• Journal of the Korean Ceramic Society
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• v.40 no.12
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• pp.1154-1158
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• 2003

Hydrothermal deposition of hydroxyapatite coatings on $Al_2$O$_3$ substrates was studied using aqueous solutions of Ca(NO$_3$)$_2$ㆍ4$H_2O$ and (NH$_4$)$_2$HPO$_4$ containing EDTA disodium salt as a chelating agent for $Ca^{2+}$. For the precipitation of the coatings the EDTA-Ca$^{2+}$ chelates were dissociated thermally at 20$0^{\circ}C$ or decomposed by oxidation with $H_2O$$_2$ at 9$0^{\circ}C$. Scanning electron microscopy and X-ray diffraction were used to investigate the deposition behavior and the phase of the coatings. Hydroxyapatite coatings were not deposited with the thermal dissociation method, whereas uniform deposition of the coatings (about 0.7 $\mu\textrm{m}$ thickness) was obtained with the oxidative decomposition method. The coatings consisted of fine rod-like hydroxyapatite crystals (hexagonal structure) with 60-80 nm diameters, having some preferred orientation with their length (i.e., the c axis) perpendicular to the substrate.ate.

• Journal of the Korean Society for Heat Treatment
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• v.28 no.1
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• pp.17-23
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• 2015

Hydroxyapatite coatings were fabricated by a room temperature spray method on zirconia substrates and the influence of heat-treatment on their microstructure was also investigated. Phase composition of coated hydroxyapatite films was similar to the starting powder, but the grain size of hydroxyapatite particles was reduced to the size of nano-scale about 100 nm. Grain size, particle compactness, and adhesiveness to zirconia of hydroxyapatite coatings were increased with heat-treatment temperature, but some of cracks by heat-treatment above $1100^{\circ}C$ were initiated between hydroxyapatite coatings and zirconia substrate. Heat-treated hydroxyapatite layers show the dissolution in SBF solution for 5 days. Hydroxyapatite-coated specimen heat-treated at $1100^{\circ}C$ for 1 h has a good biocompatibility, which specimen induced the nanocrystalline hydroxyapatite precipitates on the coating surface by the immersion in SBF solution for 5 days.

• Proceedings of the Materials Research Society of Korea Conference
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• 2012.05a
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• pp.102.2-102.2
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• 2012

Different layers of zirconium nitride (ZrN) and hydroxyapatite (HA) coatings were prepared on cp Ti substrate for biomedical applications. The main idea is to improve the mechanical strength as well as the biocompatibility of the coating. ZrN is known for its high mechanical strength, corrosion resistance. HA is well known for its biocompatibility properties. Hence, in this study, both materials were coated on a cp Ti substrate with bottom layer with ZrN for good bonding with substrate and the top layer with HA for induce bioactivity. Middle layer was formed by a composite of HA and ZrN. Detail analyses of the layered coatings for its structural, morphological, topographical properties were carried out. Then the mechanical property of the layered coatings was analyzed by nanoindentation. Biomimetic growths of apatite on the functionally graded coatings were determined by simulated body fluid method. This study provides promising results to use this kind of coatings in biomedical field.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2003.10a
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• pp.59-59
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• 2003

In recent, various functional coatings on artificial tooth implants have been conducted to enhance the bonding strength between implants and bones. Despite of these efforts, some previous reports argued that an adhesion strength between titanium implant and the final coatings like hydroxyapatite(HA) is weaker than the strength between coating and bone. In order to increase the adhesion force between the final coating and implant surface, TiN/DLC based functionally graded coating, which has higher mechanical strength than the titanium implant, was applied as a middle layer between titanium implant and final coating. Particularly we finally coated a biocompatible hydroxyapatite film on the DLC layer and examined the mechanical properties. As a result, TiN/DLC based functionally graded coating showed the higher adhesion strength compared with hydroxyapatite single layer coating on the titanium implant.

• Journal of the Korean Ceramic Society
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• v.43 no.8 s.291
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• pp.463-468
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• 2006

Hydrothermal deposition of hydroxyapatite coatings on two types of $ZrO_2$ substrates (3 mol% $Y_2O_3$-doped and 13 mol% $CeO_2$-doped tetragonal $ZrO_2s$) was studied using aqueous solutions of $Ca(NO_3)_2\;4H_2O$ and $(NH_4)_2HPO_4$ containing EDTA (ethylene diamine tetra acetic acid) disodium salt as a chelating agent for $Ca^{2+}$ ions. For the precipitation of the coatings, the $EDTA-Ca^{2+}$ chelates were decomposed by oxidation with $H_2O_2$ at $90^{\circ}C$. The deposition behavior, morphology, and orientation of the coatings were investigated while varying the solution pH using scanning electron microscopy and X-ray diffractometry. For the two sub-strates, sparse deposition of the coating was obtained at pH 5.5, whereas a uniform deposition was obtained at pH 7.1, 9.8, and 11.4 with a denser microstructure for the higher pH. The coating consisted of thin needle-like or plate-like crystals ($1-2{\mu}m$ length or diameter) at pH 7.1, but fine rod-like crystals ($1-2{\mu}m$ length, $0.1{\mu}m$ diameter) at pH 9.8 and 11.4. The coatings were $1-3{\mu}m$ thick and showed a preferred orientation of the hydroxyapatite crystals with their c axis (i.e., the elongated direction) perpendicular to the substrate surface especially for pH 9.8 and 11.4.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2017.05a
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• pp.79-79
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• 2017

