• 한국재료학회:학술대회논문집
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• 한국재료학회 2011년도 추계학술발표대회
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• pp.36.2-36.2
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• 2011

Titanium and its alloys have been widely used for orthopedic implants because of their good biocompatibility. We have previously shown that the crystalline titania layers formed on the surface of titanium metal via anodic oxidation can induce apatite formation in simulated body fluid, whereas amorphous titania layers do not possess apatite-forming ability. In this study, hot water and heat treatments were applied to transform the titania layers from an amorphous structure into a crystalline structure after titanium metal had been anodized in acetic acid solution. The apatite-forming ability of titania layers subjected to the above treatments in simulated body fluid was investigated. The XRD and SEM results indicated hot water and/or heat treatment could greatly transform the crystal structure of titania layers from an amorphous structure into anatase, or a mixture of anatase and rutile.The abundance of Ti-OH groups formed by hot water treatment could contribute to apatite formation on the surface of titanium metals, and subsequent heat treatment would enhance the bond strength between the apatite layers and the titanium substrates. Thus, bioactive titanium metals could be prepared via anodic oxidation and subsequent hot water and heat treatment that would be suitable for applications under load-bearing conditions.

• 한국재료학회지
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• 제15권10호
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• pp.671-677
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• 2005

Ti and Ti alloys are known to have excellent corrosion properties, which is an important aspect for biocompability of these implants in human body. In our study, four types of samples (Cp-Ti, Ti-6Al-4V, $0.5wt.\%$ Fe-Ti and ECAP Ti) were tested for their apatite forming ability and corrosion properties. The micropolished samples were treated with 5M NaOH solution at $60^{\circ}C$ for 24 hours. Each samples was gently washed with distilled water and heat-treated at 600"C for 1 hour. The heat-treated samples were soaked in Simulated Body Fluid (SBF) solution at $36.5^{\circ}C$ in an incubator for different period of time. The test revealed that $0.5 wt.\%$ Fe-Ti showing faster apatite growth on the surface (7th day) compared to other samples. Polarization curve test (PCT) was also carried out to determine the corrosion resistance of each samples in SBF solution. ECAP-Ti showed highest corrosion resistance compared to any other samples. $0.5wt.\%Fe-Ti$ showed higher corrosion potential and corrosion current compared to other samples.

• 한국재료학회:학술대회논문집
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• 한국재료학회 2004년도 춘계학술발표대회 및 제6회 신소재 심포지엄
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• pp.48-48
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• 2004

• 한국재료학회지
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• 제19권7호
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• pp.362-368
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• 2009

Ti scaffolds with a three-dimensional porous structure were successfully fabricated using powder metallurgy and modified rapid prototyping (RP) process. The fabricated Ti scaffolds showed a highly porous structure with interconnected pores. The porosity and pore size of the scaffolds were in the range of 66$\sim$72% and $300\sim400\;\mu$m, respectively. The sintering of the fabricated scaffolds under the vacuum caused the Ti particles to bond to each other. The strength of the scaffolds depended on the layering patterns. The compressive strength of the scaffolds ranged from 15 MPa to 52 MPa according to the scaffolds' architecture. The alkali treatment of the fabricated scaffolds in an aqueous NaOH solution was shown to be effective in improving the bioactivity. The surface of the alkali-treated Ti scaffolds had a nano-sized fibre-like structure. The modified surface showed a good apatite forming ability. The apatite was formed on the surface of the alkali treated Ti scaffolds within 1 day. The thickness of the apatite increased when the soaking time in a simulated body fluid (SBF) solution increased. It is expected that the surface modification of Ti scaffolds by alkali treatment could be effective in forming apatites in vivo and can subsequently enhance bone formation.

• 한국결정성장학회지
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• 제8권1호
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• pp.169-178
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• 1998

