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A process for coating a surface of a metal-containing substrate with a bioceramic material includes activating the surface of the metal-containing substrate by applying a voltage to the substrate in a liquid containing an electrolyte; and, immersing the substrate in a deposition solution containing the bioceramic material or precursors for the bioceramic material. The coated substrate may be heat treated to enhance coating bond strength. The bioceramic material may be hydroxyapatite. Coated substrates are useful for the fabrication of prostheses.
1. Process for coating a surface of a metal-containing substrate with a bioceramic material comprising: activating the surface of the metal-containing substrate by applying a voltage to the substrate in an aqueous solution of an alkali metal hydroxide; and, immersing the substrate in a deposition solution containing the bioceramic material or precursors for the bioceramic material to form a coated substrate.
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19. Process for coating a surface of a Ti-containing substrate with hydroxyapatite, comprising: activating the surface of the Ti-containing substrate by applying a DC voltage of 7.5-12.5 V at a current density in a range of from 0.08 A/cm2 to 0.18 A/cm2 to the substrate for 30 minutes or more in an aqueous solution having an alkali metal hydroxide concentration in a range of from 5 M to 15 M; and, immersing the substrate in an aqueous solution of hydroxyapatite precursors at a pH in a range of from 6 to 8 to form a coated substrate.
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The present invention is related to coating of a metal-containing substrate with a bioceramic material.
Materials implanted in vivo essentially have direct contact with the human body through the interface between the implant surface and bones, tissues and extracellular body fluids. The surface of the implant therefore plays a very important role related to surface chemistry, topography and micro/nano structure, and tribological properties. Major issues related to surface modification processes include corrosion and wear resistance of the implant and biocompatibility and bioactivity. Chloride ion concentration in body fluid is 113 mEql−1 and in interstitial fluid is 117 mEql−1, which may corrode metallic materials. Body fluids contain amino acids and proteins that tend to accelerate corrosion. Toxicity and allergy occur if metallic materials are corroded by fluid, if metallic ions are released into the fluid for a long time, or if ions combine with biomolecules such as proteins and enzymes. Loosening of implant could occur due to the wear of the implant. All of these factors lead to premature implant failures, debilitating pain, and surgical revisions.
Both corrosion and wear are related to the surface of implants. Extensive studies have been reported on surface modifications to understand and enhance the performance of implants. One approach is to modify the surface topography by creating a rough or porous surface on the implant to increase the surface area available for bone/implant apposition, which improves the fixation of the implant in the bone. A natural consequence of increasing the surface area is an increase in metal ion release, due to an increased surface contact with corrosive media. A further complication is the increase in wear debris due to increased surface friction, which also results in increased ion release rates and loosening of the implants. Another approach to surface modification is to coat the implant surface with hard materials focusing on increasing the wear resistance. Titanium nitride was extensively reported for implant surface modification using chemical vapor deposition (CVD) and physical vapor deposition (PVD). Although these methods provide the implant articulating surfaces with excellent wear resistance, the deposited layers often suffer from lack of adherence and are not associated with bone/implant apposition. Low energy nitrogen ion bombardment-plasma nitriding is one of the most up-to-date methods for improving the wear and corrosion behavior of metallic alloy. In plasma nitriding, a Ti-based substrate is directly involved in the reaction of coating formation, which results in an excellent adhesion of the coating to the substrate. However, the inherent high cost of plasma nitriding equipment and its operation reduces its cost-effectiveness.
Other surface coatings have been tried to improve the bone/implant interface bonding. These include hydroxyapatite (HA) coatings produced by plasma spray or ion implantation. Hydroxyapatite, (Ca10(PO4)6(OH)2), is characterized by a hexagonal structure (a=9.423 Å, c=6.875 Å, Space Group: P63m) with a density of 3.16 g/cm3. It is one of the three main components of the human body (HA, water and collagen) and is able to integrate bone structure and support bone ingrowth. For this reason, coatings of hydroxyapatite are often applied to metallic implants to alter the surface properties. In this manner the body sees the hydroxyapatite-type material as a compatible material. Without the coating, the body would see a foreign body and either isolate it from surrounding tissues or induce a tissue reaction.
However, HA coatings formed by plasma spray, the most popular commercially available technique for HA coating on implants, generated some long term concerns. A study has revealed that even though uncemented HA-coated hip prostheses had better survivorship than cemented, the HA cups with follow-up longer than 6 years revealed an increased surgical revision rate (replacement of the primary implant). Also in a study about polyethylene wear, osteolysis and acetabular loosening with HA-coated prostheses, there were no stem revisions but 24% of the acetabular components required revision. HA debris might accelerate the wear of the high density polyethylene material (HDPE) of the acetabular component. Another study of HA coating on a G.B. acetabular cup found a high rate of debonding and failure. Yet another study reporting on the evaluation of 6 revisions of HA-coated acetabular cups showed HA granules embedded in the HDPE, which may produce severe clinical problems.
There are a variety of known techniques to produce HA coatings on substrate surfaces. Plasma spray advantageously produces high density coatings, but disadvantageously is a line-of-sight process and oxidation of powder when conducted in air leads to poor adhesion and low purity coating. High velocity oxyfuel advantageously provides good coating bond strength, but disadvantageously is a line-of-sight process and produces low purity coatings. Ion bean assisted deposition advantageously uses low deposition temperature, provides high adhesion and provides good control of stress level, microstructure and composition, but disadvantageously is a line-of-sight process and is higher in cost. Pulsed laser deposition advantageously provides high purity coatings, but disadvantageously is a line-of-sight process, requires high capital investment and maintenance costs and provides a low deposition rate. Chemical vapor deposition advantageously is not line-of-sight dependent, readily provides coatings at near theoretical density and permits control of preferred grain orientation and grain size, but disadvantageously is a high temperature process in most cases leading to low purity HA coatings. Electrodeposition is advantageously low cost and simple and provides uniform coatings of high purity and low porosity, but disadvantageously is a line-of-sight process to some extent and is a two-step process that must be followed by hydrothermal treatment to obtain HA coatings. Electrophoresis deposition advantageously is not a line-of-sight process, is low cost and simple, provides high deposition rate and produces a wide range of coating thicknesses (from <1 um to >500 um), but disadvantageously is a two-step process requiring densification by sintering which may reduce the purity of the HA coating. Sol-gel deposition advantageously permits coating of complex shapes with coatings having increased homogeneity and fine-grained structures, but disadvantageously requires firing leading to reduced purity of the HA coating. Bio-mimetic deposition advantageously is a low temperature process applicable to any heat sensitive surface including polymers, permits formation of bone-like apatite crystals with high bioactivity and permits incorporation of bone growth stimulating factors and antibiotics, but disadvantageously is a very slow process requiring precise control of process parameters in which obtaining uniform coating is a practical challenge.
Finally, chemical deposition is a process mainly used to prepare HA powders but not to coat HA on a substrate. Few studies of chemical deposition of bioceramic materials are available and process kinetics are poorly understood. In theory, chemical deposition may be able to provide uniform coatings of unlimited thickness on complex shapes, be used to deposit HA on polymer surfaces, and produce a porous top layer to encourage bone ingrowth. No suitable chemical processes are commercially available for coating.
Of the processes described above, most are line-of-sight dependent and/or involve high temperature (over 15,000� C. for plasma spray). It is a challenge for any process that is line-of-sight in nature to produce uniform coating, particularly on sloped and curved surfaces. As for processes that rely on high temperature, they cause decomposition of HA which leads to the formation of impurities such as tetracalcium phosphate (Ca4P2O9), amorphous calcium phosphate, α-tricalcium phosphate (Ca3(PO4)2), and β-tricalcium phosphate (Ca3(PO4)2). These impurities are unstable in the body fluids and cause serious concerns for localized corrosion. The selective dissolution of these impurities may result in an accelerated wear caused by the roughening/scoring of the articulating surface, and this debris will, in turn, make the wear a more severe issue.
It is apparent from the processes described above that biomimetic and chemical processes are neither line-of-sight dependant nor involve high temperature operation. Biomimetic coating is an approach that consists of immersion of metal implants in simulated body fluids (SBF) at a physiologic temperature and pH. HA coating, the major component of bone, grows in a way similar to the natural bone growth in our body. This process produces HA coating with desirable properties such as high purity and bioactivity. Another uniqueness of this process is its capability to incorporate antibiotics (e.g. tobramycin), proteins and bone growth stimulators (e.g. osteogenics). However, although SBF mimics the inorganic composition, pH, and temperature of human blood plasma, achieving a reasonable coating thickness for practical applications takes a long time. Long immersion time (7-14 days) with daily refreshment of SBF's is required. The difficulty results from the metastability of SBF and the process requires replenishment and a constant pH to maintain supersaturation for apatite crystal growth. As a result of the low solubility product of HA and the limited concentration range for the metastable phase, this operation is extremely difficult and might lead to local precipitation or uneven coatings. Such an intricate and long process can hardly be tolerated in the prostheses coating industry.
Chemical coating processes produce HA coatings at low temperature and are line-of-sight independent. Theoretically, chemical processes can produce uniform coatings of unlimited thickness on complex shapes. The deposition rate of chemical HA coating is significantly higher than the biomimetic process due to significantly higher and controllable process parameters. Unfortunately, little is known about its chemical reaction kinetics and the process is used mainly for producing HA powder.
