersed substantially evenly throughout. 18. The method of claim 17, wherein the ingredients comprise at least one of calcium carbonate or ascorbic acid, and the method further comprises heating the mixture to a temperature that ranges from 285° F. to 300° F. for a period of 2 seconds to 6 seconds. 19. The method of claim 17, wherein the method further comprises pasteurizing the mixture. 20. A composition, comprising:
a soy extract having a protein:oil ratio of greater than 2.3, the soy extract comprising between 30% and 90% of the composition; one or more ingredients selected from the group consisting of stabilizers, vitamins, minerals, flavors, functional ingredients, salts, antioxidants, sugar, the one or more ingredients comprising between 0.4% and 7% of the composition; and water comprising the balance of the composition; wherein the composition comprises hexanal levels of less than 50 parts per billion (ppb). | 1,700 |
3,490 | 15,168,657 | 1,722 | A method for producing a positive electrode sheet is provided with a positive current collecting foil made of aluminum and a battery positive active material layer containing positive active material particles made of LiNiMn based spinel and applied and dried on the current collecting foil. The positive active material layer includes a first binder made of polyacrylic acid with a molecular weight of 50,000 or less and a second binder made of polyacrylic acid with a molecular weight of 300,000 or more. The first positive electrode paste forming the positive active material layer satisfies expressions (1) to (3):
α≧1.7 (1)
β≧0.9 (2)
α+βv≦3.0 (3)
where α is an additive amount of the first binder in pts. wt. and β is an additive amount of the second binder in pts. wt. when other solid content is 100 pts. wt. | 1. A method for producing a positive electrode sheet for a lithium ion secondary battery, the positive electrode sheet comprising:
a positive current collecting sheet made of aluminum; and a positive active material layer applied and dried on the positive current collecting sheet, the positive active material layer containing positive active material particles made of LiNiMn based spinel, wherein the positive active material layer includes a first positive active material layer provided in contact with the positive current collecting sheet, and the first positive active material layer includes:
a first binder made of polyacrylic acid having a molecular weight of 50,000 or less; and
a second binder made of polyacrylic acid having a molecular weight of 300,000 or more,
wherein the method includes a first applying and drying step of applying a first positive electrode paste to the positive current collecting sheet, the first positive electrode paste having been prepared by mixing the positive active material particles with water-based solvent, and drying the first positive electrode paste to form the first positive active material layer, and the first positive electrode paste includes the first binder and the second binder, and satisfies expressions (1) to (3):
α≧1.7 (1)
β>0.9 (2)
α+β≦3.0 (3)
where α is an additive amount of the first binder in parts by weight and β is an additive amount of the second binder in parts by weight when a solid content except the first binder and the second binder in a solid content of the first positive electrode paste is 100 parts by weight. 2. The method for producing a positive electrode sheet for a lithium ion secondary battery according to claim 1, wherein the second binder is made of polyacrylic acid having a molecular weight of 800,000 or more. 3. The method for producing a positive electrode sheet for a lithium ion secondary battery according to claim 1, wherein
the first applying and drying step includes forming the first positive active material layer having a thickness of 3 μm or more, and the method further comprises a second applying and drying step of applying a second positive electrode paste to the first positive active material layer, the second positive electrode paste having been prepared by mixing the positive active material particles with water-based solvent so that the second positive electrode paste is above pH 9.0, and drying the second positive electrode paste to form a second positive active material layer. 4. The method for producing a positive electrode sheet for a lithium ion secondary battery according to claim 2, wherein
the first applying and drying step includes forming the first positive active material layer having a thickness of 3 μm or more, and the method further comprises a second applying and drying step of applying a second positive electrode paste to the first positive active material layer, the second positive electrode paste having been prepared by mixing the positive active material particles with water-based solvent so that the second positive electrode paste is above pH 9.0, and drying the second positive electrode paste to form a second positive active material layer. 5. The method for producing a positive electrode sheet for a lithium ion secondary battery according to claim 3, wherein
the second positive electrode paste contains a third binder made of polyacrylic acid and satisfies expression (4):
0<γ<α+β (4)
where γ is an additive amount of the third binder in parts by weight when a solid content except the third binder in a solid content of the second positive electrode paste is 100 parts by weight. 6. The method for producing a positive electrode sheet for a lithium ion secondary battery according to claim 4, wherein
the second positive electrode paste contains a third binder made of polyacrylic acid and satisfies expression (4):
0<γ<α+β (4)
where γ is an additive amount of the third binder in parts by weight when a solid content except the third binder in a solid content of the second positive electrode paste is 100 parts by weight. 7. A positive electrode sheet comprising:
a positive current collecting sheet made of aluminum; and a positive active material layer applied and dried on the positive current collecting sheet, the positive active material layer containing positive active material particles made of LiNiMn based spinel, wherein the positive active material layer includes a first positive active material layer provided in contact with the positive current collecting sheet, and the first positive active material layer includes:
a first binder made of polyacrylic acid having a molecular weight of 50,000 or less; and
a second binder made of polyacrylic acid having a molecular weight of 300000 or more, and
the first positive active material layer satisfies expressions (1) to (3):
α≧1.7 (1)
β≧0.9 (2)
α+β≦3.0 (3)
where α is an additive amount of the first binder in parts by weight and β is an additive amount of the second binder in parts by weight when a solid content except the first binder and the second binder in a solid content of the first positive active material layer is 100 parts by weight. | A method for producing a positive electrode sheet is provided with a positive current collecting foil made of aluminum and a battery positive active material layer containing positive active material particles made of LiNiMn based spinel and applied and dried on the current collecting foil. The positive active material layer includes a first binder made of polyacrylic acid with a molecular weight of 50,000 or less and a second binder made of polyacrylic acid with a molecular weight of 300,000 or more. The first positive electrode paste forming the positive active material layer satisfies expressions (1) to (3):
α≧1.7 (1)
β≧0.9 (2)
α+βv≦3.0 (3)
where α is an additive amount of the first binder in pts. wt. and β is an additive amount of the second binder in pts. wt. when other solid content is 100 pts. wt.1. A method for producing a positive electrode sheet for a lithium ion secondary battery, the positive electrode sheet comprising:
a positive current collecting sheet made of aluminum; and a positive active material layer applied and dried on the positive current collecting sheet, the positive active material layer containing positive active material particles made of LiNiMn based spinel, wherein the positive active material layer includes a first positive active material layer provided in contact with the positive current collecting sheet, and the first positive active material layer includes:
a first binder made of polyacrylic acid having a molecular weight of 50,000 or less; and
a second binder made of polyacrylic acid having a molecular weight of 300,000 or more,
wherein the method includes a first applying and drying step of applying a first positive electrode paste to the positive current collecting sheet, the first positive electrode paste having been prepared by mixing the positive active material particles with water-based solvent, and drying the first positive electrode paste to form the first positive active material layer, and the first positive electrode paste includes the first binder and the second binder, and satisfies expressions (1) to (3):
α≧1.7 (1)
β>0.9 (2)
α+β≦3.0 (3)
where α is an additive amount of the first binder in parts by weight and β is an additive amount of the second binder in parts by weight when a solid content except the first binder and the second binder in a solid content of the first positive electrode paste is 100 parts by weight. 2. The method for producing a positive electrode sheet for a lithium ion secondary battery according to claim 1, wherein the second binder is made of polyacrylic acid having a molecular weight of 800,000 or more. 3. The method for producing a positive electrode sheet for a lithium ion secondary battery according to claim 1, wherein
the first applying and drying step includes forming the first positive active material layer having a thickness of 3 μm or more, and the method further comprises a second applying and drying step of applying a second positive electrode paste to the first positive active material layer, the second positive electrode paste having been prepared by mixing the positive active material particles with water-based solvent so that the second positive electrode paste is above pH 9.0, and drying the second positive electrode paste to form a second positive active material layer. 4. The method for producing a positive electrode sheet for a lithium ion secondary battery according to claim 2, wherein
the first applying and drying step includes forming the first positive active material layer having a thickness of 3 μm or more, and the method further comprises a second applying and drying step of applying a second positive electrode paste to the first positive active material layer, the second positive electrode paste having been prepared by mixing the positive active material particles with water-based solvent so that the second positive electrode paste is above pH 9.0, and drying the second positive electrode paste to form a second positive active material layer. 5. The method for producing a positive electrode sheet for a lithium ion secondary battery according to claim 3, wherein
the second positive electrode paste contains a third binder made of polyacrylic acid and satisfies expression (4):
0<γ<α+β (4)
where γ is an additive amount of the third binder in parts by weight when a solid content except the third binder in a solid content of the second positive electrode paste is 100 parts by weight. 6. The method for producing a positive electrode sheet for a lithium ion secondary battery according to claim 4, wherein
the second positive electrode paste contains a third binder made of polyacrylic acid and satisfies expression (4):
0<γ<α+β (4)
where γ is an additive amount of the third binder in parts by weight when a solid content except the third binder in a solid content of the second positive electrode paste is 100 parts by weight. 7. A positive electrode sheet comprising:
a positive current collecting sheet made of aluminum; and a positive active material layer applied and dried on the positive current collecting sheet, the positive active material layer containing positive active material particles made of LiNiMn based spinel, wherein the positive active material layer includes a first positive active material layer provided in contact with the positive current collecting sheet, and the first positive active material layer includes:
a first binder made of polyacrylic acid having a molecular weight of 50,000 or less; and
a second binder made of polyacrylic acid having a molecular weight of 300000 or more, and
the first positive active material layer satisfies expressions (1) to (3):
α≧1.7 (1)
β≧0.9 (2)
α+β≦3.0 (3)
where α is an additive amount of the first binder in parts by weight and β is an additive amount of the second binder in parts by weight when a solid content except the first binder and the second binder in a solid content of the first positive active material layer is 100 parts by weight. | 1,700 |
3,491 | 14,897,332 | 1,724 | A sulfide solid electrolyte material having a high Li ion conductivity is provided. A sulfide solid electrolyte material includes Li, P, I and S, having peaks at 2θ=20.2° and 23.6°, not having peaks at 2θ=21.0° and 28.0° in an X-ray diffraction measurement using a CuKα ray, and having a half width of the peak at 2θ=20.2° of 0.51° or less. | 1-8. (canceled) 9. A sulfide solid electrolyte material comprising
