An apparatus and method for collecting whole blood and then separating it into components for subsequent use or storage. A self-contained bag set is used to collect the sample, which may then be placed into a device adapted to fit into a centrifuge for separation of components. Each component is then sequentially extracted according to density, with a sensor present in the device to control the operation of valves directing the collection of each component. The sensor may be reading one or more of the following characteristics: infrared, optics, density, weight, radioactive, fluorescence, color, magnetism, ultrasonic, capacitance wherein the characteristic is inherent in the blood and blood component or is an additive. Each component may then be separated into its own storage container. The preferred sensors include optics and weight. Besides blood density separation, the device may contain a solution including cells, proteins, subcellular particles or viruses which may be mixed with affinity media or antibodies prior to separation.

Blood collection is always important, particularly in times of emergency (immediate use), but whole blood may only be stored for about 30 days before it is "outdated". For long term storage, the ability to separate the whole blood into its major components (white blood cells, platelets, red blood cells and plasma) is of paramount importance because the long term storage condition for each component is different in terms of temperature and storage media. The most important component separations occurring after collection is the separation of red blood cells (RBC), white blood cells (WBC), platelets, and plasma from one another. Within the WBC it is sometimes important to separate the granulocytes from the lymphocytes and monocytes. After separation and extraction of particular components, a fraction of the blood may be returned to the patient.
It is possible to separate the various components of whole blood either under or after centrifugation, due to their differing densities. Some prior art methods, such as that in U.S. Pat. No. 4,120,448, utilize a chamber connected to a centrifuge. The centrifuged blood separates in the chamber, and a plurality of collection means are positioned at various locations in the chamber corresponding to the areas where each component congregates, which is density-dependent.
The present (prior art) technique for sequestering white blood cells from whole blood: requires skilled technicians, is labor intensive in that it requires 16 steps conducted over the span of one hour, and produces inconsistent results because of the requirements placed on the technician in the exercise of technique. Most significantly, however, the 16 step present technique is "open"; that is, the blood product is processed in a manner that does not maintain the sterility of the product because the need to obtain samples or add sedimenting agents or cryoprotectants at the various stages of production can not be accomplished with allowing the outside environment access to the interior, meaning potential contamination of the product:
The 16 steps are:
1. Collect placental blood into collection bag (range 60-200 ml).
2. Add HES to collection bag (20% v/v).
3. Load collection bag into special centrifuge cup supports.
4. Centrifuge at 50 G for 13 min. to raise WBC from RBC (up to 6 units at one time).
5. Spike or sterile dock collection bag to expressor and processing bag set to scale.
6. Gently transfer collection bag to expressor and processing bag set to scale.
7. Express off WBC rich plasma and 10-15 ml of the top layer of RBC into processing bag—leaving excess RBC.
8. Remove collection bag with excess RBC.
9. Load processing bag set in special centrifuge cup supports.
10. Centrifuge processing bag set at 400 G for 10 min. (up to 6 units at one time).
11. Gently transfer processing bag to expressor.
12. Express off excess plasma leaving 20 ml WBC concentrate.
13. Remove excess plasma bag from processing set.
14. Add 5 ml cryoprotectant to WBC in processing bag at 4° C.
15. Transfer cryoprotected WBC to freezing bag.
16. Tube seal and separate freezing bag from processing bag.
The following prior art reflects the state of the art of which applicant is aware and is included herewith to discharge applicant's acknowledged duty to disclose relevant prior art. It is stipulated, however, that none of these references teach singly nor render obvious when considered in any conceivable combination the nexus of the instant invention as disclosed in greater detail hereinafter and as particularly claimed.
PAT. NO.ISSUE DATEINVENTOR4,120,448Oct. 17, 1978Cullis4,720,284Jan. 19, 1988McCartyDes. 314,824Feb. 19, 1991Moon5,674,173Oct. 7, 1997Hlavinka et al.5,723,050Mar. 3, 1998Unger et al.5,792,038Aug. 11, 1998Hlavinka5,921,950Jul. 13, 1999Toavs et al.6,315,706Nov. 13, 2001Unger et al.6,348,031Feb. 19, 2002Unger et al.6,652,475Nov. 25, 2003Sahines et al.WO95/01842Published: Jan. 15, 1995Unger
The prior art references listed above but not specifically described teach other devices for blood processing and further catalog the prior art of which the applicant is aware. These references diverge even more starkly from the reference specifically distinguished above.

Instrumentality for sequestering liquids based on density:method and apparatus


An apparatus for chipping material, particularly wood, includes a plurality of knife carriers are arranged around a mutual axis that form the boundaries of a cutting chamber while forming a comminution path. On the knife carriers, the slicing knives, under inclusion of a cutting angle δ, are detachably attached to the comminution path. The blades of the slicing knives uniformly project into the cutting chamber. To adjust the cutting angle δ so as to adapt it to the prevailing conditions, a control element for determining the cutting angle δ is detachably arranged between the slicing knives and the knife carriers.

1. Field of the Invention
The present invention relates to an apparatus for chipping materials having an adjustable cutting angle.
2. Description of the Background Art
Devices of this class are known from a wide variety of models. DE 101 25 922 A1, for example, has a knife ring chipper for timber. Its chipping unit has a chipping chamber around which a ring of knives are arranged. The chipping unit includes two ring wheels, which are concentrically arranged around an axis of rotation, the ring wheels being connected to axis-parallel knife carriers, which are distributed around a perimeter of the ring wheels in a circular fashion. With their base facing the axis of rotation, the knife carriers form the boundary of the chipping chamber. Due to the spacing between the knife carriers, axis-parallel slots are formed. Each knife carrier has a bearing surface that is angled towards its base for an accurate incorporation of the slicing knife. In this position, the slicing knife extends through the axial slot with a predetermined blade length projecting into the chipping chamber, and with the backside of the preceding knife carrier forms a comminution channel for the passage of the chipped material. The angle of inclination between the slicing knife and the base of the knife carrier is equal to the cutting angle, which typically is in the range of approximately 30° to 45° and is immutably determined by the geometry of the knife carrier.
A similar device is known from DE 198 48 233 A1, which also discloses a knife ring chipper, and in which small-particle material is fed in an airflow to the knife ring. For the comminution of the material, a striker wheel acts jointly with the knife ring, both of which rotate in opposite directions and thus move the small-particle material past the blades of the slicing knives. Apart from counter-rotating chipping tools, simpler models are also known, whereby the knife ring is stationary and only the striker wheel rotates, or whereby only the knife ring rotates and the blades are moved past a stationary counter-knife. All of these devices have in common that the structure of the knife ring is basically as previously described, in particular, that the knife carriers have a rigid bearing surface for the slicing knives that determines the cutting angle.
Conventional cutting disks have a comminution unit that includes a rotating disk with an opening that is arranged in a semi-radial direction along which the knife carriers with slicing knives are arranged. The knife carriers, in turn, have a bearing surface that is inclined towards the disk plane for attaching the slicing knife, whose inclination determines the cutting angle. Such a cutting disk is known from DE 100 48 886 C1, for example, wherein a cutting disk is used in a first stage of comminution. The special feature of this device is the combination with a second stage of comminution, which is formed from a ring of knives as previously described.
All of the conventional art previously described have in common that the position of the slicing knife in relation to the chipping chamber, and therefore the cutting angle, are immutably determined by the fixed geometry of the knife carrier. In many areas of application, this constant cutting angle may be sufficient. However, increased demands regarding the quality of the chips and the economical operation of comminution devices make it imperative to continue to improve devices of this class.

Chipping apparatus having an adjustable cutting angle


A magnetic field sensor for measuring the rotational speed of a rotating gear component is disclosed. The sensor includes a Hall probe, at least one permanent magnet and housing. The Hall probe is arranged in the influence area of the magnetic field of the permanent magnet. The intent is to produce the magnetic field sensor in a less complex manner. This is achieved by virtue of the fact that the permanent magnet is secured to the housing. One particular advantage of the device is that it is extraordinarily robust and is only slightly sensitive to vibrations.