There remains a need in the art for a chemical process for coating a bioceramic material, e.g. hydroxyapatite (HA), on a surface of a substrate.
There is provided a process for coating a surface of a metal-containing substrate with a bioceramic material, comprising: activating the surface of the metal-containing substrate by applying a voltage to the substrate in a liquid containing an electrolyte; and, immersing the substrate in a deposition solution containing the bioceramic material or precursors for the bioceramic material to form a coated substrate.
There is further provided a process for coating a surface of a metal-containing substrate with a bioceramic material, comprising: activating the surface of the metal-containing substrate by applying a voltage to the substrate in a liquid containing an electrolyte; immersing the substrate in a deposition solution containing the bioceramic material or precursors for the bioceramic material to form a coated substrate; and heat treating the coated substrate.
There is yet further provided a metal-containing substrate coated with a bioceramic material.
There is still yet further provided a prosthesis comprising a metal-containing substrate coated with a bioceramic material.
In comparison to prior art processes, e.g. plasma spray processes, processes of the present invention advantageously permit the formation of purer bioceramic coatings which contain fewer impurities leading to fewer imperfections or holes in the coating leading to more durable coatings. Further, uniform coatings on complex geometries may be achieved with relative ease. Also, smaller particle sizes in the coating may be obtained. Furthermore, the present processes are simpler and less expensive than prior art processes. The present processes may be conducted at lower temperatures; they are not line-of-sight dependent; they have excellent scalability; and they incur low capital investment and lower maintenance and operation cost.
Activation of the Substrate:
The present processes involve activating the surface of a metal-containing substrate by applying a voltage to the substrate in a liquid containing an electrolyte. Electrochemical activation of the surface sensitizes the surface to deposition of the bioceramic material during the coating process.
Voltage may be applied to the substrate by DC current. Applied voltage may result in polarization of the surface of the substrate. Preferably the substrate is used as an anode and the voltage is applied anodically. If desired, an AC perturbation may be superimposed over the applied voltage. The applied voltage (or applied average voltage in the case of an applied voltage with an AC perturbation) is preferably in a range of from about 1 V to about 25 V, preferably from about 1 V to about 20 V, more preferably from about 2 V to about 20 V, even more preferably from about 7.5 V to about 12.5 V. Application of too high a voltage during activation may ultimately result in poor coating performance.
Voltage may be applied for any time duration that suitably activates the surface, preferably not less than about 1 minute. More preferably, the duration over which voltage is applied is about 30 minutes or more. Current density is preferably in a range of from about 0.05 A/cm2 to about 0.2 A/cm2, more preferably from about 0.08 A/cm2 to about 0.18 A/cm2, even more preferably from about 0.1 A/cm2 to about 0.15 A/cm2.
Magnitude of applied voltage, time duration and current density during activation of the substrate surface may ultimately affect coating thickness. Activation may be conducted at any convenient temperature provided the liquid containing the electrolyte remains in a substantially liquid state.
Activation of the surface of the substrate is performed in a liquid-based system, for example a solution of an electrolyte or a molten electrolyte. Solution-based systems are preferred. Solution-based systems have a solvent, for example water, ammonia, etc., and an electrolyte The electrolyte is chosen to provide a negative charge to the surface of the substrate. For example, the electrolyte may be a basic electrolyte that generates anions in the solvent, the anions providing a negative charge on the surface of the substrate. The solvent system is preferably water. The electrolyte is preferable a base or mixture of bases, for example alkali metal hydroxides, alkaline earth metal hydroxides or mixtures thereof. Some suitable electrolytes are sodium hydroxide, potassium hydroxide, lithium hydroxide, calcium hydroxide or mixtures thereof. Sodium hydroxide, potassium hydroxide or mixtures thereof are particularly preferred.
In solution-based systems, the electrolyte may be present in any suitable concentration that results in activation of the surface of the substrate. Preferably, the concentration is in a range of from about 0.1 M to about 20 M, more preferably from about 5 M to about 15 M.
In one embodiment of the invention, activation of the substrate surface may be performed with DC current having a current density of about 0.1 A/cm2 at an applied voltage of about 10 V for about 30 minutes in a 10 M aqueous solution of sodium hydroxide.
Activation may also include sonication. Sonication during activation, for example with ultrasound, may enhance the coating process when coating is performed over longer periods of time (e.g. 24 hours or more).
The metal-containing substrate is any material comprising a metal which can be activated as previously described and on to which a bioceramic material can be coated. The metal-containing material may be, for example, a pure metal, an alloy or a metal-containing composite. Metal-containing composites may be, for example, metal-containing ceramics, or composites of one or metals and a polymer.
Examples of some metals that may be present in the metal-containing substrate are Ti, Zr, Cr, Co, Au, Pt, Ag, Ni, Cu, Mg, Ca, and stainless steel. Metal-containing substrates containing a Group 4B metal are of particular note. In one embodiment, the metal-containing substrate contains Ti, Zr or mixtures thereof. Ti-containing materials are preferred, for example Ti alloys or Ti-containing composites (e.g. Ti-HDPE composite). A particularly preferred substrate is Ti6Al4V alloy.
Coating of the Substrate:
In order to coat the substrate to form a coated substrate, the activated substrate is immersed in a deposition solution containing bioceramic material or precursors for the bioceramic material. Precursors are chemical entities which when combined, for example through chemical reaction, form the bioceramic material. The bioceramic material forms on to the surface of the substrate forming a coating.
The bioceramic material deposited on the surface of the substrate is preferably hydroxyapatite (HA). Preferably, the deposition solution contains precursors for HA, for example calcium ions and orthophosphate ions. Calcium ions and orthophosphate ions may be accompanied by counter ions. The deposition solution may contain other components, for example other salts (e.g. sodium, potassium and/or magnesium salts having counter-anions, for example chloride, bicarbonate and/or sulfate).
The deposition solution comprises a solvent and either bioceramic material, precursors for the bioceramic material or a mixture thereof dissolved therein. For HA coating, the solvent is preferably water. HA has a tendency to precipitate from aqueous solution, particularly at high pH. It is desirable to deactivate the deposition solution by reducing the pH of the solution to enhance selective formation of HA coating on the substrate. At the same time, it is preferable to have a saturated solution of HA or HA precursors to increase deposition rate of the HA on to the substrate. Preferably, the pH is less than about 8, more preferably in a range of from about 6 to about 8. If the pH of the deposition solution is too low, the solution may act to deactivate the surface of the substrate leading to poorer coating performance.
The pH of the deposition solution may be lowered with pH adjusting agents, for example acids (e.g. hydrochloric acid, phosphoric acid, etc.) to reduce unwanted precipitation of HA. In one embodiment buffers containing HCl or TRIS (tris-hydroxymethyl aminomethan) are used to adjust the pH.
During deposition it is desirable, although not necessary, to replenish the deposition solution with more HA or HA precursors in order to maintain a saturated solution of HA or HA precursors to keep the HA deposition rate substantially constant. Replenishment of the deposition solution may be conducted at any suitable time. Preferably, replenishment occurs at regular intervals, for example every 5 to 60 minutes. Replenishment increases coating growth on the substrate, and more frequent replenishments lead to more coating.
Activation of the substrate surface together with deactivation of the deposition solution leads to coating of the substrate surface rather than precipitation of HA in the solution. Further, by selectively activating a part of the substrate, it is possible to selectively coat that part. Surprisingly, the coating process appears to be �autocatalytic� in that the initial covering of the surface of the substrate does not inhibit further coating.
Additional materials may be incorporated into the coating. Such incorporation may be achieved by including one or more of the additional materials in the deposition solution. Inclusion of the one or more additional materials may be effected at any time during the coating process. For example, additional material may be included in the solution throughout the coating process, only at the beginning of the coating process, only at the end of the coating process, in the middle of the coating process, or at staggered intervals during the coating process For medical applications, additional materials may be, for example, bone growth stimulating factors, antibiotics, proteins, hormones, etc.
The substrate may be immersed in the deposition solution for any suitable length of time to form a coating on the substrate surface. Longer immersion times lead to thicker coatings. The substrate may be immersed in the deposition solution for a duration of 0.5 hours or more. Durations of 10 hours or more, preferably 15 hours or more lead to coating thicknesses acceptable for medical applications. Coating thicknesses of up to 50 μm or more can be achieved.
Coatings produced by the present process have excellent morphological characteristics. For example, average grain size is smaller than in coatings produced by prior art processes. By the process of the present invention it is possible for the coating to have an average grain size in the nano-scale, for example less than 20 nm in size, particularly in a range of about 10-20 nm in size. Further, nanoporous structures can be formed having pore diameters less than 800 nm, for example 200-500 nm. Such pore sizes are favourable for encouraging bone growth into the surface of a coated implant.
One of the problems with prior art processes is that HA decomposes, particularly at high temperatures, to form other calcium phosphate compounds which contaminate the coating. Such contaminants lead to imperfections or holes in the coating leading to a decrease in durability. The present process permits deposition of very pure HA coatings with significantly reduced levels of contaminants since HA is selectively deposited on the substrate under gentle conditions, leading to more durable coatings.