an ion conductor having Li, P and S, and having a PS4 3− structure as a main component of an anion structure, and at least one of LiI, LiBr, and LiCl, wherein the sulfide solid electrolyte material contains a high Li ion conducting phase having peaks at 2θ=20.2° and 23.6°, does not contain low Li ion conducting phase having peaks at 2θ=21.0° and 28.0° in an X-ray diffraction measurement using a CuKα ray, and has a half width of the peak at 2θ=20.2° of 0.51° or less. 10. The sulfide solid electrolyte material according to claim 9, comprising the LiBr,
wherein LiBr/(LiI+LiBr) is in the range of 25 mol % to 50 mol %. 11. The sulfide solid electrolyte material according to claim 9, comprising the LiCl,
wherein LiCl/(LiI+LiCl) is in the range of 15 mol % to 50 mol %. 12. The sulfide solid electrolyte material according to claim 9, using a raw material composition which contains Li2S, P2S5, LiI, and at least one of LiBr and LiCl,
wherein Li2S/(Li2S+P2S5) is in the range of 76 mol % to 78 mol %. 13. A sulfide glass, the sulfide glass being used for the sulfide solid electrolyte material according to claim 9,
wherein an exothermic peak of the high Li ion conducting phase (c1) and an exothermic peak of the low Li ion conducting phase (cx) are observed by differential thermal analysis, and the sulfide glass satisfies Tcx−Tc1≧55° C. when temperature of the exothermic peak of the c1 is Tc1 and temperature of the exothermic peak of the cx is Tcx in differential thermal analysis. 14. The sulfide glass according to claim 13, comprising: the ion conductor; the LiI; and the LiBr,
wherein LiBr/(LiI+LiBr) is in the range of 25 mol % to 50 mol %. 15. A solid state lithium battery comprising: a cathode active material layer containing a cathode active material; an anode active material layer containing an anode active material; and a solid electrolyte layer formed between the cathode active material layer and the anode active material layer,
wherein at least one of the cathode active material layer, the anode active material layer, and the solid electrolyte layer contains the sulfide solid electrolyte material according to claim 9. 16. A method for producing a sulfide solid electrolyte material, the sulfide solid electrolyte material being the sulfide solid electrolyte material according to claim 9, the method comprising steps of:
an amorphizing step of obtaining a sulfide glass by amorphization of a raw material composition that contains Li2S, P2S5, LiI, and at least one of LiBr and LiCl; and a heat treatment step of heating the sulfide glass, wherein the method for producing a sulfide solid electrolyte material uses the sulfide glass in which an exothermic peak of the high Li ion conducting phase (c1) and an exothermic peak of the low Li ion conducting phase (cx) are observed by differential thermal analysis; and the sulfide glass satisfies Tcx−Tc1≧55° C. when temperature of the exothermic peak of the c1 is Tc1 and temperature of the exothermic peak of the cx is Tcx in differential thermal analysis. | A sulfide solid electrolyte material having a high Li ion conductivity is provided. A sulfide solid electrolyte material includes Li, P, I and S, having peaks at 2θ=20.2° and 23.6°, not having peaks at 2θ=21.0° and 28.0° in an X-ray diffraction measurement using a CuKα ray, and having a half width of the peak at 2θ=20.2° of 0.51° or less.1-8. (canceled) 9. A sulfide solid electrolyte material comprising
an ion conductor having Li, P and S, and having a PS4 3− structure as a main component of an anion structure, and at least one of LiI, LiBr, and LiCl, wherein the sulfide solid electrolyte material contains a high Li ion conducting phase having peaks at 2θ=20.2° and 23.6°, does not contain low Li ion conducting phase having peaks at 2θ=21.0° and 28.0° in an X-ray diffraction measurement using a CuKα ray, and has a half width of the peak at 2θ=20.2° of 0.51° or less. 10. The sulfide solid electrolyte material according to claim 9, comprising the LiBr,
wherein LiBr/(LiI+LiBr) is in the range of 25 mol % to 50 mol %. 11. The sulfide solid electrolyte material according to claim 9, comprising the LiCl,
wherein LiCl/(LiI+LiCl) is in the range of 15 mol % to 50 mol %. 12. The sulfide solid electrolyte material according to claim 9, using a raw material composition which contains Li2S, P2S5, LiI, and at least one of LiBr and LiCl,
wherein Li2S/(Li2S+P2S5) is in the range of 76 mol % to 78 mol %. 13. A sulfide glass, the sulfide glass being used for the sulfide solid electrolyte material according to claim 9,
wherein an exothermic peak of the high Li ion conducting phase (c1) and an exothermic peak of the low Li ion conducting phase (cx) are observed by differential thermal analysis, and the sulfide glass satisfies Tcx−Tc1≧55° C. when temperature of the exothermic peak of the c1 is Tc1 and temperature of the exothermic peak of the cx is Tcx in differential thermal analysis. 14. The sulfide glass according to claim 13, comprising: the ion conductor; the LiI; and the LiBr,
wherein LiBr/(LiI+LiBr) is in the range of 25 mol % to 50 mol %. 15. A solid state lithium battery comprising: a cathode active material layer containing a cathode active material; an anode active material layer containing an anode active material; and a solid electrolyte layer formed between the cathode active material layer and the anode active material layer,
wherein at least one of the cathode active material layer, the anode active material layer, and the solid electrolyte layer contains the sulfide solid electrolyte material according to claim 9. 16. A method for producing a sulfide solid electrolyte material, the sulfide solid electrolyte material being the sulfide solid electrolyte material according to claim 9, the method comprising steps of:
an amorphizing step of obtaining a sulfide glass by amorphization of a raw material composition that contains Li2S, P2S5, LiI, and at least one of LiBr and LiCl; and a heat treatment step of heating the sulfide glass, wherein the method for producing a sulfide solid electrolyte material uses the sulfide glass in which an exothermic peak of the high Li ion conducting phase (c1) and an exothermic peak of the low Li ion conducting phase (cx) are observed by differential thermal analysis; and the sulfide glass satisfies Tcx−Tc1≧55° C. when temperature of the exothermic peak of the c1 is Tc1 and temperature of the exothermic peak of the cx is Tcx in differential thermal analysis. | 1,700 |
3,492 | 15,108,913 | 1,783 | Provided is a decorative sheet for decreased thickness, and ensure superior molding processability and designability including external appearance (including the finished state) and texture (feel). The present invention relates to a decorative sheet, comprising a base sheet formed of a polyester resin or a polyolefin resin; and an ornamental layer and a surface-protecting layer provided on the base sheet in this order, the decorative sheet having a total thickness of 70 to 135 μm, at least the surface-protecting layer having recesses, the maximum depth of each recess being 15 to 100% based on the total thickness and not less than 15 μm, the ratio of a tensile elastic modulus at 120° C. to a tensile elastic modulus at 20° C. being 1:12 to 1:160, and the ratio of a maximum point load at 120° C. to a maximum point load at 20° C. upon 30-mm stretching being 1:1.7 to 1:30. | 1. A decorative sheet, comprising a base sheet formed of a polyester resin or a polyolefin resin; and an ornamental layer and a surface-protecting layer provided on the base sheet in this order;
the decorative sheet having a total thickness of 70 to 135 μm, at least the surface-protecting layer having recesses, the maximum depth of each recess being 15 to 100% based on the total thickness and not less than 15 μm, the ratio of a tensile elastic modulus at 120° C. to a tensile elastic modulus at 20° C. being 1:12 to 1:160, and the ratio of a maximum point load at 120° C. to a maximum point load at 20° C. upon 30-mm stretching being 1:1.7 to 1:30. 2. The decorative sheet according to claim 1, wherein the decorative sheet further comprises a resin layer between the base sheet and the surface-protecting layer. 3. The decorative sheet according to claim 1, wherein the base sheet is formed of a polyolefin resin. 4. The decorative sheet according to claim 2, wherein the resin layer is formed of a polyolefin resin. 5. The decorative sheet according to claim 1, wherein the surface-protecting layer is a cured ionizing radiation-curable resin composition. 6. The decorative sheet according to claim 1, wherein the decorative sheet having the base sheet, the ornamental layer, the resin layer, and the surface-protecting layer in this order, and the resin layer and the surface-protecting layer are transparent. 7. The decorative sheet according to claim 1, wherein the decorative sheet is used for lamination or wrapping. 8. A decorative member, wherein a surface on the base sheet side of the decorative sheet according to claim 1 is adhered to an adherend via an adhesive layer. 9. The decorative sheet according to claim 2, wherein the base sheet is formed of a polyolefin resin. 10. The decorative sheet according to claim 3, wherein the resin layer is formed of a polyolefin resin. 11. The decorative sheet according to claim 9, wherein the resin layer is formed of a polyolefin resin. 12. The decorative sheet according to claim 2, wherein the surface-protecting layer is a cured ionizing radiation-curable resin composition. 13. The decorative sheet according to claim 3, wherein the surface-protecting layer is a cured ionizing radiation-curable resin composition. 14. The decorative sheet according to claim 4, wherein the surface-protecting layer is a cured ionizing radiation-curable resin composition. 15. The decorative sheet according to claim 2, wherein the decorative sheet having the base sheet, the ornamental layer, the resin layer, and the surface-protecting layer in this order, and the resin layer and the surface-protecting layer are transparent. 16. The decorative sheet according to claim 3, wherein the decorative sheet having the base sheet, the ornamental layer, the resin layer, and the surface-protecting layer in this order, and the resin layer and the surface-protecting layer are transparent. 17. The decorative sheet according to claim 2, wherein the decorative sheet is used for lamination or wrapping. 18. The decorative sheet according to claim 3, wherein the decorative sheet is used for lamination or wrapping. 19. A decorative member, wherein a surface on the base sheet side of the decorative sheet according to claim 2 is adhered to an adherend via an adhesive layer. 20. A decorative member, wherein a surface on the base sheet side of the decorative sheet according to claim 3 is adhered to an adherend via an adhesive layer. | Provided is a decorative sheet for decreased thickness, and ensure superior molding processability and designability including external appearance (including the finished state) and texture (feel). The present invention relates to a decorative sheet, comprising a base sheet formed of a polyester resin or a polyolefin resin; and an ornamental layer and a surface-protecting layer provided on the base sheet in this order, the decorative sheet having a total thickness of 70 to 135 μm, at least the surface-protecting layer having recesses, the maximum depth of each recess being 15 to 100% based on the total thickness and not less than 15 μm, the ratio of a tensile elastic modulus at 120° C. to a tensile elastic modulus at 20° C. being 1:12 to 1:160, and the ratio of a maximum point load at 120° C. to a maximum point load at 20° C. upon 30-mm stretching being 1:1.7 to 1:30.1. A decorative sheet, comprising a base sheet formed of a polyester resin or a polyolefin resin; and an ornamental layer and a surface-protecting layer provided on the base sheet in this order;