The invention relates to a magnetic field sensor, in particular for measurement of the rotation speed of a rotating transmission component, having a Hall probe having at least one permanent magnet, with the Hall probe being located in the area of influence of the magnetic field of the permanent magnet, having a housing which surrounds the Hall probe, wherein the permanent magnet is attached to the housing, wherein the housing is at least partially composed of plastic and the permanent magnet is in the form of a ring or hollow cylinder, wherein the longitudinal axis of the permanent magnet and an induction axis of the Hall sensor essentially coincide, with the induction axis being oriented at right angles to the electrical field direction of the Hall voltage and to the electrical main current direction in the Hall probe.
Magnetic field sensors of the type mentioned above are preferably used for rotation speed monitoring in goods vehicles, because the signal transmitters, in which field plates or Hall generators are used as active elements, have the advantage over induction transmitters that it is possible to detect relatively low rotation speeds or movements in the stationary range. In addition to being used for rotation speed measurement in a motor vehicle transmission, magnetic field sensors according to the invention can also be used to monitor other movements, for example rotary movements or translations.
A magnetic field sensor of a conventional type is already known from EP 0 546 355 B1. The extraordinarily accurate operation of this component can be achieved only on the basis of a highly complex manufacturing and assembly process. The large number of work steps include, inter alia, the attachment of the permanent magnet to a holder which has a push fit with the permanent magnet, by means of a UV-curing adhesive following previous accurate adjustment of the position of the Hall probe with respect to the permanent magnet. The normally extraordinary operating conditions of these magnetic field sensors, in particular with regard to considerable temperature fluctuations from −40° C. to +150° C. and with regard to mechanical vibration and shock loads, require the permanent magnet to be mounted in the magnetic field sensor with extraordinary robustness. Adequate strength of the joint between the heavy permanent magnet and the holder which is provided for this purpose can be achieved, for example, by the contact points being activated by means of a primer, before the application of the UV-curing adhesive. After the UV-curing, additional thermal curing must be carried out for at least three hours at room temperature in order to make it possible to ensure that the joint is of the necessary quality. In order to ensure that the pulse width of the signals which are generated by the Hall probe as it passes over a gear wheel or a similar magnetic field concentrator is as desired, the Hall probe, which is normally in the form of a Hall IC, must be aligned exactly with respect to the permanent magnet, which is preferably in the form of a ring magnet. The disadvantage of the large amount of effort for assembly and manufacture of conventional magnetic field sensors is evident from the large number of work steps, only some of which have been mentioned here, but which must be carried out with very high precision.
Against the background of the problems and disadvantages of the prior art, the invention is based on the object of providing a magnetic field sensor which can be produced with less effort and which is less susceptible to defects.
A magnetic field transmitter of the type mentioned in the introduction is already known from German Utility Model DE 295 16 373 U1, in which an annular permanent magnet is inserted into a sleeve-like housing such that it is aligned, and the Hall probe is then adjusted in a complex manner in particular in the direction of the magnetic axis of the permanent magnet, and is finally fixed to the permanent magnet and to the housing by means of an encapsulation compound.
The International Patent Application WO 03/040659 A1, U.S. Pat. 6,291,990 B1 and German Laid-Open Specification DE 101 46 157 A1 each disclose arrangements with a sensor, in which the Hall probe of a sensor is arranged off a magnetic null axis, which requires the sensor to be positioned very accurately in some way with respect to a rotating component which measurably varies the magnetic flux in the area of the Hall probe of the sensor, as a significant change. The signal from a sensor arrangement such as this must furthermore be of special quality, since the arrangement of the probe in the area which is magnetically not neutral results in a permanent basic signal whose magnitude is highly dependent on the magnetic properties of the area surrounding the sensor, and the signal which is actually to be evaluated is highly dependent on the distance between the sensor and the actual pulse-transmitting marks.


A method and system for administering a secure, Internet based examination at remote sites is disclosed. The examination is dynamic and potentially adaptive. During the examination session, the state of the examination is maintained with the use of cookies, which are updated and stored on the central server at a predefined interval during the examination. Individual examination sessions may be restored to their previous state in the event of a malfunction.

Administer an examination to measure a candidate's qualifications has become standard in almost all professions. Generally, the process of administering a written examination, and reviewing the test results extends over a period of several months. The examination procedure includes preprinted examination papers and printed test results, which contribute to the expense and inefficiency of written examinations.
Computer based testing has grown in popularity in the past few years. Computer based testing (CBT) simply means a test situation where the candidate utilizes a computer terminal rather a printed examination. Generally, the questions appear on the screen and the candidate answers them by typing at the keyboard or clicking a mouse on the appropriate answer. This format has a number of advantages over the conventional paper and pencil examination.
Candidates complete CBT examinations with much more speed and efficiency than conventional examinations. This is due to the inherent ease of clicking with a mouse. Also, the candidate is not required to constantly shift his eyes from question sheet to answer sheet.
Perhaps the most compelling advantage of CBT is its inherent flexibility—the design and format can be easily modified to adapt different circumstances. Customization to meet special needs is possible.
video, etc. can all be used to enhance the testing experience.
The most obvious difference between traditional testing and CBT is that a computer based examination's content can be generated in real time according to some set criteria. This means that each candidate might receive the same questions in a different order or perhaps even a different examination altogether.
CBT examinations also provide more options in reporting results. The raw scores and processed results can be provided in whatever format is desired.
In addition, CBT results in cost savings in printing, storing, distribution and collecting examinations.
Following the introduction of the Internet, computer based testing evolved into Internet based testing (IBT). In Internet based testing, the candidate is seated at a computer that is connected to the Internet. Usually, the software running is a World Wide Web (WWW) browser such as Netscape Navigator® or Microsoft Internet Explorer®. A connection is established with a remote web server which sends to the browser a series of web pages. Again the candidate answers by clicking the mouse or entering information at the keyboard. By submitting the answers, the candidate sends the answers back to the web server for processing and the process continues.
IBT offers further advantages from CBT. The Internet and especially the WWW is well suited to the delivery of multimedia content. Designed to be easy to navigate and to incorporate a variety of multimedia elements the Web has become virtually synonymous with the Internet in the public eye. The point and click approach to navigation on the WWW lends itself extremely well to an examination situation. Modern universities all have computer labs full of Internet-enabled computers and candidates enjoy the convenience of taking the examination using existing university facilities instead of travelling to outside centres. By electing to use the Internet as the vehicle for its examination, the testing organization will be able to assert greater control over the process and will not have to contract with a private testing institution.
While the Internet has undergone explosive growth in the past few years, in many ways it is still at an early stage of development. Therefore, there are still many development issues for IBT.
Problems with IBT include security, user interaction and reliability.
Imposing security on Internet transactions means taking specific steps to plug security holes and using software to make it as difficult as possible to intercept transmissions. There are three main areas where security must be imposed. The first is at the server, by monitoring incoming and outgoing traffic to ensure only legitimate transactions are allowed. The second is on the client side, by proctoring for the log in, ensuring that candidates can not store information about the examination. The third area is during transmission, by encrypting transactions to prevent monitoring by intruders.
The WWW is designed to be a non-linear medium. Hypertext links allow users to follow any topic of interest at any time and to easily retrace their steps whenever they want. An examination, however, is inherently liner. It starts at a specific time and ends at a specific time. More importantly, a candidate should not be able to click the back button, change answers already submitted and then proceed to another section of the examination.
IBT also should be easy to use, particularly considering that some candidates will have had little to no prior exposure to computers. Therefore, the user interface should be designed to be user friendly and intuitive.
It is also important to ensure that the examination is reliable. The examination should continue to function in the event that the candidate does something unpredictable or if some kind of technical malfunction occurs. It is almost inevitable that technical problems could arise. In this event, a mechanism must be provided to restore the examination to a previously computed state so that the candidate's work is not for naught.
For example, there is the prospect of a power failure. In this situation, candidates should be able to pick up where they left off at some later time. A power failure could also affect the server or the server could experience a technical malfunction.
Therefore, there is a need for an improved method of computer based testing that addresses the above mentioned problems.

Method and apparatus for administering an internet based examination to remote sites


An ignitable pyrotechnic transmission line, when ignited, actuates a vehicle safety device. A microdet receives a firing signal indicative of a vehicle collision and generates combustion products to ignite the pyrotechnic transmission line. A blocking member in the form of a slidable spool is interposed between the microdet and the pyrotechnic transmission line. The spool has a blocking position in which the spool prevents transmission of combustion products from the microdet to the pyrotechnic transmission line. The spool also has a non-blocking position in which the spool allows transmission of combustion products from the microdet to the pyrotechnic transmission line to ignite the pyrotechnic transmission line. The movement of the spool from the blocking position to the non-blocking position is controlled so that it moves only in the event of vehicle deceleration above a predetermined rate. Alternatively, the blocking member may be in the form of a pendulum interposed between the microdet and the pyrotechnic transmission line.

1. Technical Field
The present invention relates to an apparatus for protecting an occupant of a vehicle during a collision, and is particularly directed to an apparatus for preventing false ignition of an ignitable pyrotechnic transmission line which, when ignited, actuates a safety device.
2. Background Art
The use of an ignitable pyrotechnic transmission line to actuate a vehicle safety device is known. Typically, a pyrotechnic transmission line has one end connected to the safety device and the other end connected to a firing manifold. An ignitable blasting cap known as a microdet is disposed in the firing manifold. The microdet ignites when subjected to a firing signal of sufficient magnitude and duration. The firing signal of sufficient magnitude and duration is provided by a sensor which senses a vehicle collision. When ignited, the microdet generates gas and flame. The gas and flame ignite the pyrotechnic transmission line which in turn actuates the safety device.
A problem can arise if no actual vehicle collision has occurred, but the microdet nonetheless ignites. The resulting ignition of the pyrotechnic transmission line would cause undesired actuation of the safety device. Thus, it is desirable to ignite the pyrotechnic transmission line only in the event of an actual vehicle collision.

Apparatus for preventing undesired ignition of a pyrotechnic transmission line


A vehicle seat including a pivot bracket, a back frame, a linear adjustment mechanism, a striker, and a latch. The back frame is pivotally connected to the pivot bracket and configured to pivot about a pivot axis. The back frame includes a first end spaced apart from the and disposed below the pivot axis. The latch is configured to selectively attach the linear adjustment mechanism to the first end of the back frame so that as the first linear adjustment mechanism translates, the back frame pivots from a first use position and a second use position, and selectively detach the linear adjustment mechanism from the first end of the back frame so that the back frame is pivotable to a non-use position.

Vehicles such as sport utility vehicles may include second and third row seats that are configured to support an occupant when in use and move to a non-use position to provide additional space in the vehicle cabin. Second and third row seats may include a cushion support and a back frame that may be configured to pivot with respect to the cushion carrier. Second and third row seats may also include tracks or rails that allow longitudinal adjustment of the cushion carrier.