Heat Treatment of the Coated Substrate:
After coating the substrate with the bioceramic material, it may be desirable to heat treat the coated substrate to increase bond strength of the coating on the substrate. Heat treatment is preferably performed at a temperature below the temperature at which HA begins to decompose, which is about 800� C. More preferably, the heat treatment temperature is in a range of from about 350� C. to about 800� C., for example from about 350� C. to about 650� C., or from about 350� C. to about 600� C., or from about 350� C. to about 550� C., or from about 500� C. to about 650� C., or from about 500� C. to about 600� C., or from about 550� C. to about 650� C. In one embodiment, a temperature of about 550� C. may be used. Heat treatment is preferably conducted in a gaseous medium, for example air, argon, neon, helium, nitrogen or mixtures thereof. In situations where only part of a substrate is to be coated, it is sometimes desirable to conduct heat treatment in a gas that is inert to the substrate to reduce the possibility of damaging the substrate, for example through oxidation. Heat treatment may be conducted for any suitable length of time, for example for 0.5 hours or more, particularly for about 1-2 hours. Heat treatment can lead to an increase in coating bond strength of over four times. Coating bond strengths of 24 MPa or more can be achieved.
Processes of the present invention are useful for any application in which the coating of a bioceramic material on a metal-containing substrate is desired. The processes are particularly useful in the fabrication of medical devices, e.g. prostheses, especially prosthesis for replacing bone tissue. Prostheses include, for example, replacements for limbs (e.g. arms and legs), digits (e.g. fingers and toes), facial bones, hip bones, spinal bones, and parts thereof. Prostheses may be fully or partially implanted in a body of an animal, for example a human.
Further features of the invention will be described or will become apparent in the course of the following detailed description.
In order that the invention may be more clearly understood, embodiments thereof will now be described in detail by way of example, with reference to the accompanying drawings, in which:
Other advantages that are inherent to the structure are obvious to one skilled in the art. The embodiments are described herein illustratively and are not meant to limit the scope of the invention as claimed. Variations of the foregoing embodiments will be evident to a person of ordinary skill and are intended by the inventor to be encompassed by the following claims.
Preparation of Substrate:
A 10 mm�10 mm�1.7 mm plate of Ti6Al4V-ELI (extra-low interstitial) alloy formed in accordance with ASTM standard F136-98 having a chemical composition (wt %) of C 0.02, N 0.008, Fe 0.213, Al 6.16, V 3.92, O 0.12 and Ti balance (available from RMI Titanium Company, Mississauga, Canada), was mechanically polished using SiC paper #400 and #600, and 9 μm Al2O3 paper. A titanium wire was spot-welded to the plate for handling. The plate was ultrasonically cleaned for 10 minutes in acetone, then 10 minutes in ethanol and then 10 minutes in deionized water. The cleaned plate was then etched for 10 minutes in a dilute HF acid solution, rinsed in deionized water, ultrasonically cleaned in deionized water for 10 minutes and then dried with cold air.
One Ti6Al4V alloy plate prepared as described above was used as the working electrode in an electrochemical cell in the activation of the plate surfaces. Two other Ti6Al4V plates cleaned in ethanol were used as counter electrodes, but the plates of the counter electrode had surface areas that were at least twice as large as the surface areas of the plates of the working electrode. Activation of plate surfaces of the working electrode for each example was accomplished electrochemically by application of a DC voltage to the plates immersed in an aqueous solution of NaOH according to parameters listed in Table 1. In experiments where the effect of ultrasound was investigated, ultrasound at a frequency of 40�2 KHz was applied during activation. In experiments where the effect of ultrasound was not under investigation, ultrasound was not used.
Procedure for Coating:
Deposition solutions saturated with hydroxyapatite (HA) precursors were prepared by dissolving sodium chloride (Fluka, ≧99.5%), sodium bicarbonate (Sigma-Aldrich, ≧99.7%), potassium chloride (Fisher, ≧99.6%), sodium orthophosphate (Sigma-Aldrich, >99.0%) and magnesium chloride hexahydrate (Sigma-Aldrich, >99.0%) in deionized water, followed by the addition of 1 M hydrochloric acid to reduce the pH to about 6, then the addition of calcium chloride hexahydrate (Fisher, ≧99.5%) and sodium sulfate (Anachemia, >99.0), and then the addition of 1 M TRIS (tris-hydroxymethyl aminomethan) to adjust the pH of the solution to 6.5. Calcium chloride was added after acidification with hydrochloric acid to reduce the possibility of precipitating hydroxyapatite (HA). Alternatively, the calcium chloride could be added before acidification and the sodium orthophosphate added after acidification.
The various reagents and deionized water were used in amounts to provide a deposition solution with the following concentrations of ions:
Concentrations of the ions in the deposition solution are generally similar to concentrations found in blood plasma and simulated body fluid (SBF), although the concentration of calcium ions (Ca2+) and orthophosphate ions (HPO4 2−) in the deposition solution are five times their concentration in blood plasma and SBF.
To coat a substrate, 175 ml of the deposition solution in a 250 ml beaker were placed in a water bath at 37� C. for 3 min to raise the temperature of the deposition solution to 37� C. Activated Ti6Al4V alloy plates were weighed to five decimal places and immersed in the deposition solution by hanging them in the solution for a desired length of time. After the desired length of time elapsed, coated Ti6Al4V alloy plates were air dried and weighed. The difference between the weight of the coated and uncoated plates gave the weight of the coating material.
Effect of NaOH Concentration in the Activating Solution:
Activated Ti6Al4V alloy plates prepared in accordance with Examples A1-A6 were coated with HA over 30 minutes in accordance with the procedure for coating described above. A graph of coating thickness (μm) as a function of NaOH concentration (M) is provided in
Effect of Magnitude of Applied Voltage During Activation:
Activated Ti6Al4V alloy plates prepared in accordance with Examples A7-A14 were coated with HA over 5 hours in accordance with the procedure for coating described above. A graph of coating thickness (μm) as a function of applied voltage (volts) is provided in
Effect of Duration of Applied Voltage During Activation:
Activated Ti6Al4V alloy plates prepared in accordance with Examples A15-A24 were coated with HA over 5 hours in accordance with the procedure for coating described above. A graph of coating thickness (μm) as a function of activation time (minutes) is provided in
Effect of Current Density During Activation:
Activated Ti6Al4V alloy plates prepared in accordance with Examples A25-A33 were coated with HA over 5 hours in accordance with the procedure for coating described above. A graph of coating thickness (μm) as a function of DC current density (A/cm2) is provided in
Effect of Temperature During Activation:
Activated Ti6Al4V alloy plates prepared in accordance with Examples A34-A38 were coated with HA over 5 hours in accordance with the procedure for coating described above. A graph of coating thickness (μm) as a function of activation temperature (� C.) is provided in
Effect of Replenishing HA Solutions During Coating:
The procedure for coating described above was carried out with replenishment of the deposition solution every half hour with freshly made solution. The coated substrates were taken out of solution at time periods of 0.5, 1, 2, 3, 4 and 5 hours. A graph of coating thickness (μm) as a function of time (hours) illustrating effect of replenishing the deposition solution at half hour intervals on the growth rate of the HA coating is provided in
Two similar experiments, one in which replenishment was not done and one in which replenishment was done at 1 hour intervals confirmed that more frequent replenishing leads to a greater amount of coating on the substrate surface.
In the experiment where replenishment was done at half hour intervals, SEM indicated that morphologies of coated Ti6Al4V substrates at different time periods have a bone-like structure, and to some extent a crystal-like structure, covering the whole surface of the substrate. After 3 hours, the coating grows to such a thickness that the coating starts to crack, likely due to either internal stress or drying. The morphology of the coating at a half hour indicates that HA coating initiates from some active areas and grows in a spherical shape extruding on the surface. Gradually valleys around the spherical extrusions start to be covered by HA coating leading to a more uniform coating surface with time.
HA coating after 5 hours of coating with replenishing solution every one hour leads to more crystal-like coating morphologies, compared to the bone-like or less crystal-like morphologies indicated above. There are more cracks in the coating with less frequent replenishing.
Growth of HA Coatings:
A longer term coating process was performed in which HA was coated on a Ti6Al4V substrate for 15 hours with replenishment of the deposition solution every half hour. A linear relationship between coating duration and coating thickness was observed. Within 15 hours the coating thickness reached about 50 μm, which is an acceptable thickness for hydroxyapatite coating in medical applications. Observed coating thickness was measured from an SEM of a cross-section of the coated substrate. Coating thickness was not a calculated value in this case. The coating looks dense and tightly attached to the substrate, and only a small amount of coating close to the substrate was broken off during grinding and polishing processes. Coating thickness at 10 hours of coating was determined to be about 33 μm as indicated by energy dispersive X-ray spectroscopy (EDX) based on analysis of Ca content.
Relationship Between Calculated and Observed Coating Thickness:
A comparison between calculated and observed coating thicknesses was undertaken. Coating experiments were conducted in which activation was done at room temperature in a 10 M NaOH solution at a constant DC voltage of 10 V for 30 minutes. Coating was performed at pH 6.50 at a temperature of 37� C. in a deposition solution as described in the procedure for coating above. The deposition solution was replenished every half hour. Results are provided in
Characterization of HA Coatings:
HA coatings on Ti6Al4V substrates produced in accordance with the present invention are of very high purity and are strongly bonded to the substrate.
