• Journal of Dental Rehabilitation and Applied Science
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• v.21 no.1
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• pp.33-42
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• 2005

This study was performed to investigate the surface properties and in vitro biocompatibility of electrochemically oxidized Ti-6Al-7Nb alloy by anodic spark discharge technique. Discs of Ti-6Al-7Nb alloy of 20 mm in diameter and 2 mm in thickness were polished sequentially from #300 to 1000 SiC paper, ultrasonically washed with acetone and distilled water for 5 min, and dried in an oven at $50^{\circ}C$ for 24 hours. Anodizing was performed using a regulated DC power supply. The applied voltages were given at 240, 280, 320, and 360 V and current density of $30mA/cm^2$. Hydrothermal treatment was conducted by high pressure steam at $300^{\circ}C$ for 2 hours using a autoclave. Samples were soaked in the Hanks' solution with pH 7.4 at $36.5^{\circ}C$ during 30 days. The results obtained were summarized as follows; 1. The oxide films were porous with pore size of $1{\sim}5{\mu}m$. The size of micropores increased with increasing the spark forming voltage. 2. The main crystal structure of the anodic oxide film was anatase type as analyzed with thin-film X-ray diffractometery. 3. Needle-like hydroxyapatite (HA) crystals were observed on anodic oxide films after hydrothermal treatment at $300^{\circ}C$ for 2 hours. The precipitation of HA crystals was accelerated with increasing the spark forming voltage. 4. The precipitation of the fine asperity-like HA crystals were observed after being immersed in Hanks' solution at $37^{\circ}C$. The precipitation of HA crystals was accelerated with increasing the spark forming voltage and the time of immersion in Hanks' solution. 5. The Ca/P ratio of the precipitated HA layer was equivalent to that of HA crystal as increasing the spark forming voltage and the time of immersion in Hanks' solution.

• Journal of Dental Rehabilitation and Applied Science
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• v.22 no.1
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• pp.101-110
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• 2006

This study was performed to investigate the surface properties and in vitro biocompatibility of electrochemically oxidized Ti-6Al-7Nb alloy by anodic spark discharge technique. Discs of Ti-6Al-7Nb alloy of 20 mm in diameter and 2 mm in thickness were polished sequentially from #300 to 1000 SiC paper, ultrasonically washed with acetone and distilled water for 5 min, and dried in an oven at $50^{\circ}C$ for 24 hours. Anodizing was performed using a regulated DC power supply. The applied voltages were given at 240, 280, 320, and 360 V and current density of $30mA/cm^2$. Hydrothermal treatment was conducted by high pressure steam at $300^{\circ}C$ for 2 hours using a autoclave. Samples were soaked in the Hanks' solution with pH 7.4 at $36.5^{\circ}C$ during 30 days. The results obtained were summarized as follows; 1. The oxide films were porous with pore size of $1{\sim}5{\mu}m$. The size of micropores increased with increasing the spark forming voltage. 2. The main crystal structure of the anodic oxide film was anatase type as analyzed with thin-film X-ray diffractometery. 3. Needle-like hydroxyapatie (HA) crystals were observed on anodic oxide films after hydrothermal treatment at $300^{\circ}C$ for 2 hours. The precipitation of HA crystals was accelerated with increasing the spark forming voltage. 4. The precipitation of the fine asperity-like HA crystals were observed after being immersed in Hanks' solution at $37^{\circ}C$. The precipitation of HA crystals was accelerated with increasing the spark forming voltage and the time of immersion in Hanks' solution. 5. The Ca/P ration of the precipitated HA layer was equivalent to that of HA crystal as increasing the spark forming voltage and the time of immersion in Hanks' solution.