Linear recliner mechanism for a vehicle seat

Brose Fahrzeugteile SE & Co. Kommanditgesellschaft, Coburg


The invention comprises an integrated circuit structure, and a process for making same, comprising a via/contact opening in a dielectric layer; a CVD layer of titanium nitride having a thickness of at least about 50 Angstroms, but not exceeding about 200 Angstroms, on the sidewall and bottom surfaces of the via/contact opening to provide adherence of the filler material to the underlying and sidewall surface of the opening; a CVD barrier layer of tungsten, having a thickness of about 50 Angstroms, but not exceeding about 300 Angstroms, formed over the titanium nitride layer; and the remainder of the via/contact opening filled with a highly conductive metal selected from the group consisting of copper, CVD aluminum, and force-filled aluminum.

1. Field of the Invention
This invention relates to a via/contact opening for an integrated circuit structure filled with conductive metal and a process for making same. More particularly this invention relates to a via/contact opening for an integrated circuit structure filled with highly conductive metal, with thin barrier layers separating the highly conductive metal in the via/contact opening from underlying silicon, and a process for making the structure.
2. Description of the Related Art
In the construction of integrated circuit structures on semiconductor substrates such as a silicon substrate, vias or contact openings are formed through an insulation or dielectric layer, e.g., silicon oxide (SiO.sub.2), to electrically connect a metal pattern or wiring on the insulation layer either with a lower level of metal wiring or with elements of active devices, e.g., a source/drain region or a gate electrode of an MOS device, formed in the underlying silicon substrate.
Typically, such vias or contact openings are filled with aluminum metal. To avoid diffusion of the aluminum filler material into the underlying silicon substrate (and diffusion of the silicon into the aluminum) a titanium nitride barrier layer can be formed between the exposed portion of the substrate and the aluminum used to fill the opening. Sometimes this is accomplished by deposition of a titanium layer followed by an anneal in nitrogen to form the titanium nitride barrier layer as well as to form titanium silicide beneath the titanium nitride and in contact with the underlying silicon surface to thereby reduce the contact resistance.
However, as the diameters of the vias or contact openings become smaller, and aspect ratios increase (depth of opening divided by width), it has become more difficult to adequately fill the opening with sputtered aluminum. To solve this problem, it has been proposed to fill the opening with tungsten metal. However, since tungsten does not adhere well to the underlying silicon either an intermediate layer of titanium nitride or a dual layer of titanium silicide/titanium nitride is usually formed over the silicon and beneath the tungsten filler or plug in the opening. The use of titanium silicide can also reduce the contact resistance, for example, from over 100 .OMEGA. to as little as 1 .OMEGA. for a 0.5 .mu.m diameter contact opening. Such tungsten-filled via/contact openings are shown, for example, in Pintchovski et al. U.S. Pat. No. 4,822,753; Sun et al. U.S. Pat. No. 4,994,410; Lifshitz et al. U.S. Pat. No. 5,149,672; Somekh et al. U.S. Pat. No. 5,250,467; Somekh et al. U.S. Pat. No. 5,356,835; Yu et al. U.S. Pat. No. 5,380,678; Kim U.S. Pat. No. 5,397,742; Marangon et al. U.S. Pat. No. 5,407,861; Fujita U.S. Pat. No. 5,413,669; and Chen U.S. Pat. No. 5,462,895.
The underlying titanium nitride layer used in such tungsten-filled via/contact openings is usually either deposited onto the surface of the via/contact opening (as well as the exposed surface of the silicon substrate at the bottom of the contact opening), or a layer of titanium metal is deposited followed by annealing in nitrogen gas, causing the titanium layer to react with the nitrogen to form titanium nitride (as well as titanium silicide wherever the titanium metal layer is in contact with silicon). The aforementioned Pintchovski et al. U.S. Pat. No. 4,822,753, for example, describes the deposition of titanium nitride over an insulating layer, as well as the sidewall and bottom surfaces of an opening in the insulating layer, by CVD prior to filling the opening with a tungsten plug. The above-mentioned Lifshitz et al. U.S. Pat. No. 5,149,672, for example, teaches the sputter deposition of tungsten nitride over a silicon oxide layer followed by deposition of a tungsten layer by CVD (using WF.sub.6 and H) over the titanium nitride layer, with aluminum then optionally sputtered over the wafer.
When titanium metal is deposited and then converted to titanium silicide/nitride, care must be taken to not expose the titanium metal surface to oxygen prior to the annealing step. To avoid this, the aforementioned Sun et al. U.S. Pat. No. 4,994,410 sputters a thin layer of tungsten over the titanium and then anneals in nitrogen to form the underlying titanium silicide/titanium nitride layers, with the nitrogen gas penetrating the tungsten layer to reach the underlying titanium layer. Sun et al. then fill the remainder of the via with CVD tungsten (which cannot be deposited directly over the titanium metal without undesirable side reactions between the titanium metal and the fluorine in the WF.sub.6 used to form the CVD tungsten layer). However, the sputtering of tungsten over a titanium metal layer cannot be used satisfactorily with small openings (e.g., diameters less than about 0.5 .mu.m or aspect ratios larger than 2.5).
While the use of tungsten as a filler material for vias and contact openings has been, in the main, satisfactory, there has now arisen a need for faster devices and the higher resistance of tungsten (CVD tungsten resistance is about 11 .mu..OMEGA.cm) compared to other metals has resulted in consideration of copper (resistivity about 2 .mu..OMEGA.cm) as a metal filler material for vias and contact openings. For example, Gelatos et al. U.S. Pat. No. 5,391,517 shows a via filled with copper. However, as is well known to those skilled in the art, copper is a fast diffuser in silicon and silicon oxide, much faster than aluminum. Furthermore, the copper diffusion is not only vertical, e.g., potentially into the underlying silicon substrate, but also horizontal as well, e.g., into the dielectric material forming the sidewall of the via or contact opening. To obtain proper adherence of the copper to the device substrate and to avoid such undesirable diffusion of the copper, Gelatos et al. provide a composite interface layer comprising a first titanium layer, which is sputtered onto the dielectric to a thickness of about 100-300 Angstroms, followed by a sputter deposition of titanium nitride to a thickness of about 300-500 Angstroms. Another titanium layer is then sputtered over the titanium nitride layer to a thickness of about 100-300 Angstroms. Copper is then deposited over the second layer of titanium to completely fill the opening, and the structure is then annealed to cause the copper to form a titanium copper alloy with the underlying second layer of titanium.
While such a structure apparently adequately protects the Gelatos et al. substrate and opening sidewalls from diffusion of the copper filler, the formation of 300-500 Angstroms of titanium nitride in contact openings as small as 0.5 .mu.m in diameter would be difficult to accomplish by sputtering, and CVD titanium nitride has a high resistance of .about.400 .mu..OMEGA.cm, compared to .about.2 .mu..OMEGA.cm for CVD copper (CVD copper is 200 times more conductive than CVD titanium nitride), and therefore the use of CVD titanium nitride would be counterproductive to the use of a high conductivity copper filler material.
However, the need for faster devices, coupled with the need to avoid diffusion of via/contact opening filler materials into either the underlying substrate or the sidewalls of the opening, as well as the shrinkage in the diameter of the via/contact openings and an increase in the aspect ratios of such openings, has created difficulties. It would, therefore, be desirable to provide an integrated circuit structure with via/contact openings having a low resistance filler in the via/contact opening and adequately protected against diffusion of the filler material into either the underlying substrate or the sidewalls of the dielectric in which the opening is formed, even with via/contact opening diameters as small as 0.5 .mu.m and aspect ratios as high as 2.5.

Metal-filled via/contact opening with thin barrier layers in integrated circuit structure for fast response, and process for making same


Aqueous two-component binder systems, its first component comprising a water-soluble polyester AB and its second component comprising a blocked polyfunctional isocyanate C, where the blocking agent C2 is selected from the group consisting of primary alcohols C21 having 3 to 10 carbon atoms, in which the carbon atom adjacent to the hydroxymethylene group carries a double bond, oximes C22 of linear, branched or cyclic aliphatic ketones having 3 to 15 carbon atoms, CH-acidic compounds C23, in which the carbon atom carrying the active hydrogen carries at least one further group selected from R1xe2x80x94COxe2x80x94, R2xe2x80x94Oxe2x80x94COxe2x80x94, xe2x80x94NO2 and R3xe2x80x94SO2xe2x80x94, R1, R2 and R3 independently of one another may be linear, branched or cyclic alkyl groups having 1 to 18 carbon atoms or aryl groups having from 5 to 15 carbon atoms, and NH-acidic compounds C24.

