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Zirconia dental implants require excellent biocompatibility and high bonding strength. In this study, we attempted to fabricate biocompatible zirconia ceramics through surface modification by hydroxyapatite (HA) slurry coating. A hydroxyapatite slurry for spin coating was prepared using two sizes of hydroxyapatite particles. The hydroxyapatite slurry was obtained by adjusting the solid loading, pH range, and dispersant content. The surface roughness of the HA-coated layers on the zirconia substrate depended on the change in microstructural evolution and coating thickness. With repeated coating, the coating thickness gradually increased for both small and large particles. The specimen with two coatings had the maximum surface roughness but displayed different values depending on the size of the HA particles. High surface roughness (Ra; 0.49 μm) could be obtained from the slurry of small particles compared with that of the large particles (Ra; 0.35 μm). During a 14 days in vitro experiment in SBF solution at pH 7.4, no changes were observed in the surface microstructure of the HA coating layer on the zirconia substrate.

Two types of dense and toughened 3Y-TZP zirconia implants were fabricated by the sintering of green compacts. Then, the sintered properties of the two implants were compared. Slip-cast and post-sintered all-ceramic zirconia implants were fabricated by the heat treatment at 1450 °C for 2 h using optimal slurry conditions (60 wt% solid content, 1 wt% dispersant, and pH 12). Computer-aided design and manufacturing (CAD/CAM)-machined and post-sintered zirconia crowns, supplied by a dental hospital, were obtained by sintering at 1650 °C for 5 h. The X-ray diffraction results indicated that the phase composition of the slip-casted specimen was completely tetragonal, but the CAD/CAM machined sample was composed of mixed phases of main tetragonal and minor monoclinic crystals. The sintered density and Vickers hardness of the slip-casted specimen were 6.07 g/cm3 and 1367 Hv, respectively, and these were higher than those of the CAD/CAM machined specimen. From the comparative results of the surface microstructure, hardness, and roughness between the two sintered specimens, the slip-casted specimen was found to have higher surface roughness and mechanical hardness, smaller grain size, and less surface micro-cracks than the CAD/CAM machined specimen.

Dense zirconia compacts were fabricated by slip casting and sintering of nanoscale zirconia powders, and the effect of the powder characteristics (crystallite size, specific surface area, yttria content, and agglomeration) on the slurry and sintered properties was investigated. Three types of commercial 3 mol% yttria-stabilized tetragonal zirconia polycrystals powders were used as the starting powders after the powder characteristic analysis. A zirconia slurry for slip casting was prepared by mixing zirconia powder (solid loading of 60, 65, and 70 wt.%), distilled water, and a dispersant of Darvan C. The green compacts obtained from slip casting were cold isostatic pressed to enhance the close packing and densified by sintering at 1450 °C for 2 h. Highly dense zirconia compacts with a relative density of 99.5% and grain size of 350 nm were obtained based on the powder type and solid loading in the slurry. The microstructure and mechanical hardness of the sintered specimen after slip casting were dependent on the yttria content in the 3 mol% yttria-stabilized tetragonal zirconia polycrystal powder and the solid loading within the slurry.

Highly surface-roughened zirconia substrates were obtained from additive zirconia powder coating by room temperature spray processing. Homogeneous and dense zirconia coatings were deposited on sintered zirconia substrates with strong bonding by a powder spray coating method. The thickness and surface roughness of the coating layers on zirconia substrates increased with increasing coating cycles, which was confirmed from atomic force microscopy (AFM) and roughness analyses. The tetragonal phase and chemical composition of the zirconia coating layers were similar to those of the raw 3Y-TZP powder used as a raw material, indicating that no phase or composition changes occurred during the spray process.

Dental zirconia implants are typically manufactured by mechanical machining of a zirconia block into a tooth shape. Many cracks are created by this machining process on the surface of the green body, which induces deterioration of mechanical strength and reliability of the sintered zirconia implant. In this study, we fabricated a dense zirconia specimen by slip casting and sintering. The zirconia slurry for slip casting was prepared by mixing yttria-stabilized zirconia powder with an average particle size of 20 nm, distilled water, and dispersant. Slurry viscosity was controlled by varying pH, dispersant concentration, and solid content; the lower viscosity being achieved at pH 11 controlled by ammonium hydroxide. With a dispersant content of 0.4-0.8 wt%, the viscosity was reduced from 190 cP to 40 cP at pH 11. After casting and sintering at 1550 °C for 2 h, the sintered body reached a density of 5.70-6.01 g/cm³ and a grain size of 300-700 nm, depending on the slurry preparation conditions.

Zirconia ceramics has a bioinert property with low bioactivity. So, it is necessary to improve its low bioactivity by the surface modification using effective coating methods. In this study, we fabricated the hydroxyapatite-coated zirconia substrate by room temperature spray processing to improve the bioactivity of the zirconia implant and investigated its coating effect on the biological performance of zirconia substrate via an in vitro test in simulated body fluid (SBF) solution. Before the room temperature spray coating was completed, size-controlled hydroxyapatite powder that had an average size of 4.5 μm, was obtained by the calcination and milling of a commercial powder. By controlling the processing parameters, such as spraying distance, and deposition cycles, we fabricated homogeneous and dense hydroxyapatite coatings on zirconia substrate. Surface morphology, coating thickness, and microstructure were dependent on deposition cycles, and were related to surface roughness and bioactivity. Zirconia substrates with wave-patterned and roughened hydroxyapatite coatings demonstrated high bioactivity in their in vitro tests. Via the immersion test in an SBF solution, surface dissolution and new precipitates of hydroxyapatite were observed on coated zirconia substrate, indicating the degree of bioactivity.

