• Bulletin of the Korean Chemical Society
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• 제32권10호
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• pp.3730-3734
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• 2011

The degree of self-assembly and the size variation of nanotubular structures in anodic titanium oxide prepared by the anodization of titanium in ethylene glycol containing 0.25 wt % $NH_4F$ at 40 V were investigated as a function of anodization time. We found that the degree of self-assembly and the size of the nanotubes were strongly dependent on thickness deviation and thus indirectly on anodization time, as the thickness deviation was caused by the dissolution of the topmost tubular structures at local areas during long anodization. A large deviation in thickness led to a large deviation in the size and number of nanotubes per unit area. The dissolution primarily occurred at the bottoms of the nanotubes ($D_{bottom}$) in the initial stage of anodization (up to 6 h), which led to the growth of nanotubes. Dissolution at the tops ($D_{top}$) was accompanied by $D_{bottom}$ after the formed structures contacted the electrolyte after 12 h, generating the thickness deviation. After extremely long anodization (here, 70 h), $D_{top}$ was the dominant mode due to increase in pH, meaning that there was insufficient driving force to overcome the size distribution of nanotubes at the bottom. Thus, the nanotube array became disorder in this regime.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2012년도 춘계학술발표회 논문집
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• pp.255-255
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• 2012

The interactions between cells and nanotopographies are increasingly interested as nanotopographies that may be more efficient in promoting cell functions and, titanium nanotubes have attracted much attention. Titanium nanotube can be fabricated easily with precisely controlled diameters and lengths. Titanium nanotubes with the suitable tube dimensions have been observed to enhance bone cell functions, whereas, there is still some controversy. These nanotubes can also serve as carriers for drugs such as growth factors, antibacterial agents and other drugs and show promise in bone implant applications.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2007년도 하계학술대회 논문집 Vol.8
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• pp.372-372
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• 2007

Titanium oxide nanotube arrays were fabricated by the anodization of pure titanium thin film deposited at $500^{\circ}C$ on silicon substrates. The titania nanotubes were grown by anodization in nonaqueous-base electrolytes at different potentials between 5 V and 30 V. $TiO_2$ nanotube array with a small pore diameter of 40 nm and long titanium oxide layer of $4\;{\mu}m$ was obtained. The $TiO_2$ nanotube array was used as a porous electrode for quartz crystal microbalance (QCM). Nanoporous morphology of electrode will increase the sensitivity of microbalance.

• 대한금속재료학회지
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• 제46권11호
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• pp.730-736
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• 2008

$TiO_2$ nanotubes fabricated in aqueous HF-based electrolytes have been generally grown only to about 500nm in length because of the strong dissolubility of HF acid. In this paper, ethylene glycol solution has been applied for increasing the length of the anodic $TiO_2$ nanotubes, and the growth behaviors of the nanotubes according to water contents has been investigated. Anodization of Ti in ethylene glycol + 1 wt% $NH_4F$ (EG solution) with water additions up to 10 wt% were carried out at the constant voltage of 20 V. The results show that a thin titanium oxide layer is formed in the initial stage and the nanotube structure grows underneath the initial layer. And the length of $TiO_2$ nanotubes decreases with the increasing water content in the solution. It can be ascribed to the locally acidified circumstance around the barrier layer inside the nanopore due to $H^+$ ion originated from water. The XPS for the nanotubes suggests that the spectra of Ti2p and O1s are the major chemical bonding states of the $TiO_2$, and those for F1s, N1s and C1s come from the compound of $(NH_4)_2TiF_6$.

• 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.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2007년도 추계학술대회 논문집
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• pp.306-306
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• 2007

The surface was transformed to porous titanium oxide by the anodization of pure titanium. Titanium was anodized in non-aqueous and aqueous electrolytes at different potentials between 5 V and 150 V. Various electrolytes were compose of ethylene glycerol, $H_2SO_4,\;NH_4F\;and\;H_2O$. We obtained titania nanotube arrays on the micro pore of titanium. Micro pores and nano tubes were obtained by anodization at high potentials and low potentials, respectively. Morphologies of nanotubes and micro pore were characterized by FE-SEM. The unique surface structure is very attractive to electrical and medical applications such as gas sensor, biosensor, dental implant and stent.