The invention relates to two-component systems comprising water-soluble polyesters and blocked isocyanates that are suitable as binders for aqueous baking varnishes.
Baking varnishes comprise reactive resin binders and curatives which only on baking, i.e., at relatively high temperatures, react with the reactive groups of the resins to form crosslinked structures. Aqueous baking binders are known, for example, from EP-A 0 218 906, which describes combinations of copolymers of free-radically polymerizable monomers and crosslinker resins such as amino resins, phenolic resins or blocked isocyanates. Blocking agents mentioned for the isocyanates are aliphatic and aromatic monoalcohols such as methanol, ethanol, butanol, (cyclo)hexanol and benzyl alcohol, oximes, lactams and phenols. The binder is a water-dilutable mixture comprising mass fractions of from 60 to 95% of the copolymer and from 40 to 5% of the crosslinker. By adding pigments it is also possible to prepare pigmented paints possessing high storage stability. The blocking of the isocyanates is so efficient that the crosslinking reaction in the mixture does not proceed with any notable speed at standard (room) temperature.
EP-A 0 496 210 discloses two-component systems for producing baking coatings which comprise aqueous/organic solutions of anionically modified polyacrylate resins and organic polyisocyanates which are not blocked and therefore no blocking agents are liberated on curing.
According to EP-A 0 537 568, certain aqueous polyester resins containing sulfonate and hydroxyl groups may be formulated to aqueous two-component binders using polyfunctional isocyanates containing free isocyanate groups as curatives. Water-dilutable paints in the form of two-component systems based on water-soluble polyesters or other water-soluble resins and unblocked isocyanates in combination with water-soluble or water-dispersible, partially etherified amino resins are known from Austrian patent application A-2173/99.
When unblocked isocyanates are used, however, a number of disadvantages arise. For instance, in the paint, the aqueous solvent always competes with the OH groups of the resin for reaction with the unblocked isocyanate groups within the processing period. This activity may lead on the one hand to formation of unwanted secondary products (by reaction of water and isocyanate, substantially amines, and subsequently ureas); on the other hand, the carbon dioxide formed when the isocyanates are decomposed by the action of water produces gas bubbles which often result in defects in the baked paint film. The secondary products formed (amines, ureas) may also additionally impair the properties of the baked paint film.
The losses of isocyanate groups as a result of secondary reactions are normally compensated by using stoichiometric excessxe2x80x94often considerablexe2x80x94of the isocyanates. This is economically undesirable. The processing of unblocked isocyanates in the two-component process, moreover, also presents workplace hygiene (toxicological) problems.
In practice, usually unblocked, polyfunctional aliphatic isocyanates are used in two-component systems. The reaction between water and the unblocked aromatic isocyanates is generally so rapid that processing within the necessary time is impossible. Aromatic unblocked isocyanates are therefore not usually used for a 2K application.
It has been found that not only aliphatic but also aromatic polyfunctional isocyanates can in fact be used in two-component systems if they are blocked with blocking agents which lead to highly reactive reaction products which undergo deblocking at comparatively low baking temperatures. The isocyanates blocked in this way may be so reactive that formulation with water-soluble, hydroxyl group-containing resins (e.g., polyesters) in the form of one-component systems is no longer possible because of their instability to hydrolysis. On the other hand, curing of two-component paints which comprise these isocyanates to give crosslinked films is possible at baking temperatures which are all the lower. Compounds which have been found particularly appropriate for use as blocking agents are highly activated C-H acidic compounds, certain reactive alcohols, and certain oximes, as elucidated later on below. Similar adducts with aliphatic isocyanates are described for example in Houben-Weyl, Methoden der Organischen Chemie, Vol. XIV/2, Makromolekulare Stoffe [macromolecular substances], 4th ed. 1963, pages 62 and 63.
The present invention therefore provides aqueous two-component binders, its first component comprising a water-dilutable polyester AB having a hydroxyl number of at least 10 mg/g and its second component comprising a blocked polyfunctional isocyanate C, wherein the blocked isocyanate C is prepared by reaction of an aromatic isocyanate C1 and a blocking agent C2 for the isocyanate, C2 being selected from primary alcohols C21 having 3 to 10 carbon atoms, in which the carbon atom adjacent to the hydroxymethylene group carries a double bond, oximes C22 of linear, branched or cyclic aliphatic ketones having 3 to 15 carbon atoms, CH-acidic compounds C23, in which the carbon atom which carries the active hydrogen carries at least one further group selected from R1xe2x80x94COxe2x80x94, R2xe2x80x94Oxe2x80x94COxe2x80x94, xe2x80x94NO2 and R3xe2x80x94SO2xe2x80x94, R1, R2 and R3 independently of one another denoting linear, branched or cyclic alkyl groups having 1 to 18 carbon atoms or aryl groups having 5 to 15 carbon atoms, and NH-acidic compounds C24 such as, for example, 3,5-dimethylpyrazole, succinimide or phthalimide. Examples of suitable blocking agents C21 are hydroxyacetone, allyl alcohol, 2-methylallyl alcohol (xcex2-methallyl alcohol), 3-methyl-2-buten-1-ol, 2-penten-1-ol and 2-hexen-1-ol. Examples of suitable blocking agents C22 are the oximes of acetone, 2-butanone, 2- and 3-pentanone and methyl isobutyl ketone. Particularly suitable blocking agents C23 are acetyl acetone, acetoacetates, malonates and cyanoacetates.
The water-dilutable polyesters AB may be prepared either conventionally by polycondensation of polyfunctional, especially difunctional, organic hydroxy compounds AB1 and polyfunctional, especially difunctional, organic acids AB2 or by partial condensation of hydroxyl group-containing compounds B which per se are insoluble in water with organic compounds A containing acid groups, especially carboxyl groups. The compounds A are per se soluble in water or dispersible in water following at least partial neutralization of the acid groups. Partial condensation means here that the reaction of the compounds A and B is conducted to a point such that the resulting condensation product AB still contains both hydroxyl groups and acid groups. The amount of the acid groups in AB corresponds preferably to an acid number of from about 10 to 60 mg/g, preferably from 15 to 55, and in particular from 20 to 50 mg/g. The amount of the hydroxyl groups in AB corresponds to a hydroxyl number of at least 10 mg/g, preferably from 15 to 200 mg/g, and in particular from 25 to 150 mg/g. The polycondensate AB normally has a Staudinger index J0 of from 5 to 25 cm3/g, preferably from 7 to 22, and in particular from 10 to 20 cm3/g, as measured in dimethylformamide at 20xc2x0 C.
A substance termed xe2x80x9cwater-solublexe2x80x9d here is one which in contact with ten times the amount of water at room temperature (20xc2x0 C.) is dissolved in the aqueous phase to an extent such that the mass fraction of this substance in the aqueous phase after equilibrium has been reached is not less than 1%. A substance termed xe2x80x9cwater-dispersiblexe2x80x9d is one which with ten times the mass of water formsxe2x80x94under shearingxe2x80x94a dispersion which when stored at room temperature shows no macroscopic separation over a period of 14 days. Substances referred to as xe2x80x9cwater-dilutablexe2x80x9d are soluble in water and/or dispersible in water.
The compounds or resins A containing carboxyl groups are preferably selected from polyester resins A1, polyurethane resins A2, the so-called maleate oils A3, fatty acids and fatty acid mixtures A4 grafted with unsaturated carboxylic acids, and acrylate resins A5. Instead of or in a mixture with resins containing carboxyl groups, it is also possible to use epoxy resins modified with phosphoric acid and/or phosphonic acids, or similarly modified reaction products of epoxy resins with fatty acids, referred to collectively as A6. Preferably, the acid number of the resins A is from 100 to 230 mg/g, in particular from 70 to 160 mg/g. Their Staudinger index, measured in dimethylformamide as solvent at 20xc2x0 C., is generally from about 6.5 to 12 cm3/g, preferably from 8 to 11 cm3/g.
Suitable polyester resins A1 may be prepared in a conventional manner from polyols A11 and polycarboxylic acids A12, where optionally somexe2x80x94preferably up to 25%xe2x80x94of the amount of substance of the polyols and polycarboxylic acids can be replaced by hydroxycarboxylic acids A13. By appropriate choice of the type and amount of the starting materials A11 and A12 it is ensured that the resulting polyester has a sufficient number of acid groups, in accordance with the acid number indicated above. The polyols A11 are preferably selected from the aliphatic and cycloaliphatic alcohols having 2 to 10 carbon atoms and on average at least two hydroxyl groups per molecule; glycol, 1,2- and 1,3-propanediol, 1,4-butanediol, 1,6-hexanediol, neopentyl glycol, di- and triethylene glycol, di- and tripropylene glycol, glycerol, trimethylolpropane and trimethylolethane are particularly suitable. Suitable polycarboxylic acids A12 are aliphatic, cycloaliphatic and aromatic polycarboxylic acids such as adipic acid, succinic acid, cyclohexane-dicarboxylic acid, phthalic acid, isophthalic and terephthalic acid, trimellitic acid, trimesic acid and benzophenonetetracarboxylic acid. It is also possible to use compounds having both carboxylic acid groups and sulfonic acid groups, such as sulfoisophthalic acid, for example.
Suitable polyurethane resins A2 may be prepared by reacting aliphatic polyols A21, as defined under A11, hydroxyalkanecarboxylic acids A22 having at least one, preferably two, hydroxyl groups and a carboxyl group which under esterification conditions is less reactive than adipic acid; preference is given to the use of dihydroxymonocarboxylic acids selected from dimethylol-acetic acid, dimethylolbutyric acid and dimethylol-propionic acid; oligomeric or polymeric compounds A25 having on average at least two hydroxyl groups per molecule, which may be selected from polyether polyols A251, polyester polyols A252, polycarbonate polyols A253, saturated and unsaturated dihydroxyaliphatic compounds A254, which are obtainable by oligomerizing or polymerizing dienes having 4 to 12 carbon atoms, especially butadiene, isoprene and dimethylbutadiene, followed by functionalization in a known manner, and also polyfunctional isocyanates A23, selected preferably from aromatic, cycloaliphatic and also linear and branched aliphatic difunctional isocyanates such as tolylene diisocyanate, bis(4-isocyanatophenyl)methane, tetramethylxylylene diisocyanate, isophorone diisocyanate, bis(4-isocyanatocyclohexyl)methane, hexamethylene diisocyanate and 1,6-diisocyanato-3,5,5- and -3,5,5-trimethylhexane.
Particular preference is given to those polyurethane resins A2 which are prepared by reacting a mixture of one or more polyols A21 with a hydroxyalkanecarboxylic acid A22 and at least one polyfunctional isocyanate A23 which has been at least partly blocked, usually to the extent of more than 20%, preferably to the extent of more than 35% and, in particular, to the extent of 50% or more with monohydroxy compounds A24 selected from polyalkylene glycol monoalkyl ethers HOxe2x80x94(R1xe2x80x94O)nxe2x80x94R2, where R1 is a linear or branched alkylene radical having 2 to 6, preferably 2 to 4 carbon atoms and R2 is an alkyl group having 1 to 8, preferably 2 to 6 carbon atoms, n being a number between 2 and 10, and oximes of aliphatic ketones having 3 to 9 carbon atoms. The degree of blocking is stated here as the ratio of the number of blocked isocyanate groups to the total number of isocyanate groups (blocked and unblocked) present in the isocyanate A23. It is further preferred to prepare the polyurethane resins A21 by reacting a mixture of a polyfunctional isocyanate and a polyfunctional isocyanate blocked as described above with the hydroxyalkanecarboxylic acid A22 and the polyols A21 and A25, the mixing ratios being chosen so that each molecule of the polyurethane A21 contains on average one or more than one terminal blocked isocyanate group.