The zirconia used in dental implants requires excellent mechanical and chemical properties such as high strength, high biological performance, corrosion resistance, and phase stability. In this study, after we prepared a highly fluidized solution of calcium phosphate, we fabricated a hydroxyapatite (HA) coating layer on a zirconia substrate using the sol–gel method to enhance its biocompatibility and bone-bonding ability. We dipped the zirconia substrate into the calcium phosphate sol to obtain the HA-coated film, which was dried at room temperature. The phase change and microstructural evolution were examined while the coating dried and during heat treatment. The biological activity of the coated and as-received substrates was evaluated using an in vitro experiment and the results were compared. The HA-coated film showed a highly dense and uniform layer structure, while its physical and biological properties depended on the starting substrate, coating times, and processing conditions.

Dental implants are typically composed of 3Y-TZP (3 mol% yttria-stabilized tetragonal zirconia polycrystals). Most dental zirconia implants are currently fabricated via mechanical machining. However, during the machining of zirconia green bodies, many cracks form on the surface. To prevent surface crack formation on the implants, shape forming of the zirconia is necessary using methods such as slip casting. Herein, we fabricated green compacts using slip casting, candidate forming process to reduce surface cracking. To fabricate an optimal 3Y-TZP implant by slip casting and sintering, we prepared a suitable 3Y-TZP slurry for slip casting by adjusting the viscosity via pH, dispersant agent content, and solid loading refinement. Green compacts were prepared by the slip casting of all-ceramic zirconia implants fabricated using optimal slurry conditions, for example, 60 wt% solid content, 1 wt% dispersant, pH 12 and post-sintering at 1450 °C for 2 h. All sintered bodies contained a tetragonal phase with a high sintered density of approximately 6.07 g/cm3, good mechanical hardness of approximately 1367 Hv, grain size of 220 nm, and high surface roughness without cracks.

Nanoscale yttria-stabilized zirconia (Y-TZP) powder was synthesized by homogeneous precipitation via urea hydrolysis, and the influence of a dispersing agent and the initial ZrOCl2 concentration on the powder characteristics was investigated. A precipitated gel was obtained from the reaction of the precursor solution with zirconium oxychloride, yttrium chloride, and urea with heating at 110 °C for 5 h. The initial ZrOCl2 concentration was controlled from 0.25 to 1 M. To observe the effect of adding a dispersing agent on the agglomeration of primary particles, we used two starting compositions, one with and the other without a dispersing agent, ammonium polymethacrylate. Two crystalline powders were obtained after drying, calcination, and milling the gel, and we investigated the powder characteristics, such as particle agglomeration, the specific surface area, the microstructure, and phase composition. Two scales of agglomerates were observed in the particle size distribution, namely, 190 to 362 nm at the primary scale and 1.6-4.0 μm at the secondary scale. The amount of secondary agglomerate increased from 6 to 20 vol% with the increasing initial ZrOCl2 concentration. The size of both types of agglomerate and the amount of secondary agglomerates decreased due to the addition of the dispersing agent, especially the primary agglomerate size. The sintered density and microstructure of Y-TZP were affected by the agglomeration behavior, especially the amount of secondary agglomerates.

Nanocrystalline zirconia with high surface area and pure tetragonal crystalline phase was prepared using ethylene diamine (EDA), which acts as both precipitating agent and dispersant of the zirconium precursor. The yttria stabilized zirconia (Y-TZP) is a very attractive material due to its excellent biocompatibility, high fracture toughness, high strength and low wear rates. So zirconyl chloride octahydrate (ZrOCl2 · 8H2O) and yttrium chloride hexahydrate (YCl3 · 6H2O) in different molar ratios were used as starting solution. The detailed effects of various process parameters such as reaction time, concentration of the precursor solution, amount of ethylene diamine, and calcination temperature on the structural properties of the zirconia powders were investigated. The preparation conditions significantly affected the structural stability, crystal size, and crystal phase of the final material. Increases in the reaction time and amount of ethylene diamine led to a substantial increase of the crystal growth rate, the specific surface area, and the tetragonal content of the zirconia.

Organic/inorganic biocomposite materials for biodegradable fixation medical devices require osteoconductivity, biocompatibility, and adequate mechanical properties with biodegradation behavior. The objective of this study was to investigate the effect of Si ions substituted in β-tricalcium phosphate (β-TCP) on the mechanical properties of organic/inorganic biocomposites. Biodegradable composite materials were prepared with polylactic acid (PLA) as the matrix and nano Si-substituted β-TCP as the osteoconductive filler by solvent mixing and conventional molding. The nanostructured Si-substituted β-TCP powders were synthesized by co-precipitation, controlling the quantity of Si ions. The amount of nanostructured Si-substituted β-TCP powders in composites was varied in the 0-40 wt% range and the material properties were compared with those of pure β-TCP/PLA composites. The influence of Si ions on the mechanical properties of the composites was evaluated by tensile and flexural tests.