Strong bonding between the coating and the substrate results from formation of a strong initial layer with inter-diffusion of elements from both the substrate and the coating. EDX line analysis conducted as a line scan perpendicular to the boundary line from the coating to the substrate confirms the existence of a 2-3 μm thick initial diffusion layer close to the substrate. EDX analysis conducted as a line scan parallel to the boundary line between the coating and the substrate further confirms that the initial diffusion layer is an inter-diffusion layer of Ti, Ca and P.
EDX point analysis also confirms that the inter-diffusion layer exists. Referring to
Measurement 4 shows that Ca, Ti and V co-exist at the initial coating layer. Since Measurements 1, 2 and 5 are away from the inter-diffusion layer, EDX analysis of these points is not influenced by the substrate and the ratio of Ca/P should be the actual ratio of Ca and P existing in the coating. The average of Measurements 1, 2 and 5 is 1.67, which is exactly the atomic ratio of Ca/P in stoichometric hydroxyapatite (Ca10(PO4)6(OH)2). This confirms that the formed coating is pure HA.
Measurements 3 and 4 are influenced by the inter-diffusion layer and the Ca/P ratio is far away from hydroxyapatite. There is no P detected at Measurement 3 and much more Ca than P is detected at Measurement 4, possibly indicating that Ca first reacts with titanium oxide and favorably deposits on the substrate at the activated substrate surface as amorphous CaTiO3, while the P participates at a later stage as the CaTiO3 incorporates phosphate ion to form hydroxyapatite on the surface. Measurement 3 is closer than Measurement 4 to the substrate, thus there is no P detected at Measurement 3. P gradually deposits and is detected at Measurement 4.
X-ray diffraction (XRD) analyses of commercial crystallized hydroxyapatite powder (PENTAX Corporation, Tokyo, Japan) and of powders obtained from coatings of the present invention confirm that the coatings of the present invention are substantially pure hydroxyapatite (HA). The commercial HA XRD pattern matches very well with the standard XRD pattern of HA in the JCPDF card (Joint Committee on Powder Diffraction Standards�Powder Diffraction Files). Major patterns of the powders from coatings of the present invention match very well with the commercial HA powders.
Coatings formed on substrate surfaces were analyzed with a Perkin Elmer FTIR (Fourier Transform Infrared Spectroscopy) Instrument (Spectrum BX), in a scanning range between 4000 cm−1 and 400 cm−1 with 216 scans per sample. Spectra obtained show characteristic bands of HA along with additional bands ascribed to associated H2O.
Characteristic FTIR bands of hydroxyapatite corresponding to the stretching vibration of PO4 3− can be observed in the range of 1200-900 cm−1, which in this investigation are at 1119 cm−1, 1048 cm−1, 1036 cm−1 and 979 cm−1. Deformation vibrations of PO4 3− are at 603 cm−1, 572 cm−1, 471 cm−1 and 422 cm−1. Hydroxyl (OH−) bands are at 3458 cm−1 and 617 cm−1. Bands located in the range of 3900 cm−1 to 3500 cm−1 and 1900 cm−1 to 1400 cm−1 can be assigned to associated H2O in the coating, the result of a long period of exposure in the atmosphere.
With increasing duration of coating, intensities of the hydroxyapatite FTIR bands significantly increase, indicating a significant increase in coating thickness starting from a time of about 180 minutes. The characteristic bands of HA split after about 180 minutes, indicating that the formed HA may be starting to crystallize. Broad and not-split bands of HA at 120 minutes illustrate that the initially deposited HA is in an amorphous or poorly crystallized phase. The characteristic FTIR band of CO3 2− is not very intense up to about 120 minutes of coating, and is significantly more intense after 180 minutes of coating, indicating an increase in carbonate content as coating proceeds.
Scanning electron microscopy (SEM) of the formed HA coating (
Diffraction pattern from transmission electron microscopy (TEM) analysis (
Heat Treatment:
HA-coated Ti6Al4V substrates were prepared by coating an activated substrate of Example A31 using the Procedure for Coating described above. Coated substrates were heat treated in a furnace (Pyradia, Quebec, Canada) in air for 1 hour. Heat treatment experiments were performed at temperatures of 350� C., 450� C., 550� C., 650� C., 750� C. and 850� C.
Scanning electron microscopy (SEM) analysis before and after heat-treatment indicate that surface morphologies are similar before and after heat-treatment at temperatures in a range of from about 350� C. to 550� C. After a temperature of 650� C., heat-treatment widens cracks on the surface of the coating and the coating becomes porous. Widening of cracks may be a result of a mismatch between the coefficients of thermal expansion (CTE) of the Ti6Al4V substrate, TiO2 and HA layers. Heat-treatment may cause a small amount of contraction between the substrate and the TiO2 layer, while large expansion between the TiO2 layer and the HA layer may result in severe stresses, which may be released by cracking.
X-ray diffraction (XRD) patterns of heat-treated and untreated samples indicate that crystallinity of the HA coating increases at temperatures of 450� C. and 550� C. with the appearance of new peaks. At 650� C. one new phase appears, which was found to be tricalcium phosphate (TCP), and the coating is mixture of HA and TCP. With increasing temperature beyond 650� C., the concentration of TCP increases. TCP is more readily dissolvable than HA in human body fluids, thus the formation of the TCP is not favorable for medical applications. SEM observations also show that heat treatment at and above 650� C. can cause some morphology changes.
Fracture surface analysis of hydroxyapatite (HA) coatings with and without heat-treatment after adhesion testing indicates that some of the coating still adheres to the substrate, i.e. fractures happen inside the coating instead of between the coating and the substrate, indicating that bonding is strong between the coating and the substrate. More of the coating adheres to the substrate with an increase in heat-treatment temperature, indicating that bonding becomes stronger with an increase on heat-treatment temperature, i.e. heat-treatment strengthens the bonding between the coating and the substrate.
Incorporation of Protein Into HA Coatings:
Attempts were made to incorporate Bone Morphogenic Protein (BMP2) into HA coatings on Ti6Al4V substrates at concentrations of BMP2 of 1 μg/L, 10 μg/L and 50 μg/L by the following general procedure. Step 1: Coating of activated Ti6Al4V substrates was performed in 175 ml beakers for 2 hours with a regular deposition solution without addition of protein. The deposition solution was replenished at half hour intervals. Step 2: Further coating of coated substrates from Step 1 was performed in 50 ml beakers for 3 hours with addition of protein at different concentration. The deposition solution was replenished at one hour intervals. For comparison, other coated substrates from Step 1 were further coated with HA under various conditions without addition of protein. Coating conditions are listed in Table 4 and the coating weight gain is listed in Table 5.
SEM indicates that all coatings from Step 1 have a bone-like morphology. For Step 2, SEM indicates that the morphology of HA coatings after coating with solutions having protein at concentrations of 1 μg/L and 10 μg/L is fine and hairy, but the protein is not present in the coating. SEM indicated that the addition of 50 μg/L of protein significantly changed the morphology to a very fine bone-like structure with a large presence of protein. It appears that incorporation of protein into the HA coating may be initiated at a certain minimum concentration of protein. High SEM magnification indicates that protein and HA mingle together in the coating, which is good to sustain protein in the coating. Heat treatment of coatings containing protein may result in protein denaturation or pyrolysis.
Coating of Ti-HDPE Composite:
A Ti-composite was fabricated by infiltrating high density polyethylene (HDPE) at elevated temperature into a porous Ti disk, which was sintered from micro-scale Ti powders. The disks were polished using #400 SiC paper to form a flat surface, and then the disks were subjected to sand-blasting on all the surfaces using #10 alumina powders. To make a through activation on the disks due to the porosities, the activation process was performed for 45 minutes. A regular Ti6Al4V alloy was subjected to the same treatments and coating procedures.
Table 6 shows the weight gain of hydroxyapatite after coating process. More HA coating formed on porous Ti and Ti-HDPE composite disks than on the regular Ti6Al4V alloy. More HA coating formed on the porous Ti than on the Ti-HDPE composite, possibly due to its greater porosity in which some NaOH was trapped, resulting in a more alkaline surface, which is favorable for the formation of HA coating on the surface. Even though more HA coating formed on porous Ti, the surface is not fully covered and the coating is not even. HA coatings on porous Ti have some uncovered areas on the bottoms, and it is difficult to form coatings on the edges and surrounding surfaces. In contrast, HA coating is evenly distributed on the surface of Ti-HDPE composite disks, with the bottoms, edges and surrounding surfaces all fully covered.
Other advantages that are inherent to the structure are obvious to one skilled in the art. The embodiments are described herein illustratively and are not meant to limit the scope of the invention as claimed. Variations of the foregoing embodiments will be evident to a person of ordinary skill and are intended by the inventor to be encompassed by the following claims.
Patent Citations
Non-Patent Citations
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Craig A. Pieratt, 49, LaGrange, died Monday, April 9, 2012 in the Orlando, Fla., area.
Israel Eugene "Izzy" Yoder, 21, Ligonier, died April 5, 2012 as the result of a swimming accident in Haiti while serving on a mission trip.
Rodney L. Sawyer,50, rural LaGrange County, died on Thursday, April 12, 2012 at his residence.