xe2x80x9cMaleate oilxe2x80x9d A3 is a term used to denote reaction products of (drying) oils A31 and olefinically unsaturated carboxylic acids A32, especially dicarboxylic acids. Oils A31 used are preferably drying and semidrying oils such as linseed oil, tallow oil, rapeseed oil, sunflower oil and cottonseed oil, having iodine numbers of from about 100 to about 180 cg/g. The unsaturated carboxylic acids A32 are selected so that under the customary conditions they graft free-radically (following addition of initiators or following heating) onto the initial charge of oils with a yield (fraction of the unsaturated carboxylic acids bonded to the oil after the reaction, based on the amount used for the reaction) of more than 50%. Particularly suitable is maleic acid in the form of its anhydride, as are tetrahydrophthalic anhydride, acrylic acid and methacrylic acid, and also citraconic acid, mesaconic acid and itaconic acid.
Equally suitable resins A4 are fatty acids or fatty acid mixtures A41 grafted with the unsaturated acids specified under A32, said fatty acids or fatty acid mixtures A41 being obtainable in industrial amounts by saponification of fats. The suitable fatty acids have at least one olefinic double bond in the molecule; those which may be listed by way of example include oleic acid, linoleic and linolenic acid, ricinoleic acid and elaidic acid, and also the stated technical grade mixtures of such acids.
Further suitable resins A5 are the acidic acrylate resins obtainable by copolymerization of olefinically unsaturated carboxylic acids A51 and other vinyl or acrylic monomers A52. The carboxylic acids are those already mentioned under A32, and also vinylacetic acid and also crotonic and isocrotonic acid and the monoesters of olefinically unsaturated dicarboxylic acids, such as monomethyl maleate and monomethyl fumarate, for example. Suitable monomers A52 are the alkyl esters of acrylic and methacrylic acid having preferably 1 to 8 carbon atoms in the alkyl group, (meth)acrylonitrile, hydroxyalkyl (meth)acrylates having 2 to 6 carbon atoms in the alkyl group, styrene, vinyltoluene, and also vinyl esters of aliphatic linear and branched carboxylic acids having 2 to 15 carbon atoms, especially vinyl acetate and the vinyl ester of a mixture of branched aliphatic carboxylic acids having on average 9 to 11 carbon atoms. It is also advantageous to copolymerize the monomers specified under A51 and A52 in the presence of compounds A53 which react with the unsaturated carboxylic acids with addition and formation of a carboxyl- or hydroxyl-functional, copolymerizable compound. Examples of such compounds are lactones A531, which react with the carboxylic acids A51 with ring opening to form a carboxyl-functional unsaturated compound, and epoxides A532, especially glycidyl esters of xcex1-branched saturated aliphatic monocarboxylic acids having 5 to 12 carbon atoms, such as of neodecanoic acid or neopentanoic acid, which react with the acid A51 with addition to give a copolymerizable compound containing a hydroxyl group. The amounts of substance of the compounds used should be such that the required acid number is reached. If this compound A53 is introduced as the initial charge and the polymerization is conducted so that this compound is used as (sole) solvent, solvent-free acrylate resins are obtained.
The epoxy resins modified with phosphoric acid or phosphonic acids or with likewise-modified adducts of epoxy resins and fatty acids, A6, are prepared by reacting phosphoric acid or organic phosphonic acids which are at least dibasic with epoxy resins or adducts of epoxy resins and fatty acids, preferably in a solvent. The amount of substance of the phosphoric or phosphonic acid used is normally such that all of the epoxide groups are consumed by the reaction with the acid and such that a sufficient number of acid groups is still available after the reaction. The resulting resin has hydroxyl groups (from the reaction of the oxirane group with the acid function), these hydroxyl groups being positioned xcex2 to the ester group, and also acid groups of the phosphoric or phosphonic acid which were not consumed by the reaction with the epoxide. Examples of suitable phosphoric or phosphonic acids are orthophosphoric acid H3PO4, phosphorous acid H3PO3, and alkanephosphonic acids having 1 to 18, especially 1 to 6, carbon atoms.
Suitable hydroxyl group-containing compounds or resins B are, in particular, polyesters B1, acrylate resins B2, polyurethane resins B3 and epoxy resins B4. The hydroxyl number of the resins B is generally from about 50 to 500 mg/g, preferably from about 60 to 350 mg/g, and with particular preference from 70 to 300 mg/g. Their Staudinger index, measured at 20xc2x0 C. in dimethylformamide as solvent, is preferably from 8 to 13 cm3/g, in particular from 9.5 to 12 cm3/g.
Like the component A1, the polyesters B1 are prepared by polycondensation; in this case all that is necessary is to select the type and amount of the starting materials such that there is an excess of hydroxyl groups over the acid groups, as the condensation product needs to have the hydroxyl number indicated above. This may be achieved by using polyhydric alcohols containing on average at least two, preferably at least 2.1, hydroxyl groups per molecule, with dicarboxylic acids or with a mixture of polycarboxylic and monocarboxylic acids containing on average not more than two, preferably from 1.5 to 1.95, acid groups per molecule. Another possibility is to use a corresponding excess of hydroxyl components (polyols) B11 over the acids B12. The polyols B11 and the polyfunctional acids B12 which are reacted in the polycondensation reaction to give the hydroxyl group-containing polyesters B1 are selected from the same groups as the polyols A11 and the acids A12. It is likewise possible here to replace some of the polyols and acids by hydroxy acids in accordance with A13. The aim is for the acid number of component B not to exceed 20 mg/g and to be preferably below 18 mg/g. The acid number may be reduced, for example, by reacting the condensed polyester B1 with a small amount of monohydric aliphatic alcohols A14 under esterification conditions. The amount of alcohols A14 is such that, although the acid number is reduced below the limit, the Staudinger index does not fall below the stated lower limit. Examples of suitable aliphatic alcohols are n-hexanol, 2-ethylhexanol, isodecyl alcohol and tridecyl alcohol.
The hydroxyl group-containing acrylate resins B2 are obtainable by usually free-radically initiated copolymerization of hydroxyl group-containing acrylic monomers B21 with other vinyl or acrylic monomers B22 without such functionality. Examples of the monomers B21 are esters of acrylic and methacrylic acid with aliphatic polyols, especially diols having 2 to 10 carbon atoms, such as hydroxyethyl and hydroxypropyl (meth)acrylate. Examples of the monomers B22 are the alkyl esters of (meth)acrylic acid with 1 to 10 carbon atoms in the alkyl group, such as methyl, ethyl, n-butyl and 2-ethylhexyl (meth)acrylate, (meth)acrylonitrile, styrene, vinyltoluene, vinyl esters of aliphatic monocarboxylic acids having 1 to 10 carbon atoms, such as vinyl acetate and vinyl propionate. Preference is also given to those acrylate resins prepared not, as is usual, in solution but instead in a bulk polymerization in which the initial charge comprises a liquid cyclic compound which acts as solvent during the polymerization reaction and which by means of ring opening forms a copolymerizable compound on reaction with one of the monomers used. Examples of such compounds are glycidyl esters of xcex1-branched aliphatic monocarboxylic acids, especially the acids or acid mixtures available commercially as neopentanoic acid or neodecanoic acid, and also lactones such as xcex5-caprolactone or xcex4-valerolactone. Where these glycidyl esters are used, it is necessary during the polymerization to use comonomers containing acid groups, such as (meth)acrylic acid, in a fraction which is at least equimolar to the amount of substance of the epoxide groups. The lactones may be used, with ring opening, both with hydroxyl group-containing comonomers and with comonomers containing acid groups.
Hydroxyl group-containing polyurethane resins B3 are obtainable in a known manner by addition of oligomeric or polymeric polyols B31, selected from polyester polyols, polyether polyols, polycarbonate polyols and polyolefin polyols, and, if desired, low molar mass aliphatic diols or polyols B33 having 2 to 12 carbon atoms, such as ethylene glycol, 1,2- and 1,3-propylene glycol, 1,4-butanediol, 1,6-hexanediol, di- and triethylene and/or propylene glycol, neopentyl glycol, trimethylolpropane, pentaerythritol, and polyfunctional isocyanates B32, the latter being used in a substoichiometric amount such that the number of hydroxyl groups in the reaction mixture is greater than the number of isocyanate groups. Suitable polyols are, in particular, oligomeric and polymeric dihydroxy compounds having a number-average molar mass Mn of from about 200 to 10000 g/mol. By means of polyaddition with polyfunctional, especially difunctional, isocyanates, they are built up to the target value for the Staudinger index of at least 8 cm3/g, preferably at least 9.5 cm3/g.
Epoxy resins B4 obtainable by reacting epichlorohydrin with aliphatic or aromatic diols or polyols, especially bisphenol A, bisphenol F, resorcinol, novolaks or oligomeric polyoxyalkylene glycols having 2 to 4, preferably 3, carbon atoms in the alkylene group have at least one hydroxyl group per epichlorohydrin molecule used. Instead of the reaction of epichlorohydrin with diols it is also possible to prepare the appropriate epoxy resins by the so-called advancement reaction from diglycidyl ethers of diols (such as those mentioned above) or diglycidyl esters of dibasic organic acids with the stated diols. All known epoxy resins may be used here, provided they satisfy the condition for the hydroxyl number.
On its own, the blocked isocyanate C is preferably not water-soluble or water-dispersible. It can be prepared by reacting the aforementioned blocking agents C2 with polyfunctional isocyanates C1 which are aromatic (i.e., the isocyanate groups are each attached to an aromatic carbon atom) and contain at least two, preferably from 2 to 4, isocyanate groups per molecule. Examples that may be mentioned of the preferred aromatic polyfunctional isocyanates are 1,3-phenylene diisocyanate, 1,4-phenylene diisocyanate, 2,4-tolylene diisocyanate (2,4-TDI), 2,6-tolylene diisocyanate (2,6-TDI), and mixtures (TDI) of these isomers, 4,4xe2x80x2-biphenylene diisocyanate, 1,5-naphthylene diisocyanate, 1,4-naphthylene diisocyanate, 4,4xe2x80x2-diisocyanatodiphenyl ether, and bis(4-isocyanatophenyl) methane (MDI) which may be reacted further with at least trihydric linear or branched aliphatic alcohols to give oligomeric compounds, which then contain preferably from 2 to 4 isocyanate groups per molecule. Examples of suitable polyhydric alcohols which are intended to result in highly hydrolysis-stable bonds include glycerol, trimethylolpropane, trimethylolethane, pentaerythritol, dimethylolpropane and -ethane. Uretdiones and isocyanurates of above diisocyanates, allophanates and biurets derived from above diisocyanates, and mixtures of such di- or polyisocyanates may likewise be used. Particular preference is given to the diisocyanates, especially TDI, and to the uretdiones, isocyanurates, allophanates and biurets derived from them.
Depending on the performance requirements it is also possible to use aliphatic isocyanates such as hexamethylene diisocyanate instead of the aromatic isocyanates preferred herexe2x80x94in that case the baking temperatures required for curing will of course be higher.
The two-component systems of the invention are mixed immediately prior to application. The pot life of the mixtures is more than 8 hours. The customary additives, known in paint technology, may be added to these mixtures.
The two-component binders of the invention can be used to formulate coating materials for substrates such as metal, wood, plastics, mineral substrates such as clay, concrete, unglazed porcelain, or else for cardboard. Preference is given to their use as binders for clearcoat materials on metallic substrates; in this application the varnish films formulated with binders of the invention exhibit particularly good adhesion.
It is also possible to replace some of the blocked isocyanate groups by water-soluble melamine resins or other amino resins which react when heated with the hydroxyl groups of the polyester AB, with crosslinking. In this case, on heating, curing takes place in a number of stages, with the isocyanate-induced curing which begins even at a relatively low temperature being able to prevent running of the precrosslinked coating film on inclined surfaces. The amino resins, especially melamine resins, may be added to the polyester component or, preferably, to the blocked isocyanates. In these compositions the mass fractions of solids in the binder mixture are preferably from 60 to 90% for the component AB, from 10 to 40% for the blocked isocyanates C, and from 0 to 15% for the amino resin component.