Metallic biomaterials have been mainly used for the fabrication of medical devices for the replacement of hard tissue such as artificial hip joints, bone plates, and dental implants. Because they are very reliable on the viewpoint of mechanical performance. This trend is expected to continue. Especially, Ti and Ti alloys are bioinert. So, they do not chemically bond to the bone, whereas they physically bond with bone tissue. For their poor surface biocompatibility, the surface of Ti alloys has to be modified to improve the surface osteoinductivity. Recently, ceramic-like coatings on titanium, produced by plasma electrolytic oxidation (PEO), have been developed with calciumand phosphorus-enriched surfaces. A lso included the influences of coatings, which can accelerate healing and cell integration, as well as improve tribological properties. However, the adhesions of these coatings to the Ti surface need to be improved for clinical use. Particularly Silicon (Si) has been found to be essential for normal bone, cartilage growth and development. This hydroxyapatite, modified with the inclusion of small concentrations of silicon has been demonstrating to improve the osteoblast proliferation and the bone extracellular matrix production. Strontium-containing hydroxyapatite (Sr-HA) was designed as a filling material to improve the biocompatibility of bone cement. In vitro, the presence of strontium in the coating enhances osteoblast activity and differentiation, whereas it inhibits osteoclast production and proliferation. The objective of this work was to study Morphology of bone-like apatite formation on Sr and Si-doped hydroxyapatite surface of Ti-6Al-4V alloy after plasma electrolytic oxidation. Anodized alloys was prepared at 270V~300V voltages with various concentrations of Si and Sr ions. Bone-like apatite formation was carried out in SBF solution. The morphology of PEO, phase and composition of oxide surface of Ti-6Al-4V alloys were examined by FE-SEM, EDS, and XRD.

• Korean Journal of Metals and Materials
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• v.47 no.1
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• pp.13-20
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• 2009

This work presents functionally graded coatings (FGC) of hydroxyapatite (HA) and metallic powders on Ti-6Al-4V implants using plasma spray coating method. HA has been the most frequently used coating material due to its excellent compatibility with human bones. However, because of the abrupt changes in thermomechanical properties between HA and the metallic implant across an interface, and residual stress induced on cooling from coating temperture to room temperature, debonding at the interface occurs in use sometimes. In this work, FGC of HA and Ti or Ti-alloy powders is made to mitigate the abrupt property changes at the interface and the effect of FGC on residual stress release is investigated by evaluating the mechanical bond strength between the implant and the HA coating layers. Thermal annealing is done after coating in order to crystallize the HA coating layer which tends to have amorphous structure during thermal spray coating. The effects of types and compositional ratio of metallic powders in FGC and annealing conditions on the bond strength are also evaluated by strength tests and the microstructure analysis of coating layers and interfaces. Finally, biocompatibility of the coating layers are tested under ISO 10993-5.

• Journal of the Korean Ceramic Society
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• v.36 no.10
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• pp.1087-1093
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• 1999

Bioglass which is one of the surface active bionmaterials has a good biocompatibility but a poor mechanical strength, In the present work therefore two types of fluoride-containing bioglasses were coated on an alumina to improve mechanical strength. Crystallization of the coating layer and the hydroxyapatite formation on the bioactive glass coatings in tris-buffer solution were studied. When bioactive glass coated alumina was heat-treated Na2CaSi3O8 crystal was formed on the layer at lower temperature while wollastonite(CaSIO3) was obtained at higher temperature. Hydroxyapatite forming rate on the coating layer with Na2CaSi3O8 crystal was delayed with SiO2 contents in glass composition. However the hydroxyapatite was developed in 20minutes regardless SiO2 contents when the coating layer crystallized into wollastonite. More amount of P3+ ions were leached out of the coating layer with wollastonite than that with Na2CaSi3O8 crystal while Na+ and Ca2+ ions were leached out more easily from the Na2CaSi3O8 crystal containing coating layer.

• Journal of Technologic Dentistry
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• v.26 no.1
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• pp.139-144
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• 2004

In the present study, a simple method was successfully used for hydroxyapatite coatings on Ti-6Al-4V substrates deposited by using a sol-gel derived precursor. Prior to hydroxyapatite coating the samples were micropolished (0.1 micron) and divided into three sets. The first set,were the micropolished samples kept as such. The second set were coated with titania sol and the third set was treated with 5M NaOH. After three repetitions of hydroxyapatite coating procedures on each set and heat treatment at 600 $^{\circ}\Delta C$, the formation of hydroxyapatite has been confirmed by XRD analyses and the substrate material was found to be oxidized with negligible amount of CaO in the coating. The SEM studies revealed surface morphology. Hydroxyapatite, calcined at 600$^{\circ}\Delta C$, displaying a porous structure arisen from heating of the bulk. But, it is very meaningful in trying to approach morale management plans with an object of dental technicians. It is necessary that dental technicians should make efforts to control themselves.

• Journal of the Korean institute of surface engineering
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• v.32 no.3
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• pp.307-311
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• 1999

The well-crystalline hydroxyapatite($Ca_{10}(PO_4)_6(OH)_2$ ; HAp) layer having a biocompatibility was successfully coated onto titanium substrate using a radio-frequency magnetron sputtering, and effects of sputtering gas and the thickness of HAp film on a crystal growth of the HAp layers were investigated. The deposition rate of the layer sputtered with water-vapour gas was slower than that of the layer sputtered with argon gas. The results of X-ray diffraction demonstrated that the about $0.8\mu\textrm{m}$ thick HAp film under water-vapour gas was an amorphous phase, the about $1.2\mu\textrm{m}$ thick film was (100) plane-oriented HAp, and the about $1.5\mu\textrm{m}$ thick film was (001)plane-oriented HAp. FT-IR analysis proved that hydroxyl group of the layer sputtered with argon gas was defected, but that of the layer sputtered with water-vapour gas was not defected. From these results, it was favorable to use water-vapour gas on the HAp coatings onto metal surface.