• Korean Journal of Metals and Materials
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• v.46 no.6
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• pp.370-376
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• 2008

The formation of anodic oxide film of titanium (Ti) was studied at a variety of electrolyte concentrations and current density to clarify their effects on morphology, microstructure and composition of Ti oxide layer. For the analysis of the Ti oxide films, a scanning electron microscopy (SEM), X-ray diffractometer (XRD), and X-ray photoelectron spectroscopy (XPS) were used. The results showed that the concentration of phosphoric acid played a crucial role in the crystalline structure of the Ti oxide layer while the current density gave a critical effect on the thickness and diameter of its pore. In particular, the crystalline anatase phase with a thickness larger than $2{\mu}m$, which is quite desirable for a dental implant application, could be readily prepared at the phosphoric acid concentration of 0.5 M and current density higher than $2.0A/dm^2$.

• Corrosion Science and Technology
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• v.6 no.6
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• pp.316-321
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• 2007

The effect of annealing on the pitting corrosion resistance of anodized Al-Mg alloy (AA5052) processed by equal-channel angular pressing (ECAP) was investigated by electrochemical techniques in a solution containing 0.2 mol/L of $AlCl_3$ and also by surface analysis. The Al-Mg alloy was annealed at a fixed temperature between 473 and 573 K for 120 min in air after ECAP. Anodizing was conducted for 40 min at $100-400A/m^2$ at 293 K in a solution containing 1.53 mol/L of $H_2SO_4$ and 0.0185 mol/L of $Al_2(SO_4)_3$. The internal stress generated in anodic oxide films during anodization was measured with a strain gauge to clarify the effect of ECAP on the pitting corrosion resistance of anodized Al-Mg alloy. The time required to initiate the pitting corrosion of anodized Al-Mg alloy was shorter in samples subjected to ECAP, indicating that ECAP decreased the pitting corrosion resistance. However, the pitting corrosion resistance was greatly improved by annealing after ECAP. The time required to initiate pitting corrosion increased with increasing annealing temperature. The strain gauge attached to Al-Mg alloy revealed that the internal stress present in the anodic oxide films was compressive stress, and that the stress was larger with ECAP than without. The compressive internal stress gradually decreased with increasing annealing temperature. Scanning electron microscopy showed that cracks occurred in the anodic oxide film on Al-Mg alloy during initial corrosion and that the cracks were larger with ECAP than without. The ECAP process of severe plastic deformation produces large internal stresses in the Al-Mg alloy; the stresses remain in the anodic oxide films, increasingthe likelihood of cracks. It is assumed that the pitting corrosion is promoted by these cracks as a result of the higher internal stress resulting from ECAP. The improvement in the pitting corrosion resistance of anodized AlMg alloy as a result of annealing appears to be attributable to a decrease in the internal stresses in anodic oxide films

• Corrosion Science and Technology
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• v.6 no.6
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• pp.275-281
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• 2007

The effect of annealing on the pitting corrosion resistance of anodized Al-Mg alloy (AA5052) processed by equal-channel angular pressing (ECAP) was investigated by electrochemical techniques in a solution containing 0.2 mol/L of $AlCl_3$ and also by surface analysis. The Al-Mg alloy was annealed at a fixed temperature between 473 and 573 K for 120 min in air after ECAP. Anodizing was conducted for 40 min at $100-400A/m^2$ at 293 K in a solution containing 1.53 mol/L of $H_2SO_4$ and 0.0185 mol/L of $Al_2(SO_4)_3$. The internal stress generated in anodic oxide films during anodization was measured with a strain gauge to clarify the effect of ECAP on the pitting corrosion resistance of anodized Al-Mg alloy. The time required to initiate the pitting corrosion of anodized Al-Mg alloy was shorter in samples subjected to ECAP, indicating that ECAP decreased the pitting corrosion resistance. However, the pitting corrosion resistance was greatly improved by annealing after ECAP. The time required to initiate pitting corrosion increased with increasing annealing temperature. The strain gauge attached to Al-Mg alloy revealed that the internal stress present in the anodic oxide films was compressive stress, and that the stress was larger with ECAP than without. The compressive internal stress gradually decreased with increasing annealing temperature. Scanning electron microscopy showed that cracks occurred in the anodic oxide film on Al-Mg alloy during initial corrosion and that the cracks were larger with ECAP than without. The ECAP process of severe plastic deformation produces large internal stresses in the Al-Mg alloy; the stresses remain in the anodic oxide films, increasingthe likelihood of cracks. It is assumed that the pitting corrosion is promoted by these cracks as a result of the higher internal stress resulting from ECAP. The improvement in the pitting corrosion resistance of anodized AlMg alloy as a result of annealing appears to be attributable to a decrease in the internal stresses in anodic oxide films

• Korean Journal of Materials Research
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• v.17 no.11
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• pp.593-600
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• 2007