Osteoconductive, biocompatible, and resorbable organic/inorganic composites are most commonly used in fixation medical devices, such as suture anchors and interference screws, because of their unique physical and chemical properties. Generally, studies on biodegradable composites have focused on their mechanical properties based on the composition and the individual roles of organic and inorganic biomaterials. In this study, we prepared biodegradable organic/inorganic nanocomposite materials using the solvent mixing process and conventional molding. We used polylactic acid (PLA) as the matrix and nano-sized hydroxyapatite (nano-HAp) as the osteoconductive filler. The content of nano-HAp was varied in 0-30 wt% and its influence on the In-Vitro mechanical performance of PLA/HAp nanocomposites was evaluated. The In-Vitro mechanical properties of nanocomposites were evaluated using standardized tensile and flexural tests after different immersion times in simulated body fluid.

Highly roughened surfaces on dental implants enhance the bone-bonding ability and in vivo cell adhesion on the implant surface. In this study, zirconia substrates were coated by powder coating using room temperature spray processing to improve their surface properties. Processing factors (particle size of the starting powder, number of repetitions of the deposition cycle, and spraying distance) were controlled to form a dense coating layer with high surface roughness on the zirconia substrate. Starting zirconia powders for coating were heat-treated at high temperature to control the particle size and kinetic energy. The coating layer fabricated from starting powder with a particle size of about 1.52 μm shows a homogeneous and dense microstructure, and it has a maximum surface roughness about 0.37 μm. The surface roughness of the film coatings increased with the number of times that the deposition cycle was repeated. No phase changes between the starting powder and the coating layer were observed, and all of the materials show identical tetragonal phases.

Dental zirconia implants fabricated by the mechanical machining and sintering of zirconia blocks have many surface cracks that lead to the deterioration of mechanical strength and the failure of the implant in the body. In this study, we attempted to manufacture an extremely dense and crack-free zirconia specimen by slip casting and pressureless sintering. After the preparation of zirconia slurry by control of its viscosity and by solid loading, highly dense zirconia specimens could be obtained by pressureless sintering at 1450 °C for 2 h. Slurry viscosity was controlled by adjusting the mixing ratio of 3Y-TZP powder, a dispersant, and a pH adjustment agent. Highly dense 3Y-TZP specimens with a relative density of 99% and small grain size of 200-400 nm could be obtained at a solid loading of 50-65 wt%. An optimally dense specimen was fabricated from zirconia slurry with 60 wt% solid loading that had the highest apparent density of 6.07 g/cm³ (99.5%).

Active nanoscale powders of cubic phase zirconia stabilized with yttria, gadolinia, and scandia were successfully prepared by urea hydrolysis. Synthetic cubic zirconia powders had homogeneous, nanoscale, and less-agglomeration characteristics. Dense pellets of grain size about 0.4 μm exhibited grain boundary blocking resistance compared to the high frequency bulk resistance. Gadolinium doped system exhibited highest ionic resistivity. Yttria stabilized zirconia by urea hydrolysis in this work showed smaller ionic resistivity than the sample prepared from the commercial powder.

Hydroxyapatite (HA) is widely used as a bioactive ceramics as it forms a chemical bond with bone. However, the drawback to using this material is its inferior mechanical properties. In this research, surface corrosion and disintegration of nanoscaled HA in a dog were studied, and the mechanism by which phase-pure HA dissolved In Vivo was investigated. Biological properties of HA In Vivo are affected by the grain-boundary dissolution followed by a surface corrosion and microstructural disintegration. This kind of dissolution process, apparently evidenced at the grain boundary, causes particle generation, which indicates that both long-term bone in-growth and mechanical properties can dramatically deteriorate. Implant dissolution by osteoclasts In Vivo is also observed on the surface of hydroxyapatite. Implant surface showed an aggressive corrosion by an osteoclast resorption. Severe and deeper dissolution underwent close to osteoclast resulting in formation of smaller and more round particle shape.

Surface modification with a biphasic composition of hydroxyapatite (HA) and tricalcium phosphate (TCP) was performed on a zirconia substrate using a sol-gel method. An initial calcium phosphate sol was prepared by mixing a solution of Ca(NO3)2 · 4H20 and (C2H5O)3P(O), while both porous and dense zirconia were used as substrates. The sol-gel coating was performed using a spin coater. The coated porous zirconia substrate was re-sintered at 1350 °C 2 h, while coated dense zirconia substrate was heat-treated at 750 °C 1 h. The microstructure of the resultant HA/TCP coatings was found to be dependent on the type of zirconia substrate used. With porous zirconia as a starting substrate, numerous isolated calcium phosphate particles (TCP and HA) were uniformly dispersed on the surface, and the particle size and covered area were dependent on the viscosity of the calcium phosphate sol. Conversely, when dense zirconia was used as a starting substrate, a thick film of nano-sized HA particles was obtained after heat treatment, however, substantial agglomeration and cracking was also observed.

A throat plug is a device in a shock tunnel to prevent fragments, produced by the bursting of the primary diaphragm, from entering the nozzle and damaging the model. In the present study, a series of experimental and numerical studies has been carried out to investigate the flows around stationary throat plugs in a shock tunnel. For this purpose, conical, circular, and double circular stationary throat plugs that have a 19.4% areal blockage were used as the test models. The primary shock velocity was set at 1.19 km/s, and the shock generated a tailored condition when helium and air were used as the driver and driven gases at room temperature. In the experiment, the nozzle reservoir pressure and the pitot pressure at the nozzle exit were measured to examine the influence of the throat plug. It was found that, from both the experiment and the calculation, all types of the plugs generate a pressure bump in the nozzle reservoir during the transient period of interaction between the reflected shock and the pl...