Two-component systems based on water-soluble polyesters and blocked isocyanates for aqueous baking varnishes


The present disclosure includes apparatus, systems and techniques relating to detecting sync marks. In some implementations, an apparatus includes phase locking circuitry that includes a phase calculator to identify a phase of sampled data, and a phase-locked loop to generate an output signal and phase-lock the generated output signal with the calculated phase of the sampled data to produce a phase-locked signal. The apparatus includes detector circuitry to receive phase information of the phase-locked output signal. The detector circuitry includes a detector to generate a stream of decision bits for the sampled data with each bit in the stream being associated with a different phase. The detector circuitry includes an output selector to select at least one bit from the stream based on the received phase information of the phase-locked output signal.

The present disclosure describes systems and techniques relating to recording data on a computer readable medium.
In magnetic-medium-based storage devices, data can be stored on circular, concentric tracks on a magnetic disk surface. A read-write head can retrieve and record data on a magnetic layer of a rotating disk as the read-write head flies on a cushion of air over the disk surface. When retrieving data, magnetic field variations can be converted into an analog electrical signal, which can then be amplified and converted to a digital signal for signal processing. To guarantee the quality of the information stored on and read back from the disk, the read-write head should be precisely positioned at substantially the center of a track during both writing and reading. A closed-loop servo system, driven by servo information embedded in a dedicated portion of the track, can be used as a reference for positioning the head.
The servo information generally defines the position of the data tracks and is generally written with great accuracy to ensure that the read-write head servo system operates properly. The servo information can be written on each surface as a radially extending set of spokes or wedges. The portion of a servo wedge at a particular track location may contain a sync field, an index mark, a gray coded track number, and two or more fine-positioned offset bursts configured in an echelon across the track. Read-write head positioning relative to a track center can be determined and corrected, if necessary, by reading and noting the respective amplitudes and timings of the offset bursts.
Conventionally, a servo writer is used to write the embedded servo information on the disk surface. A servo writer can include a large base (e.g., granite base) to minimize the effects of vibration. The servo writer also may use precision fixtures to hold the target drive, a precision, laser-interferometer-based actuator arm positioning mechanism to place the arms radially with respect to the axis of rotation of the disks in the drive, and an external clock head to position the servo wedges in time. Conventional servo writers are typically large in size and expensive. Further, as track density increases, the servo writing time required by a servo writer to write the servo information also increases, which can create a bottleneck in the disk drive manufacturing process.
Various attempts have been made to reduce usage of such servo writers. For example, some servo writing techniques have used a servo writer to generate high quality seed wedges, from which additional servo wedges can be generated by the disk drive itself using propagation self-servo write techniques. Other approaches have tried to eliminate the traditional servo writer altogether by pre-writing the disk with a low frequency reference pattern. Yet another approach has been to attempt an increase in throughput per servo writer by writing a spiral servo pattern on the disk, from which servo wedges can be generated by the disk drive itself.

Spiral servo detection with phase-locked loop (PLL)


A plastic container closure package with a linerless sealing closure system comprising a plastic container having a threaded finish for receiving a closure having a base wall and an internal skirt with complementary threads on the skirt. The plastic container is made by a process wherein a tube of molten plastic is inflated and blown to form the container and thereafter the tube is trimmed to form the sealing surface of the finish of the container. The closure includes an annular flange that extends downwardly from the underside of the base wall of the closure and radially inwardly of the closure for engagement with the container. The annular flange includes a smooth continuous frustoconical surface that faces the finish of the container and engages the inner edge at the juncture of the top surface and inside surface of the finish of the container. An annular stop extends axially from the underside of the base wall of the closure to limit the flexing of the annular flange. The width of the flange is such that the free end thereof normally extends beyond the inner edge of the finish into sealing engagement intermediate the free edge and the end of the flange.

When plastic containers are utilized to retain liquids such as oil or water, it has been found that it is necessary that the closure utilized with the container have a separate liner in order to provide an adequate seal. The problem of sealing is made even more complex where the plastic container is made by closing molds about a tube of molten plastic material and blowing the tube followed by thereafter cutting and trimming the portion of the tube that has been blown into a finish to provide a sealing surface on the upper end of the finish. The trimming process often results in variation in the plane of the finish at circumferentially spaced points along the sealing surface as well as non-uniformity in a radial direction. The trimming process can result in variations in height circumferentially of the finish, known as "trim slant". The trimming can also result in the top surface being inclined rather than being perpendicular to the longitudinal axis of the container. In addition, in such a molding process wherein the tube is extruded variations in diameter of the finish can occur circumferentially known as ovality. Each of these conditions can result in failure of the seal so that it has thought to be necessary to utilize a sealing liner in the closure. Sealing on such a container is also made more difficult due to variations or imperfections in the seam produced adjacent the juncture of the closed molds.
Various patents have been proposed including flanges extending radially outwardly and inwardly as shown in U.S. Pat. Nos. 3,053,406, 3,067,900, 3,255,909, 3,393,818 3,802,590, 4,069,937, 4,196,818, 4,220,250, 4,398,645, 4,422,947, 4,450,973, 4,598,835, 4,739,893 and 4,872,304.
As far as the present inventor is aware, none of these patents has been directed to the problems of the present invention or resulted in a satisfactory package for liquids.
Among the objectives of the present invention are to provide a package for a plastic container made by the aforementioned process which does not require a separate liner and utilizes a linerless sealing closure system which will compensate for any unevenness and out-of-round top surfaces on the finish of the container; and which container package will be capable of packaging oil, water or similar fluids.
In accordance with the invention a plastic container closure package with a linerless sealing closure system comprising a plastic container having a threaded finish for receiving a closure having a base wall and an internal skirt with complementary threads on the skirt. The plastic container is made by a process wherein a tube of molten plastic is inflated and blown to form the container and thereafter the tube is trimmed to form the sealing surface of the finish of the container. The closure includes an annular flange that extends downwardly from the underside of the base wall of the closure and radially inwardly of the closure for engagement with the sealing surface on the container. The annular flange includes a smooth continuous frustoconical surface that faces the finish of the container and engages the inner edge at the juncture of the top surface and inside surface of the finish of the container. An annular stop extends axially from the underside of the base wall of the closure to limit the flexing of the annular flange. The width of the flange is such that the free end thereof normally extends beyond the inner edge of the finish surface into sealing engagement intermediate the free edge and the end of the flange.