A group of 20 eighth grade students and seven parent and teacher chaperones from Lakeland Middle School traveled to Washington, D.C. during spring break.
Twenty-four Lakeland High School students participated in Hispanic Day on Campus March 23 at Ancilla College.
The Lakeland and Prairie Heights softball squads braved the cold and wind Tuesday afternoon in a hotly contested battle for their NECC opener.
The Prairie Heights girls track squad nipped visiting Lakeland, 63-61, and lost to the Angola squad, 95-32. Angola's girls also topped Lakeland, 99-33.
The Lakeland boys track squad defeated both the host Prairie Heights squad and Angola teams in a three-way track meet Tuesday afternoon.
A caucus to appoint the replacement for the position of LaGrange County Clerk is scheduled for 6 p.m. on Monday, April 23, at the LaGrange County Library.
Debbie Bontrager
President, Animal Welfare Association, Inc.
As Indiana's spring turkey season approaches, DNR Wildlife Research Biologist Steve Backs said hunters should plan to work a little harder this year.
Cassidy Sabelhouse
Women of the Moose
Library Closings…
All branches of the library will be closed on May 28 due to Memorial Day.
Troy Sutton
To the Editor:
Melvin Lee Mullett, 75, Topeka, died Monday, April 9, 2012 at his residence.
Max Sherck, 82, Middlebury, died Monday, April 9, 2012 at Courtyard Healthcare of Goshen.
Patricia C. Stiles, 82, LaGrange, died Sunday, April 8, 2012 at Parkview LaGrange Hospital.
Mary Louise Miller, 77, Wakarusa, died Sunday, April 8, 2012 at Greencroft Healthcare.


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The start of High School football means Lobo Recruiting kicks into high gear. Today's focus is Brad Sorenson from Colton CA. I had a chance to speak to Coach Harold Strauss of Colton High, concerning his star in the making. Brad Sorenson
TRM: Coach, what is an accurate height and weight for Brad?
Coach Strauss: Funny you should ask, Brad grew 4 1/2 and gained 35 lbs since the end of last football season. He's now 6' 4" 1/2 and 205 lbs. He has grown into the prototypical Pro Style QB.
TRM: That's pretty incredible.
Coach Strauss: Because of his growth spurt, I think a lot of teams were waiting until after his first game to see how he would do.
TRM: So how did he do?
Coach Strauss: He had an outstanding game. He was 7-10 for 270 yards and 3 Touchdowns.
TRM: Coach, I have to ask why only 10 pass attempts?
Coach Strauss: Well we only ran 32 offensive plays and we have great running back, Charisse Wright (consensus top 10 national RB), who ran for 200+ yards
TRM: So what schools are currently recruiting Brad?
Coach Strauss: BYU, Utah, Utah St, UNM, and all the Ivy League. He is a very good student, on and off the football field. BYU and Utah are recruiting him the heaviest, but I received lots of requests for game tape since our first game. Even Pete Carroll, USC head coach, was at the first game and really liked what he saw from Brad.
Brad sounds like the new type of UNM QB, see Steve Harris and Donovan Porterie. Brad is able to run an offense effectively with a stud RB in the backfield. Stay tuned as the TheRedMenace.com brings you more recruiting news!!!!!


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Experience the magic of old time radio as Charles Dickens' "A Christmas Carol" is staged one night only, Wednesday, December 17 at 7:30pm at the Millspace in the Newmarket Mills. General admission is $12 or $10 for students and seniors with all proceeds going to the arts and culture civic center. The feel of a 1940's radio broadcast will be created with the help of sound effects performed live in front of the audience. As in the era of old time radio, a table of bells, shoes, and other objects will be orchestrated to bring the Victorian era tale to life. John Herman directs. SECURE YOUR TICKETS NOW:
Wrong Brain Holidaze Bizaare
Call to Vendors!
WHAT'S HAPPENING: 3rd Annual Wrong Brain Holidaze Bizaare
WHO THEY NEED: Call to Vendors, Artists and Performers
WHEN IS IT: Saturday, December 13, 11am-5pm
WHERE IS IT: Millspace, bottom level of the Newmarket Mills, Newmarket, NH
The Wrong Brain Bizaare is a semiannual multimedia arts open market, pop up gallery, music exhibition and creative celebration! They aim to bring you the strange, unconventional, underground, alternative and emerging of the Seacoast.
They are seeking vendors who offer – original art, prints, zines, RECYCLED/HANDMADE: pins, patches, clothing, accessories, toys, VINTAGE/LOCAL: clothing, records and cassettes, comics, books, skincare, food, etc. Other items are absolutely acceptable as long as they fit the theme.
They are seeking pop-up gallery exhibitors with original art in frames or hanging fixtures.
They are seeking musicians and readers for live entertainment.
Vendor Space Information:
10×10 – $60
6×4 – $30
Bring your own tables and chairs.
Some electricity is available upon request only.
Most spaces have access to wooden beams for hanging.
To apply to be a vendor, please submit the following:
Business/artist name & location
What do you do?
What products will you sell?
Why do you fit the theme?
10×10 or 6×4?
Please attach 3-5 high quality, clear images.
Link to your website/blog/portfolio.
If you plan on sharing a space, please submit ONE application with BOTH of your info.
To apply to the pop-up gallery, please submit the following:
Artist name & location
Up to 4 original works with title, size, medium, dimensions, price, and attached image for each piece.
To apply to perform music or readings, please submit the following:
Artist/band name & location
Short bio. Why do you fit the theme?
Link to hear your music/read your writing.
For other installation or performance ideas, please submit a proposal and we will talk!
EMAIL SAM: email@example.com
WEBSITE: wrongbrain.net
Not all who apply will be accepted. Space and time are limited and they are seeking only those who are Wrong Brained.
Notifications of acceptance will be emailed by Wednesday, October 29.
Harvest! A deliciously fun-filled evening
Harvest! was a great success and we want to thank everyone who came out to celebrate all things fresh and local with us on Saturday, September 27. We had an incredible array of dishes made with ingredients from dozens of area farms and gardens. One guest shared "It made me conscientious about how I prepared my dish. I knew I had to get to a farm stand to shop." Local restaurants The Joinery and Basil Leaf Thai Cuisine graciously donated amazing dishes to our table and our dinner guests sipped on iced tea blends from White Heron.
Our guest speakers also gave us much to think about. Local nutritionist Ranan Cohen encouraged us to think globally while eating locally. Some of our most nutrient dense foods come from miles away, but we can combine them with extraordinary local foods. Sara-Zoe Patterson of Seacoast Eat Local challenged us to introduce someone new to a farm stand. She shared the impact of our choices is to local farmers and growers. SNAP/EBT cards are also now accepted at several area farmers markets so that everyone has access to locally sourced foods. Jeff Cantara of New Roots Farm shared his perspective on the unexpected nature of farming and the continuous lesson of perseverance. We cleared the tables from the center of the hall to make room for dancing as our evening was wrapped up by the fantastic sounds of Computer Beach Party.
We appreciate the tremendous support of our amazing Executive Chef sponsor Appledore Real Estate as well as Rebecca Proctor of RSP Studio Custom Framing who organized the incredible Harvest! gallery inside Millspace. She has graciously donated her time and talents in framing several of the pieces from local artist. We also loved teaming with Mr. Fox Composting to assist in our efforts to make this a zero waste event. We hope you will consider them at your next gathering.
This delicious event had something for every pallet and we cannot wait to do it again during the next Harvest! season. In the meantime, we hope you will take the time to make the healthy choice for you, your family, and the local economy and visit one of several area Winter Farmers' Markets to support local growers and farmers.
We thank you for your continued support of Newmarket Millspace as we embark on our first year. We can't wait to see you again!
Join us at Harvest!
We are less than a week away from our evening of all things fresh in the community. Doors will open at 5pm and dinner will begin at 6. There is still time to get your tickets! We have a few important things we need you to remember for this exciting event.
"Pack Your Picnic Basket"
Harvest! is teaming up with Mr. Fox Composting to make this a zero wast event. Pleas bring your own plates, bowls, silverware, napkins and glasses. Consider a tablecloth, vase of flowers, or gourds to decorate your table. Opt for more sustainable choices for your dish like decomposable was paper muffin cups instead of aluminum, or us a dish towel to cover your salad instead of plastic wrap.
Bring Your Own Beverage
We will have pitchers of water available but you are welcom to bring your own beverage of choice. Beer and wine are acceptable. Cheers!
Label Your Dish
We want to make sure everyone can enjoy all of the amazing food being prepared, so please bring your recipe or list of ingredients on a card or you can fill one out when you come. This way people with allergies can be informed.
Where's Your Favorite Local Farm?
We will be keeping a list of where your ingredients came from, so we can recognize and support local growers…even if it's your own backyard garden!
We are accepting donations of flowers for our tables as well as items for our raffle such as a jar of your famous canned pickles or jam, a basket of goodies from your garden, or baked items. You have creative license here!
We sincerely thank you for your support of Newmarket Millspace and look forward to fun-filled evening of community, guest speakers, art and live music!
Harvest! Millspace
Newmarket Millspace will be hosting Harvest! a celebration of community and the local food movement on September 27th from 5-10pm. Come fill up on an evening of food and fun at this unique event. We are asking you to create a dish to share using ingredients that are locally sourced and/or harvested. In return we will provide you with dynamic speakers involved in this movement: nutritionist Ranan Cohen, author Sara-Zoe Patterson of Seacoast Eat Local, and farmer Jeff Cantara of New Roots Farm in Newmarket. Live and local music will wrap up the evening for your enjoyment and dancing.