• Proceedings of the KOSOMBE Conference
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• v.1998 no.11
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• pp.231-232
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• 1998

The purpose of this study was to examine whether the precipitation of calcium phosphate on titanium surface was affected by surface modification. To improve the bone conductivity, of titanium, samples were devided into 4 groups. Group 1 was immersed in 5M-NaOH solution at $60^{\circ}C$ for 24 hours. Group 2 was immersed in 5M-NaOH solution at $60^{\circ}C $ for 24 hours and heat-treated at $600^{\circ}C$ for 1 hour. Group 3 was anodized in Hanks' solution at 1V, $25^{\circ}C$ for 1 hour. Group 4 was anodized in Hanks' solution at 5V, $80^{\circ}C$ for 5 minutes. And then, all specimens were immersed in the MEM Eagle's medium whose composition was similar to that of extracellular fluid for 30 days. The precipitation of the calcium phosphate on implant surface was increased by the immersion in the NaOH solution, and more highly accelerated by heat treatment at $600^{\circ}C$. The precipitation of the calcium phosphate on titanium implant was increased with the treatment of the anodic oxidation in Hanks' solution at 5V, $80^{\circ}C$.

• The Journal of Korean Academy of Prosthodontics
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• v.44 no.5
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• pp.617-627
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• 2006

Statement of problem: HA has been used as a coating material on Ti implants to improve osteoconductivity. However. it is difficult to form uniform HA coatings on implants with complex surface geometries using a plasma spraying technique. Purpose : To determine if Ti6Al4V sintered porous-surfaced implants coated with HA sol-gel coated and hydrothermal treated would accelerate osseointegration. Materials and Methods : Porous implants which were made by electric discharge were used in this study. Implants were anodized and hydrothermal treatment or HA sol-gel coating was performed. Hydrothermal treatment was conducted by high pressure steam at $300^{\circ}C$ for 2 hours using a autoclave. To make a HA sol, triethyl phosphite and calcium nitrate were diluted and dissolved in anhydrous ethanol and mixed. Then anodized implant were spin-coated with the prepared HA sols and heat treated. Samples were soaked in the Hanks solution with pH 7.4 at $37^{\circ}C$ for 6 weeks. The microstructure of the specimens was observed with a scanning electron microscope (SEM), and the composition of the surface layer was analyzed with an energy dispersive spectroscope (EDS). Results : The scanning electron micrographs of HA sol-gel coated and hydrothermal treated surface did not show any significant change in the size or shape of the pores. After immersion in Hanks' solution the precipitated HA crystals covered macro- and micro-pores The precipitated Ca and P increased in Hanks' solution that surface treatment caused increased activity. Conclusion : This study shows that sol-gel coated HA and hydrothermal treatment significantly enhance the rate of HA formation due to the altered surface chemistry.

• The Journal of Korean Academy of Prosthodontics
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• v.43 no.5
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• pp.684-693
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• 2005

Statement of problem: Ti-6Al-7Nb alloy is used instead of Ti-6Al-4V alloy that was known to have toxicity. Purpose: This study was performed to investigate the effect of electrolyte concentration on the surface characteristics of anodized and hydrothermally-treated Ti-6Al-7Nb alloy Materials and methods: Discs of Ti-6Al-7Nb alloy of 20 mm in diameter and 2 mm in thickness were polished sequentially from #300 to 1,000 SiC paper ultrasonically washed with acetone and distilled water for 5 min, and dried in an oven at $50^{\circ}C$ for 24 hours. Anodizing was performed at current density $30mA/cm^2$ up to 300 V in electrolyte solutions containing $\beta-glycerophosphate$ disodium salt hydrate $(\beta-GP)$ and calcium acetate (CA). Hydrothermal treatment was conducted by high pressure steam at $300^{\circ}C$ for 2 hours using a autoclave. All samples were soaked in the Hanks' solution with pH 7.4 at $36.5^{\circ}C$ for 30 days. Results and conclusion: The results obtained were summarized as follows: 1. After hydrothermal treatment, the precipitated HA crystals showed the dense fine needle shape. However, with increasing the concentration of electrolyte they showed the shape of thick and short rod. 2. When the dense fine needle shape crystals was appeared after hydrothermal treatment, the precipitation of HA crystals in Hanks' solution was highly accelerated. 3. The crystal structures of $TiO_2$ in anodic oxide film were composed of strong anatase peak and weak rutile peak as analyzed with thin-film X-ray diffractometery. 4. The Ca/P ratio of the precipitated HA layer was equivalent to that of HA crystal in Hanks' solution.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.22 no.2
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• pp.99-104
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• 2012

