• The Journal of Korean Academy of Prosthodontics
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• v.47 no.1
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• pp.39-45
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• 2009

Statement of problem: Recently precalcification treatment has been studied to shorten the period of the implant. Purpose: This study was performed to evaluate the effect of precalcification treatment of $TiO_2$ Nanotube formed on Ti-6Al-4V Alloy. Material and methods: Specimens of $20{\times}10{\times}2\;mm$ in dimensions were polished sequentially from #220 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. The nanotubular layer was processed by electrochemical anodic oxidation in electrolytes containing 0.5 M $Na_2SO_4$ and 1.0 wt% NaF. Anodization was carried out using a regulated DC power supply (Kwangduck FA, Korea) at a potential of 20 V and current density of $30\;㎃/cm_2$ for 2 hours. Specimens were heat-treated at $600^{\circ}C$ for 2 hours to crystallize the amorphous $TiO_2$ nanotubes, and precalcified by soaking in $Na_2HPO_4$ solution for 24 hours and then in saturated $Ca(OH)_2$ solution for 5 hours. To evaluate the bioactivity of the precalcified $TiO_2$ nanotube layer, hydroxyapatite formation was investigated in a Hanks' balanced salts solution with pH 7.4 at $36.5^{\circ}C$ for 2 weeks. Results: Vertically oriented amorphous $TiO_2$ nanotubes of diameters 48.0 - 65.0 ㎚ were fabricated by anodizing treatment at 20 V for 2 hours in an 0.5 M $Na_2SO_4$ and 1.0 NaF solution. $TiO_2$ nanotubes were composed with strong anatase peak with presence of rutile peak after heat treatment at $600^{\circ}C$. The surface reactivity of $TiO_2$ nanotubes in SBF solution was enhanced by precalcification treatment in 0.5 M $Na_2HPO_4$ solution for 24 hours and then in saturated $Ca(OH)_2$ solution for 5 hours. The immersion in Hank's solution for 2 weeks showed that the intensity of $TiO_2$ rutile peak increased but the surface reactivity decreased by heat treatment at $600^{\circ}C$. Conclusion: This study shows that the precalcified treatment of $TiO_2$ Nanotube formed on Ti-6Al-4V Alloy enhances the surface reactivity.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2013.05a
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• pp.111-111
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• 2013

골이식 부위에서 연조직의 붕괴를 막아주면서 골이식재를 위한 안정적인 공간을 확보하기 위해서 타이타늄 메쉬가 적용된다. 본 연구에서 생체 불활성의 특성을 보이는 타이타늄 차폐막에 양극산화와 석회화 순환처리에 의해서 생체활성을 부여한 결과, 골형성을 촉진하는 결과를 보여주었다.

• The korean journal of orthodontics
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• v.44 no.5
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• pp.246-253
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• 2014

Objective: To evaluate the bioactivity, and the biomechanical and bone-regenerative properties of Ti6Al4V miniscrews subjected to anodization, cyclic precalcification, and heat treatment (APH treatment) and their potential clinical use. Methods: The surfaces of Ti6Al4V alloys were modified by APH treatment. Bioactivity was assessed after immersion in simulated body fluid for 3 days. The hydrophilicity and the roughness of APH-treated surfaces were compared with those of untreated (UT) and anodized and heat-treated (AH) samples. For in vivo tests, 32 miniscrews (16 UT and 16 APH) were inserted into 16 Wistar rats, one UT and one APH-treated miniscrew in either tibia. The miniscrews were extracted after 3 and 6 weeks and their osseointegration (n = 8 for each time point and group) was investigated by surface and histological analyses and removal torque measurements. Results: APH treatment formed a dense surface array of nanotubular TiO2 layer covered with a compact apatite-like film. APH-treated samples showed better bioactivity and biocompatibility compared with UT and AH samples. In vivo, APH-treated miniscrews showed higher removal torque and bone-to-implant contact than did UT miniscrews, after both 3 and 6 weeks (p < 0.05). Also, early deposition of densely mineralized bone around APH-treated miniscrews was observed, implying good bonding to the treated surface. Conclusions: APH treatment enhanced the bioactivity, and the biomechanical and bone regenerative properties of the Ti6Al4V alloy miniscrews. The enhanced initial stability afforded should be valuable in orthodontic applications.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2013.05a
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• pp.215-215
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• 2013