Microfluidics technology has been exploited in single cell study because of its ability to manipulate particles and control over culture conditions. Two drawbacks of the existing studies are that (1) they require large supporting equipment like an incubator and a syringe pump; which involves more culture media volume, and that (2) the trapped cells are isolated from one another that cell interaction is obstructed or not considered. These limit the applications and advantages of microfluidics compared to conventional petri dish method. In this study, centrifugal microfluidics is utilized to trap single cells of primary cultures of neonatal rat cardiomyocyte with controlled separation distance. Cell growth, coupling, and beating are successfully observed and monitored in the fabricated microfluidic device without large supporting equipment. Coupling and decoupling dynamics, that is a first to be observed in cardiomyocyte cell microfluidics, can be proven useful in the headway of controlled cell growth and orientation research. Furthermore, these findings can be applied to future chip design and operation for cardiomyocyte studies and high-throughput lab on-a-chip devices.

Densification and mechanical properties of dental zirconia ceramics were evaluated by different sintering methods. Y-TZP zirconia block was used in this study. Sintering were performed in electric heating furnace and microwave sintering furnace, and then experimented and analyzed on a change in densification according to the sintering time, a change in densification according to thickness, flexural strength and micro-structure of zirconia specimens. Microwave sintering was very effective in considerable mechanical properties such as flexural strength and bulk density was drastically increased than conventional electric heating method. It is also shown that microwave sintering was faster and more economical than common method to be present in qualities which equal or exceed. It will be important to seek the accurate sintering condition of dental zirconia by microwave sintering method and the continuous research is necessary for the study of relationship between sintering methods and mechanical properties.

In this study, we investigated the crack nucleation and growth and propagation on the surface of Y-TZP during isothermal phase transformation by low temperature ageing. Crack initiation and growth on the surface of Y-TZP specimen was dependent on the sintered microstructure, i.e, sintered density, grain size, pore structure, residual stress etc.. In the case of Y-TZP with 2mol % yttria content, phase transformation of tetragonal to monoclinic began on the surface and induced a crack nucleation of specimen at the initial stage of low temperature ageing. Most of cracks in 2Y-TZP by low temperature ageing were firstly formed on the surface of specimens (free surface, weak bonding grains, etc.) where the change of strain free energy for a tetragonal to monoclinic transformation was small, and surface cracks grew into the bulk interior through the grain boundaries.

We present herein a first proof of concept demonstrating the potential of a protein nanopore-based technique for real-time detection of selected Gram-negative bacteria (Pseudomonas aeruginosa or Escherichia coli) at a concentration of 1.2 × 108 cfu/mL. The anionic charge on the bacterial outer membrane promotes the electrophoretically driven migration of bacteria towards a single α-hemolysin nanopore isolated in a lipid bilayer, clamped at a negative electric potential, and followed by capture at the nanopore’s mouth, which we found to be described according to the classical Kramers’ theory. By using a specific antimicrobial peptide as a putative molecular biorecognition element for the bacteria used herein, we suggest that the detection system can combine the natural sensitivity of the nanopore-based sensing techniques with selective biological recognition, in aqueous samples, and highlight the feasibility of the nanopore-based platform to provide portable, sensitive analysis and monitoring of bacterial pathogens. Electronic supplementary material The online version of this article (doi:10.1186/s11671-016-1715-z) contains supplementary material, which is available to authorized users.

In situ preparation of magnesium (Mg) substituted biphasic calcium phosphate (BCP) of hydroxyapatite (HAp)/β-tricalcium phosphate (β-TCP) were carried out through aqueous co-precipitation method. The concentrations of added magnesium were varied with the calcium in order to obtain constant (Ca + Mg)/P ratios of 1.602. X-ray diffraction (XRD) and Fourier transformed infrared (FTIR) spectroscopy were used to characterize the structure of synthesized magnesium substituted BCP powders. The results have shown that substitution of magnesium in the calcium deficient apatites revealed the formation of biphasic mixtures of different HAp/β-TCP ratios after heating at 1000 °C. The ratios of the formation of phase mixtures were dependent on the content of magnesium. After immersing in Hanks’ balanced salt solution (HBSS) for 1 week, 1 wt% magnesium substituted BCP powders were degraded and precipitation started to be formed with small granules consisting of number of flake-like crystal onto the surface of synthesized powders. On the other hand, in the case of pure BCP powders, the formation of new precipitates was detected after immersion in HBSS for 2 weeks. On the basis of these results, magnesium substituted BCP could be able to develop a new apatite phase on the surface in contact with physiological fluids faster than BCP does. In addition, the retention time to produce the new apatite phase in implantation operation for the BCP powder could be controlled by the amount of magnesium substitution.

