• 대한금속재료학회지
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• 제47권2호
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• pp.91-98
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• 2009

The titania nanotubular layer for photocatalytic application was synthesized by anodization process in HF solution and the photocatalytic efficiencies of nanotubular film were evaluated by the decomposition rate of aniline blue. In order to facilitate the photocatalytic reaction, the electron acceptors such as potassium bromate, hydrogen peroxide and ammonium persulfate were added to aniline blue solution and the effects of electron acceptors on the dye degradation efficiency were evaluated. The results showed that the photocatalytic efficiency has markedly improved by adding the electron acceptors.

• 대한치과보철학회지
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• 제49권1호
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• pp.16-21
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• 2011

연구 목적: 높은 외력이 작용하는 부위의 임플란트 재료로서 사용되고 있는 Ti-6Al-7Nb 합금의 골유착을 개선하기 위한 방법의 하나로서 나노튜브 $TiO_2$ 층 생성하고 전석회화 처리한 다음 유사체액 중에서의 활성도를 알아보고자 하였다. 연구 재료 및 방법: 양극산화처리는 glycerol에 20 wt% $H_2O$와 1 wt% $NH_4F$를 혼합하여 준비한 전해질 수용액에 전압 20 V, 전류밀도 20 mA/$cm^2$의 조건에서 1시간동안 통전하였다. 전석회화처리는 $80^{\circ}C$의 $Na_2HPO_4$ 수용액에 30분 동안 침적하고, 이어서$100^{\circ}C$의 $Ca(OH)_2$ 포화 수용액에 30분 동안 침적하였으며, $500^{\circ}C$에서 2시간 동안 열처리하였다. 전석회화처리 후 표면층의 생체활성도를 조사하기 위해 $36.5^{\circ}C$, pH 7.4의 유사체액에 10일 동안 침적하였다. 결과: 1. 나노튜브 $TiO_2$ 층은 높은 자기정렬 형태를 갖고 큰 직경의 튜브들 사이 공간에 상대적으로 작은 직경의 튜브들이 생성되는 형태로 치밀한 구조를 이루었으며, 상부에서 하부로 갈수록 직경 감소를 보였다. 2.1 wt% $NH_4F$와 20 wt% $H_2O$를 함유하는 glycerol 전해액에서 20V의 전압을 인가하여 생성된 나노튜브들의 평균 길이는 $517.0{\pm}23.2\;nm$를 보였다. 3. 나노튜브 $TiO_2$ 층의 생체활성도는 $80^{\circ}C$의 0.5 M$Na_2HPO_4$ 수용액과 $100^{\circ}C$의 $Ca(OH)_2$ 포화 수용액에 침적하는 전석회화처리 군의 경우에 크게 개선되어, 아파타이트의 석출 과정에서 나타나는 치밀한 돌기상과 이들을 가로지르는 미세 균열상이 관찰되었다. 결론: Ti-6Al-7Nb 합금을 나노튜브 $TiO_2$ 층 생성 후 전석회화 처리한 결과 생체활성도가 개선되었다.

• 대한금속재료학회지
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• 제50권2호
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• pp.164-170
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• 2012

Nanotubular structure formation on the Ti-6Al-4V and Ti-Ta alloy surfaces by electrochemical methods has been studied using the anodizing method. A nanotube layer was formed on Ti alloys in 1.0 M $H_3PO_4$ electrolyte with small additions of $F^-$ ions. The nanotube nucleation and growth of the ${\alpha}$-phase and ${\beta}$-phase appeared differently, and showed different morphology for Cp-Ti, Ti-6Al-4V and Ti-Ta alloys. In the ${\alpha}$-phase of Cp-Ti and martensite ${\alpha}^{\prime}$ and in the ${\alpha}^{{\prime}{\prime}}$ and ${\beta}$-phase of the Ti-Ta alloy, the nanotube showed a clearly highly ordered $TiO_2$ layer. In the case of the Ti-Ta alloy, the pore size of the nanotube was smaller than that of the Cp-Ti due to the ${\beta}$-stabilizing Ta element. In the case of the Ti-6Al-4V alloy, the ${\alpha}$-phase showed a stable porous structure; the ${\beta}$-phase was dissolved entirely. The nanotube with two-size scale and high order showed itself on Ti-Ta alloys with increasing Ta content.