임플란트 소재로서 순 타이타늄은 높은 응력이 발생하는 부위에는 그 강도가 충분하지 않은 것으로 지적되었으며, 이러한 이유로 인해서 그의 대용합금에 대한 연구가 진행되고 있다. 본 연구에서 ${\beta}$형 타이타늄 합금 Ti-32Nb-5Zr 합금을 시험재료로 선택한 다음 양극산화와 석회화 순환처리에 의해서 표면을 개질한 결과, HAp 석출이 빠르게 가속되었을 뿐만 아니라 신생골 생성량과 골결합력이 크게 개선된 결과를 보여주었다.

• The Journal of Korean Academy of Prosthodontics
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• v.49 no.1
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• pp.16-21
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• 2011

Purpose: The purpose of this study was to investigate the bioactivity of precalcified nanotubular $TiO_2$ layer on Ti-6Al-7Nb alloy. Materials and methods: Anodic oxidation was carried out at a potential of 20 V and current density of 20 mA/$cm^2$ for 1 hour. The glycerol solution containing 1 wt% $NH_4F$ and 20 wt% deionized water was used as an electrolyte. Precalcification treatment was obtained by soaking in $Na_2HPO_4$ solution at $80^{\circ}C$ for 30 minutes followed by soaking in saturated $Ca(OH)_2$ solution at $100^{\circ}C$ for 30 minutes, followed by heat treatment at $500^{\circ}C$ for 2 hours. To evaluate the activity of precalcified nanotubular $TiO_2$ layer, specimens were immersed in a simulated body fluid with pH 7.4 at $36.5^{\circ}C$ for 10 days. Results: 1. Nanotubular $TiO_2$ layer showed the highly ordered dense structure by interposing small diameter nanotubes between large ones, the shape of nanotubes was enlarged as going down. 2. The mean length of nanotubes was $517.0{\pm}23.2\;nm$ innm glycerol solution containing 1 wt% $NH_4F$ and 20 wt% $H_2O$ at 20 V for 1 hour. 3. The bioactivity of Ti-6Al-7Nb alloy was improved with formation of nanotubular $TiO_2$ layer and precalcification treatment in $80^{\circ}C$ 0.5 M $Na_2HPO_4$ and saturated $100^{\circ}C$ $Ca(OH)_2$ solution. Conclusion: Bioactivity of precalcified nanotubular $TiO_2$ layer on Ti-6Al-7Nb alloy was improved.

• Korean Journal of Dental Materials
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• v.45 no.4
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• pp.243-256
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• 2018

The purpose of this study was to investigate the effects of the anodization and cyclic calcification treatment on the surface characteristic and bioactivity of the titanium thin sheet in order to obtain basic data for the production of bioactive titanium membrane. A $30{\times}20{\times}0.08mm$ titanium sheets were prepared, and then they were pickled for 10 seconds in the solution which was mixed with $HNO_3:HF:H_2O$ in a ratio of 12: 7: 81. The $TiO_2$ nanotube layer was formed to increase the specific surface area of the titanium, and then the cyclic calcification treatment was performed to induce precipitation of hydroxiapatite by improvement of the bioactivity. The corrosion resistance test, wettability test and immersion test in simulated body solution were conducted to investigate the effect of these surface treatments. The nanotubes formed by the anodization treatment have a dense structure in which small diameter tubes are formed between relatively large diameter tubes, and their inside was hollow and the outer walls were coupled to each other. The hydroxyapatite precipitates were well combined on the nanotubes by the penetration into the nanotube layer by successive cyclic calcification treatment, and the precipitation of hydroxyapatite tended to increase proportionally after immersion in simulated body solution as the number of cycles increased. In conclusion, it was confirmed that induction of precipitation of hydroxyapatite by cyclic calcification treatment after forming the nanotube $TiO_2$ nanotube layer on the surface of the titanium membrane can contribute to improvement of bioactivity.