In situ preparation of silicon (Si) substituted biphasic calcium phosphate (BCP) of hydroxyapatite (HAp)/ β-tricalcium phosphate (β-TCP) were carried out through aqueous co-precipitation method. The concentrations of added silicon were varied with the phosphor in order to obtain constant Ca/(P+Si) ratios of 1.602. X-ray diffraction (XRD) and Fourier transformed infrared (FTIR) spectroscopy were used to characterize the structure of synthesized silicon substituted BCP powders. The characterization revealed that the formation of biphasic mixtures of different HAp/ β-TCP ratios was dependent on the content of silicon. After immersing in Hanks' balanced salt solution (HBSS) for 1 week, 3 wt% silicon substituted BCP powders were degraded and precipitation started to be formed with small granules consisting of number of flake-like crystal onto the surface of synthesized powders. In the case of 1 wt% silicon substituted BCP powders, the degradation behavior was detected after immersion in HBSS for 3 weeks. On the other hand, silicon unsubtituted BCP powders were not degraded even after that duration. On the basis of these results, silicon substituted BCP is able to develop a new apatite phase on the surface in contact with physiological fluids faster than BCP does. This enhanced reactivity resulted in reduction for the stability of the β-TCP structure due to SiO 4 tetrahedral distortion and disorder at the hydroxyl site when silicon incorporates into BCP.

Bone ash-derived hydroxyapatite (HA) ceramics were prepared by pressureless sintering and hot pressing, and their dissolution behavior was examined in buffered water. HA powder was obtained by soaking bone ash in a 0.1M NaOH solution at 80 °C, followed by calcination at 1000 °C to completely remove the organic material. The crystal structure of the HA powder with a particle size of approximately 1 μm was mainly hydroxyapatite with a minimal amount of α-tricalcium phosphate. To improve densification, the powder was hot-pressed at 1000 °C for 0.5 h under a pressure of 30 MPa in an Ar atmosphere. The sintered density of the hot-pressed HA was 95 % of the theoretical density, which is much higher than the 70% obtained for the pressureless-sintered compact. In the porous HA ceramics obtained by pressureless sintering, dissolution occurred adjacent to the pores rather than in the dense part, which increased the residual porosity. On the other hand, the hot-pressed HA showed grain boundary dissolution followed by particle loosening.

Titanium alloys are superior of biocompatibility, mechanical properties and chemical stability. The biocompatibility of Ti alloy is related to the surface effect between human tissue and implant. Therefore, the purpose of this study is to investigate the bioactivity of Ti alloy by alkali and acid chemical surface treatment; and the biocompatibility of Ti alloy was evaluated by in vitro test. Higher bone-bonding ability and bioactivity of the substrate were obtained by the formation of apatite layers on the Ti alloy in simulated body fluid. The microstructures of apatite layer were investigated by scanning electron microscope (SEM) and the formed phases were analyzed with X-ray diffraction (XRD).

Titanium-based nitride coatings on cutting tools, press molds and dies can be used to prolong their life cycle because of their superior corrosion and oxidation resistance. TiAlN/ZrN and TiCrN/ZrN multilayer coatings were prepared by RF magnetron sputtering, and their microstructural evolution and corrosion resistance during heat treatment were investigated. The TiAlN/ZrN and TiCrN/ZrN multilayer coatings are degraded by heating up to 600 °C with the formation of oxides particles on the surface. During the heat treatment, the TiCrN/ZrN and TiAlN/ZrN multilayer coatings show the lowest corrosion current density and the highest polarization resistance at temperature range of 400–500 °C. Consequently, the TiAlN/ZrN and TiCrN/ZrN multilayer coatings show good corrosion resistance at temperature range of 400–500 °C during heating.

A small amount of misch metal was added to Cu-Zn-Al alloy in order to study its effect on grain refinement, mechanical properties, phase transformation behavior and stabilization of martensite. It is found that the addition of misch metal is very effective for reducing the grain size. The coarse grains over 1 000 μm are refined to the size of 30 μm by the addition of 0.43% (mass fraction) misch metal. The grain size of thermo-mechanically treated alloys is barely affected by cold working. The fracture strength and ductility increase significantly with the increase of misch metal content when tensile test is carried out below M f temperature. Also, the fracture strength is larger in the case of post-quench ageing treatment than that in the case of direct quench ageing treatment. The fracture mode is changed from transgranular brittle fracture to ductile fracture with void formation and coalescence by the addition of misch metal.

Hydroxyapatite (HA) has generated a great deal of interest as a promising implant material. However, its poor mechanical properties induced by severe dissolution in biological milieu limit medical applications and lead to clinical failure. In this study, HA ceramics with 30P2O5-30CaO-40Na2O glass (1.0 wt.% and 2.5 wt.%) were prepared to improve the resistance of monophase HA. The monophase HA sintered body showed microstructural degradation due to grain boundary dissolution in buffered water. However, the dissolution-resistance of HA/glass composites was significantly improved and showed no apparent evidence of dissolution. This suggests that a less soluble glass phase should be placed at grain boundaries to protect HA from dissolution.

Dissolving behavior of hydroxyapatite (HA) ceramics prepared from bovine bone (BHA) was investigated and compared with synthetic HA. BHA power was obtained by calcining at 800 °C for 1 h to remove organics and then attritor-milling for 24 h. Synthetic HA and BHA powders were prepared by hot-pressing at 1000 °C for 0.5 h under the pressure of 30 MPa in Ar atmosphere. Sintered densities of the synthetic HA and the BHA were about 96% and 95%, respectively. The BHA consisted of mainly HA and small amount of magnesium oxide. Immersion test revealed that there was no clear evidence of dissolution for the BHA, whereas extensive dissolution on the surface of the synthetic HA occurred in buffered water. Accordingly, dense hydroxyapatite from bovine bone was more stable than synthetic HA in liquid environment.

