• 한국세라믹학회지
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• 제41권3호
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• pp.202-209
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• 2004

침전법 및 솔젤법에 의하여 10- l5 nm 및 500 nm 크기의 구형 TiO$_2$ 분말을 제조하고 수열합성법으로 50-70 nm 및 120-250 nm 크기의 침상 hydroxyapatite(이하 HA라 표기) 입자를 각각 제조한 다음, 두 분말의 조성비를 달리한 세 종류(HA/TiO$_2$비; 75/25, 50/50, 25/75wt%)의 HA/TiO$_2$ 복합분말을 planetary 볼밀로 혼합하여 각각 제조하였다. 복합분말을 탄소몰드에 넣고 hot-press를 사용하여 가압소결로 치밀체를 제조하였는데, 가압도중 대부분의 HA가 tricalcium phosphate(이하 TCP라 표기)로 분해되면서 $\beta$-TCP/TiO$_2$ 복합체가 제조되었다. 제조된 복합체의 미세구조와 소결밀도는 복합분말의 형태와 조성에 따라 변화하였는데, 입자가 균질하게 분산되어 있는 미세구조를 갖는 복합분말을 소결한 경우, 치밀한 소결체를 얻을 수 있었으며, 소결온도가 증가할수록 균질한 미세구조를 나타내었다. 또한 복합분말 내 HA 함량이 증가하면서 소결체의 입자크기가 증가한 반면, 소결밀도가 감소하고, 미세구조는 불균질하였다. 반대로 HA분말에 비하여 TiO$_2$분말의 함량이 큰 시편은 전체적으로 작은 입자크기와 균질한 미세구조를 나타냈으며, 소결밀도 또한 증가하였다.

• 대한금속재료학회지
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• 제50권1호
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• pp.86-91
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• 2012

Ti-6Al-4V extra low interstitial (ELI) alloy has been widely used as an orthopedic implant material because of its excellent biocompatibility, corrosion resistance and mechanical properties. However, V-free titanium alloys such as Ti-6%Al-7%Nb and Ti-5%Al-2.5%Fe have recently been developed because of the toxicity of V. Hydroxyapatite (HA) is used as a coating material on Ti or Ti biomaterials due to its good biocompatibility. However, HA coated on Ti alloy causes a problem for tissue by peeling off during usage. Therefore, such peeling off during long time usage can be suppressed by adding HA in Ti or Ti alloy composites. The aim of this study was to manufacture an ultra fine grained (UFG) Ti-Nb-HA bulk alloy, which is usually difficult to fabricate using melting and casting technology, by rapid sintering process using high energy mechanical milled (HEMM) powder.

• 대한금속재료학회지
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• 제47권8호
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• pp.508-515
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• 2009

Ti-6Al-4V biomaterial is widely used as a bone alternative. However, Ti-6Al-4V ELI alloy suffers from numerous problems such as a high elastic modulus and high toxicity. Therefore, non-toxic biomaterials with low elastic moduli need to be developed. Ti-HA(hydroxyapatite) composites were fabricated in the present work by pulsed current activated sintering (PCAS) at $1000^{\circ}C$ under 60 MPa using mixed Ti and HA powders. The effects of HA content on the physical and mechanical properties of the sintered Ti-HA composites have been investigated. X-ray diffraction(XRD) analysis of the Ti-HA composites, including Ti-40 wt%HA in particular, revealed new phases, $Ti_{2}O$, CaO, $CaTiO_3$, and TixPy, formed by chemical reactions between Ti and HA during sintering. The hardness of the Ti-HA composites decreased with an increase in HA content. The corrosion resistance of these composites was observed to be an excellent candidate as a commercial Ti-6Al-4 V ELI alloy. A Ti-5 wt%HA composite fabricated by PCAS is recommended as a new biomaterial, because it offers good corrosion resistance, compressive strength, wear resistance, and biocompatibility, and a low Young's modulus.