In an effort to make this a zero waste evening we are partnering with Mr. Fox Composting. This is also a BYOB and BYOPS event– Bring Your Own Beverage of choice; beer and wine are acceptable and Bring Your Own Place Settings as well as containers for leftovers. You will be able to come to Millspace early to set your place at the table. Doors officially open at 5pm and dinner begins at 6pm.
Tickets are available here through our Go Fund Me site. We chose this format to offer different levels of participation and to ensure that we have a variety of dishes for everyone to enjoy. Please be prepared to provide a list of ingredients so that we may alert those guests who may have food allergies or preferences. Follow us on Facebook and Twitter for updates on Harvest at Newmarket Millspace. Set a space for you and your family at our table for this unique event today!
Join us at the Heritage Festival!
May 31, 2014: The Newmarket Heritage Festival is back!
The award-winning Newmarket Heritage Festival, New Hampshire's favorite international block party, returns on May 31—and you're invited! Celebrate the arts, culture, history and community spirit in a new location this year—inside the historic Newmarket Mills at 55 Main St. in downtown Newmarket.
Great Performance Line-Up: The 2014 Heritage Festival features a great line-up of multicultural performers: music of the old country with legendary accordion master Gary Sredzienski, the dazzling Chinese Folk Art Workshop, and the high-energy rhythms of the Akwaaba African drummers; Irish music and dancing with the New England Irish Harp Orchestra and the McDonough-Grimes Dancers; flamenco dancing, Indian and Laotian dancing, a hip hop dance demo and more!
Artisans at Work: Watch (and try!) blacksmithing, barrel making, letterpress printing, pottery, Chinese calligraphy, woodcarving, wool felting, and more. Meet these talented artisans and learn about the tools and traditions of their work.
Vendors: The festival also features dozens of vendors, including Main Street merchants and Newmarket Mills merchants, who will be open for business and offering festival specials! Don't miss this chance to stock up on handcrafted gifts, specialty items—and good eats!
Activities: The Bristol S-Gauge model trains will be running in the American Legion building, strolling musicians will play on the sidewalks, and a band of medieval knights will be roaming the streets. Also around town, the Newmarket Gardeners will hold their annual plant sale and the Community Church will host a Soup and Chowder Supper.
Location: Inside the Newmarket Mills, 55 Main St., Newmarket, NH
Hours: 10 am – 8 pm
Admission: Adults $5, adults; children $2 (ages 6-12); under 6 free.
Parking: Free parking and free trolley at the Newmarket High School (213 S. Main St.)
Handicap accessible? Yes
More info: http://www.heritage-festival.org
Contact: 603-659-5588, email@example.com
The festival is produced by the Newmarket Main Street Corporation (NMSC), a nonprofit group dedicated to strengthening and revitalizing the historic and cultural characteristics of the community and to preserving the legacy of Newmarket for future generations. The NMSC is a 501 (c) (3) organization and all contributions are tax deductible.
Explore the gundalow at our Family Day!
Join us at the Newmarket Millspace on Saturday May 17 from 10-1 for a Family Day in celebration of the newly built gundalow Piscataqua during its stay in Newmarket! You can board the Piscataqua and take a guided tour by the crew. The sea faring sounds of the Great Bay Sailors will be performing on the Rivermoor Docks. Head inside the Millspace and learn more about the gundalow, mill history, ecology, and more, through a variety of workshops and hands on activities. Artist Adam Kelley will be offering workshops to our visitors who want to learn how to capture the gundalows images through drawing. Find local artist Susan Adams at her easel as she creates a painting of the gundalow. Join in the artistic celebration by participating in our coloring event. Bring your colored page into the Bloom'n Cow (between now and Sunday, May 18th) located on the first level of the Newmarket Mills where your own work of art will be displayed. Tour a mini gallery provided by the New Market Historical Society to learn first hand about Newmarket's history.
This free event is sponsored by the Newmarket Millspace and the Newmarket Historical Society for all to enjoy. We can't wait to see you there!!
Come Celebrate and Welcome the gundalow, Piscataqua to Newmarket!
Photograph courtesy of The Gundalow Company
The Newmarket Millspace and The New Market Historical Society are delighted to welcome the newly built gundalow, Piscataqua to Newmarket as it makes its way up the Lamprey River the weekend of May 16-18 and docks just behind the mills downtown. The weekend will be full of events to celebrate the gundalow's visit.
Enjoy a sail on the Piscataqua from the mills or Adams point. There are various sailing opportunities throughout the weekend for you to choose from. Tickets are $40 per person and proceeds will benefit two nonprofit organizations, the Gundalow Company and the New Market Historical Society. Tickets to sail can be purchased at: www.gundalow.org.
Saturday, May 17 from 10:00 – 1:00 p.m. is Family Day and there will be a FREE open house and hand on activities within the Millspace and onboard the Piscataqua for families to celebrate and learn more about the gundalows and the history of the Mills.
Come help us welcome and celebrate this historic vessel to Newmarket's shore!
Millspace opening night attracts hundreds
Thank you. We did it.
We have started a new chapter in a story that is well over a hundred years old. We hope for the Millspace to be a testament to the rich, cultural heritage of the community and its centuries-old tradition of melding history, art, industry, and technology.
Thank you again to the incredible individuals, organizations, and businesses that have been a part of the planning of this space. It is important to note that just the planning for this space has been ongoing for over ten years and the sheer number of people involved that deserve recognition is immense.
Thank you to Access Sports Medicine and Orthopedic Medicine. This project began with a dedicated group of local leaders, entrepreneurs, artists, and neighbors developing a vision. And the dream is ever closer because of your generous contribution, as well as the contributions of Chinburg Properties, The Newmarket Community Development Corporation, Proulx Oil and Propane, Boston Education Network, Caprioli Painting, and The Pao Café.
Thank you to the past and present members of the Lamprey Arts & Culture Alliance, the Newmarket Main Street Corporation, the Newmarket Heritage & Cultural Center Committee, and the New Market Historical Society.
Thank you to all the volunteers who have contributed ideas and worked over the many years simply because of a desire to give back to the community.
We have only just completed Phase 1 of construction. What does that mean? It means that you can legally be in the Millspace… but we still need bathrooms. We still need a dedicated heating system. Our ultimate plans include a theater, exhibition space, classrooms, and more. If you can help out, then let us know. We'd love to keep you informed of our progress. Help us spread the word by directing people right here to Millspace.org. Follow us on Twitter and Facebook.
Thank you to Eric Wentworth, illustrator and designer at Winter Crow Studio, for creating the Millspace logo.
Thank you to everyone who made the opening night special, including our jazz duo (Greg Rothwell and Mack Walters), our host for the evening (and event organizer!) John Herman, and finally our dynamic roster of local notables who came to speak on their passions: W. Jeffrey Bolster, Kath Gallant, Brady Carlson, Sam Paolini, Michael Provost, John Pittman, Greg Kretchmar, Matthew Carano, and Jen Chinberg.
And thank YOU.
NEWS: Newmarket Millspace "Ignites" the Community with Dynamic Speakers, Jazz, and Art
Newmarket Millspace "Ignites" the Community with Dynamic Speakers, Jazz, and Art
An evening of art, jazz, and speakers including NHPR All Things Considered host Brady Carlson officially kicks open the doors to the Millspace, a new civic center for arts, culture, and history in the Newmarket Mills. The inaugural event, "Ignite: Millspace," is Saturday, January 25th at 7:30pm, presented through the generous support of Access Sports Medicine & Orthopaedic Medicine. Tickets are $10. Purchase them at http://buytickets.at/millspace
"This is not just a cultural event, but it is a historic one for the community," says event host John Herman. "This once derelict building is alive again, and at its heart is the Millspace. We want this civic center to ignite passions. There will be speakers on a wide range of topics. Each talk will be brief and illuminating. Some are new ideas and visions. Others will look to the past."
Speakers include popular host of "Greg and the Morning Buzz" Greg Kretschmar, Music video director and comic book writer Alex De Campi, 2013 Bancroft Prize for History winner W. Jeffrey Bolster, visual artist Sam Paolini, and more. Each speaker will present personal passions in the form of an Ignite talk, a fast paced presentation style popular around the world.
The evening will also feature a display of the Bridge Board Project, a collection of art generated from weathered boards and beams recovered from an old covered bridge spanning the Lamprey River that washed out in the Mothers Day flood of 2006. Artists and craft persons brought boards home and got creative by painting, drawing, and carving the unique pieces.
"Ignite: Millspace" marks the successful completion of the center's first phase of construction. "We are grateful to Access Sports Medicine & Orthopaedics for their generous donation which made this important first phase of construction possible and allows us to host events in the space. Right now the center is a big empty room," says Herman. "Our goal with this huge kick off is to get the community inside the space and inspire them to dream about the possibilities."
ABOUT MILLSPACE –Plans for the civic center include a theater, lobby, gallery, information desk, meeting room, large function area, and concessions cafe. Learn more about the upcoming center and take a look at a virtual walk-through at Millspace.org.