Networking and density of silver particles is a great importance to obtain low electrical resistivity of silver paste. In order to improve packing density, interconnectivity and conductivity at low sintering temperature, silver paste was prepared from bimodal silver particles, i.e., consisting of micro- and nano-sized particles. In order to fit nano-Ag particle into the interstices of the micro-Ag particles of 1.6 microm in size, the interstices need to be approximate below 360 nm in size. Therefore, we prepared nano-Ag particles of 100-300 nm in size by chemical reduction method. The silver paste prepared by mixing the bimodal powders, Pb-free frit and vehicle were printed on an alumina substrate by screen printing and sintered at temperature of 400-500 degrees C. As increasing the amount of nano-Ag particles and sintering temperature, packing density and electrical conductivity were increased. The nano-Ag particles placed between the micro-Ag particles contributed to improve interconnectivity and densification of the printed films. Accordingly, as the amount of nano-Ag particles was increased, the electrical resistivity were decreased. The thick film at sintered 500 degrees C showed the lowest electrical resistivity of 3.9 microomega cm which can be compatible for application in microelectronics devices.

Silver thick films were prepared from lead-free silver paste adding silver nanoparticles for low sintering temperature, and the effect of glass frit content on conductivity in the films was investigated. Silver pastes with different glass contents were prepared by mixing micron-scale silver powder of 1.6 microm and nanoparticles of 30-50 nm in size. To prepare lead-free silver paste, 5 wt% of the silver nanoparticles as a sintering aid were added to the micron-scale silver powder. Then, 3 wt%, 6 wt%, and 9 wt% of lead-free frits were added to the mixed powders. Using the paste, thick films were prepared by a screen printing on an alumina substrate and then the films were sintered at temperatures from 300 degrees C to 550 degrees C. As increasing the sintering temperature and content of lead-free frit, the thick films showed dense microstructure. The glass frit enhanced to develop denser microstructure by liquid phase sintering. However, excess of glass content increased sheet resistivity due to the formation of glass pool separated from particle network. Furthermore, the nanoparticles can assist to develop a conductive network in the film. The films with 6 wt% of glass frit had the best conductive network and the lowest sheet resistivity of 3.2 microomega cm.

Dissolving behavior of hydroxyapatite (HA) ceramics prepared from bovine bones (BHA) was investigated and compared with artificial HA. BHA and artificial HA were sintered at 1200 °C for 1 h, and they were immersed in distilled water at 37 °C for 3, 7, 14 and 28 days. Detectable peaks in artificial HA were only identical to HA phase, however, BHA consists of mostly HA phase and small amount of MgO. Sintered density of BHA was lower than that of artificial HA. Dissolution of artificial HA was founded after 7 days. The grain boundaries on the surface of artificial HA appeared to initiate dissolution, and grains are pulled out of the artificial HA surface at the end of the immersion period, however, there is no evidence of BHA surface at the end of the immersion period. It was found that HA from bovine bone was more stable than artificial HA in a liquid environment.

Hydroxyapatite (HA) has been of interest in many industrial applications, such as ion exchange, catalysis and biomaterials. Chelating agents have often been used to prepare inorganic powders in the form of sphere, rod, whisker and fiber. In this study, HA whiskers were synthesized directly from typically shaped HA powders by refluxing at 80 and 100 °C for 24 h using ethylenediamine tetraacetic acid (EDTA). 3% or 6% of hydrogen peroxide (H 2 O 2 ) was used to promote precipitation of HA crystals. The pH of the solution was adjusted at 7 or 9 by adding ammonia solution. The higher the H 2 O 2 concentration, pH value and refluxing temperature, the longer and thinner whiskers were formed. The whiskers produced at 100 °C with 6% of H 2 O 2 and pH 9 had the highest aspect ratio of about 50–60 (a length of 3 μm and a width of 0.05 μm).

A small amount of misch metal was added to CuZnAl alloy in order to study the effect of grain refinement and mechanical properties, phase transformation behavior and stabilization of martensite. It was found that the addition of misch metal was very effective for reducing the grain size. The coarse grains over 1000 μm have been refined to the size of 30 μm by the addition of 0.43wt% misch metal. The grain size of thermo-mechanically treated alloys was barely affected by cold working. The fracture strength and ductility have been significantly increased with the increase of misch metal content when tensile test is carried out below Mf temperature. Also, the fracture strength has been more increased in the case of post-quench ageing treatment than the direct quench ageing treatment. The fracture mode has been changed from transgranular brittle fracture to ductile fracture with void formation and coalescence by the addition of misch metal.

Titanium-based nitride coatings on cutting tools, press molds and dies can prolong their life cycle because of superior corrosion and oxidation resistance of coatings. In this study, TiAlN/ZrN and TiCrN/ZrN multilayer coatings were prepared by R.F magnetron sputtering, and microstructural evolution and corrosion resistance of the coatings were investigated during heat treatment. The TiAlN/ZrN and TiCrN/ZrN multilayer coatings were degraded by heating up to 600 oC with formation of oxides particles on the surface. During the heat treatment, the TiCrN/ZrN and TiAlN/ZrN multilayer coatings showed the lowest corrosion current density and the highest polarization resistance at temperature range of 400 oC and 500 oC. Consequently, the TiAlN/ZrN and TiCrN/ZrN multilayer coatings showed good corrosion resistance at temperature range of 400°C and 500°C during heating.