Plastic container package with linerless sealing closure system


Protective strips for use in the manufacture of upholstered furniture include a fastening strip portion, a cover strip portion and a hinge portion which flexibly connects the fastening and cover strip portions to one another. In use, the protective strips may be positioned such that a portion of the upholstery fabric is sandwiched between the fastening strip portion thereof and a portion of the furniture frame to which the fabric is to be attached. Suitable fasteners (e.g., staples, tacks, nails, brads and like fasteners) may then be physically driven through the fastening strip portion and the underlying fabric portion into the furniture frame and thereby fasten the fabric portion physically to the frame. Once the fastening strip portion has been fastened to the furniture frame, the remaining fabric portion may be doubled over the fastened tail portion which in turn causes the cover strip portion to be folded over the fastening strip portion. In such a manner, the heads of the fasteners are physically covered by the cover strip portion so as to prevent contact with the overlaid fabric. As such, rubbing of the fabric against the fastener heads is prevented so as to thereby preclude (or at least substantially minimize) fabric abrasion and wear.

During the manufacture of upholstered furniture, it is conventional to employ tacks and staples to fasten upholstery fabric to the underlying furniture frame. Various tack strips are known for such purpose. For example, conventional tack strips include a ribbon of metal from which generally triangularly shaped nails or tacks are punched and bent at right angles. See, U.S. Pat. Nos. 6,647,610, 6,857,178 and 6,989,186 (the entire contents of each such patent and patent application being expressly incorporated hereinto by reference).
Sometimes tack and/or staple guns are employed so as to fasten upholstery fabric to the furniture frame by means of individual fasteners such as staples, tacks, brads and/or nails. In this regard, a tail portion of the fabric is typically first fastened to the furniture frame by means of the fasteners so that the remaining portion may be folded over, and thereby cover, the fastener heads. It can be appreciated however that over time pressure or rubbing of the covering fabric portion on the tack or staple head will result in fabric wear.
It has been conventional practice to place a paperboard strip against the fabric tail and then drive the individual fasteners through the paperboard strip and fabric tail to secure the fabric to the underlying furniture frame. Such conventional practice has however not been entirely satisfactory Specifically, the fastener heads are still placed in contact with the covering fabric section and thus cause localized fabric abrasion and wear to occur. The likelihood of fabric abrasion and wear is more acute even with such a conventional paperboard strip in those instances where the tack or staple does not fully penetrate into the wood frame of the furniture piece or bends due to improper and/or incomplete installation.
Therefore, it would especially be desirable if upholstery fabric wear due to underlying tack and staple heads could be eliminated if not significantly minimized. It is toward fulfilling such a need that the present invention is directed.
Broadly, the present invention is embodied in a protective strip for use in the manufacture of upholstered furniture comprised of a fastening strip portion, a cover strip portion and a hinge portion which flexibly connects the fastening and cover strip portions to one another. In use, therefore, the protective strip of the present invention may be positioned such that a portion of the upholstery fabric is sandwiched between the fastening strip portion thereof and a region of the furniture frame to which the fabric is to be attached. Suitable fasteners (e.g., staples, tacks, nails, brads and the like) may then be physically driven through the fastening strip portion and the underlying fabric portion into the furniture frame. In such a manner, the fabric portion is attached physically to the furniture frame.
Once the fastening strip portion has been attached to the furniture frame, the remaining fabric portion may be doubled over the fastened tail portion which in turn causes the cover strip portion to be folded over the fastening strip portion. The heads of the fasteners are therefore physically covered by the cover strip portion so as to prevent contact with the overlaid fabric. As such, rubbing of the fabric against the fastener heads is prevented so as to thereby preclude (or at least substantially minimize) fabric abrasion and wear.
These and other aspects and advantages will become more apparent after careful consideration is given to the following detailed description of the preferred exemplary embodiments thereof.


A liquid crystal display, comprising: a liquid crystal display panel and a backlight module. The backlight module comprising: a reflection unit, a light emitting unit, and a compound diffusion plate structure. The light emitting unit has a plurality of light emitting components installed within the installation space of the reflection unit. The compound diffusion plate structure is placed on one side of the light emitting unit, comprising: a body unit and a printing micro diffusion unit. The body unit has a main layer, and a plurality of micro diffusion particles formed inside the body unit, allowing light to diffuse within the body unit. The printing micro diffusion unit has a plurality of convex lens units formed on a light entrance plane or a light exit plane of the body unit by means of printing.

1. Field of the Invention
The present invention is related to a compound diffusion plate structure, backlight module, and liquid crystal display; in particular, to a compound diffusion plate structure capable of increasing brightness and range of angle of view, as well as a backlight module and a liquid crystal display using the compound diffusion plate structure.
2. Description of Related Art
Since the demand on the size of backlight module keeps increasing, conventional small to middle size backlight modules of side-light type have been gradually substituted by direct-light type backlight modules. In a backlight module of side-light type, light enters on one side of light guiding plate, and repeatedly reflects and diffuses inside the light guiding plate based on the total reflection principle in order to enhance the light range and uniformity; afterward, the total reflection is broken by an optically designed micro structure to uniformly emit light out of the light guiding plate, light is then diffused through a diffusion film, and concentrated via an enhancing film to a positive angle of view, then after reflection, providing the required light for the light crystal panel, which does not generate light in itself for image display operations. Since the lamps used in the side-light module are hidden on the side of the light guiding plate and covered by masks, human eye will not directly see these lamps, thus uniformity thereof can be conveniently controlled by the design of the light guiding plate; wherein, the lamps are restricted to the thickness of the light guiding plate, so brightness is usually insufficient, thus enhancing film is needed to increase brightness. However, in general cases, due to the shrinkage of angle of view caused by using the concentrating plate, the final angle of view may not be suitable for multiple viewers to see at the same time. In terms of the direct-light type backlight module applied in current LCD-TV's, as the required size becomes larger, the requirements on injection smoothness in large-sized light guiding plate and tonnage of the injection machines make it more and more difficult to successfully achieve the necessary manufacturing processes for direct-light type backlight module, and the overall weight of the product becomes much heavier; therefore, it is common to see side-light light guiding plate with insufficient brightness used in large-size televisions because the manufacturing process difficulty and cost of direct-light type backlight module is much higher; furthermore, the larger the surface area is, the greater the demand for brightness or luminosity becomes, which means the number of lamps needed increases accordingly, and because the side-light light guiding plate with the side-light type space limitation problem can not accommodate more lamps therein, thus it is incapable of meeting the requirements on large surface and high brightness in present television market. It should be noted that large size liquid crystal televisions no longer use the backlight module of side-light type which requires light guiding plate, but employ direct-light type backlight module of multiple lamps to fulfill the demand for televisions with high brightness and wide angle of view features.
The backlight module, in essence, provides the liquid crystal panel with a light source of uniformity and high brightness, whose basic principle is that it converts a common, similar point-wise or linear light source into a planar light source product with high luminosity and uniform brightness through a terse and effective optical mechanism. The optical design of a general side-light type structure uses a linear light source from a Cold Cathode Fluorescent Lamp in which the emitted light passes through a reflection mask and enters into the light guiding plate, converted from linear light source distribution into a uniform planar light source, then made to subject to the light equalization performed by a diffusion plate and light concentration performed by a prism sheet, in order to enhance the brightness and uniformity in the light source.
In general, light passes through a diffusion plate after emitting from a light source, with poorer orientation in the light emitted from the diffusion plate; therefore, it is necessary to use a prism sheet to correct the direction of light which applies the geometric structure in its design to allow light to refract and totally reflect to achieve the objectives of light concentration and frontal brightness enhancement. However, the effect of brightness increase in the backlight achieved by the above method is merely based on the light convergence from a wider angle of view to a narrower one; consequently the angle of view shrinks, causing a problem of reduced angle range of view when watching the display, so that the user can only view with a limited angle range of view or otherwise it is impossible to clearly see the images shown on the screen of the display, resulting in inconvenience for users to a certain extent. As such, currently there also provides a novel Dual Brightness Enhancement Film (DBEF), which applies the principle of multi-film interference, to achieve the design of brightness enhancement on total angle of view without compressing angle of view. For the liquid crystal television using the direct-light type backlight module, since the plurality of lamps in the backlight module are directly places in the lamp box of the backlight module, light emitted from the lamp will be directly seen by human eyes; so, suppose simply placing the lamp into the box without the design of light equalization, it can not be used as a backlight source since this may cause poor uniformity in the backlight module and brightness variation may occur, resulting in so-called un-even lamp image and lamp phenomenon (referred as MURA problem in Japan). The condition occurring in the lamp source of the direct-light type backlight module is rather analogous to when people directly look at a fluorescent light: the place where people see the fluorescent light tube is most bright, but the brightness in the dark zone between light tubes decrease dramatically. Therefore, the direct-light type backlight module needs a diffusion plate and multiple diffusion films, or even micro structure diffusion films, to mask or diffuse lamp images so as to achieve the purpose of uniform backlight source. Only by this uniform backlight module can the uneven effect in the liquid crystal image display be avoided. The compound diffusion plate according to the present invention can reduce or eliminate the MURA problem, thus providing required uniform illumination for future use in various backlight modules, advertisement light boxes, lighting devices, road lamps, and etc.
Accordingly, having noticed the above-discussed improvable defects and utilized solid long-term relevant experiences in practical operations, together with prudent and insightful observations and researches, in conjunction with, theoretical applications as well, the inventors of the application herein propose the present invention to offer reasonable design for being able to effectively amend the aforementioned defects.

