• Journal of Korean Society of Environmental Engineers
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• v.30 no.3
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• pp.339-344
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• 2008

Titanium dioxide nanotubes were fabricated by self-organized electrochemical potentiostatic anodization of titanium thin film with an electrolyte solution of sodium sulfate 1M and sodium flouride 0.5wt% aqueous solution at 20$^{\circ}C$ for 20min. Field Emmision Scanning Electron Microscopy(FE-SEM) and X-ray Diffractometer(XRD) were used to evaluate the micromorphology and crystalline structure of the titanium dioxide nanotube thin film. Titanium dioxide nanotube were fabricated with diameters approx. 100nm and tube length from appox. 1 $\mu$m. Titanium dioxide films formed through anodization and annealing process at 450$^{\circ}C$ contained a phase of anatase. Also, this study was performed to evaluate the application of titanium dioxide thin film for treating humic acid dissolved in water. The reaction tended to follow the Langmuir-Hinshelwood kinetics with zero order. Comparative experiments with thin film and anatase powder showed the same zero order kinetics when 0.3g of powder had been used.

• Journal of Dental Rehabilitation and Applied Science
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• v.25 no.2
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• pp.183-190
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• 2009

The aim of this study is to find the condition of forming the favorable nanotubes by anodizing with NaF and $H_3PO_4$. Machined Ti discs were used for anode, and Platinum net was used for cathode. For electrolyte, $H_3PO_4$ and NaF solution were mixed. We controlled voltage, electrolyte concentration, anodizing time and formed nanotubes on Ti discs. After that, these were washed with distilled water for 24 hours and dried in the $40^{\circ}C$ oven for 24 hours. The surface structure of specimens were analyzed. The results were as follows : At 0.5 wt % NaF, according as increasing voltage and anodizing time, early state of nucleating pores were generated. At 1.0 wt % NaF, 20 V, 20 & 25 min, well-formed nanotubes were observed. At 1.0 wt % NaF, 30 V, structure of nanotube became bigger and interconnected. At 2.0 wt % NaF, no nanotubes were formed and it was unrelated with voltage and time. At 1.0 wt % NaF, 20 V, 20 - 25 min, well-ordered nanotubes were generated on Ti discs. For the formation of favorable nanotubes, it is considered that proper parameters such as electrolyte concentration, voltage, anodizing time are necessary according to the kind of electrolytes.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2012.05a
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• pp.319-319
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• 2012

수용액에서 양극산화법을 이용하여 티타늄 표면에 $TiO_2$ 나노튜브를 형성시켰고, XRD 및 전자현미경을 통해 열처리를 한 $TiO_2$ 나노튜브 소재표면, 계면구조를 관찰하였으며, 이는 향후 나노튜브의 결정구조를 제어할 수 있는 자료로 활용 될 것으로 기대된다.

• Applied Chemistry for Engineering
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• v.28 no.4
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• pp.375-382
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• 2017

In the present review, we provide an overview of the research trend of anodic $TiO_2$ nanostructures. To date, most anodic $TiO_2$ nanostructure formation has focused on the fluoride ion electrolyte system to form nanotube layers. Recently, a novel approach that describes the formation of thick, self-organized $TiO_2$ nanostructures was reported. These layers can be prepared on Ti metal by anodization in a hot organic/$K_2HPO_4$ electrolyte. This nanostructure consists of a strongly interlinked network of nanosized $TiO_2$, and thus provides a considerably higher specific surface area than that of using anodic $TiO_2$ nanotubes. This review describes the formation mechanism and novel properties of the new nanostructures, and introduces potential applications.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2018.06a
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• pp.28-28
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• 2018

수전해(electrochemical water splitting)는 연료전지의 가역적 역반응을 이용하여 물로부터 수소와 산소를 발생시키는 기술이다. 산소는 음극에서 발생하는데, 이 때 음극 표면은 고농도의 산소 음이온 및 라디칼에 장시간 노출된다. 때문에 기계적, 화학적 내구성이 우수한 전극재를 사용할 필요가 있다. 불용성 전극 (dimensionally stable anode, DSA)은 이러한 기술적 요구사항을 잘 만족하는 상용화 된 전극이다. 티타늄이나 티타늄 합금 표면에 촉매를 미량 반복 살포하여 산화물 형태의 매우 견고한 표면을 형성함으로서 내구성을 확보한다. 그러나, 보통 DSA 제조 기법의 특징에 따라 다공성 표면 구조를 사용하지는 않기 때문에 생산 과정이 복잡하고 비용이 많이 발생하는 문제를 여전히 나타내고 있다. 본 연구는 상기 문제를 개선하기 위한 수전해용 음극 제조 기술에 관한 연구이다. 티타늄과 티타늄 합금은 동일한 양극산화 기술 적용이 가능하다는 점을 이용하여 티타늄 기판으로부터 다공성 구조를 형성함으로써 바인더의 사용을 배제하였다. 단일공정양극산화기법 (single-step anodization)을 이용하여 $IrO_2$와 $RuO_2$를 도핑함으로써 TiO2에 촉매능을 부여하였다. 제조된 나노튜브들의 구조적 특징을 HR-TEM (High-resolution transmission electron microscope)과 FE-SEM (Field-emission scanning electron microscope)으로 분석하고 SAED (selective area electron diffraction) 패턴을 분석하여 전극재의 결정성을 확인하였다. 알칼라인 분위기에서 일으킨 산소발생반응 (oxygen evolution reaction, OER)의 LSV (linear sweep voltammetry) 결과를 XPS (X-ray photoelectron microscoscopy) 결과와 연관지어 촉매 표면 구조와 과전압의 관계를 해석하였다. LSV 결과로부터 Tafel 분석을 연달아 수행함으로써 전극의 속도결정단계를 정의하였다. 최종적으로 사이클 테스트 통하여 DSA로써의 성능을 평가하였다.