Hydroxyapatite (HA) has been widely used as a coating for orthopedic metal implants. An important concern regarding HA coating is its degradation of the biological milieu. In this study, the microstructure of a retrieved HA-coated acetabular cup implanted for four years after total hip arthroplasty (THA) was investigated by field emission scanning electron microscopy. In order to understand the underlying mechanism, of degradation and exfoliation of the HA coating, degradation of phase-pure and dense HA ceramics was also observed byin vitro andin vivo testing. The surface morphology and fracture surfaces of HA ceramics revealed that the dissolution starting at the surface extended inwards resulting in particle loosening and microstructural-level degradation. The dissolution features of HA ceramics were similar to the case of HA coating. It was found that extensive dissolution of the coating occurred and most of the coating disappeared. The majority of the remaining graints were fractured by the intergranular mode, suggesting that grain boundaries should be predominantly dissolved. These observations may explain the mechanism through which the biological stability of the HA coated layer becomes unexpectedly poor.

Fabrication of paste at low temperature has been developed in order to apply for various electronic devices, such as bus electrode and address electrode in PDP, especially for enlargement of a screen size. In this study, nano-sized silver particles with 10 - 30 nm were synthesized from silver nitrate (AgNO3) by a chemical reduction method. To prepare Pb-free silver paste, the silver nanoparticles were mixed with conventional silver powder with an average particle size of 1.6 and conventional Pb-free frit. Thick films were fabricated from silver paste by a screen printing on alumina substrate and the films were fried at temperatures ranging from 550 °C to 600 °C. Microstructures of the fried thick films were analyzed by FE-SEM. Sheet resistivity of fried thick films was measured and also the relationship between sinterability and conductivity of these films were investigated.

The reaction-sintered alumina and zirconia-alumina ceramics with low firing shrinkage were prepared from Al 2 O 3 /Al and ZrO 2 (C a -PSZ)/Al powder mixture by attrition milling and the effect of the characteristics of used ceramic powders was investigated. Flaky Al powders mixed with coarse alumina powders could be effectively pulverized due to high hardness of alumina powders. On the contrary fused Ca-PSZ/Al powder mixture could not be effectively comminuted due to lower hardness than alumina powders. So by using hard alumina ball media or coarse Al 2 O 3 powders rather than Al, the milling efficiency could be much more increased. After attrition milling the Al 2 O 3 /Al specimens were oxidized at 1200°C for 8 hours and followed by sintering at 1550°C for 3 hours. Because mixed powders of Al with alumina were much more effectively comminuted, more than 97% theoretical density of sintered body could be achieved. In the case of fused Ca-PSZ powder reaction-sintered with Al at 1550°C for 3 hours, the reaction-sintering and densification were a little more difficult than Al 2 O 3 /Al specimens because of the insufficient milling. And the unstabilization of Ca-PSZ body which caused the cracks in the specimens was brought by the diffusion of Ca ion from Ca-PSZ grains to alumina.

Nano-sized silver particles are considered to apply a silver paste for electrode because of its high conductivity on sintering at low temperature. In this study, silver nanoparticles as seeds were prepared by chemical reduction method with capping agent. Silver particles were prepared using SDS (Sodium dodecyl sulfate) as a surfactant and silver nanoparticles as seeds and reacted with ascorbic acid as a reduction agent. The silver seeds with 10-20 nm in size with uniform distribution were formed and the size and shape of silver particles were strongly dependent on the concentration of surfactant.

This research has been performed to investigate the effect of ageing onto the grain refinement of 82wt%Cu-13.5wt%Al-4.5wt%Ni-0.1wt% misch metal alloy with ageing temperature and time. The variation of transformation temperature with ageing has been found to be heavily dependent on ageing time and temperature. In the second reversed transformation cycle, the temperature of Ms point decreases with ageing time at 300, but no variation at 100. The temperature of As point increases with ageing time at both temperatures. After the second reversed transformation cycle, the transformation temperature does not show any significant changes in martensitic phase with ageing, the temperature of Ms point being the same afterwards. Parent phase after ageing appears to show M18R and N2H martensitic phases depending on the ageing time and temperature. It is also found that α and γ2 phases are formed only at the condition of 300 and 24h.

Effective micro-organisms (EM) increase the natural resistance of soil and plants, and it considerably improves the quality and fertility of soil as well as the growth and quality of crops. In this study, we prepared two types of porous ceramics with high and low porosity, and observed the attaching behavior of micro-organisms to the surface of ceramics. In the case of highly porous ceramics with large pore (80% in porosity), many of micro-organisms were observed in the pores of interior as well as on the ceramic surfaces. However, most of micro-organisms attached on the surface of the low porous ceramics with small pore (45% porosity), and only a few micro-organisms observed in pore inside.