• 한국재료학회:학술대회논문집
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• 한국재료학회 2011년도 춘계학술발표대회
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• pp.239.1-239.1
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• 2011

Dye sensitized solar cells (DSC) are promising devices for inexpensive, nontoxic, transparent, and large-scale solar energy conversion. Generally thick $TiO_2$ nanoporous films act as efficient photoanodes with their large surface area for absorbing light. However, electron transport through nanoparticle networks causes the slowdown and the loss of electron transport because of a number of interparticle boundaries inside the conduction path. We have studied DSCs with precisely dimension-controlled $TiO_2$ nanotubes array as photoanode. $TiO_2$ nanotubes array is prepared by template-directed fabrication method with atomic layer deposition. Well-ordered nanotubes array provides not only large surface area for light absorbing but also direct pathway for electrons with minimalized grain boundaries. Large enlongated anatase grains in the nanotubes could enhance the conductivity of electrons, but also suppress the recombination with holes through defect sites during diffusion into the electrode. To study the effect of grain boundaries, we fabricated two kinds of nanotubes which have different grain sizes by controlling deposition conditions. And we studied electron conduction through two kinds of nanotubes with different grain structures. The solar cell performance was studied as a function of thickness and grain structures. And overall solar-to-electric energy conversion efficiencies of up to 7% were obtained.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2013년도 제45회 하계 정기학술대회 초록집
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• pp.75.2-75.2
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• 2013

Atomic layer deposition (ALD), utilizing self-limiting surface reactions, could offer promising perspectives for future efficient energy conversion devices. The capabilities of ALD for surface/interface modification and construction of novel architectures with sub-nanometer precision and exceptional conformality over high aspect ratio make it more valuable than any other deposition methods in nanoscale science and technology. In the context, a variety of researches on fabrication of active materials for energy conversion applications by ALD are emerging. Among those materials, one-dimensional nanotubular titanium dioxide, providing not only high specific surface area but also efficient carrier transport pathway, is a class of the most intensively explored materials for energy conversion systems, such as photovoltaic cells and photo/electrochemical devices. The monodisperse, stoichiometric, anatase, TiO2 nanotubes with smooth surface morphology and controlled wall thickness were fabricated via low-temperature template-directed ALD followed by subsequent annealing. The ALD-grown, anatase, TiO2 nanotubes in alumina template show unusual crystal growth behavior which allows to form remarkably large grains along axial direction over certain wall thickness. We also fabricated dye-sensitized solar cells (DSCs) introducing our anatase TiO2 nanotubes as photoanodes, and studied the effect of blocking layer, TiO2 thin films formed by ALD, on overall device efficiency. The photon convertsion efficiency ~7% were measured for our TiO2 nanotubebased DSCs with blocking layers, which is ~1% higher than ones without blocking layer. We also performed open circuit voltage decay measurement to estimate recombination rate in our cells, which is 3 times longer than conventional nanoparticulate photoanodes. The high efficiency of our ALD-grown, anatase, TiO2 nanotube-based DSCs may be attributed to both enhanced charge transport property of our TiO2 nanotubes photoanode and the suppression of recombination at the interface between transparent conducting electrode and iodine electrolytes by blocking layer.

• 한국재료학회지
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• 제29권12호
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• pp.790-797
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• 2019

To improve photocatalytic performance, CdS nanoparticle deposited TiO₂ nanotubular photocatalysts are synthesized. The TiO₂ nanotube is fabricated by electrochemical anodization at a constant voltage of 60 V, and annealed at 500 for crystallization. The CdS nanoparticles on TiO₂ nanotubes are synthesized by successive ionic layer adsorption and reaction method. The surface characteristics and photocurrent responses of TNT/CdS photocatalysts are investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD), UV-Vis spectrometer and LED light source installed potentiostat. The bandgaps of the CdS deposited TiO₂ photocatalysts are gradually narrowed with increasing of amounts of deposited CdS nanoparticles, which enhances visible light absorption ability of composite photocatalysts. Enhanced photoelectrochemical performance is observed in the nanocomposite TiO₂ photocatalyst. However, the maximum photocurrent response and dye degradation efficiency are observed for TNT/CdS30 photocatalyst. The excellent photocatalytic performance of TNT/CdS30 catalyst can be ascribed to the synergistic effects of its better absorption ability of visible light region and efficient charge transport process.