the decorative sheet having a total thickness of 70 to 135 μm, at least the surface-protecting layer having recesses, the maximum depth of each recess being 15 to 100% based on the total thickness and not less than 15 μm, the ratio of a tensile elastic modulus at 120° C. to a tensile elastic modulus at 20° C. being 1:12 to 1:160, and the ratio of a maximum point load at 120° C. to a maximum point load at 20° C. upon 30-mm stretching being 1:1.7 to 1:30. 2. The decorative sheet according to claim 1, wherein the decorative sheet further comprises a resin layer between the base sheet and the surface-protecting layer. 3. The decorative sheet according to claim 1, wherein the base sheet is formed of a polyolefin resin. 4. The decorative sheet according to claim 2, wherein the resin layer is formed of a polyolefin resin. 5. The decorative sheet according to claim 1, wherein the surface-protecting layer is a cured ionizing radiation-curable resin composition. 6. The decorative sheet according to claim 1, wherein the decorative sheet having the base sheet, the ornamental layer, the resin layer, and the surface-protecting layer in this order, and the resin layer and the surface-protecting layer are transparent. 7. The decorative sheet according to claim 1, wherein the decorative sheet is used for lamination or wrapping. 8. A decorative member, wherein a surface on the base sheet side of the decorative sheet according to claim 1 is adhered to an adherend via an adhesive layer. 9. The decorative sheet according to claim 2, wherein the base sheet is formed of a polyolefin resin. 10. The decorative sheet according to claim 3, wherein the resin layer is formed of a polyolefin resin. 11. The decorative sheet according to claim 9, wherein the resin layer is formed of a polyolefin resin. 12. The decorative sheet according to claim 2, wherein the surface-protecting layer is a cured ionizing radiation-curable resin composition. 13. The decorative sheet according to claim 3, wherein the surface-protecting layer is a cured ionizing radiation-curable resin composition. 14. The decorative sheet according to claim 4, wherein the surface-protecting layer is a cured ionizing radiation-curable resin composition. 15. The decorative sheet according to claim 2, wherein the decorative sheet having the base sheet, the ornamental layer, the resin layer, and the surface-protecting layer in this order, and the resin layer and the surface-protecting layer are transparent. 16. The decorative sheet according to claim 3, wherein the decorative sheet having the base sheet, the ornamental layer, the resin layer, and the surface-protecting layer in this order, and the resin layer and the surface-protecting layer are transparent. 17. The decorative sheet according to claim 2, wherein the decorative sheet is used for lamination or wrapping. 18. The decorative sheet according to claim 3, wherein the decorative sheet is used for lamination or wrapping. 19. A decorative member, wherein a surface on the base sheet side of the decorative sheet according to claim 2 is adhered to an adherend via an adhesive layer. 20. A decorative member, wherein a surface on the base sheet side of the decorative sheet according to claim 3 is adhered to an adherend via an adhesive layer. | 1,700 |
3,493 | 14,344,840 | 1,733 | Disclosed are ruthenium nanoparticles having an essentially face-centered cubic structure. Disclosed is a method for producing ruthenium nanoparticles having an essentially face-centered cubic structure. This production method includes a step (i) of maintaining a solution containing ruthenium (III) acetylacetonate, polyvinylpyrrolidone, and triethylene glycol at a temperature of 180° C. or higher. | 1. Ruthenium nanoparticles having an essentially face-centered cubic structure. 2. A carbon monoxide oxidation catalyst comprising the ruthenium nanoparticles according to claim 1. 3. A method for producing ruthenium nanoparticles having an essentially face-centered cubic structure, the method comprising a step (i) of maintaining a solution containing ruthenium (III) acetylacetonate, polyvinylpyrrolidone, and triethylene glycol at a temperature of 180° C. or higher. 4. The method according to claim 3, wherein, in the step (i), the solution is maintained at a temperature ranging from 180° C. to 220° C. 5. The method according to claim 3, wherein
the step (i) comprises: a step (a) of preparing a first organic solution containing polyvinylpyrrolidone and triethylene glycol and a second organic solution containing ruthenium (III) acetylacetonate; and a step (b) of spraying the second organic solution into the first organic solution heated to a temperature ranging from 200° C. to 220° C. | Disclosed are ruthenium nanoparticles having an essentially face-centered cubic structure. Disclosed is a method for producing ruthenium nanoparticles having an essentially face-centered cubic structure. This production method includes a step (i) of maintaining a solution containing ruthenium (III) acetylacetonate, polyvinylpyrrolidone, and triethylene glycol at a temperature of 180° C. or higher.1. Ruthenium nanoparticles having an essentially face-centered cubic structure. 2. A carbon monoxide oxidation catalyst comprising the ruthenium nanoparticles according to claim 1. 3. A method for producing ruthenium nanoparticles having an essentially face-centered cubic structure, the method comprising a step (i) of maintaining a solution containing ruthenium (III) acetylacetonate, polyvinylpyrrolidone, and triethylene glycol at a temperature of 180° C. or higher. 4. The method according to claim 3, wherein, in the step (i), the solution is maintained at a temperature ranging from 180° C. to 220° C. 5. The method according to claim 3, wherein
the step (i) comprises: a step (a) of preparing a first organic solution containing polyvinylpyrrolidone and triethylene glycol and a second organic solution containing ruthenium (III) acetylacetonate; and a step (b) of spraying the second organic solution into the first organic solution heated to a temperature ranging from 200° C. to 220° C. | 1,700 |
3,494 | 14,696,879 | 1,727 | A membrane electrode assembly for a fuel cell that includes a membrane electrode unit with a membrane and two electrodes which make surface contact with both faces of the membrane. The membrane electrode assembly has a seal support that surrounds the periphery of the membrane and that overlaps the latter. The membrane electrode also has a connecting layer which continuously overlaps the membrane and the seal support, an inner edge section of the connecting layer being bonded to the membrane electrode unit and an outer edge section of the connecting layer being bonded to the seal support on the same flat face of the connecting layer. A seal is connected outside the membrane to the seal support. A fuel cell is provided that includes a plurality of membrane electrode assemblies. A motor vehicle includes the fuel cell and a method is provided for producing the membrane electrode assembly. | 1. A membrane electrode arrangement for a fuel cell, comprising:
a membrane electrode assembly that includes a membrane and two electrodes that make surface contact with both sides of the membrane; a seal support that circumferentially surrounds and overlaps the membrane; a connecting layer that circumferentially overlaps the membrane and the seal support, an inner edge section of the connecting layer being integrally connected to the membrane electrode assembly, and an outer edge section of the connecting layer being integrally connected to the seal support on a same flat side of the connecting layer; and a seal that is connected to the seal support outside the membrane. 2. The membrane electrode arrangement according to claim 1, wherein the connecting layer is disposed on a flat side of the membrane opposite the seal support. 3. The membrane electrode arrangement according to claim 1, wherein the integral connection is an adhesive bond. 4. The membrane electrode arrangement according to claim 1, wherein the connecting layer is coated with an adhesive or a self-adhesive film. 5. The membrane electrode arrangement according to claim 1, wherein an inner edge of the connecting layer ends in an offset against an inner edge of the seal support or projects beyond it. 6. The membrane electrode arrangement according to claim 1, wherein the seal support has a perforation along which the seal extends on both sides of the seal support, wherein a first subsection of the seal is disposed on a first flat side and a second subsection is disposed on the second flat side of the seal support, and wherein the first and second subsections are connected to each other as a single piece via the perforation. 7. A fuel cell comprising a plurality of alternately stacked bipolar plates and a membrane electrode arrangement according to claim 1. 8. A motor vehicle comprising a fuel cell according to claim 7. 9. A method for manufacturing a membrane electrode arrangement according to claim 1, the method comprising:
manufacturing the seal in a region of the seal support; and integrally connecting the inner edge section of the connecting layer to the membrane electrode assembly and the outer edge section of the connecting layer to the seal support. 10. The method according to claim 9, wherein the seal is overmolded onto the seal support. | A membrane electrode assembly for a fuel cell that includes a membrane electrode unit with a membrane and two electrodes which make surface contact with both faces of the membrane. The membrane electrode assembly has a seal support that surrounds the periphery of the membrane and that overlaps the latter. The membrane electrode also has a connecting layer which continuously overlaps the membrane and the seal support, an inner edge section of the connecting layer being bonded to the membrane electrode unit and an outer edge section of the connecting layer being bonded to the seal support on the same flat face of the connecting layer. A seal is connected outside the membrane to the seal support. A fuel cell is provided that includes a plurality of membrane electrode assemblies. A motor vehicle includes the fuel cell and a method is provided for producing the membrane electrode assembly.1. A membrane electrode arrangement for a fuel cell, comprising:
a membrane electrode assembly that includes a membrane and two electrodes that make surface contact with both sides of the membrane; a seal support that circumferentially surrounds and overlaps the membrane; a connecting layer that circumferentially overlaps the membrane and the seal support, an inner edge section of the connecting layer being integrally connected to the membrane electrode assembly, and an outer edge section of the connecting layer being integrally connected to the seal support on a same flat side of the connecting layer; and a seal that is connected to the seal support outside the membrane. 2. The membrane electrode arrangement according to claim 1, wherein the connecting layer is disposed on a flat side of the membrane opposite the seal support. 3. The membrane electrode arrangement according to claim 1, wherein the integral connection is an adhesive bond. 4. The membrane electrode arrangement according to claim 1, wherein the connecting layer is coated with an adhesive or a self-adhesive film. 5. The membrane electrode arrangement according to claim 1, wherein an inner edge of the connecting layer ends in an offset against an inner edge of the seal support or projects beyond it. 6. The membrane electrode arrangement according to claim 1, wherein the seal support has a perforation along which the seal extends on both sides of the seal support, wherein a first subsection of the seal is disposed on a first flat side and a second subsection is disposed on the second flat side of the seal support, and wherein the first and second subsections are connected to each other as a single piece via the perforation. 7. A fuel cell comprising a plurality of alternately stacked bipolar plates and a membrane electrode arrangement according to claim 1. 8. A motor vehicle comprising a fuel cell according to claim 7. 9. A method for manufacturing a membrane electrode arrangement according to claim 1, the method comprising:
manufacturing the seal in a region of the seal support; and integrally connecting the inner edge section of the connecting layer to the membrane electrode assembly and the outer edge section of the connecting layer to the seal support. 10. The method according to claim 9, wherein the seal is overmolded onto the seal support. | 1,700 |
3,495 | 13,859,236 | 1,788 | An adhesive bonding film comprises at least one layer of thermally curable resin. The thermally curable resin includes embedded metal particles adapted to be excited to produce heat for curing the resin. | 1. An adhesive bonding film, comprising:
at least one layer of thermally curable resin, the thermally curable resin including embedded metal particles adapted to be excited to produce heat for curing the resin. 2. The adhesive bonding film of claim 1, wherein the embedded metal particles are nano-particulate iron. 3. The adhesive bonding film of claim 1, wherein:
the thermally curable resin includes a thickening material, and the metal particles are encapsulated within the thickening material. 4. The adhesive bonding film of claim 3, wherein the thickening material is a hydrophobic fumed silica. 5. The adhesive bonding film of claim 1, wherein the thermally curable resin includes a thermally activated catalyst. 6. The adhesive bonding film of claim 1, including a scrim embedded in the layer of thermally curable resin. 7. The adhesive bonding film of claim 1, wherein the metal particles are dispersed substantially throughout the layer of thermally curable resin. 8. The adhesive bonding film of claim 1, wherein the embedded metal particles may be excited to produce heat by an electromagnetic field. 9. The adhesive bonding film of claim 1, wherein the metal particles are ferromagnetic. 10. The adhesive bonding film of claim 1, wherein the metal particles are encapsulated in a glass. 11. The adhesive bonding film of claim 10, wherein the glass is a hydrophobic fumed silica. 12. A method of making an adhesive bonding film, comprising:
forming a layer of an adhesive resin that may be thermally activated to cure; mixing metal particles into the layer of the adhesive resin; generating heat by exciting the metal particles using an electro-magnetic field; and using the heat generated by excitation of the metal particles to thermally cure the layer of the adhesive. 13. The method of claim 12, further comprising:
encapsulating the metal particles in a glass. 14. The method of claim 13, wherein encapsulating the metal particles includes a coating the metal particles in a hydrophobic fumed silica. 15. The method of claim 12, wherein excitation of the metal particles is performed by electromagnetic induction. 16. The method of claim 12, wherein the mixing is performed by introducing a dispersion of nano-particles into the adhesive resin 17. An adhesive bonding film made by the method of claim 12. 18. A method of bonding together first and second composite parts, comprising:
introducing a dispersion of ferromagnetic nano-particles into a layer of adhesive resin; placing the layer of adhesive resin between two bonding surfaces respectively of the first and second composite parts; and thermally curing the adhesive resin by exciting the ferromagnetic nano-particles. 19. The method of claim 18, wherein exciting the ferromagnetic nano-particles is performed by electromagnetic induction. 20. The method of claim 19, wherein the electromagnetic induction is performed by:
using an alternating current driven induction coil to generate an electromagnetic field, and coupling the electromagnetic field with the nano-particles. | An adhesive bonding film comprises at least one layer of thermally curable resin. The thermally curable resin includes embedded metal particles adapted to be excited to produce heat for curing the resin.1. An adhesive bonding film, comprising:
at least one layer of thermally curable resin, the thermally curable resin including embedded metal particles adapted to be excited to produce heat for curing the resin. 2. The adhesive bonding film of claim 1, wherein the embedded metal particles are nano-particulate iron. 3. The adhesive bonding film of claim 1, wherein:
the thermally curable resin includes a thickening material, and the metal particles are encapsulated within the thickening material. 4. The adhesive bonding film of claim 3, wherein the thickening material is a hydrophobic fumed silica. 5. The adhesive bonding film of claim 1, wherein the thermally curable resin includes a thermally activated catalyst. 6. The adhesive bonding film of claim 1, including a scrim embedded in the layer of thermally curable resin. 7. The adhesive bonding film of claim 1, wherein the metal particles are dispersed substantially throughout the layer of thermally curable resin. 8. The adhesive bonding film of claim 1, wherein the embedded metal particles may be excited to produce heat by an electromagnetic field. 9. The adhesive bonding film of claim 1, wherein the metal particles are ferromagnetic. 10. The adhesive bonding film of claim 1, wherein the metal particles are encapsulated in a glass. 11. The adhesive bonding film of claim 10, wherein the glass is a hydrophobic fumed silica. 12. A method of making an adhesive bonding film, comprising:
forming a layer of an adhesive resin that may be thermally activated to cure; mixing metal particles into the layer of the adhesive resin; generating heat by exciting the metal particles using an electro-magnetic field; and using the heat generated by excitation of the metal particles to thermally cure the layer of the adhesive. 13. The method of claim 12, further comprising:
encapsulating the metal particles in a glass. 14. The method of claim 13, wherein encapsulating the metal particles includes a coating the metal particles in a hydrophobic fumed silica. 15. The method of claim 12, wherein excitation of the metal particles is performed by electromagnetic induction. 16. The method of claim 12, wherein the mixing is performed by introducing a dispersion of nano-particles into the adhesive resin 17. An adhesive bonding film made by the method of claim 12. 18. A method of bonding together first and second composite parts, comprising:
introducing a dispersion of ferromagnetic nano-particles into a layer of adhesive resin; placing the layer of adhesive resin between two bonding surfaces respectively of the first and second composite parts; and thermally curing the adhesive resin by exciting the ferromagnetic nano-particles. 19. The method of claim 18, wherein exciting the ferromagnetic nano-particles is performed by electromagnetic induction. 20. The method of claim 19, wherein the electromagnetic induction is performed by:
using an alternating current driven induction coil to generate an electromagnetic field, and coupling the electromagnetic field with the nano-particles. | 1,700 |
3,496 | 14,736,505 | 1,711 | A rodder assembly to be moved through an underground conduit includes a tube adapted to receive fluid under pressure. In some embodiments the rodder assembly includes at least one rigid rod, and a nozzle is attached to the tube to discharge fluid from the tube. | 1. Apparatus to be moved through an underground conduit comprising a rodder assembly, said rodder assembly including a tube adapted to receive fluid under pressure, and means to discharge fluid from said tube. 2. The apparatus of claim 1, said rodder assembly including a rigid rod attached to said tube. 3. The apparatus of claim 2 wherein said rodder assembly includes a sleeve surrounding said tube and said rod to attach said tube to said rod. 4. The apparatus of claim 1 wherein said means to discharge fluid from said tube includes a nozzle attached to said tube. 5. The apparatus of claim 1, said rodder assembly including at least one rigid rod positioned within said tube. 6. The apparatus of claim 5 wherein said means to discharge fluid from said tube includes a nozzle attached to said tube. 7. The apparatus of claim 1, said rodder assembly including a plurality of rods positioned in the wall of said tube. 8. The apparatus of claim 7 wherein said means to discharge fluid from said tube includes a nozzle attached to said tube. 9. The apparatus of claim 1 wherein said tube has a closed end and said means to discharge fluid includes an opening in said closed end. 10. The apparatus of claim 1 wherein said means to discharge fluid includes a plurality of openings spaced along said tube. 11. A method to be performed in an underground conduit comprising the steps of inserting a tube into the conduit, providing fluid under pressure to the tube, and emitting fluid from the tube. 12. The method of claim 11 further comprising the step of attaching a rigid rod to the tube. 13. The method of claim 12 further comprising the step of attaching a nozzle to the tube to perform the step of emitting fluid. 14. The method of claim 11 further comprising the step of inserting at least one rigid rod into the tube. 15. The method of claim 14 further comprising the step of attaching a nozzle to the tube to perform the step of emitting fluid. 16. The method of claim 11 further comprising the step of inserting a plurality of rigid rods in the wall of the tube. 17. The method of claim 16 further comprising the step of attaching a nozzle to the tube to perform the step of emitting fluid. 18. The method of claim 11 wherein the tube has a closed end and further comprising the step of forming an opening in the closed end to perform the step of emitting fluid. 19. The method of claim 11 further comprising the step of forming a plurality of spaced openings along the tube to perform the step of emitting fluid. | A rodder assembly to be moved through an underground conduit includes a tube adapted to receive fluid under pressure. In some embodiments the rodder assembly includes at least one rigid rod, and a nozzle is attached to the tube to discharge fluid from the tube.1. Apparatus to be moved through an underground conduit comprising a rodder assembly, said rodder assembly including a tube adapted to receive fluid under pressure, and means to discharge fluid from said tube. 2. The apparatus of claim 1, said rodder assembly including a rigid rod attached to said tube. 3. The apparatus of claim 2 wherein said rodder assembly includes a sleeve surrounding said tube and said rod to attach said tube to said rod. 4. The apparatus of claim 1 wherein said means to discharge fluid from said tube includes a nozzle attached to said tube. 5. The apparatus of claim 1, said rodder assembly including at least one rigid rod positioned within said tube. 6. The apparatus of claim 5 wherein said means to discharge fluid from said tube includes a nozzle attached to said tube. 7. The apparatus of claim 1, said rodder assembly including a plurality of rods positioned in the wall of said tube. 8. The apparatus of claim 7 wherein said means to discharge fluid from said tube includes a nozzle attached to said tube. 9. The apparatus of claim 1 wherein said tube has a closed end and said means to discharge fluid includes an opening in said closed end. 10. The apparatus of claim 1 wherein said means to discharge fluid includes a plurality of openings spaced along said tube. 11. A method to be performed in an underground conduit comprising the steps of inserting a tube into the conduit, providing fluid under pressure to the tube, and emitting fluid from the tube. 12. The method of claim 11 further comprising the step of attaching a rigid rod to the tube. 13. The method of claim 12 further comprising the step of attaching a nozzle to the tube to perform the step of emitting fluid. 14. The method of claim 11 further comprising the step of inserting at least one rigid rod into the tube. 15. The method of claim 14 further comprising the step of attaching a nozzle to the tube to perform the step of emitting fluid. 16. The method of claim 11 further comprising the step of inserting a plurality of rigid rods in the wall of the tube. 17. The method of claim 16 further comprising the step of attaching a nozzle to the tube to perform the step of emitting fluid. 18. The method of claim 11 wherein the tube has a closed end and further comprising the step of forming an opening in the closed end to perform the step of emitting fluid. 19. The method of claim 11 further comprising the step of forming a plurality of spaced openings along the tube to perform the step of emitting fluid. | 1,700 |
3,497 | 14,971,878 | 1,761 | Methodologies and equipment for using a hypochlorite solution to remove menstrual fluid, underarm perspiration or other hard-to-remove stains from soft fabric articles with reduced damage to the fabric articles when compared with popular chlorine bleaches. The soft fabric articles preferably are in white, although the present invention can also be applied to articles in other colors. In one embodiment, the weight concentration ratio of the alkali metal hydroxide over the hypchlorite salt in the hypochlorite solution is no less than 1:12.5. The hypochlorite solution may contain at least 0.2% by weight of sodium hydroxide and/or have a pH of at least 11.8. | 1-130. (canceled) 131. A method for ascertaining the natural fabric effect quality of a hypochlorite bleach composition, said quality in the range of fabric-damaging to abated-damaging to cotton-safe, said composition in the process of formulation or already existing,
wherein the amounts of the essential components of a bleach composition are expressed in a ratio value as wt % alkali-metal hydroxide over wt % alkali-metal hypochloride-salt, or the reciprocal, which ratio value is selected to define the desired natural fabric effect quality of the composition (eg., 1:30 —fabric-damaging, 1:2 —cotton-safe, etc.), wherein a bleach composition so composed and set with a natural fabric effect quality must be characterized by the selected ratio value that defines said fabric effect quality, wherein said ratio value and the amount of an essential component are expressed as known factors of the ratio equation by which the amount of the other essential component is determined and limited, whereas, for an existing bleach composition the natural fabric effect quality is identified by the value of the bleach ratio calculated as the unknown term of a ratio equation, said calculated ratio value determined and limited by the amounts of the two essential components as known factors of the ratio equation, wherein a bleach composition composed with a pre-selected natural fabric effect quality in the range of damaging to abated-damaging to cotton-safe comprises,
(a) an amount of an alkali-metal hypochlorite -salt, as a known factor of a ratio equation, said amount effective for cleaning stain from a soft-fabric article,
(b) an amount of an alkali-metal hydroxide as an unknown term of the ratio equation, said amount calculated by (a) and (c),
(c) a ratio value, as a known factor of the ratio equation, said value selected in the range 1:30 to 1:1, or reciprocal value selected in the range 30:1 to 1.1, to set the pre-selected quality of natural fabric effect of the bleach composition in the range of fabric-damaging to abated-damaging to cotton-safe;