TiO2 photocatalyst has attracted much attention in recovering valuable metal ions from industrial wastewater because TiO2 shows chemical stability and good wear resistant, and a photocatalytic reaction occurs by illumination of the sun or fluorescent light. In this study, Au removal and recovery in a gilding wastewater using TiO2 photocatalyst was evaluated. Commercially obtained TiO2 powder and TiO2 film prepared by spray and screen print method were used for Au adsorption. The cyanide existed in a plating wastewater was firstly removed with peroxide or persulfate because a driving force for Au ion reduction during photocatalytic process could decrease by the existed cyanide. Compared with persulfate, peroxide shows relatively slow removal rate of cyanide but no precipitation occurs. With respect to photocatalytic reaction of TiO2 powder and film for Au removal and recovery, it was found that the addition of 10 vol% of methanol as a hole scavenger increases the rates of Au ion reduction and Au adsorption on the TiO2 powder and film, subsequently the reaction of Au photoadsorption was completed within 60 min. Au lumps on the TiO2 particles obtained by photocatalytic reduction of TiO2 was confirmed by XRD analysis and TEM observation.

The effect of Ca/P ratio on surface dissolution of hydroxyapatite [Ca10(PO4)6(OH)2, HA] in distilled water was investigated. The stoichiometric HA powder and desired Ca/P ratio achieved by adding either Ca3(PO4)2 for a Ca/P ratio of 1.62 or CaO for a Ca/P ratio of 1.72 were used as starting materials. Dense HA ceramics were obtained by sintering at 1200 oC for 2 h in air with under moisture protection. The sintered specimens were then placed into 40 ml of pH 7.4 distilled water. After immersing for certain period of time at 37 oC, crystal structure, weight loss and microstructure of the specimens were investigated. As increasing the immersion time, circular cavities similar to that normally attributed to osteoclast resorption lacunae were observed. As a result, it was found that the dissolution of HA along the grain boundary and subsequently microstructural disintegration was more distinct in 1.62 and 1.72 samples compared to pure HA.

In this work, tricalcium phosphate [TCP, β-Ca3(PO4)2]/titania composite were prepared with different ratio of 75/25, 50/50 and 25/75 (HA/TiO2, wt %). The TiO2 and hydroxyapatite (HA) powders, as starting materials, were synthesized by precipitation and hydrothermal methods, respectively. The sintered bodies of β-TCP/TiO2 composite were prepared by hot pressing at pressure of 30 MPa and temperature of 800-1000 oC for 30 min under the pressure of 30 MPa in N2 atmosphere. During the sintering process, hydroxyapatite was decomposed to β-TCP and CaTiO3 at elevated temperature because TiO2 could accelerate the decomposition of hydroxyapatite. The hot-pressed composite with 98% of sintered density, showed high value of 1080 Hv in hardness, compared with the pure hydroxyapatite (600 Hv) before immersion in distilled water. Increasing sintering temperature led densification of the composite with moderately uniform microstructures. As increasing the amount of TiO2, the surface of the composite was less damaged or dissolved.

Commercial hydroxyapatite (HA) powders were calcined at the temperature range of 1000-1350 °C in air and the calcined powders were immersed in simulated body fluid (SBF) at 37 °C for 3 or 7 days. At 1200°C, HA gradually releases its OH' ions and transforms into oxyhydroxyapatite (Ca 10 (PO 4 ) 6 O x (OH)2-2x, OHAP). HA initiated to decompose to a-tricalcium phosphate (a-TCP) and tetracalcium phosphate (TTCP) phase at 1350°C. The surface dissolution of HA powders was accelerated by non-stoichiometric composition such as a-TCP, TTCP and the powders with smooth surface appeared to be dissolved on the edge showing fiber-like particles, followed by separation of the large particle to small one with the immersion time. The fiber-like particles consisted of new phases such as, carbonated-apatite (CHA) and octacalcium phosphate (OCP).

CuAlNi shape memory alloy with Cu-13.5Al-4.5Ni(wt%) composition was prepared by cross-rolling method and the aging effect, phase transformation characteristics, microstructural variation were investigated. Transformation temperature was greatly increased in aged specimens at 250°C. Transformation temperature was not changed after the second reversed transformation, and Ms point was same in most specimens with third reversed transformation cycle. The variation of Ms point was not seen with aging at 100°C, but it was decreased with aging at 250°C. Transformation temperatures appear to be constant, to an measurable extent, in specimens prepared by both hotrolling and cross-rolling at 900°C. Plate shaped-specimen with the thickness of about 1mm was prepared by cross-rolling treatment at 350°C. The transformation temperatures did not change after the second transformation-reverse transformation cycling, and specially transformation start temperature was the same in most specimens experiencing third thermal cycle and thereafter. Undesirable tweed-like structure was observed in 250°C-aged specimen after a cross-rolling at 350°C. On aging the specimen prepared by cross-rolling, G.P zone was formed easier than that of γ2 phase. This phase was transformed to plate-like θ phase during aging.

In this study, it was demonstrated how second phases with small amount, which are hardly detected by XRD analysis, affect grain boundary dissolution and related mechanical properties of HA. All HA disks sintered at 1200 oC for 2 h in air with under moisture protection were phase pure and had Ca/P molar ratio of 1.67. Following certain period of exposure to the distilled water, the surface dissolution initiated at grain boundaries and particle loosening, subsequently resulting in decrease in mechanical properties of HA. In order to understand the dissolution mechanism, grain boundary structure of HA was identified by transmission electron microscopy (TEM) and high resolution TEM observation. From the analysis, it was found that the non-stoichiometric phase as α-tricalcium phosphate (TCP) transformed from β-TCP was existed at grain boundaries and caused surface dissolution of HA. From the XRD analysis, it was found that (211) and (112) planes of hydroxyapatite were susceptible to dissolution, whereas (300) plane was relatively stable.