The co-precipitation technique has been applied to synthesize biphasic calcium phosphate (BCP). $Ca(NO_3)_2{\cdot}4H_2O$ and $(NH_4)_2HPO_4$ as the starting materials was used. X-ray diffraction (XRD) and Fourier transformed infrared (FT-IR) spectroscopy were used to characterize the structure of as-synthesized and calcined BCP powders. After immersion in Hanks' Balanced Salt Solution (HBSS), for 1 week a precipitation started to be formed with individual small granules on the specimen surface. An MTT assay indicated that BCP powders have no cytotoxic effects on MG-63 cells, and that they have good biocompatibility.

• Korean Journal of Materials Research
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• v.14 no.9
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• pp.607-613
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• 2004

This study was to investigate the surface properties of electrochemically oxidized Ti-6Al-7Nb alloy by anodic spark discharge technique. Anodizing was performed at current density 30 $mA/cm^2$ up to 300 V in electrolyte solutions containing $DL-{\alpha}$-glycerophosphate disodium salt hydrate($DL-{\alpha}$-GP) and calcium acetate (CA). Hydrothermal treatment was done at $300^{\circ}C$ for 2 hrs to produce a thin outermost layer of hydroxyapatite (HA). The bioactivity was evaluated from HA formation on the surfaces in a Hanks' solution with pH 7.4 at $36.5^{\circ}C$ for 30 days. The size of micropores and the thickness of oxide film increased and complicated multilayer by increasing the spark forming voltage. Needle-like HA crystals were observed on anodic oxide film after the hydrothermal treatment at $300^{\circ}C$ for 2 hrs. When increasing $DL-{\alpha}$-GP in electrolyte composition, the precipitated HA crystals showed the shape of thick and shorter rod. However, when increasing CA, the more fine needle shape HA crystals were appeared. The bioactivity in Hanks' solution was accelerated when the oxide films composed with strong anatase peak with presence of rutile peak. The increase of amount of Ca and P was observed in groups having bioactivity in Hanks' solution. The Ca/P ratio of the precipitated HA layer was equivalent to that of HA crystal and it was closer to 1.67 as increasing the immersion time in Hanks' solution.

• Journal of the Korean Ceramic Society
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• v.48 no.3
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• pp.217-221
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• 2011

Glass-ceramic materials, which consist of glass matrix phase containing crystalline ${\beta}-Ca_3(PO_4)_2$ and ${\beta}-Ca_2P_2O_7$, have been prepared by heating at $750-900^{\circ}C$ of calcium phosphate invert glasses in the silica-free $CaO-P_2O_5-TiO_2-Na_2O$, system. With increasing heating temperature from 750 to $900^{\circ}C$, the crystallite size of precipitated ${\beta}-Ca_3(PO_4)_2$ in glass with $55CaO{\cdot}35P_2O_5{\cdot}3TiO_2{\cdot}7Na_2O$ (mol%) composition increased from 48 to 91 nm. With the extension of the immersion time in dilute acetic acid solution (pH = 5) to ${\geq}$200 min, the degree of dissolution of $Ca^{2+}$ and $P^{5+}$ ions in the glass-ceramics was linearly increased and the solution was constantly maintained at pH = ~7. Biomimetic nanostructured (62-88 nm in average dia.), sphere-shaped hydroxyapatite was homogeneously formed on the surface of the glass-ceramics when socked for 7-14 days in a Hanks' solution, indicating bioactivity of the prepared glass-ceramics.