wherein the pH of said composition is at least 11. 132. The method according to claim 131, further comprising: providing an instruction for a consumer on contacting the cleaning composition with said stain on said soft fabric article. 133. The method according to claim 132, wherein said instruction instructs a consumer on duration of application of said cleaning composition on said stain on said soft fabric article. 134. The method according to claim 133, wherein said duration is at least 1 minute. 135. The method according to claim 133, wherein said duration is at least 5 minutes. 136. The method according to claim 133, wherein said duration is at least 15 minutes. 137. The method according to claim 131, wherein the stain is due to body fluids. 138. The method according to claim 131, wherein said cleaning composition is contained in a container having an instruction thereon regarding said cleaning composition and use thereof. 139. The method according to claim 131, wherein the alkali metal hydroxide is sodium hydroxide, and the hypochlorite salt is sodium hypochlorite. 140. The method according to claim 139, wherein the weight concentration ratio of sodium hydroxide over sodium hypochlorite in the cleaning composition is in the range of 1:1 to 1:30, inclusive. 141. The method according to claim 139, wherein the cleaning composition includes at least 0.2 weight percent of sodium hydroxide. 142. The method according to claim 139, wherein the cleaning composition includes at least 0.5 weight percent of sodium hypochlorite. 143. The method according to claim 131, wherein the soft fabric article comprises cotton. 144. The method according to claim 131, wherein said cleaning composition is contained in a container, said container comprising a spray bottle, whereby said solution is sprayed onto said soft fabric article. 145. An aqueous hypochlotie-salt bleach product for cleaning stain from a soft fabric article, the bleach product with two unique features;
(i) a natural fabric safety quality on contacting a soft fabric article, said natural quality in the range of fabric-damaging to abated-damaging to cotton-safe; (ii) a weight concentration ratio, weight % alkali-metal hydroxide over weight % alkali-metal hypochlorite-salt, or the reciprocal, wherein the selected value of said ratio defines the natural fabric safety quality of the bleach product which can be sorted by the ratio value, wherein the aqueous bleach product comprises, (a) an amount of an alkali-metal hypochlorite -salt, effective for cleaning stain from a soft-fabric article, (b) an amount of an alkali-metal hydroxide as determined by (a), (c), and a ratio equation, (c) a ratio value, said value selected in the range 1:30 to 1:1, or reciprocal value selected in the range 30:1 to 1:1, to set the quality of natural fabric safety of the bleach product in the range of fabric-damaging to abated-damaging to cotton-safe; wherein the pH of said product is at least 11. 146. The bleach product according to claim 145, further comprising: an instruction for removing a stain from a soft fabric article employing said cleaning composition. 147. The bleach product according to claim 146, wherein said instruction instructs a consumer on duration of application of said cleaning composition on a stain on said soft fabric article. 148. The bleach product according to claim 147, wherein said duration is at least 1 minute. 149. The bleach product according to claim 147, wherein said duration is at least 5 minutes. 150. The bleach product according to claim 147, wherein said duration is at least 15 minutes. 151. The bleach product according to claim 145, wherein said cleaning composition is contained in a container having an instruction thereon regarding said cleaning composition and use thereof. 152. The bleach product according to claim 145, wherein the weight concentration ratio of alkali metal hydroxide over hypochlorite salt is in the range of 1:1 to 1:30, inclusive. 153. The bleach product according to claim 145, wherein said cleaning composition is contained in a container, said container comprising a spray bottle, whereby said cleaning composition is sprayed onto said soft fabric article. | Methodologies and equipment for using a hypochlorite solution to remove menstrual fluid, underarm perspiration or other hard-to-remove stains from soft fabric articles with reduced damage to the fabric articles when compared with popular chlorine bleaches. The soft fabric articles preferably are in white, although the present invention can also be applied to articles in other colors. In one embodiment, the weight concentration ratio of the alkali metal hydroxide over the hypchlorite salt in the hypochlorite solution is no less than 1:12.5. The hypochlorite solution may contain at least 0.2% by weight of sodium hydroxide and/or have a pH of at least 11.8.1-130. (canceled) 131. A method for ascertaining the natural fabric effect quality of a hypochlorite bleach composition, said quality in the range of fabric-damaging to abated-damaging to cotton-safe, said composition in the process of formulation or already existing,
wherein the amounts of the essential components of a bleach composition are expressed in a ratio value as wt % alkali-metal hydroxide over wt % alkali-metal hypochloride-salt, or the reciprocal, which ratio value is selected to define the desired natural fabric effect quality of the composition (eg., 1:30 —fabric-damaging, 1:2 —cotton-safe, etc.), wherein a bleach composition so composed and set with a natural fabric effect quality must be characterized by the selected ratio value that defines said fabric effect quality, wherein said ratio value and the amount of an essential component are expressed as known factors of the ratio equation by which the amount of the other essential component is determined and limited, whereas, for an existing bleach composition the natural fabric effect quality is identified by the value of the bleach ratio calculated as the unknown term of a ratio equation, said calculated ratio value determined and limited by the amounts of the two essential components as known factors of the ratio equation, wherein a bleach composition composed with a pre-selected natural fabric effect quality in the range of damaging to abated-damaging to cotton-safe comprises,
(a) an amount of an alkali-metal hypochlorite -salt, as a known factor of a ratio equation, said amount effective for cleaning stain from a soft-fabric article,
(b) an amount of an alkali-metal hydroxide as an unknown term of the ratio equation, said amount calculated by (a) and (c),
(c) a ratio value, as a known factor of the ratio equation, said value selected in the range 1:30 to 1:1, or reciprocal value selected in the range 30:1 to 1.1, to set the pre-selected quality of natural fabric effect of the bleach composition in the range of fabric-damaging to abated-damaging to cotton-safe;
wherein the pH of said composition is at least 11. 132. The method according to claim 131, further comprising: providing an instruction for a consumer on contacting the cleaning composition with said stain on said soft fabric article. 133. The method according to claim 132, wherein said instruction instructs a consumer on duration of application of said cleaning composition on said stain on said soft fabric article. 134. The method according to claim 133, wherein said duration is at least 1 minute. 135. The method according to claim 133, wherein said duration is at least 5 minutes. 136. The method according to claim 133, wherein said duration is at least 15 minutes. 137. The method according to claim 131, wherein the stain is due to body fluids. 138. The method according to claim 131, wherein said cleaning composition is contained in a container having an instruction thereon regarding said cleaning composition and use thereof. 139. The method according to claim 131, wherein the alkali metal hydroxide is sodium hydroxide, and the hypochlorite salt is sodium hypochlorite. 140. The method according to claim 139, wherein the weight concentration ratio of sodium hydroxide over sodium hypochlorite in the cleaning composition is in the range of 1:1 to 1:30, inclusive. 141. The method according to claim 139, wherein the cleaning composition includes at least 0.2 weight percent of sodium hydroxide. 142. The method according to claim 139, wherein the cleaning composition includes at least 0.5 weight percent of sodium hypochlorite. 143. The method according to claim 131, wherein the soft fabric article comprises cotton. 144. The method according to claim 131, wherein said cleaning composition is contained in a container, said container comprising a spray bottle, whereby said solution is sprayed onto said soft fabric article. 145. An aqueous hypochlotie-salt bleach product for cleaning stain from a soft fabric article, the bleach product with two unique features;
(i) a natural fabric safety quality on contacting a soft fabric article, said natural quality in the range of fabric-damaging to abated-damaging to cotton-safe; (ii) a weight concentration ratio, weight % alkali-metal hydroxide over weight % alkali-metal hypochlorite-salt, or the reciprocal, wherein the selected value of said ratio defines the natural fabric safety quality of the bleach product which can be sorted by the ratio value, wherein the aqueous bleach product comprises, (a) an amount of an alkali-metal hypochlorite -salt, effective for cleaning stain from a soft-fabric article, (b) an amount of an alkali-metal hydroxide as determined by (a), (c), and a ratio equation, (c) a ratio value, said value selected in the range 1:30 to 1:1, or reciprocal value selected in the range 30:1 to 1:1, to set the quality of natural fabric safety of the bleach product in the range of fabric-damaging to abated-damaging to cotton-safe; wherein the pH of said product is at least 11. 146. The bleach product according to claim 145, further comprising: an instruction for removing a stain from a soft fabric article employing said cleaning composition. 147. The bleach product according to claim 146, wherein said instruction instructs a consumer on duration of application of said cleaning composition on a stain on said soft fabric article. 148. The bleach product according to claim 147, wherein said duration is at least 1 minute. 149. The bleach product according to claim 147, wherein said duration is at least 5 minutes. 150. The bleach product according to claim 147, wherein said duration is at least 15 minutes. 151. The bleach product according to claim 145, wherein said cleaning composition is contained in a container having an instruction thereon regarding said cleaning composition and use thereof. 152. The bleach product according to claim 145, wherein the weight concentration ratio of alkali metal hydroxide over hypochlorite salt is in the range of 1:1 to 1:30, inclusive. 153. The bleach product according to claim 145, wherein said cleaning composition is contained in a container, said container comprising a spray bottle, whereby said cleaning composition is sprayed onto said soft fabric article. | 1,700 |
3,498 | 14,641,948 | 1,734 | A lightweight, selectively degradable composite material is disclosed. The composite material comprises a compacted powder mixture of a first powder, the first powder comprising first metal particles comprising Mg, Al, Mn, or Zn, or an alloy of any of the above, or a combination of any of the above, having a first particle oxidation potential, a second powder, the second powder comprising low-density ceramic, glass, cermet, intermetallic, metal, polymer, or inorganic compound second particles, and a third metal powder, the third metal powder comprising third metal particles having an oxidation potential that is different than the first particle oxidation potential. The compacted powder mixture has a microstructure comprising a matrix comprising the first metal particles, the second particles and third particles dispersed within the matrix, the third particles comprising a network of third particles extending throughout the matrix, the composite material having a density of about 3.5 g/cm 3 or less. | 1. A lightweight, selectively degradable composite material comprising a compacted powder mixture of a first powder, the first powder comprising first metal particles comprising Mg, Al, Mn, or Zn, or an alloy of any of the above, or a combination of any of the above, having a first particle oxidation potential, a second powder, the second powder comprising low-density ceramic, glass, cermet, intermetallic, metal, polymer, or inorganic compound second particles, and a third metal powder, the third metal powder comprising third metal particles having an oxidation potential that is different than the first particle oxidation potential, the compacted powder mixture having a microstructure comprising:
a matrix comprising the first metal particles; and the second particles and third particles dispersed within the matrix, the third particles comprising a network of third particles extending throughout the matrix, the lightweight, selectively degradable composite material having a density of about 3.5 g/cm3 or less. 2. The composite material of claim 1, wherein the third particles are substantially homogeneously dispersed within the matrix, and the network is substantially discontinuous, wherein adjacent third particles are not in touching contact with one another. 3. The composite material of claim 1, wherein the third particles are substantially homogeneously dispersed within the matrix, and wherein the network is partially continuous and adjacent third particles are in touching contact with one another throughout at least a portion of the matrix. 4. The composite material of claim 1, wherein the third particles are substantially homogeneously dispersed within the matrix, and wherein the network is locally continuous and adjacent third particles are in touching contact with one another throughout a localized portion of the matrix. 5. The composite material of claim 1, wherein the third particles are substantially homogeneously dispersed within the matrix, and wherein the network is continuous and adjacent third particles are in touching contact with one another throughout the matrix. 6. The composite material of claim 1, wherein a portion of the third particles are in touching contact with adjacent third particles and comprise an interconnected network of third particles within the matrix. 7. The composite material of claim 1, wherein the first particle oxidation potential is about 0.7 volts or more, and the third particle oxidation potential is about 0.5 volts or less. 8. The composite material of claim 1, wherein a difference between the first particle oxidation potential and the third particle oxidation potential is about 0.7 to about 2.7 volts. 9. The composite material of claim 1, wherein the lightweight, selectively degradable composite material has a density of about 1.5 to about 3.5 g/cm3. 10. The composite material of claim 1, wherein the composite material has an ultimate compressive strength of at least 80 ksi. 11. The composite material of claim 1, wherein the composite material has an ultimate compressive strength of at least 100 ksi. 12. The composite material of claim 1, wherein the first metal particles have an average size of about 5 to about 300 μm. 13. The composite material of claim 1, wherein the first metal particles have an average size of about 75 to about 150 μm. 14. The composite material of claim 1, wherein the first metal particles comprise a magnesium-base alloy. 15. The composite material of claim 14, wherein the magnesium-base alloy comprises an Mg—Si, Mg—Al, Mg—Zn, Mg—Mn, Mg—Al—Zn, Mg—Al—Mn, Mg—Zn—Zr, or Mg—X alloy, where X comprises a rare earth element, or an alloy thereof, or any other combination of the aforementioned. 16. The composite material of claim 15, wherein the third metal particles comprise Ni, Fe, Cu, or Co, or an alloy thereof, or any combination thereof. 17. The composite material of claim 1, wherein the second particles have a density of about 0.1 to about 4.0 g/cm3. 18. The composite material of claim 1, wherein the metal second particles comprise hollow metal particles. 19. The composite material of claim 1, wherein the metal second particles comprise pure Ti or a Ti alloy. 20. The composite material of claim 1, wherein the metal second particles have an average particle size of about 10 to about 200 μm. 21. The composite material of claim 1, wherein the ceramic, glass, polymer, or inorganic compound particles are hollow or porous. 22. The composite material of claim 1, wherein the ceramic particles comprise metal carbide, nitride, or oxide particles, or a combination thereof. 23. The composite material of claim 1, wherein the ceramic particles comprise silicon carbide particles. 24. The composite material of claim 1, wherein the silicon carbide particles have an average particle size of about 5 to about 200 μm. 25. The composite material of claim 1, wherein the second particles comprise substantially spherical particles. 26. The composite material of claim 1, wherein the second particles comprise substantially non-spherical particles having rounded edges. 27. A selectively degradable article, comprising:
a lightweight, selectively degradable composite material, the composite material comprising a compacted powder mixture of a first powder, the first powder comprising first metal particles comprising Mg, Al, Mn, or Zn, or an alloy of any of the above, or a combination of any of the above, having a first particle oxidation potential, a second powder, the second powder comprising low-density ceramic, glass, cermet, intermetallic, metal, polymer, or inorganic compound second particles, and a third metal powder, the third metal powder comprising third metal particles having an oxidation potential that is different than the first particle oxidation potential, the compacted powder mixture having a microstructure comprising: a matrix comprising the first metal particles; and the second particles and third particles dispersed within the matrix, the third particles comprising a network of third particles extending throughout the matrix, the lightweight, selectively degradable composite material having a density of about 3.5 g/cm3 or less. 28. The article of claim 27, wherein the composite material comprises a selectively degradable downhole article. 29. The article of claim 28, wherein the selectively degradable downhole article comprises a selectively degradable flow inhibition tool or component. 30. The article of claim 29, wherein the selectively degradable flow inhibition tool or component is selected from the group consisting of a frac plug, bridge plug, wiper plug, shear out plug, debris barrier, atmospheric chamber disc, swabbing element protector, sealbore protector, screen protector, beaded screen protector, screen basepipe plug, drill in stim liner plug, inflow control device plug, flapper valve, gaslift valve, transmatic plugs, float shoe, dart, diverter ball, shifting/setting ball, ball seat, plug seat, dart seat, sleeve, teleperf disk, direct connect disk, drill-in liner disk, fluid loss control flapper, shear pin, screw, bolt, and cement plug. 31. The article of claim 30, wherein the article is used in a method comprising at least partially inhibiting a fluid flow in a wellbore. 32. A lightweight, selectively degradable composite material comprising a first matrix of a first metal comprising Mg, Al, Mn, or Zn, or an alloy of any of the above, or a combination of any of the above, having a first oxidation potential, a second powder, the second powder comprising low-density ceramic, glass, cermet, intermetallic, metal, polymer, or inorganic compound second particles, and a third metal powder, the third metal powder comprising third metal particles having an oxidation potential that is different than the first oxidation potential, the composite material having a microstructure comprising:
the matrix of the first metal; and the second particles and third particles dispersed within the matrix, the third particles comprising a network of third particles extending throughout the matrix, the lightweight, selectively degradable composite material having a density of about 3.5 g/cm3 or less. 33. The composite material of claim 32, wherein the third particles are substantially homogeneously dispersed within the matrix, and the network is substantially discontinuous, wherein adjacent third particles are not in touching contact with one another. 34. The composite material of claim 32, wherein the third particles are substantially homogeneously dispersed within the matrix, and wherein the network is partially continuous and adjacent third particles are in touching contact with one another throughout at least a portion of the matrix. 35. The composite material of claim 32, wherein the third particles are substantially homogeneously dispersed within the matrix, and wherein the network is locally continuous and adjacent third particles are in touching contact with one another throughout a localized portion of the matrix. 36. The composite material of claim 32, wherein the third particles are substantially homogeneously dispersed within the matrix, and wherein the network is continuous and adjacent third particles are in touching contact with one another throughout the matrix. 37. The composite material of claim 32, wherein a portion of the third particles are in touching contact with adjacent third particles and comprise an interconnected network of third particles within the matrix. 38. The composite material of claim 32, wherein the first particle oxidation potential is about 0.7 volts or more, and the third particle oxidation potential is about 0.5 volts or less. 39. The composite material of claim 32, wherein the microstructure of the matrix is an as-cast microstructure. 40. The composite material of claim 32, wherein the first metal comprises a magnesium-base alloy. 41. The composite material of claim 40, wherein the magnesium-base alloy comprises an Mg—Si, Mg—Al, Mg—Zn, Mg—Mn, Mg—Al—Zn, Mg—Al—Mn, Mg—Zn—Zr, or Mg—X alloy, where X comprises a rare earth element, or an alloy thereof, or any other combination of the aforementioned. 42. The composite material of claim 41, wherein the third metal particles comprise Ni, Fe, Cu, or Co, or an alloy thereof, or any combination thereof. 43. The composite material of claim 32, wherein the second particles have a density of about 0.1 to about 4.0 g/cm3. 44. The composite material of claim 32, wherein the metal second particles comprise hollow metal particles. 45. The composite material of claim 32, wherein the metal second particles comprise pure Ti or a Ti alloy. 46. A selectively degradable article, comprising:
a lightweight, selectively degradable composite material comprising a first matrix of a first metal comprising Mg, Al, Mn, or Zn, or an alloy of any of the above, or a combination of any of the above, having a first oxidation potential, a second powder, the second powder comprising low-density ceramic, glass, cermet, intermetallic, metal, polymer, or inorganic compound second particles, and a third metal powder, the third metal powder comprising third metal particles having an oxidation potential that is different than the first oxidation potential, the composite material having a microstructure comprising:
the matrix of the first metal; and
the second particles and third particles dispersed within the matrix, the third particles comprising a network of third particles extending throughout the matrix, the lightweight, selectively degradable composite material having a density of about 3.5 g/cm3 or less. 47. The article of claim 46, wherein the composite material comprises a selectively degradable downhole article. 48. The article of claim 47, wherein the selectively degradable downhole article comprises a selectively degradable flow inhibition tool or component. 49. The article of claim 48, wherein the selectively degradable flow inhibition tool or component is selected from the group consisting of a frac plug, bridge plug, wiper plug, shear out plug, debris barrier, atmospheric chamber disc, swabbing element protector, sealbore protector, screen protector, beaded screen protector, screen basepipe plug, drill in stim liner plug, inflow control device plug, flapper valve, gaslift valve, transmatic plug, float shoe, dart, diverter ball, shifting/setting ball, ball seat, plug seat, dart seat, sleeve, teleperf disk, direct connect disk, drill-in liner disk, fluid loss control flapper, shear pin, screw, bolt, and cement plug. 50. The article of claim 46, wherein the article is used in a method comprising at least partially inhibiting a fluid flow in a wellbore. | A lightweight, selectively degradable composite material is disclosed. The composite material comprises a compacted powder mixture of a first powder, the first powder comprising first metal particles comprising Mg, Al, Mn, or Zn, or an alloy of any of the above, or a combination of any of the above, having a first particle oxidation potential, a second powder, the second powder comprising low-density ceramic, glass, cermet, intermetallic, metal, polymer, or inorganic compound second particles, and a third metal powder, the third metal powder comprising third metal particles having an oxidation potential that is different than the first particle oxidation potential. The compacted powder mixture has a microstructure comprising a matrix comprising the first metal particles, the second particles and third particles dispersed within the matrix, the third particles comprising a network of third particles extending throughout the matrix, the composite material having a density of about 3.5 g/cm 3 or less.1. A lightweight, selectively degradable composite material comprising a compacted powder mixture of a first powder, the first powder comprising first metal particles comprising Mg, Al, Mn, or Zn, or an alloy of any of the above, or a combination of any of the above, having a first particle oxidation potential, a second powder, the second powder comprising low-density ceramic, glass, cermet, intermetallic, metal, polymer, or inorganic compound second particles, and a third metal powder, the third metal powder comprising third metal particles having an oxidation potential that is different than the first particle oxidation potential, the compacted powder mixture having a microstructure comprising:
a matrix comprising the first metal particles; and the second particles and third particles dispersed within the matrix, the third particles comprising a network of third particles extending throughout the matrix, the lightweight, selectively degradable composite material having a density of about 3.5 g/cm3 or less. 2. The composite material of claim 1, wherein the third particles are substantially homogeneously dispersed within the matrix, and the network is substantially discontinuous, wherein adjacent third particles are not in touching contact with one another. 3. The composite material of claim 1, wherein the third particles are substantially homogeneously dispersed within the matrix, and wherein the network is partially continuous and adjacent third particles are in touching contact with one another throughout at least a portion of the matrix. 4. The composite material of claim 1, wherein the third particles are substantially homogeneously dispersed within the matrix, and wherein the network is locally continuous and adjacent third particles are in touching contact with one another throughout a localized portion of the matrix. 5. The composite material of claim 1, wherein the third particles are substantially homogeneously dispersed within the matrix, and wherein the network is continuous and adjacent third particles are in touching contact with one another throughout the matrix. 6. The composite material of claim 1, wherein a portion of the third particles are in touching contact with adjacent third particles and comprise an interconnected network of third particles within the matrix. 7. The composite material of claim 1, wherein the first particle oxidation potential is about 0.7 volts or more, and the third particle oxidation potential is about 0.5 volts or less. 8. The composite material of claim 1, wherein a difference between the first particle oxidation potential and the third particle oxidation potential is about 0.7 to about 2.7 volts. 9. The composite material of claim 1, wherein the lightweight, selectively degradable composite material has a density of about 1.5 to about 3.5 g/cm3. 10. The composite material of claim 1, wherein the composite material has an ultimate compressive strength of at least 80 ksi. 11. The composite material of claim 1, wherein the composite material has an ultimate compressive strength of at least 100 ksi. 12. The composite material of claim 1, wherein the first metal particles have an average size of about 5 to about 300 μm. 13. The composite material of claim 1, wherein the first metal particles have an average size of about 75 to about 150 μm. 14. The composite material of claim 1, wherein the first metal particles comprise a magnesium-base alloy. 15. The composite material of claim 14, wherein the magnesium-base alloy comprises an Mg—Si, Mg—Al, Mg—Zn, Mg—Mn, Mg—Al—Zn, Mg—Al—Mn, Mg—Zn—Zr, or Mg—X alloy, where X comprises a rare earth element, or an alloy thereof, or any other combination of the aforementioned. 16. The composite material of claim 15, wherein the third metal particles comprise Ni, Fe, Cu, or Co, or an alloy thereof, or any combination thereof. 17. The composite material of claim 1, wherein the second particles have a density of about 0.1 to about 4.0 g/cm3. 18. The composite material of claim 1, wherein the metal second particles comprise hollow metal particles. 19. The composite material of claim 1, wherein the metal second particles comprise pure Ti or a Ti alloy. 20. The composite material of claim 1, wherein the metal second particles have an average particle size of about 10 to about 200 μm. 21. The composite material of claim 1, wherein the ceramic, glass, polymer, or inorganic compound particles are hollow or porous. 22. The composite material of claim 1, wherein the ceramic particles comprise metal carbide, nitride, or oxide particles, or a combination thereof. 23. The composite material of claim 1, wherein the ceramic particles comprise silicon carbide particles. 24. The composite material of claim 1, wherein the silicon carbide particles have an average particle size of about 5 to about 200 μm. 25. The composite material of claim 1, wherein the second particles comprise substantially spherical particles. 26. The composite material of claim 1, wherein the second particles comprise substantially non-spherical particles having rounded edges. 27. A selectively degradable article, comprising:
a lightweight, selectively degradable composite material, the composite material comprising a compacted powder mixture of a first powder, the first powder comprising first metal particles comprising Mg, Al, Mn, or Zn, or an alloy of any of the above, or a combination of any of the above, having a first particle oxidation potential, a second powder, the second powder comprising low-density ceramic, glass, cermet, intermetallic, metal, polymer, or inorganic compound second particles, and a third metal powder, the third metal powder comprising third metal particles having an oxidation potential that is different than the first particle oxidation potential, the compacted powder mixture having a microstructure comprising: a matrix comprising the first metal particles; and the second particles and third particles dispersed within the matrix, the third particles comprising a network of third particles extending throughout the matrix, the lightweight, selectively degradable composite material having a density of about 3.5 g/cm3 or less. 28. The article of claim 27, wherein the composite material comprises a selectively degradable downhole article. 29. The article of claim 28, wherein the selectively degradable downhole article comprises a selectively degradable flow inhibition tool or component. 30. The article of claim 29, wherein the selectively degradable flow inhibition tool or component is selected from the group consisting of a frac plug, bridge plug, wiper plug, shear out plug, debris barrier, atmospheric chamber disc, swabbing element protector, sealbore protector, screen protector, beaded screen protector, screen basepipe plug, drill in stim liner plug, inflow control device plug, flapper valve, gaslift valve, transmatic plugs, float shoe, dart, diverter ball, shifting/setting ball, ball seat, plug seat, dart seat, sleeve, teleperf disk, direct connect disk, drill-in liner disk, fluid loss control flapper, shear pin, screw, bolt, and cement plug. 31. The article of claim 30, wherein the article is used in a method comprising at least partially inhibiting a fluid flow in a wellbore. 32. A lightweight, selectively degradable composite material comprising a first matrix of a first metal comprising Mg, Al, Mn, or Zn, or an alloy of any of the above, or a combination of any of the above, having a first oxidation potential, a second powder, the second powder comprising low-density ceramic, glass, cermet, intermetallic, metal, polymer, or inorganic compound second particles, and a third metal powder, the third metal powder comprising third metal particles having an oxidation potential that is different than the first oxidation potential, the composite material having a microstructure comprising:
the matrix of the first metal; and the second particles and third particles dispersed within the matrix, the third particles comprising a network of third particles extending throughout the matrix, the lightweight, selectively degradable composite material having a density of about 3.5 g/cm3 or less. 33. The composite material of claim 32, wherein the third particles are substantially homogeneously dispersed within the matrix, and the network is substantially discontinuous, wherein adjacent third particles are not in touching contact with one another. 34. The composite material of claim 32, wherein the third particles are substantially homogeneously dispersed within the matrix, and wherein the network is partially continuous and adjacent third particles are in touching contact with one another throughout at least a portion of the matrix. 35. The composite material of claim 32, wherein the third particles are substantially homogeneously dispersed within the matrix, and wherein the network is locally continuous and adjacent third particles are in touching contact with one another throughout a localized portion of the matrix. 36. The composite material of claim 32, wherein the third particles are substantially homogeneously dispersed within the matrix, and wherein the network is continuous and adjacent third particles are in touching contact with one another throughout the matrix. 37. The composite material of claim 32, wherein a portion of the third particles are in touching contact with adjacent third particles and comprise an interconnected network of third particles within the matrix. 38. The composite material of claim 32, wherein the first particle oxidation potential is about 0.7 volts or more, and the third particle oxidation potential is about 0.5 volts or less. 39. The composite material of claim 32, wherein the microstructure of the matrix is an as-cast microstructure. 40. The composite material of claim 32, wherein the first metal comprises a magnesium-base alloy. 41. The composite material of claim 40, wherein the magnesium-base alloy comprises an Mg—Si, Mg—Al, Mg—Zn, Mg—Mn, Mg—Al—Zn, Mg—Al—Mn, Mg—Zn—Zr, or Mg—X alloy, where X comprises a rare earth element, or an alloy thereof, or any other combination of the aforementioned. 42. The composite material of claim 41, wherein the third metal particles comprise Ni, Fe, Cu, or Co, or an alloy thereof, or any combination thereof. 43. The composite material of claim 32, wherein the second particles have a density of about 0.1 to about 4.0 g/cm3. 44. The composite material of claim 32, wherein the metal second particles comprise hollow metal particles. 45. The composite material of claim 32, wherein the metal second particles comprise pure Ti or a Ti alloy. 46. A selectively degradable article, comprising:
a lightweight, selectively degradable composite material comprising a first matrix of a first metal comprising Mg, Al, Mn, or Zn, or an alloy of any of the above, or a combination of any of the above, having a first oxidation potential, a second powder, the second powder comprising low-density ceramic, glass, cermet, intermetallic, metal, polymer, or inorganic compound second particles, and a third metal powder, the third metal powder comprising third metal particles having an oxidation potential that is different than the first oxidation potential, the composite material having a microstructure comprising:
the matrix of the first metal; and
the second particles and third particles dispersed within the matrix, the third particles comprising a network of third particles extending throughout the matrix, the lightweight, selectively degradable composite material having a density of about 3.5 g/cm3 or less. 47. The article of claim 46, wherein the composite material comprises a selectively degradable downhole article. 48. The article of claim 47, wherein the selectively degradable downhole article comprises a selectively degradable flow inhibition tool or component. 49. The article of claim 48, wherein the selectively degradable flow inhibition tool or component is selected from the group consisting of a frac plug, bridge plug, wiper plug, shear out plug, debris barrier, atmospheric chamber disc, swabbing element protector, sealbore protector, screen protector, beaded screen protector, screen basepipe plug, drill in stim liner plug, inflow control device plug, flapper valve, gaslift valve, transmatic plug, float shoe, dart, diverter ball, shifting/setting ball, ball seat, plug seat, dart seat, sleeve, teleperf disk, direct connect disk, drill-in liner disk, fluid loss control flapper, shear pin, screw, bolt, and cement plug. 50. The article of claim 46, wherein the article is used in a method comprising at least partially inhibiting a fluid flow in a wellbore. | 1,700 |
3,499 | 15,296,755 | 1,744 | An ink composition for use in digital offset printing including a white colorant, a translucent colorant, or a combination thereof; wherein the white colorant, translucent colorant, or combination thereof is present in an amount of at least 50 percent by weight based on the total weight of the ink composition; at least one component selected from the group consisting of a curable monomer and a curable oligomer; at least one phase change agent; an optional dispersant; an optional photoinitiator. A process of digital offset printing including applying the ink composition onto a re-imageable imaging member surface at an ink take up temperature, the re-imageable imaging member having dampening fluid disposed thereon; forming an ink image; transferring the ink image from the re-imageable surface of the imaging member to a printable substrate at an ink transfer temperature. | 1. An ink composition for use in digital offset printing, comprising:
a white colorant, a translucent colorant, or a combination thereof; wherein the white colorant, translucent colorant, or combination thereof is present in an amount of at least 50 percent by weight based upon the total weight of the ink composition; at least one component selected from the group consisting of a curable monomer and a curable oligomer; at least one phase change agent; an optional dispersant; and an optional photoinitiator. 2. The ink composition of claim 1, wherein the phase change agent has the characteristic of providing the ink composition with a first lower viscosity at an ink take up temperature and a second higher viscosity at an ink transfer temperature wherein the ink take up temperature is higher than the ink transfer temperature. 3. The ink composition of claim 1, wherein the ink composition has a first viscosity of from about 3,000 to about 90,000 centipoise at an ink take up temperature of from about 45° C. to about 80° C.; and
wherein the ink composition has a second viscosity of from about 100,000 to about 2,000,000 centipoise at an ink transfer temperature of from about 18° C. to about 30° C. 4. The ink composition of claim 1, wherein the ink composition has a first viscosity of from about 3,000 to about 90,000 centipoise at an ink take up temperature of from about 45° C. to about 80° C. and a relatively higher shear rate of from about 50 rad/s to about 200 rad/s; and
wherein the ink composition has a second viscosity of from about 100,000 to about 2,000,000 centipoise at an ink transfer temperature of from about 18° C. to about 30° C. and a relatively lower shear rate of from about 0.5 rad/s to about 2 rad/s. 5. The ink composition of claim 1, wherein the colorant is a white colorant present in an amount of greater than 50 percent by weight to about 85 percent by weight, based upon the total weight of the ink composition. 6. The ink composition of claim 1, wherein the colorant is selected from the group consisting of titanium dioxide, rutile, zinc oxide, zinc sulfide, calcium carbonate, clay, lithopone (a mixture of barium sulphate and zinc sulfide), and combinations thereof. 7. The ink composition of claim 1, further comprising a non-white colorant. 8. The ink composition of claim 1, further comprising a non-white colorant, wherein the non-white colorant is an inorganic metal oxide pigment; and
wherein the inorganic metal oxide pigment is present in an amount of less than 5 percent by weight based on the total weight of the ink composition. 9. The ink composition of claim 1, wherein the at least one component selected from the group consisting of a curable monomer and a curable oligomer is a component selected from the group consisting of acrylated polyesters, acrylated polyethers, acrylated epoxies, urethane acrylates, and pentaerythritol tetraacrylate, and combinations thereof. 10. The ink composition of claim 1, wherein the at least one component selected from the group consisting of a curable monomer and a curable oligomer is a component selected from the group consisting of a tetrafunctional polyester acrylate oligomer, a propoxylated trimethylolpropane triacrylate monomer, and combinations thereof. 11. A process of digital offset printing, the process comprising:
applying an ink composition onto a re-imageable imaging member surface at an ink take up temperature, the re-imageable imaging member having dampening fluid disposed thereon; forming an ink image; transferring the ink image from the re-imageable surface of the imaging member to a printable substrate at an ink transfer temperature; wherein the ink composition comprises: a white colorant, a translucent colorant, or a combination thereof; wherein the white colorant, translucent colorant, or combination thereof is present in an amount of at least 50 percent by weight based upon the total weight of the ink composition; at least one component selected from the group consisting of a curable monomer and a curable oligomer; at least one phase change agent, wherein the phase change agent has the characteristic of providing the ink composition with a first lower viscosity at an ink take up temperature and a second higher viscosity at an ink transfer temperature wherein the ink take up temperature is higher than the ink transfer temperature.; an optional dispersant; and an optional photoinitiator. 12. The process of claim 11, wherein the ink composition has a first viscosity of from about 3,000 to about 90,000 centipoise at an ink take up temperature of from about 45° C. to about 80° C.; and
wherein the ink composition has a second viscosity of from about 100,000 to about 2,000,000 centipoise at an ink transfer temperature of from about 18° C. to about 30° C. 13. The process of claim 11, wherein the colorant is a white colorant present in an amount of greater than 50 percent by weight to about 85 percent by weight, based upon the total weight of the ink composition. 14. The process of claim 11, further comprising:
a non-white colorant. 15. The process of claim 11, wherein the colorant is selected from the group consisting of titanium dioxide, rutile, zinc oxide, zinc sulfide, calcium carbonate, clay, lithopone (a mixture of barium sulphate and zinc sulfide), and combinations thereof. 16. The process of claim 11, wherein the ink composition further comprises a non-white colorant, wherein the non-white colorant is an inorganic metal oxide pigment; and
wherein the inorganic metal oxide pigment is present in an amount of less than 5 percent by weight based on the total weight of the ink composition. 17. The process of claim 11, wherein the substrate is selected from the group consisting of paper, plastic, folded paperboard, Kraft paper, and metal. 18. The process of claim 11, wherein the substrate is a label. 19. The process of claim 11, wherein applying the ink composition comprises applying the ink composition using an anilox delivery system. 20. The process of claim 11, wherein applying the ink composition comprises applying the ink composition to form an undercoat. 21. The ink composition of claim 1, wherein the phase change agent is a gellant. 22. The ink composition of claim 1, wherein the phase change agent is a non-curable gellant. 23. The ink composition of claim 1, wherein the phase change agent is an ester-terminated polyamide gellant. | An ink composition for use in digital offset printing including a white colorant, a translucent colorant, or a combination thereof; wherein the white colorant, translucent colorant, or combination thereof is present in an amount of at least 50 percent by weight based on the total weight of the ink composition; at least one component selected from the group consisting of a curable monomer and a curable oligomer; at least one phase change agent; an optional dispersant; an optional photoinitiator. A process of digital offset printing including applying the ink composition onto a re-imageable imaging member surface at an ink take up temperature, the re-imageable imaging member having dampening fluid disposed thereon; forming an ink image; transferring the ink image from the re-imageable surface of the imaging member to a printable substrate at an ink transfer temperature.1. An ink composition for use in digital offset printing, comprising:
a white colorant, a translucent colorant, or a combination thereof; wherein the white colorant, translucent colorant, or combination thereof is present in an amount of at least 50 percent by weight based upon the total weight of the ink composition; at least one component selected from the group consisting of a curable monomer and a curable oligomer; at least one phase change agent; an optional dispersant; and an optional photoinitiator. 2. The ink composition of claim 1, wherein the phase change agent has the characteristic of providing the ink composition with a first lower viscosity at an ink take up temperature and a second higher viscosity at an ink transfer temperature wherein the ink take up temperature is higher than the ink transfer temperature. 3. The ink composition of claim 1, wherein the ink composition has a first viscosity of from about 3,000 to about 90,000 centipoise at an ink take up temperature of from about 45° C. to about 80° C.; and
wherein the ink composition has a second viscosity of from about 100,000 to about 2,000,000 centipoise at an ink transfer temperature of from about 18° C. to about 30° C. 4. The ink composition of claim 1, wherein the ink composition has a first viscosity of from about 3,000 to about 90,000 centipoise at an ink take up temperature of from about 45° C. to about 80° C. and a relatively higher shear rate of from about 50 rad/s to about 200 rad/s; and
wherein the ink composition has a second viscosity of from about 100,000 to about 2,000,000 centipoise at an ink transfer temperature of from about 18° C. to about 30° C. and a relatively lower shear rate of from about 0.5 rad/s to about 2 rad/s. 5. The ink composition of claim 1, wherein the colorant is a white colorant present in an amount of greater than 50 percent by weight to about 85 percent by weight, based upon the total weight of the ink composition. 6. The ink composition of claim 1, wherein the colorant is selected from the group consisting of titanium dioxide, rutile, zinc oxide, zinc sulfide, calcium carbonate, clay, lithopone (a mixture of barium sulphate and zinc sulfide), and combinations thereof. 7. The ink composition of claim 1, further comprising a non-white colorant. 8. The ink composition of claim 1, further comprising a non-white colorant, wherein the non-white colorant is an inorganic metal oxide pigment; and
wherein the inorganic metal oxide pigment is present in an amount of less than 5 percent by weight based on the total weight of the ink composition. 9. The ink composition of claim 1, wherein the at least one component selected from the group consisting of a curable monomer and a curable oligomer is a component selected from the group consisting of acrylated polyesters, acrylated polyethers, acrylated epoxies, urethane acrylates, and pentaerythritol tetraacrylate, and combinations thereof. 10. The ink composition of claim 1, wherein the at least one component selected from the group consisting of a curable monomer and a curable oligomer is a component selected from the group consisting of a tetrafunctional polyester acrylate oligomer, a propoxylated trimethylolpropane triacrylate monomer, and combinations thereof. 11. A process of digital offset printing, the process comprising:
applying an ink composition onto a re-imageable imaging member surface at an ink take up temperature, the re-imageable imaging member having dampening fluid disposed thereon; forming an ink image; transferring the ink image from the re-imageable surface of the imaging member to a printable substrate at an ink transfer temperature; wherein the ink composition comprises: a white colorant, a translucent colorant, or a combination thereof; wherein the white colorant, translucent colorant, or combination thereof is present in an amount of at least 50 percent by weight based upon the total weight of the ink composition; at least one component selected from the group consisting of a curable monomer and a curable oligomer; at least one phase change agent, wherein the phase change agent has the characteristic of providing the ink composition with a first lower viscosity at an ink take up temperature and a second higher viscosity at an ink transfer temperature wherein the ink take up temperature is higher than the ink transfer temperature.; an optional dispersant; and an optional photoinitiator. 12. The process of claim 11, wherein the ink composition has a first viscosity of from about 3,000 to about 90,000 centipoise at an ink take up temperature of from about 45° C. to about 80° C.; and
wherein the ink composition has a second viscosity of from about 100,000 to about 2,000,000 centipoise at an ink transfer temperature of from about 18° C. to about 30° C. 13. The process of claim 11, wherein the colorant is a white colorant present in an amount of greater than 50 percent by weight to about 85 percent by weight, based upon the total weight of the ink composition. 14. The process of claim 11, further comprising:
a non-white colorant. 15. The process of claim 11, wherein the colorant is selected from the group consisting of titanium dioxide, rutile, zinc oxide, zinc sulfide, calcium carbonate, clay, lithopone (a mixture of barium sulphate and zinc sulfide), and combinations thereof. 16. The process of claim 11, wherein the ink composition further comprises a non-white colorant, wherein the non-white colorant is an inorganic metal oxide pigment; and
wherein the inorganic metal oxide pigment is present in an amount of less than 5 percent by weight based on the total weight of the ink composition. 17. The process of claim 11, wherein the substrate is selected from the group consisting of paper, plastic, folded paperboard, Kraft paper, and metal. 18. The process of claim 11, wherein the substrate is a label. 19. The process of claim 11, wherein applying the ink composition comprises applying the ink composition using an anilox delivery system. 20. The process of claim 11, wherein applying the ink composition comprises applying the ink composition to form an undercoat. 21. The ink composition of claim 1, wherein the phase change agent is a gellant. 22. The ink composition of claim 1, wherein the phase change agent is a non-curable gellant. 23. The ink composition of claim 1, wherein the phase change agent is an ester-terminated polyamide gellant. | 1,700 |
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