ABOUT IGNITE – If you had five minutes on stage what would you say? What if you only had 20 slides and they transitioned automatically every 15 seconds? Around the world people have been putting together "Ignite" nights to share ideas and passions. More information about Ignite Events held around the world can be found at O'Reilly's Ignite website, Ignite.OReilly.com.


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|Durant has another poor shooting game
|Written by Admin
|Monday, 09 July 2007 18:28
LAS VEGAS (AP) -Kevin Durant showed again he isn't afraid to shoot as he starts his professional career with the Seattle Supersonics. The shots, however, continue to be off target.
The second pick in last month's draft was 4-for-19 from the field and scored 18 points Monday night in the Sonics' 87-74 loss to the New York Knicks in the NBA's Las Vegas summer league.
``I just wasn't in the game tonight,'' Durant said. ``As the game went on, we got a little better, and that is the important thing.''
On Friday night, the 6-foot-9 Durant was 5-for-17 from the field in a 77-66 loss to the Dallas Mavericks.
The 215-pound forward struggled with New York's physical play Monday, finishing with one rebound and no assists in 34 minutes.
``It is what it is,'' he said. ``I've made some good passes, but we've just missed shots. I can't do anything about that.''
Durant was 2-for-11 from the field in the first half and he missed his first four shots in the second half before hitting a short jumper with 9:25 to play. He finished with 11 points in the fourth quarter, including a 3-pointer in the final minute and six straight free throws.
``The game is quicker and everyone is good,'' said Durant, who swept the national player of the year awards in his one season at Texas. ``You have to play hard every night.
``I'm still getting the ball where I want it in the post. I just need to execute.''


text:
Porcine plasma protein as proteinase inhibitor in bigeye snapper (Priacanthus tayenus) muscle and surimi
Article first published online: 18 JUN 2001
DOI: 10.1002/jsfa.887
© 2001 Society of Chemical Industry
Journal of the Science of Food and Agriculture
Volume 81, Issue 10, pages 1039–1046, August 2001
Additional Information
How to Cite
Benjakul, S., Visessanguan, W. and Srivilai, C. (2001), Porcine plasma protein as proteinase inhibitor in bigeye snapper (Priacanthus tayenus) muscle and surimi. J. Sci. Food Agric., 81: 1039–1046. doi: 10.1002/jsfa.887
Publication History
- Issue published online: 18 JUN 2001
- Article first published online: 18 JUN 2001
- Manuscript Accepted: 13 MAR 2001
- Manuscript Revised: 23 OCT 2000
- Manuscript Received: 4 AUG 2000
Funded by
- International Foundation for Science, Sweden. Grant Number: E/2878-1
- Prince of Songkla University
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Football: World Cup lesson from 'worst team ever', American Samoa21 May 2014 | 03:06
Search results
Mexico to make debut at Sevens
Posted Jan 28th 2011, 12:00am by Alvin Sallay
... at the March 25-27 tournament. With the International Rugby Board keen to fast-track Mexico- the country will be hosting the Pan-American Games in October with rugby sevens being a medal sport ... includes the 12 core HSBC Sevens Series teams- Argentina, Australia, England, Fiji, France, Kenya, New Zealand, Samoa, Scotland, South Africa, the United States and Wales- plus seven teams from ...http://www.scmp.com/article/736963/mexico-make-debut-sevens
Sport - Hong Kong - HONG KONG SEVENS
Samoa grab silverware but hard work lies ahead
Posted Mar 25th 2013, 12:00am by Mathew Scott
... Mathew Scott Samoa grabs silverware but hard work lies ahead Samoa might have walked away with the Plate after winning a bruising final 12-7 over Canada but captain Afa Aiono said ... teams there's no margin for error and we just can't keep giving other teams easy opportunities." Samoa won the second leg of the world series in Dubai with a stunning 26-15 Cup ...http://www.scmp.com/sport/hong-kong/article/1198936/samoa-grab-silverware-hard-work-lies-ahead
A game for sheilas no longer
Posted Nov 20th 2005, 12:00am by Mathew Scott
... the Australian football scene was struggling for existence and teams were filled with part-time locals and semi-pros who had blown in from afar. And you were hard pressed to find coverage of the sport ... among sports fans was that this was more akin to putting lipstick on a pig. You only had to scratch the surface- or go to any game- to see that nothing had really changed. The feeling ...http://www.scmp.com/node/525700
Sport - Hong Kong - HONG KONG SEVENS
We're not done yet, insists England after loss to Samoa
Posted Mar 23rd 2013, 12:00am by Alvin Sallay
... Alvin Sallay firstname.lastname@example.com England suffer a big loss against Samoa but coach vows to return stronger, while South Africa also take a beating at the hands of Argentina We're ... will meet old enemy Scotland with the pressure on their shoulders after Samoa knocked the stuffing out of them in a powerful and consummate performance which stunned most of the packed stadium ...http://www.scmp.com/sport/hong-kong/article/1197504/were-not-done-yet-insists-ryan
Posted Mar 30th 2012, 12:00am
... this now prolonged match time in what is already a very physical sport played in humid conditions. Players' associations will be watching the introduction of this new Sevens format very ... and Samoa played each other six times on Sunday... or perhaps I just had one too many Pimm's? Ralph Barnes, Sai Kung Surprised by recycled video clips May I congratulate the organisers ...http://www.scmp.com/article/997031/letters
Sport - Other Sport - RUGBY UNION
Big guns clash in World Cup 'group of death'
Posted Dec 04th 2012, 12:00am by AFP
... of the sport's traditional powers will be knocked out before the quarter-finals, with only the top two teams from each of the four pools going through to the knockout stages. Wales were beaten 14-12 ... Tonga and two as yet unqualified teams in Europe 1 and Africa 1. Asia's representative will join South Africa, Samoa, Scotland and Americas 2 in Pool B. France, beaten finalists in New ...http://www.scmp.com/sport/other-sport/article/1096896/big-guns-clash-world-cup-group-death
Sport - Rugby
Flash cuts no dash for England's Lancaster
Posted Oct 23rd 2014, 10:14pm by AFP
... Africa and Samoa visit next month. That means there is no place in the 33-man squad announced by Lancaster for either Freddie Burns or Danny Cipriani. If we take Jonny Wilkinson as the benchmark, ...http://www.scmp.com/sport/rugby/article/1623141/flash-cuts-no-dash-englands-lancaster
Sport - Rugby
England wings must take off, says David Strettle
Posted Oct 20th 2014, 10:08pm by AFP
... announcement of his squad for the November internationals. England welcome New Zealand, South Africa, Samoa and Australia to Twickenham on successive weekends next month, starting with the November ...http://www.scmp.com/sport/rugby/article/1620792/england-wings-must-take-says-david-strettle
Sport - Rugby
Winning 2015 Asian series best route to Olympics, says Dai Rees
Posted Feb 07th 2014, 11:30pm by Alvin Sallay
... Victory in the Asian Sevens Series next year will be vital as Hong Kong try to guarantee a place in the 2016 Olympics when the sport makes its Games debut, says performance chief Dai Rees. Only 12 ... competition, which would make more sense," Rees said. "But whatever the format, this competition will be tough, with every chance that we could see teams like Australia, Samoa, France, even ...http://www.scmp.com/sport/rugby/sevens/article/1423351/winning-2015-asian-series-best-route-olympics-says-dai-rees
Sport - RUGBY UNION
New Zealand up next for Wales after Samoa loss
Posted Nov 18th 2012, 12:00am by AFP
... the gloom hanging over his team after their 26-19 loss to Samoa. Wales may have won the Six Nations and the grand slam this year but are veering towards crisis point after Samoa subjected them ... Beck gave Wales a 13-6 lead with an interception try on his home debut only for Fa'atoina Autagavaia, George Pisi and Johnny Leota to cross as Samoa evoked memories of their famous World ...http://www.scmp.com/sport/article/1084855/new-zealand-next-wales-after-samoa-loss
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Vienna, Austria
Landstraßer Hauptstraße 120, 03. Landstraße, 1030 Vienna, Austria – Show map
|Room Type
|Double Room (1 Adult)
|Double Room (1 Adult)
|Double Room
|Special Offer - Double Room with Parking
|Luxury Double Room
|Triple Room
|Junior Suite (2 Adults)
|Junior Suite (3 Adults)
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915 properties in Vienna
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499 verified reviews
We verify all reviews from guests who have stayed at Hotel Eurostars Embassy. Find out more.
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Hotel Eurostars Embassy's staff speaks: Spanish, English, German
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When you book with us your details are protected by a secure connection.
Food & Drink
Bar, Breakfast in the Room
WiFi is available in public areas and is free of charge.
Public parking is available on site (reservation is not needed) and costs EUR 18 per day.
Room Service, Car Rental, Airport Shuttle (surcharge), 24-Hour Front Desk, Express Check-in/Check-out, Tour Desk, Ticket Service, Baggage Storage, Laundry, Dry Cleaning, Ironing Service, Business Center, Fax/Photocopying
Newspapers, Safe, Non-smoking Rooms, Elevator, Soundproof Rooms, Heating, Hypoallergenic room available, Air Conditioning
Spanish, English, German
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Until 12:00 PM
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Children and Extra Beds
All children are welcome.
All children under 5 years stay free of charge when using existing beds.