• 한국분말재료학회지
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• 제17권6호
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• pp.443-448
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• 2010

The $\beta$ phase Ti-Nb-Sn-HA bio materials were successfully fabricated by high energy mechanical milling and pulse current activated sintering (PCAS). Ti-6Al-4V ELI alloy has been widely used as biomaterial. But the Al has been inducing Alzheimer disease and V is classified as toxic element. In this study, ultra fine sized Ti-Nb-Sn-HA powder was produced by high energy mechanical milling machine. The $\beta$ phase Ti-Nb-Sn-HA powders were obtained after 12hr milling from $\alpha$ phase. And ultra fine grain sized Ti-Nb-Sn-HA composites could be fabricated using PCAS without grain growth. After sintering, the microstructures and phase-transformation of Ti-Nb-Sn-HA biomaterials were analyzed by scanning electron microscope (SEM) and X-ray diffraction (XRD). The relative density was obtained by Archimedes principle and the hardness was measured by Vickers hardness tester. The $\beta$-Ti phase was obtained after 12h milling. As result of hardness and relative density, 12h milled Ti-Nb-Sn-HA composite has the highest values.

• 한국재료학회지
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• 제23권7호
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• pp.353-358
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• 2013

To improve coating ability and the life of the coating, Ti based composite materials with hydroxyapatite(HA) should be developed. The raw materials of Ti-26wt%, Nb-1wt%, and Si with 10wt% HA were mixed for 24 h by a mixing machine and milled for 1 h to 6 h by planetary mechanical ball milling. Ti-26%Nb-1%Si-(10%HA) composites, composed of nontoxic elements, were fabricated successfully by spark plasma sintering(SPS) at $1000^{\circ}C$ under 70MPa. The relative density of the sintered Ti-Nb-Si-HA composites using the 24 h mixed powder, and the 6 h milled powder, was 91% and 97 %, respectively. The effects of HA contents and milling time on microstructure and mechanical properties were investigated by SEM and hardness tester, respectively. The Vickers hardness of the composites increased with increasing milling time and higher HA content. The Young's modulus of the sintered Ti-26%Nb-1%Si-10%HA composite using the 6 h-milled powder was 55.6 GPa, as obtained by compression test. Corrosion resistance of the Ti-26wt%Nb-1wt%Si composite was increased by milling and by the addition of 10wt%HA. Wear resistance was improved with increasing milling time. Biocompatibility of the Ti-Nb-Si alloys was improved by the addition of HA.

• 한국표면공학회지
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• 제41권2호
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• pp.57-62
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• 2008

Electrochemical properties of Ti-30Ta-$(3{\sim}15)$Nb alloys coated by HA/Ti compound layer have been studied by various electrochemical method. Ti-30Ta binary alloys contained 3, 7, 10, and 15 wt% Nb contents were manufactured by the vacuum furnace system. The specimens were homogenized for 24 hrs at $1000^{\circ}C$. The samples were cut and polished for corrosion test and coating. It was coated with HA/Ti compound layer by magnetron sputter. The HA/Ti non-coated and coated morphology of Ti alloy were analyzed by x-ray diffractometer(XRD) and filed emission scanning electron microscope(FE-SEM). The corrosion behaviors were investigated using potentiodynamic method in 0.9% NaCl solution at $36.5{\pm}1^{\circ}C$. The homoginazed Ti-30Ta-$(3{\sim}15wt%$)Nb alloys showed the ${\alpha}+{\beta}$ phase, and ${\beta}$ phase peak was predominantly appeared with increasing Nb content. The microstructure of Ti alloy was transformed from needle-like structure to equiaxed structure as Nb content increased. HA/Ti composite surface showed uniform coating layer with 750 nm thickness. The corrosion resistance of HA/Ti composite coated Ti-alloys were higher than those of the non-coated samples in 0.9% NaCl solution at $36.5{\pm}1^{\circ}C$. Especially, corrosion resistance of Ti-Ta-Nb system increased as Nb content increased.

• 한국표면공학회지
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• 제41권5호
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• pp.181-188
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• 2008

