양극산화와 열산화 처리로 형성된 티타늄 산화막의 표면 특성과 생체활성에 관한 연구 (A Sudy on Surface Charateristics and Bioactivity of Titanium Oxide film Formed by Anodization and thermal Oxidization Techniques)

서지정보

· 발행기관 : 대한치과재료학회
· 수록지 정보 : 대한치과재료학회지 / 31권 / 4호 / 255 ~ 265페이지
· 저자명 : 박영준, 송호준, 이용렬

초록

The purpose of this study was to evaluate the surface characteristics of titanium oxide films formed by anodization and thermal oxidation techniques, and to investigate its effects on formation of calcium phosphate. As experimental specimen groups, naturally oxidized film (AS-R), thin anodic oxidation film (ANO-L), thick anodic oxidation film (ANO-H) treated up to dielectric breakdown voltage, and thermal oxidation films of TH-L and TH-H treated at 530℃ and 800℃ in the air, respectively, were prepared.
Surface characterization was performed using field emission-scanning electron microscopy (FE-SEM), X-ray diffractometry (XRD), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS) in order to evaluate the micro-morphology, crystalline structure, chemical composition, and binding structure of the oxide films. Bioactivity of specimen groups was investigated by evaluating the degree of calcium phosphate formation after immersing the samples in MEM for 7 days.
The results were as follows: 1. Nanometer sized granular oxide particles were distributed on the surface of TH-L samples and sub-micrometer sized large crystallites were formed on TH-H samples. Irregularly shaped oxides were observed in ANO-L, and homogeneously porous oxide film having average pore size of about 0.5 ㎛ was formed in ANO-H.
2. Titanium oxide films having anatase crystalline structure were formed on ANO-L and TH-L sample surfaces. However, the preferred orientation crystal planes of ANO-L and TH-L were different to be (101) and (004) plane, respectively. Rutile crystalline structure was dominantly shown on TH-H sample, and anatase and rutile crystals were co-existed on ANO-H sample surfaces.
3. The amounts of hydroxyl group, which is related to the bioactivity of titanium implant, were higher in thermally treated specimen groups than in other groups. This result was analyzed to have close relation to the preferred orientation crystal plane and surface area of oxide films. The content of hydroxyl group increased as the density of surface titanium atoms increased, and that was least in specimen group having rutile and anatase crystalline structure in coexistence.
4. Immersion test in MEM showed that the capacity of calcium phosphate formation was dependent on total content of hydroxyl group and surface morphology of titanium oxides.

영어초록

The purpose of this study was to evaluate the surface characteristics of titanium oxide films formed by anodization and thermal oxidation techniques, and to investigate its effects on formation of calcium phosphate. As experimental specimen groups, naturally oxidized film (AS-R), thin anodic oxidation film (ANO-L), thick anodic oxidation film (ANO-H) treated up to dielectric breakdown voltage, and thermal oxidation films of TH-L and TH-H treated at 530℃ and 800℃ in the air, respectively, were prepared.
Surface characterization was performed using field emission-scanning electron microscopy (FE-SEM), X-ray diffractometry (XRD), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS) in order to evaluate the micro-morphology, crystalline structure, chemical composition, and binding structure of the oxide films. Bioactivity of specimen groups was investigated by evaluating the degree of calcium phosphate formation after immersing the samples in MEM for 7 days.
The results were as follows: 1. Nanometer sized granular oxide particles were distributed on the surface of TH-L samples and sub-micrometer sized large crystallites were formed on TH-H samples. Irregularly shaped oxides were observed in ANO-L, and homogeneously porous oxide film having average pore size of about 0.5 ㎛ was formed in ANO-H.
2. Titanium oxide films having anatase crystalline structure were formed on ANO-L and TH-L sample surfaces. However, the preferred orientation crystal planes of ANO-L and TH-L were different to be (101) and (004) plane, respectively. Rutile crystalline structure was dominantly shown on TH-H sample, and anatase and rutile crystals were co-existed on ANO-H sample surfaces.
3. The amounts of hydroxyl group, which is related to the bioactivity of titanium implant, were higher in thermally treated specimen groups than in other groups. This result was analyzed to have close relation to the preferred orientation crystal plane and surface area of oxide films. The content of hydroxyl group increased as the density of surface titanium atoms increased, and that was least in specimen group having rutile and anatase crystalline structure in coexistence.
4. Immersion test in MEM showed that the capacity of calcium phosphate formation was dependent on total content of hydroxyl group and surface morphology of titanium oxides.

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