• 한국재료학회지
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• 제23권4호
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• pp.240-245
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• 2013

Electrochemical surface treatment is commonly used to form a thin, rough, and porous oxidation layer on the surface of titanium. The purpose of this study was to investigate the formation of nanotubular titanium oxide arrays during short anodization processing. The specimen used in this study was 99.9% pure cp-Ti (ASTM Grade II) in the form of a disc with diameter of 15 mm and a thickness of 1 mm. A DC power supplier was used with the anodizing apparatus, and the titanium specimen and the platinum plate ($3mm{\times}4mm{\times}0.1mm$) were connected to an anode and cathode, respectively. The progressive formation of $TiO_2$ nanotubes was observed with FE-SEM (Field Emission Scanning Electron Microscopy). Highly ordered $TiO_2$ nanotubes were formed at a potential of 20 V in a solution of 1M $H_3PO_4$ + 1.5 wt.% HF for 10 minutes, corresponding with steady state processing. The diameters and the closed ends of $TiO_2$ nanotubes measured at a value of 50 cumulative percent were 100 nm and 120 nm, respectively. The $TiO_2$ nanotubes had lengths of 500 nm. As the anodization processing reached 10 minutes, the frequency distribution for the diameters and the closed ends of the $TiO_2$ nanotubes was gradually reduced. Short anodization processing for $TiO_2$ nanotubes of within 10 minutes was established.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2013년도 춘계학술대회 논문집
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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.

• 대한치과보철학회지
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• 제47권1호
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• pp.39-45
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• 2009

연구목적: 최근 치과용 임플란트의 임상 경향이 전체 치료기간을 줄일 수 있는 방법에 관심이 집중됨에 따라 불활성의 티타늄 임플란트 표면에 활성을 부여하기 위한 다양한 표면처리 방법이 검토되고 있다. 본 연구에서는 높은 강도가 요구되는 부위의 임플란트 재료로서 사용되고 있지만 표면 특성이 순 티타늄에 비해 떨어지는 Ti-6Al-4V 합금의 골전도성을 개선할 목적으로 시행되었다. 연구 재료 및 방법: $20{\times}10{\times}2\;mm$의 Ti-6Al-4V 합금판을 준비한 다음 $TiO_2$ 나노튜브를 형성하기 위해 DC 정전원 장치의 양극과 음극에 각각 시편과 백금판을 결선하고 0.5 M $Na_2SO_4$와 1.0 wt% NaF를 함유하는 전해액을 사용하여 전압 20 V와 전류밀도 $30\;㎃/cm^2$ 조건에서 2시간 동안 양극산화 처리하였다. $TiO_2$ 나노튜브 형성 후 산화 피막층의 결정화를 유도하기 위해 $600^{\circ}C$에서 2시간 동안 열처리하였고, 표면활성도를 개선하기 위해 0.5 M $Na_2HPO_4$ 수용액 24시간 침적과 $Ca(OH)_2$ 포화 수용액에 5시간 침적을 시행하였다. 준비한 시편의 표면 반응성을 조사하기 위해 pH와 무기이온의 농도를 사람의 혈장과 유사하게 조절한 Hanks 용액 (H2387, Sigma Chemical Co., USA)에 2주간 침적하였다. 결과: 20 V에서의 양극산화처리로 직경 48.0 - 65.0 ㎚ 범위의 무정형의 $TiO_2$ 나노튜브가 전체 표면에 걸쳐서 균일하게 생성되는 양상을 보였다. $TiO_2$ 나노튜브는 $600^{\circ}C$에서 2시간 열처리 후 상대적으로 강한 anatase 피크와 함께 rutile 피크가 관찰되었다. $TiO_2$ 나노튜브의 표면활성도는 0.5 M $Na_2HPO_4$ 수용액 24시간 침적과 $Ca(OH)_2$ 포화수용액에 5시간 침적으로 개선되었다. 열처리와 전석회화 처리 후 SBF에 침적한 결과, $TiO_2$ rutile 피크의 상대적 강도는 크게 증가되었지만 HA의 석출은 저하되는 경향을 보였다. 결론: 이상의 결과로 미루어 볼 때, 양극산화 처리한 $TiO_2$ 나노튜브는 $600^{\circ}C$에서의 열처리에 의해 피막층이 안정화되고, 0.5 M $Na_2HPO_4$ 수용액 24시간 침적과 $Ca(OH)_2$ 포화수용액에 5시간 침적으로 표면에 인산칼슘층을 형성하는 것이 표면활성도를 개선하는데 유효함을 알 수 있었다.

• 대한치과교정학회지
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• 제44권5호
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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.