A.C. impedance properties of HA/Ti compound layer coated Ti-30Ta-($3{\sim}15$)Nb alloys have been studied by electrochemical method. Ti-30Ta binary alloys contained 3, 7, 10 and 15 wt% Nb were manufactured by the vacuum furnace system. And then specimen was homogenized at $1000^{\circ}C$ for 24 hrs. The sample was cut and polished for corrosion test and coating. It was coated with HA/Ti compound layer by magnetron sputter. The non-coated and coated morphology of Ti alloy were analyzed by X-ray diffractometer (XRD), energy X-ray dispersive spectroscopy (EDX) and filed emission scanning electron microscope (FE-SEM). The corrosion behaviors were investigated using A.C. impedance test (PARSTAT 2273, USA) in 0.9% NaCl solution at $36.5{\pm}1^{\circ}C$. Ti-30Ta-($3{\sim}15\;wt%$)Nb alloys showed the ${\alpha}+{\beta}$ phase, and $\beta$ phase peak was predominantly appeared in the case of increasingly Nb contents. The microstructures of Ti alloy were transformed from needle-like structure to equiaxed structure as Nb content increased. From the analysis of coating surface, HA/Ti composite surface uniformed coating layer with 750 nm thickness. The growth directions of film were (211), (112), (300) and (202) for HA/Ti composite coating on the surface after heat treatment at $550^{\circ}C$, whereas, the growth direction of film was (110) for Ti coating. The polarization resistance ($R_p$) of HA/Ti composite coated Ti-alloys were higher than those of the Ti and HA coated samples in 0.9% NaCl solution at $36.5{\pm}1^{\circ}C$. Especially, corrosion resistance of Ti-Ta-Nb system increased as Nb content increased.

• 한국결정성장학회지
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• 제14권3호
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• pp.83-89
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• 2004

본 연구에서는 우수한 생체적합성과 높은 기계적 성질을 갖는 아파타이트 생체세라믹스를 제조하기 위하여 수산화아파타이트(HA, $Ca_{10}(PO_4)_6(OH)_2/TiO_2$ 생체복합분말을 제조하였다. HA/$TiO_2$ 생체복합분말은 침전법과 졸겔법으로 각각 제조된 $TiO_2$ 분말과 수열합성법으로 제조된 HA 분말을 1:1의 무게분율로 혼합하여 제조하였다. HA/$TiO_2$ 생체복합분말은 $TiO_2$와 HA 입자의 크기와 모양에 따라 미세구조의 차이를 나타냈으며, $TiO_2$와 HA의 입자 크기가 서로 다른 복합분말의 경우, 작은 입자는 큰 입자의 표면에 둘러싸고 있었으나, $TiO_2$와 HA의 입자 크기가 비슷한 복합분말의 경우, $TiO_2$와 HA 입자가 서로 분산되어 균일한 미세구조를 가지고 있었다 균질한 미세구조를 갖는 복합분말은 소결체 제조 시 높은-소결밀도와 우수한 기계적 특성을 나타내었다.

• 한국분말재료학회지
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• 제16권5호
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• pp.310-315
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• 2009

Ultra-fine TiC/Co composite powder was synthesized by the carbothermal reduction process without wet chemical processing. The starting powder was prepared by milling of titanium dioxide and cobalt oxalate powders followed by subsequent calcination to have a target composition of TiC-15 wt.%Co. The prepared oxide powder was mixed again with carbon black, and this mixture was then heat-treated under flowing argon atmosphere. The changes in the phase, mass and particle size of the mixture during heat treatment were investigated using XRD, TG-DTA and SEM. The synthesized oxide powder after heat treatment at 700$^{\circ}C$ has a mixed phase of TiO$_2$ and CoTiO$_3$ phases. This composite oxide powder was carbothermally reduced to TiC/Co composite powder by the solid carbon. The synthesized TiC/Co composite powder at 1300$^{\circ}C$ for 9 hours has particle size of under about 0.4 $\mu$m.

• 한국세라믹학회지
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• 제45권10호
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• pp.610-617
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• 2008

Multi-walled carbon nanotube(CNT) reinforced hydroxyapatite composite coating with a thickness of $5{\mu}m$ has been successfully deposited on Ti substrate using aerosol deposition(AD). The coating had a dense microstructure with no cracks or pores, showing good adhesion with the Ti substrate. Microstructural observation using field-emission scanning electron microscopy(FE-SEM) and transmission electron microscopy(TEM) showed that CNTs with original tubular morphology were found in the hydroxyapatite-CNT(HA-CNT) composite coating. Measurements of hardness and elastic modulus for the coating were performed by nanoindentation tests, indicating that the mechanical properties of the coating were remarkably improved by the addition of CNT to HA coating. Therefore, HA-CNT composite coating produced by AD is expected to be potentially applied to the coating for high load bearing implants.