All children under 2 years stay free of charge in a crib.
All older children or adults are charged EUR 30 per person per night for extra beds.
The maximum number of extra beds/cribs in a room is 1.
Any type of extra bed or crib is upon request and needs to be confirmed by management.
Additional fees are not calculated automatically in the total cost and will have to be paid for separately during your stay.
Pets are not allowed.
When booking more than 5 rooms, different policies and additional supplements may apply.
When booking for more than 10 people, different policies and additional supplements may apply.
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In Vienna's center, this contemporary 5-star hotel is next to City Park and across from Landstrasse Metro Station and the City Airport Train (CAT), which takes guests to Vienna Airport in 16 minutes.
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The non-smoking 4-star Leonardo Hotel Vienna is just 325 ft from the Mariahilfer Straße shopping street and a quarter mile from the Westbahnhof transportation hub.
Score from 3235 reviews Very good
Amazing bath! Amazing price/quality ratio!! Very clean and very helpful and friendly staff!!
Friendly, attentive without being intrusive, good warm rooms, fantastic showers, plenty of space. Big city guide book was nice touch.
The stay was good, nothing to dislike.
The breakfast was good.
The receptionist didn't give me a 15 minutes free "Wien Parkschein" on the arrivel. There was a stoppage in the washstand of the bathroom. There are no power point at the bed in the room.
The location, the bed, the breakfast
During 5 days of our stay we could hardly take a shower - there was no HOT WATER in the whole hotel! Actually, once there was SOME tepid water at 4:00 a.m. And we really appreciate the creativity with which the reception each time gave us thousands of explanations and incredible excuses. Finally, we got some monetary compensation for cold shivers, oh,sorry, showers...
- Perfect breakfast - Very clean rooms - Reception is very nice - Staff are very helpful - The heater in the room is great
- There was no warm water, but problem was solved the 2nd day - There was a problem with the WIFI server and even when they fixed it the signal was very bad - The heater in the bathroom wasnt working
There was no hot water for the first night and day I was there. On the last day of my stay there was no internet despite being told on a number of occasions it was fixed. I wont be staying again.
Location, room, safety.
Unprofessional staff, no hot water at all for two days, no internet connection 5 days out of 8.
This is the worst hotel I have ever live in, i have booked for 4 days but I left the hotel from the second day. Dis liked it, and the staff were not helpful at all. Very bad
Very clean and friendly. Big room a lot of space . Good position from center . In week-end easy to park
Not so far from centar - about 20-25 min walking, and clean rooms
Small tables and plates for breakfast
A classic hotel at street corner, very clean and quiet, located half an hour walk from Stephansplatz. We had a triple room quite small, but the beds was very comfortable. Not great breakfast but acceptable, served next to reception, in a space with large windows to the street.
Could not park the car in the hotel parking. We were told that only 4.20 meters shorter cars can be parked there and sent us to a public park located about 500 meters away.
They clean the room and will not change sheets or provide toiletries. I had to go buy soap for myself
Hotel is really good and clean, Staff is excellent. It has a bright and fresh rooms.
Clean , nice neighborhood , caffe across street
Large rooms, nice bathrooms, friendly staff.
No welcome water in the room, pretty far away from the centre, poor surrounding.
1. Near the centre 2. Brekfast is ok but very simple (croissant are marvelous) 3. Conditioning is really quiet
1. Cleaning of the room is not so good 2. No free water in rooms 3. No additional stuff such as toothbrush, slippers. Shampoo and shower gel are not provided on daily order
The biggest shower I've been in in Europe. The shower head was also amazing. The bead was wry comfortable, great breakfast and pretty good location. Well worth the money!
Excellent breakfast and very friendly servers.
Torn mattress that was not replaced despite complaints. We had to beg for towels every day...one towel was the standard even though there were three of us. The front desk person was extremely rude and said the reason we had poor housekeeping responses is that they were "all from the Ukraine"...I was shocked at her callous and cold attack on a group of people. We were finally given a 10% percent discount by the manager for our trouble...I would have preferred better service.
Very nice hotel, especially as we got it at app 50% discount for a late booking. We had parking included in the offer and it was very comfortable not to bother about this issue even if the hotel garage was an extremely tight entrance. Staff is friendly, also breakfast ok, rooms are comfortable and nicely furnished and clean. Good location (25 min walking from the centre and max 10 min from the metro station). Overall, it was a positive experience.
Nothing that I particularly disliked; Maybe too small flat TV or small private parking, but for parking there was also an alternative at app 500m.
Friendly staff
Smelled a bit smoke in room
Very good location which have a good transport. Many shops around the hotel and especially there is a hot dog opposite the hotel which open quite long time and no need to worry about hunger. The hotel is quite clean and we love the air-con and inside the room.
If the breakfast is free, that will be better!
They cancelled our reservation 2 days before we reached there. Thank god we managed to secure other hotel. The booking at this hotel is a hassle for us as we have to do it 4 times to secure booking (other place only one time). I suggest u look somewhere else whereas there are other hotels around that is so so so much better.
Location was very good close to metro stations
They have poor choice of breakfast & Air-conditioning never worked we had to open the window and sleep.
Outside noises (street)
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text:
South Coast Metro Center SS: 589 Anton Blvd Costa Mesa, CA 92626 714-751-2724 [Print]
GX Schedule Update for the Thanksgiving Holiday - Dear Members & Guests - Our Group X schedule will be modified from November 26th to 30th. Please check the schedule to see what classes are being offered. Have a wonderful and safe holiday!
Pool Closed for Remodel - From November 24th to December 9th, the pool area will be remodeled and unavailable to members. We appreciate your understanding.
Every Aqua Zumba and Zumba Gold class is Endorsed by Silver&Fit®
Notes: {*} - Space is limited; sign up at front desk required; {esp} - Se habla espanol


text:
Oh man, you just messed with the wrong Bandit. That's right. With a capital "B" cause I'm very badass. I'm about to tear your guts out and -
Your sword went right through my brainpan! How did that even happen?
Yeah, you go ahead and loot my body. I think I've got a few coins and some mammoth snouts in my pockets. You know, the usual. Go ahead and take it all. Know this, however: I will return. When you least expect it, a bandit will attack, and that bandit will be me. Your misadventures will soon come to an end at the hands of the true master of Skyrim!
Hey, you! If you want to cross the bridge you have to pay the toll. It's uh... 200 coins? Yeah. 200 coins. Sure, I'm with the government. It's none of your business why it says Bandit above my head.
Listen, don't try my patience. You have armor made from the bones of dragons you've personally killed. Your sword was forged by the greatest blacksmith in the land. I, however, would surely prevail because I am adorned in fur armor. That's right, fur. Some if it's from a dog, and some of it's from a goat that got away before I could finish crafting. My weapon of choice is a rusty dagger that you pass up while scrounging for loot.
No? You're not paying the toll? Fine. I'm going to enjoy seeing your guts fall out of -
UH! You yelled at me so hard I flew off the cliff!
Now I'm a vampire bandit. This is so sweet. I've got a nice little hidden cave. I've got my coffin, a book of riddles, and all the broken urns I could possibly need.
Did I just hear something? Could have sworn someone was sneaking around. And there, that sounds like an arrow being drawn. When did this awesome cave start making such weird sounds?
Just in case someone's in here, I should go next to this bright fire and crouch. That will make me invisib -
UH! Didn't even see that one. Wait, was that a 30x damage multiplier? Come on. That's just stupid.
Well, well. Look who stumbled across my awesome crumbling fort? That's right, asshole. It's me again, and this time I'm a cultist bandit.
You know how dragons were really powerful creatures that mysteriously disappeared long ago and now they're back? Remember all those weird gods and cults and civilizations that were very powerful and mysteriously disappeared long ago, until you just happened upon them in the last few days?
Well, my cult is very ancient and very powerful. There are all sorts of books written about us. You might have come across some of them, stolen them, then tried to manually drop them on your bookshelf before you realized it had an auto-sort feature. Funny thing is, our cult disappeared long ago and everyone agreed it was quite mysterious. Now we're back, and you've got to die.
You'll be so much easier to steal from when you're dea-
Saints Row The Third
Dumb in all the best ways imaginable and fueled by an impressionistic plot full of characters that are all too happy to dive headfirst into terrible plans, this makes every other game that aspires to be "over the top" seem devoid of creativity and ambition. 9/10
Need For Speed: The Run
Halfway decent driving, flashy but hollow on-foot quick time events, and not a lot of reason to care about either element. 5/10
Wait, rather than hiding in shame, these assholes assume that their brand is popular enough to warrant a piece of entertainment? 2/10
Jurassic Park: The Game
Imagine a version of Heavy Rain that actually had some charm, then stuttered at every turn and made your inputs feel more disconnected from the game than the gap between David Cage and the notion of good writing. 6/10
The Legend Of Zelda: Skyward Sword
Carry on my skyward sword / the tutorials might make you bored / lay your worries to rest / don't you waggle no more. 9/10
In a Something Awful exclusive, we reveal the true state of Darren Wilson after his harrowing encounter with Michael Brown.
gee, sun, thanks for life and warmth and light. you totally did it on purpose and aren't just a stupid exploding deathtrap
Everything I'm about to show you is art. It says nothing and is worth even less, but it's still art!
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