CaO-$SiO_2-P_2O_5$ 3성분계 유리화 영역(glass forning region)내의 여러조성(A:$SiO_2$- rich조성, B:CaO-rich조성, C:$P_2O_5$-rich조성, D, E:A, B, C의 중간조성)을 가지는 유리분말을 결정화시켰을 때 유리중에 석출되는 결정상(crystal phase)을 분말 XRD로 확인하였다. 여러조성중 apatite(($Ca_{10}(PO_4)_6O$)와 $\beta$-wollastonite($CaSiO_3$)결정이 석출되고, 굽힘강도가 우수한 E조성(CaO 49.4, $SiO_2\;36.8,\;P_2O_5$8.8wt%)을 선택하여 이 조성의 유리분말을 일방향으로 결정화 소결하였다. 제조된 결정화 소결체에 대하여 charaterization을 하고 굽힘강도를 측정하였다. 또한 결정화 소결체와 생체뼈와의 결합성을 조사하기 위하여 유사체액(simulated body fluid)내에서 침적실험을 하였으며, 결정화 소결체의 표면을 thin-film XRD, FT-IR로 분석하였다. 실험결과, apatite와 wollastonite 결정이 석출된 치밀한 결정화 소결체가 얻어졌으며, 이들 결정은 wollastonite 결정의 (202)면이 인상방향에 수직으로 성장하는 경향을 보였다. 또한 제조된 결정화 소결체는 평균 186.9MPa의 굽힘강도를 나타내어 일반적 방법으로 제조되는 결정화 소결체보다 높은 역학적 성질을 보였다. 유사체액내의 침적실험결과, 시료표면위에 apatite 결정층이 3일후부터 형성되어 생체뼈와 화학결합을 이룰 가능성이 있음을 알았다.

• 한국재료학회지
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• 제24권12호
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• pp.671-676
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• 2014

It is known that bones get damaged by accidents and aging. Since the discovery of Bioglass, various kinds of ceramics have been also found to bond to living bone; some of these ceramics are already being clinically used as bone-repairing materials. In the present study, antibacterial calcium silicate gel ($Ag-30CaO{\cdot}70SiO_2$ gel) was prepared by sol-gel method in order to control the microstructure, which is related to the dissolution rate and induction period of apatite formation in body environment. In addition, biological $Ag-30CaO{\cdot}70SiO_2$ is tested. This was done to impart antimicrobial activity to the $30CaO{\cdot}70SiO_2$. Ag ion was added during sol-gel synthesis to replace the $H_2O$ added during the making of the $30CaO{\cdot}70SiO_2$ gel, which has silver solutions of various concentration. After the sol-gel process, 1N-$HNO_3$ solution was used to wash the gel when synthesizing the gel, in order to maintain the porous structure and remove PEG, water soluble polymers. Then, the apatite forming ability of the sol-gel derived CaO-$SiO_2$ gels was investigated using simulated body fluid (SBF), which had almost the same ion concentration as that of human blood plasma. The gels were analyzed by FT-IR spectroscopy, SEM observation, XRD, and fluorescent microscopy. The apatite was successfully created even after washing the gel; apatite is present in an amorphous state, and was found to affect the concentration of the Ag ion in cells in MC3T3 live & dead assay results. From these results, it is suggested that a good material that can be used to repair defects of nature bone is $Ag-30CaO{\cdot}70SiO_2$ gel.

• 공학논문집
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• 제6권2호
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• pp.23-32
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• 2004

현재까지 사용되어가지고 있는 임플란트 재료 중 commercially pure titanium (순수티탄; Cp-Ti)과 Ti-alloy들은 생체재료로 폭넓게 사용되어지고 있는데, Ti 금속들은 경도가 강하고 점도가 높기 때문에, 치과나 정형외과 등의 하중에 잘 견디는 곳에 이용되어지고 있다고 한다. 이것들은 생체적합성과 부식에 대한 저항성도 좋은 것으로 알려져 있다. 일반적으로 Ti은 4종류의 Grade로 강도의 차이에 의하여 분류되고 Ti의 강도에 영향을 미치는 것으로는 산소, 철, 질소등이 있다. 따라서 본 연구에서는 O와 Fe의 함량을 달리한 Ti alloy시편을 사용하여 생체적합성 실험을 하였다. 먼저 실험은 시편을 micropolishing하고 5M NaOH에서 $60^{\circ}C$에서24시간 처리하여서 비표면적을 넓혔으며, 표면의 $TiO_2$을 만들어주기 위하여 $600^{\circ}C$에서 열처리하였다. 그런 시편을 $36.5^{\circ}C$의 SBF에 넣어 1~14일까지 침적한 후에 표면에 형성된 apatite를 SEM과 EDAX로 조사하였다. 조사 결과 모든 시편에서 apatite가 생성되었지만, 시편의 조성에 따라서 apatite의 형성양이 다름을 확인하였다.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2016년도 추계학술대회 논문집
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• pp.198-198
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• 2016