Compound diffusion plate structure, backlight module, and liquid crystal display


A system and method for optical switching of networks in a multi-node computing system with programmable magneto-optical switches that enable optical signal routing on optical pathways. The system includes a network of optical links interconnecting nodes with switching elements that are controlled by electrical control signals. Data transmission is along the optical links and an optical pathway is determined by the electrical control signals which are launched ahead of optical signal. If links are available, an optical pathway is reserved, and the electrical signal sets the necessary optical switches for the particular optical pathway. There is thereby eliminated the need for optical-electrical-optical conversion at each node in order to route data packets through the network. If a link or optical pathway is not available the system tries to find an alternative path. If no alternative path is available, the system reserves buffering. After transmission, all reservations are released.

The present disclosure relates generally to methods and apparatuses for optical switching of networks in multi-node computer systems using optical interconnects to enable packet routing, and by using optical switching on these interconnects.
Fast networks are essential in improving the performance of high performance computing systems. The use of optical interconnects is therefore necessary by virtue of their inherent high bandwidth. Existing high performance computing systems such as Blue Gene/L and Blue Gene/P systems available from International Business Machines Corporation utilizes buffering of packets (in memory) at every node and routing on every node with electrical switching of the networks. In those embodiments, packets are routed along hops of a route or path and stored in every node, routed and injected again into the network.
Simply using optical interconnects to replace electrical interconnects would require electrical to optical conversion at each node.
It would be desirable to provide an optical switching system that eliminates the necessity of O-E-O (optical-electrical-optical) conversion and buffering at each node of the network.

This patent is subject to a terminal disclaimer.

Multi-node system networks with optical switches


A head covering is described that is positioned on a head of a wearer to retain the wearer's hair in a desired position. The head covering comprises a hooded cap and an extension. The hooded cap includes a pair of ties and a set of straps. The hooded cap is secured to the head of the wearer using ties. The extension connects to the hooded cap on one end and includes an opposing distal end portion with a free terminal end. The extension includes a pouch and a flap. The pouch defines a first aperture in proximity to the hooded cap and a second aperture in proximity to the flap. A passageway is defined between the first aperture, the extension and the second aperture. The flap and pouch include connectors for the optional connection of the flap and pouch to secure the second aperture in a closed position. At least one strap is connected to the extension. The straps are constructed to secure the extension and hair together. The head covering has a first position wherein the head covering is passed along the hair of the wearer from a distal end of the wearer's hair to the wearer's head. The second position of the head covering includes the hooded cap positioned on the wearer's head and the hair of the wearer at least partially positioned in the passageway defined in the extension.

1. Field of the Invention
The present disclosure relates to heading covering products and their methods of application and in particular, to an apparatus and method for a head covering that can be selectively employed to retain and contain the hair of a wearer.
2. Description of the Related Art
There are many head coverings on the market today, the most popular being the du-rag. While this head covering is widely used, the du-rag is not designed to hold long hair in place, rather to lie over the hair. After an extensive patent search, we have found the following patents to be relative to the Locks Down disclosure. U.S. Pat. Nos. 7,096,510, 6,738,986, 6,735,783, 5,878,756, D135,323 and D482,843.
U.S. Pat. No. 7,096,510 to Yeadon (2004) teaches a head covering that has a three-sectioned hemispheric crown. The sections of the crown include a headband 6, securing ties 7, and a center section 3 that includes a flap extending over the neck 2. The flap extending over the neck 2 is an extension or pouch 8 form the back of the head down the neck. The pouch 8 received the long hair of the wearer. An elastic opening 10 secures the inner wall around the hair as shown in FIGS. 1-3 of the reference.
U.S. Pat. No. 6,738,986 to Martin (2004) teaches a head covering made from a single piece of material. A central top seam forms a hemispheric cap portion and a fold 36 and the securing of the edges 34 and 32 form a pouch portion. Tie members 38 and 40 are linear vertical strips of material that are integrally connected to and extend downward from the bottom front of the cap portion. Tie members 38 and 40 also have an inner edge formed from cut outs 55 (see col. 3, lines 40-51).
This head covering claims a tail compartment where there is a closure to store things in, it also claims that hair could be tucked into this compartment. This demonstrates that our method of application is inconsistent with and could not be used on this head covering. Also, this reference teaches the use of the head covering during underwater/aquatic uses such as swimming. In contrast, the present disclosure is a stylish fashion hair accessory.
U.S. Pat. No. 5,878,756 to Bilodeau (1999) teaches a cap with a hollow hemispherical configuration. The lower peripheral edge has a thin rectangular band 16 mounted thereon. Band 16 has a pair of free end 18 that extend from a rear extent of the cap, selectively tie and secure the cap to the head of the user. A hair sleeve 20 is an elongated strip 22 of flexible cloth that is connected to the cap. Hair sleeve 20 has four equally spaced pairs of rectangular tabs 24 that extend perpendicularly from the longitudinal side edges of the hair sleeve 20. Tubular sleeve 26 can thus receive and pass through the hair of the wearer. In contrast to the present disclosure, this head covering has a sleeve that ties around the long hair of the wearer and thus cannot employ the method of applying the head covering of the present disclosure.
U.S. Pat. No. D482,843 to Burnett (2003) shows triangular shaped head covering that is folded to define ties that can connect in the front or back of the head. A pouch is also shown that receives, or as claimed retains the wearer's hair. This head-covering patent claims the ornamental design for a scarf and headwear with packet for retaining hair.


A safety cap for an electrical outlet having an adhesive section can be attached to a standard outlet cover. Alternately, an outlet cover including two slidable plates including a spring or spring groove can be used to prevent access to the outlet by a child. An elongated member on one plate is used to contact a spring on the other plate. Alternately, the elongated member can fit into a spring groove to bias the plates apart into the closed position. Locking pins can be used to lock the plates onto an aperture at the base of a plug's power prong. Additionally, a recess around each electrical outlet can mate with a respective lip of a plug to provide an interlocking interface between the plug and outlet cover to prevent a child from being able to insert a metal object between the plug and the faceplate.

In residential and other structures, electrical outlets are generally positioned a short distance above the floor. This makes the outlets readily accessible to small children. A curious child is inclined to test and probe his environment and may stick objects, such as paper clips, into the prong receiving openings of an electrical outlet. This exposes him to the danger of shock or even death.
Additionally, an exposed outlet presents the problem of "carbon fires" that can occur when dust accumulates in an outlet.
In spite of generally widespread knowledge of the dangers that electrical outlets present to small children, very few devices are commercially available for denying a child access to an outlet. The most commonly available device is a small plastic disk with prongs that plug into the openings of an outlet receptacle. The disk covers the receptacle and takes the place of an electrical plug to prevent insertion of any other object in the openings. A major disadvantage of this type of device is that the disk may easily become lost or mislaid when it is temporarily removed to allow normal use of the outlet.
There have been a number of proposals for providing a permanently mounted safety cover for electrical outlets to make the prong receiving openings inaccessible to a child. Such proposals generally provide an inadequate solution either because the safety cover is too easily defeated by a child who is still too young to understand the dangers of electricity or because the covering device is unduly complicated and/or cumbersome.
It is desired to have an improved electrical outlet safety cover that avoids some of the problems of the prior art.


A new and distinct cultivar of Browallia plant named ‘UNHBR12’, characterized by numerous single flowers that are light purple in color with a white center, compact and rounded growth habit, stems that do not break or separate on the center of the mature plant, and good performance in partial shade in the garden and as a hanging basket.

The present Invention relates to a new and distinct cultivar of Browallia plant, botanically known as a Browallia artificial hybrid, and hereinafter referred to by the cultivar name 'UNHBR12'.
The new Browallia is a product of a planned breeding program conducted by the Inventor in Durham. N.H. The objective of the breeding program is to create new compact Browallia plants with attractive flowers in a range of colors, profuse flowering and reduced fruit set.
The new 'UNHBR12' originated from a hybridization made by the Inventor on Aug. 8, 2000 between a proprietary selection of Browallia speciosa, code UNH BROW1-2, not patented, used as female, and a proprietary selection of Browallia americana code UNH BROW6, not patented, used as male. Seed was sown on Feb. 2, 2001. From the progeny, a single plant B01-1, later coded as 'UNHBR12' was selected in Durham, N.H., USA, on the basis of its profuse flowering, compact growth habit and attractive flowers.
Asexual reproduction of the new cultivar by terminal vegetative cuttings since June 2001 in Durham, N.H. has shown that the unique features of this new Browallia are stable and reproduced true to type in successive generations.