• 한국신재생에너지학회:학술대회논문집
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• 2010.06a
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• pp.227.1-227.1
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• 2010

본 연구는 자외선 영역의 흡수로 전자 정공의 전하쌍을 생성함으로써 광전압 및 전류를 일으키는 티타니아 물질을 금속지지체 표면에 양극산화로 튜브형 $TiO_2$(anodized tubular $TiO_2$; ATT)로 제조한 후 나노크기의 금속 혹은 $WO_3$입자를 담지하여 광감응 재료로 활용하였다. 이는 기존의 입자나 콜로이드 형태로 광촉매 물질을 고정화하여 사용한 재료의 탈리현상 및 효율저하를 극복하기 위함이다. ATT는 전해질 내에 전기화학적 에칭율과 화학적 용해율의 비율에 의해 나노튜브 길이 성장에 영향을 미치는데 이를 유기 전해질과 불산 전해질을 사용하여 정전압 혹은 정전류의 조건에서 다양한 길이의 $TiO_2$ 나노튜브를 제조하였다. 여기에 전기분해담지(electrolytic deposition; ELD)를 통하여 정전류 조건에서 다양한 금속(Pt, Pd, Ru)을 나노크기의 형태로 담지하여 광촉매 내 생성된 전자 정공의 재결합을 줄이고자 하였고 $WO_3$의 담지를 통하여 가시광 감응을 높이고자 하였다. 제조된 여러 조건의 시료는 SEM과 EDAX를 통하여 형태와 길이, 담지량을 확인 하고 XRD를 이용하여 열처리 온도에 따른 결정화상태를 확인하였으며 광전류 측정 및 Cr(VI)의 광환원과 MB의 광분해를 통하여 광효율을 관찰하였다. 금속이 도핑되었을 경우 순수 ATT보다 보통 3배의 흡착률과 UV광원 아래 2배의 광효율을 관찰할 수 있었는데 이 중 Pt의 담지가 가장 효율이 좋았으며 흡착률에서는 담지량의 증가에 따른 증가선을 관찰 할 수 있었으나 광원 사용시 3%담지율에서 최적을 확인 할 수 있었다. 또한 $TiO_2$외 가시광감응 활성을 높이기 위한 다양한 광촉매제조가 진행 중에 있다.

• Korean Chemical Engineering Research
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• v.49 no.1
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• pp.28-34
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• 2011

Titania nanotube(TNT), which is a tube shaped thin film manufactured by anodizing titanium under $F^-$ ion electrolyte, has photo activity. Distilled water and formamide were used as solvent, and HF, NaF, $NH_4F$ were used as main $F^-$ ions for the electrolyte. The length and the diameter of TNT increased as the voltage and anodizing time increased. TNT prepared by anodizing was a very ordered tube, and had a maximum length of 13.7 ${\mu}m$ depending on the conditions of manufacturing. Titania prepared by anodizing was amorphous, and became an anatase crystal after heat treatment.

• 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.

• Korean Chemical Engineering Research
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• v.49 no.5
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• pp.652-656
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• 2011

Thin film of titania nanotubes(TNT) and titania nanofilms(TNF) was fabricated by anodizing for the study of the photo-catalytic reaction(PC) and photoelectrocatalytic reaction(PEC). Removal efficiency of methylene blue was investigated by UV radiation on the TNT coated titanium plate. Removal efficiency was increased with longer TNT length. Degradation efficiency of the PEC reaction was less sensitive than that of PC reaction. And Effect of TNT length is relatively small. Titania nanofilms(TNF) showed low efficiency than TNT. The efficiency drop of PC was larger than that of PEC.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2006.10a
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• pp.37-38
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• 2006