• Journal of Technologic Dentistry
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• v.27 no.1
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• pp.79-88
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• 2005

This study was performed to investigate the surface properties of electrochemically oxidized pure niobium by anodic oxide and hydrothermal treatment technique. Niobium specimens of $10\times10mm$ in dimension were polished sequentially from #600, #800, #1000 emery paper. The surface pure niobium specimens were anodized in an electrolytic solution that was dissolved calcium and phosphate in water. The electrolytic voltage was set in the range of 250 V and the current density was 10 $mA/cm^2$. The specimen was hydrothermal treated in high-pressure steam at 300$^{\circ}C$ for 2 hours using an autoclave. Then, specimens were immersed in the Hanks' solution with pH 7.4 at 37$^{\circ}C$ for 30 days. The surface of specimen was characterized by scanning electron microscope(SEM), energy dispersive X-ray microanalysis(EDX), potentiostat/galvanostat test, and cytotoxicity test. The results obtained was summarized as follows; According to the result of measuring corrosion behavior at 0.9% NaCl, corrosion resistance was improved more specimens treated with anodic oxide than in hydrothermal treated ones. The multi-porous oxide layer on surface treated through anodic oxidation showed a structure that fine pores overlap one another, and the early precipitation of apatite was observed on the surface of hydrothermal treated samples. According to the result of EDX after 30 days deposition in Hanks' solution, Ca/P was 1.69 in hydrothermal treated specimens. In MTT test, specimens treated through anodic oxidation and hydrothermal treated ones showed spectrophotometer similar to that of the control group. Thus no significant difference in cytotoxicity was observed (P>0.05).

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.121-121
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• 2016

치아는 인체중에서도 혹한 환경에서 부분으로 높은 하중과 타액과 같은 강 부식성 매체로 그 환경이 상상을 초월한다. 즉 반복적으로 가해지는 하중(응력)과 침식을 유발하는 타액과 음식물 등이다. 따라서 치아가 쉽게 파괴되거나 썩는 현상이 나타나게 된다. 이렇게 사용되다가 치아의 역할을 다하게 되면 인공치아를 사용하게 되는데 그 재료가 바로 타이타늄(Ti)이다. 생체매식재로 사용되는 Ti는 반응성이 높아 산소와 쉽게 결합하여 표면에 TiO, $TiO_2$, 및 $Ti_2O_3$와 같은 산화피막을 표면에 형성함으로써 뛰어난 부식저항성과 생체적합성을 가지며 생체에 독성이 없고 탄성계수가 골과 비슷하여 골과 임플란트 경계면에서 응력분산에 유리한 성질 등 물리적, 기계적 성질이 뛰어나 외과용 임플란트 재료로 가장 좋은 재료이다. 금속 임플란트의 생체적합도는 임플란트 재료 자체보다는 생체 내 산화막이 화학적으로 불안정할 때 부식이 발생하게 되고 그 결과 금속이온이 주위로 유리되어 조직반응을 일으키므로 금속의 표면을 덮고 있는 산화막에 의해 좌우된다. Ti는 생체불활성재료로서 매식재료로 사용할 경우 뼈와 잘 융합되는 골유착을 나타내나 골과 화학적결합은 하지 않고 골형성을 적극적으로 유도하지 못함으로 환자의 치유기간이 길어지게 된다. 이러한 이유로 골조직내 임플란트의 접합을 개선하기위한 연구가 이루어져 골과의 결합을 높이기 위해 골유착을 일으키는 Ti에 골성장을 유도하는 뼈성분인 하이드록시 아파타이트(HA)라는 물질을 플라즈마 코팅법을 사용하던가 아니면 Hanks' solution내에서 침적 후 HA도금을 하는 방법 등으로 처리하고 있다. 그러나 플라즈마 코팅법은 고온에서 처리를 행하고 Hanks' solution내에 침적할 경우 Ti표면에 밀착도가 저하되거나 합금의 상변화 등으로 인하여 표면처리 과정 중에서 내식성이 크게 감소될 수 있다. 이러한 여러 가지 코팅법을 통하여 골 유착을 증진시키기 위한 연구는 계속되고 있지만 임상적으로 사용 후 문제가 단시일에 발생되는 것도 아니고 수년이 지나야 나타나게 된다. 이러한 방법으로 코팅을 하게 되면 골과 잘 유착이 되어 자연차아와 같은 기능을 하게 된다. 따라서 이러한 문제를 최소화하는 방법이 나노구조를 표면에 형성시켜 골유착을 쉽게 함으로써 이를 개선할 수 있을 것으로 생각되어 본 강의에서는 임플란트의 문제와 사용되는 재료에 대하여 고찰하여 자연치아를 대체 할 수 있는지 알아보았다.