Aluminum was anodized in a $H_2SO_4$ solution, and titanium (IV) oxide ($TiO_2$) was electrodeposited into nanopores of anodic porous alumina in a mixed solution of $TiOSO_4$ and $(COOH)_2$. The photocatalytic activity of the prepared film was analyzed for photodegradation of methylene blue aqueous solution. Consequently, we found it was possible to electrodeposit $TiO_2$ onto anodic porous alumina, and synthesized it into the nanopores by hydrolysis of a titanium complex ion under AC 8-9 V when film thickness was about $15-20{\mu}m$. The photocatalytic activity of $TiO_2$-loaded anodic porous alumina ($TiO_2/Al_2O_3$) at an impressed voltage of 9 V was the highest in every condition, being about 12 times as high as sol-gel $TiO_2$ on anodic porous alumina. The results revealed that anodic porous alumina is effective as a substrate for photocatalytic film and that high-activity $TiO_2$ film can be prepared at low cost.

• Bulletin of the Korean Chemical Society
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• v.20 no.11
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• pp.1340-1344
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• 1999

The electrochemical behavior of oxide layers on aluminium was studied using electrochemical impedance spectroscopy. Impedance spectra were taken at a compact and a porous oxide layer of Al. The anodic films on Al have a variable stoichiometry with gradual reduction of oxygen deficiency towards the oxide-electrolyte interface. Thus, the interpretation of impedance spectra for oxide layers is complicated, with the impedance of surface layers differing from those of ideal capacitors. This layer behavior with conductance gradients was caused by an inhomogeneous dielectric. The frequency response cannot be described by a single RC element. The oxide layers of Al are properly described by the Young model of dielectric constant with a vertical decay of conductivity.

• Journal of the Korean institute of surface engineering
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• v.12 no.3
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• pp.167-173
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• 1979

The structure of anodic aluminium oxide films formed in 2% oxalic asid at constant temperature was studied by the oid of the transmission and replica electron microscopy. Far the initial stage of oxidations, it is observed that pores are initiated from lattice defects as subgrain boundaries, and then spread radially. Some pores merge each other and the others cease to grow until the current density reaches to the steady state. The pore diameter and the cell size are proportional to the anodizing voltages, and it is considered that the pore initiation and growth are largely controlled by the field - assisted oxide dissolution.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2006.06a
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• pp.545-546
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• 2006

This study was performed to investigate the surface properties of electrochemically oxidized pure titanium by anodic spark discharging method. Commercially pure titanium plates of $10{\times}20{\times}1[mm]$ in dimensions were polished sequentially emery paper. Anodizing was performed at current density of $76.2\;[mA/cm^2]$, application voltage of 290, 350, 400 [V] using a regulated DC power supply, which allowed automatic transition constant current when a preset maximum voltage has been reached. The Ti surface oxided films was characterized by scanning electron microscope(SEM). The precipitation of HA(Hydroxyapatite) crystals on anodized surface was greatly accelerated by hydrothermal treatment. The concentrations of DL-$\alpha$-Glycerolphosphate Magnesiurn(DL-$\alpha$-GP-Mg) salt and Ca acetate in an electrolyte was highly affected the precipitation of HA crystals converted by Ti Anodized oxide films by Shape of Impulse Voltage.

• Bulletin of the Korean Chemical Society
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• v.20 no.9
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• pp.1049-1055
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• 1999

Electrochemical oxidation of silicon (p-type Si(100)) at room temperature in ethylene glycol and in aqueous solutions has been performed by applying constant low current densities for the preparation of thin SiO2 layers. In-situ ac impedance spectroscopic methods have been employed to characterize the interfaces of electrolyte/oxide/semiconductor and to estimate the thickness of the oxide layer. The thicknesses of SiO2 layers calculated from the capacitive impedance were in the range of 25-100Å depending on the experimental conditions. The anodic polarization resistance parallel with the oxide layer capacitance increased continuously to a very large value in ethylene glycol solution. However, it decreased above 4 V in aqueous solutions, where oxygen evolved through the oxidation of water. Interstitially dissolved oxygen molecules in SiO2 layer at above the oxygen evolution potential were expected to facilitate the formation of SiO2 at the interfaces. Thin SiO2 films grew efficiently at a controlled rate during the application of low anodization currents in aqueous solutions.

• Applied Chemistry for Engineering
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• v.28 no.6
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• pp.601-606
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• 2017

One-dimensional nanostructured metal oxide can be formed through an anodic oxidation, which is a typical technique of metal surface treatment. Studies on $TiO_2$ nanotubes have been widely carried out with increasing interests in $TiO_2$, which has an excellent functionality among various metal oxides. The present article reviews the principles of formation of $TiO_2$ nanotubes, which have been studied so far. In particular, the article discussed the equilibrium relationship between the oxide formation and etching, which is a key parameter of $TiO_2$ nanotube growth, and the formation of the porous structure. Furthermore, morphological considerations of $TiO_2$ nanotubes according to electrolyte conditions will be explained to the researchers who will study the application of $TiO_2$ nanotubes formed through the anodic oxidation in the future.

• 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).