An ideal orthopedic implant should provide an excellent bone-implant connection, less implant loosening and minimum adverse reactions. Commercial pure titanium (CP-Ti) and Ti alloys have been widely utilized for biomedical applications such as orthopedic and dental implants. However, being bioinert, the integration of such implant in bone was not in good condition to achieve improved osseointegraiton, there have been many efforts to modify the composition and topography of implant surface. These processes are generally classified as physical, chemical, and electrochemical methods. Plasma electrolytic oxidation (PEO) as an electrochemical route has been recently utilized to produce this kind of composite coatings. Mg ion plays a key role in bone metabolism, since it influences osteoblast and osteoclast activity. From previous studies, it has been found that Mg ions improve the bone formation on Ti alloys. PEO is a promising technology to produce porous and firmly adherent inorganic Mg containing $TiO_2$($Mg-TiO_2$ ) coatings on Ti surface, and the amount of Mg introduced into the coatings can be optimized by altering the electrolyte composition. In this study, a series of $Mg-TiO_2$ coatings are produced on Ti-6Al-4V ELI dental implant using PEO, with the substitution degree, respectively, at 0, 5, 10 and 20%. Based on the preliminary analysis of the coating structure, composition and morphology, a bone like apatite formation model is used to evaluate the in vitro biological responses at the bone-implant interface. The enhancement of the bone like apatite forming ability arises from $Mg-TiO_2$ surface, which has formed the reduction of the Mg ions. The promising results successfully demonstrate the immense potential of $Mg-TiO_2$ coatings in dental and biomaterials applications.

• 한국재료학회:학술대회논문집
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• 한국재료학회 2009년도 춘계학술발표대회
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• pp.45.1-45.1
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• 2009

In this study, we investigated a calcium phosphate-calcium sulfate injectable bone substitute (IBS) with organic reinforcement of chitosan, citric acid and hydroxypropyl-methyl-cellulose (HPMC). The powder component of IBS consisted of tetra calcium phosphate (TTCP), dicalcium phosphate dihydrate (DCPD) and calcium sulfate dihydrate (CSD). The liquid component was a solution of citric acid and chitosan. The effect of HPMC in terms of setting time, compressive strength and apatite forming ability on this IBS was investigated. The mass content of HPMC in liquid phase was varied in array of 0%, 2%, 3% and 4%. The setting times obtained between 20 and 45 minutes. Compressive strength was achieved over 20 MPa after incubation at 370C and in 100% humidity for 28 days. Porosities were evaluated in relation with compressive strength. Elastic moduli of the 28 days after-incubation IBS were obtained around 4GPa

• Corrosion Science and Technology
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• 제15권3호
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• pp.120-124
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• 2016

The effect of alloying element Ca (0, 1, and 2 wt%) on corrosion resistance and bioactivity of the as-received and anodized surface of rolled plate AM60 alloys was investigated. A plasma electrolytic oxidation (PEO) was carried out to form anodic oxide film in $0.5mol\;dm^{-3}\;Na_3PO_4$ solution. The corrosion behavior was studied by polarization measurements while the in vitro bioactivity was tested by soaking the specimens in Simulated Body Fluid (1.5xSBF). Optical micrograph and elemental analysis of the substrate surfaces indicated that the number of intermetallic particles increased with Ca content in the alloys owing to the formation of a new phase $Al_2Ca$. The corrosion resistance of AM60 specimens improved only slightly by alloying with 2 wt% Ca which was attributed to the reticular distribution of $Al_2Ca$ phase existed in the alloy that might became barrier for corrosion propagation across grain boundaries. Corrosion resistance of the three alloys was significantly improved by coating the substrates with anodic oxide film formed by PEO. The film mainly composed of magnesium phosphate with thickness in the range $30-40{\mu}m$. The heat resistant phase of $Al_2Ca$ was believed to retard the plasma discharge during anodization and, hence, decreased the film thickness of Ca-containing alloys. The highest apatite forming ability in 1.5xSBF was observed for AM60-1Ca specimens (both substrate and anodized) that exhibited more degradation than the other two alloys as indicated by surface observation. The increase of surface roughness and the degree of supersaturation of 1.5xSBF due to dissolution of Mg ions from the substrate surface or the release of film compounds from the anodized surface are important factors to enhance deposition of Ca-P compound on the specimen surfaces.