• Advances in nano research
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• 제10권3호
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• pp.211-219
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• 2021

The evaluation of the corrosion resistance of titanium with a TiO2 nanotubes top layer was carried out (TiO2 NT). These nanostructures were evolved into anatase nanoparticles without heat treatment in an aqueous medium, which is a novel phenomenon. This work analyzes the layer between the nanotube bottom and the substrate, which is thin and still susceptible to corrosion. The bottom of TiO2 nanotubes having Fluor resulting from the synthesis process changed between amorphous to crystalline anatase with a crystallite size of about 4 nm, which influenced the corrosion rates. Four kinds of samples were evaluated. A) NT by Ti anodizing; B) NTSB for Ti plates, either modifying its surface or anodizing the modified surface; C) NT-480 for anodized Ti and heat-treated (480℃) for reaching the anatase phase; D) NTSB-480 for Ti plates, first, modifying its surface using sandblast, after that, anodizing the modified surface, and finally, heat-treated to 480℃ to compare with samples having induced crystallization and passivation. Four electrochemical techniques were used to evaluate the corrosion rates. The surfaces having TiO2 nanotubes with a sandblast pre-treatment had the highest resistance to corrosion.

• Bulletin of the Korean Chemical Society
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• 제30권8호
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• pp.1798-1804
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• 2009

In this study, we have studied on improved performance of carbon nanotubes/titanium (CNT/TiO2) structure electrode for methylene blue (MB). The composite electrodes consisting of CNTs and a titanium oxide matrix with phenol resin binder was fabricated with a mixture method. The chemical and morphological structure of CNT/Ti$O_2$ composites were characterized by means of BET surface area, X-ray diffraction (XRD), scanning electron microscopy (SEM), UV-Vis absorption technique, Raman spectroscopy and energy dispersive X-ray (EDX). The electrode showed a remarkably enhanced performance for MB oxidation under UV illumination with or without electro-chemical reaction (ECR). Such a remarkably improved performance of the CNT/Ti$O_2$ structure electrode might be due to the enhanced MB oxidation by electro- and photo-generated electrons and holes in the CNTs and Ti$O_2$ under UV illumination with or without ECR.

• 한국재료학회지
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• 제17권1호
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• pp.6-10
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• 2007

In the present study, we investigated the formation of self-organized nanostructure oxide layers on CP Ti and Ti-10Ta-10Nb alloy in an electrolyte of 1M phosphoric acid and 1.5 wt% Hydrofluoric acid. The morphology of oxide film on substrate was observed using scanning electron microscopy and transmission electron microscopy The surface roughness of titanium oxide film was analyzed by atomic force microscopy and the crystalline of specimen was investigated using X-ray diffractometer. The results of this study showed that well-aligned titanium oxide nanotubes are formed with diameter of approx. 100nm and length of approx. 500nm with CP Ti. However, it is clear that TiTaNb alloy highly irregular structure with various diameters. Transmission electron microscope investigations show that the specimens were confirmed as amorphous. Such titanium oxide nanotubes are expected a well-adhered bioacitive surface layer on titanium substrate for orthopedics and dental implants.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2018년도 춘계학술대회 논문집
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• pp.75-75
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• 2018

Commercially pure titanium (CP-Ti) and Ti-6Al-4V alloys have been widely used in implant materials such as dental and orthopedic implants due to their corrosion resistance, biocompatibility, and good mechanical properties. However, surface modification of titanium and titanium alloys is necessary to improve osseointegration between implant surface and bone. Especially, when titanium oxide nanotubes are formed on the surface of titanium alloy, cell adhesion is greatly improved. In addition, plasma electrolytic oxide (PEO) coatings have a good safety for osseointegration and can easily and quickly form coatings of uniform thickness with various pore sizes. Recently, the effects of bone element such as magnesium, zinc, strontium, silicon, and manganese for bone regeneration are researching in dental implant field. The purpose of this study was researched on the surface morphology of PEO-treated Ti-6Al-4V alloy after anodic titanium oxide treatmentusing various instruments. Ti-6Al-4V ELI disks were used as specimens for nanotube formation and PEO-treatment. The solution for the nanotube formation experiment was 1 M $H_3PO_4$ + 0.8 wt. % NaF electrolyte was used. The applied potential was 30V for 1 hours. The PEO treatment was performed after removing the nanotubes by ultrasonics for 10 minutes. The PEO treatment after removal of the nanotubes was carried out in the $Ca(CH_3)_2{\cdot}H_2O+(CH_3COO)_2Mg{\cdot}4H_2O+Mn(CH_3COO)_2{\cdot}4H_2O+Zn(CH_3CO_2)_2Zn{\cdot}2H_2O+Sr(CH_2COO)_2{\cdot}0.5H_2O+C_3H_7CaO_6P$ and $Na_2SiO_3{\cdot}9H_2O$ electrolytes. And the PEO-treatment time and potential were 3 minutes at 280V. The morphology changes of the coatings on Ti-6Al-4V alloy surface were observed using FE-SEM, EDS, XRD, AFM, and scratch tester. The morphology of PEO-treated surface in 5 ion coating solution after nanotube removal showed formation or nano-sized mesh and micro-sized pores.