• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.152-152
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• 2016

Anodizing is a technology to generate thicker and high-quality films than natural oxide films by treating metals via electrochemical methods. It is a technique to develop metals for various uses, and extensive research on the commercial use has been performed for a long time. Aluminum anodic oxide (AAO) is generate oxide films, whose sizes and characteristics depending on the types of electrolytes, voltages, temperatures and time. Electrochemical manufacturing method of nano structure is an efficient technology in terms of cost reduction, high productivity and complicated shapes, which receives the spotlight in diverse areas. The sulfuric acid was used as an anodizing electrolyte, controlling its temperature to $10^{\circ}C$. The anode was 5083 Al alloy with dimension of $5(t){\times}20{\times}20mm$ while the cathode was the platinum. The distance between the anode and the cathode was maintained at 3 cm. Agitation was introduced by magnetic stirrer at 300 rpm to prevent localized temperature rise that hinders stable growth of oxide layer. In order to observe surface characteristics with applied current density, the electrolyte temperature, concentration was maintained at constant condition for $10^{\circ}C$, 10 vol.%, respectively. To prevent hindrance of stable growth of oxide layer due to local temperature increase during the experiment, stirring was maintained at constant rate. In addition, using galvanostatic method, it was maintained at current density of $10{\sim}30mA/cm^2$ for 40 minutes. The cavitation experiment was carried out with an ultrasonic vibratory apparatus using piezo-electric effect with modified ASTM-G32. The peak-to-peak amplitude was $30{\mu}m$ and the distance between the horn tip and specimen was 1 mm. The specimen after the experiment was cleaned in an ultrasonic, dried in a vacuum oven for more than 24 hours, and weighed with an electric balance. The surface damage morphology was observed with 3D analysis microscope. As a result of the investigation, differences were observed surface hardness and anti-cavitation characteristics depending on the development of oxide film with applied current density.

• The Journal of Korean Academy of Prosthodontics
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• v.45 no.1
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• pp.85-97
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• 2007

Statement of problem: Recently, anodic oxidation of cp-titanium is a popular method for treatment of titanium implant surfaces. It is a relatively easy process, and the thickness, structure, composition, and the microstructure of the oxide layer can be variably modified. Moreover the biological properties of the oxide layer can be controlled. Purpose: In this study, the roughness, microstructure, crystal structure of the variously treated groups (current, voltage, frequency, electrolyte, thermal treatment) were evaluated. And the specimens were soaked in simulated body fluid (SBF) to evaluate the effects of the surface characteristics and the oxide layers on the bioactivity of the specimens which were directly related to bone formation and integration. Materials and methods: Surface treatments consisted of either anodization or anodization followed thermal treatment. Specimens were divided into seven groups, depending on their anodizing treatment conditions: constant current mode (350V for group 2), constant voltage mode (155V for group 3), 60 Hz pulse series (230V for group 4, 300V for group 5), and 1000 Hz pulse series (400V for group 6, 460V for group 7). Non-treated native surfaces were used as controls (group 1). In addition, for the purpose of evaluating the effects of thermal treatment, each group was heat treated by elevating the temperature by $5^{\circ}C$ per minute until $600^{\circ}C$ for 1 hour, and then bench cured. Using scanning electron microscope (SEM), porous oxide layers were observed on treated surfaces. The crystal structures and phases of titania were identified by thin-film x-ray diffractmeter (TF-XRD). Atomic force microscope (AFM) was used for roughness measurement (Sa, Sq). To evaluate bioactivity of modified titanium surfaces, each group was soaked in SBF for 168 hours (1 week), and then changed surface characteristics were analyzed by SEM and TF-XRD. Results: On basis of our findings, we concluded the following results. 1. Most groups showed morphologically porous structures. Except group 2, all groups showed fine to coarse convex structures, and the groups with superior quantity of oxide products showed superior morphology. 2. As a result of combined anodization and thermal treatment, there were no effects on composition of crystalline structure. But, heat treatment influenced the quantity of formation of the oxide products (rutile / anatase). 3. Roughness decreased in the order of groups 7,5,2,3,6,4,1 and there was statistical difference between group 7 and the others (p<0.05), but group 7 did not show any bioactivity within a week. 4. In groups that implanted ions (Ca/P) on the oxide layer through current and voltage control, showed superior morphology, and oxide products, but did not express any bioactivity within a week. 5. In group 3, the oxide layer was uniformly organized with rutile, with almost no titanium peak. And there were abnormally more [101] orientations of rutile crystalline structure, and bonelike apatite formation could be seen around these crystalline structures. Conclusion: As a result of control of various factors in anodization (current, voltage, frequency, electrolytes, thermal treatment), the surface morphology, micro-porosity, the 2nd phase formation, crystalline structure, thickness of the oxide layer could be modified. And even more, the bioactivity of the specimens in vitro could be induced. Thus anodic oxidation can be considered as an excellent surface treatment method that will able to not only control the physical properties but enhance the biological characteristics of the oxide layer. Furthermore, it is recommended in near future animal research to prove these results.

• Journal of the Korean institute of surface engineering
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• v.51 no.1
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• pp.21-26
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• 2018

The $Cu_2(btc)_3$ metal-organic frameworks (MOF) coated anodic aluminum oxide (AAO) membrane was successfully prepared by layer-by-layer technique using hand spray method. It was confirmed that the $Cu_2(btc)_3$ layer, which has the pore sized in 2-3 nm, on surface of AAO exhibited the polycrystalline thin film structure by XRD analysis. More than 100 repetitive spray cycles were required to obtain more robust and thick MOFs on AAO and it was possible to uniformly coat both the top and bottom surfaces of the AAO. It should be noted that the MOFs also could be coated on surface of pores resulting in reduce the size of pore from 52 nm to 32 nm.

• Proceedings of the Korean Institute of Information and Commucation Sciences Conference
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• 2010.05a
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• pp.814-817
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• 2010

AAO thin films prepared by a two-step anodization process have pores that are uniform in diameter, highly ordered, and perfectly vertical with respect to the plane of the nano template. Further, the pore size and interpore distance can be easily controlled by varying the anodizing voltage and acid electrolyte. When metals are electrochemically deposited in the pores, metal nanowires that are highly ordered and uniform in diameter are formed in each pore.

• Proceedings of the Materials Research Society of Korea Conference
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• 2003.11a
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• pp.128-128
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• 2003

Electrochromism (EC) is defined as a phenomenon in which a change in color takes place in the presence of an applied voltage. Because of their low power consumption, high coloration efficiency, EC devices have a variety of potential applications in smart windows, mirror, and optical switching devices. An EC devices generally consist of a transparent conducting layer, electrochromic cathodic and anodic coloring materials and an ion conducting electrolyte. EC has been widely studied in transition metal oxides(e.g., WO$_3$, NiO, V$_2$O$\sub$5/) Among these materials, WO$_3$ is a most interesting material for cathodic coloration materials due to its lush coloration efficiency (CE), large dynamic range, cyclic reversibility, and low cost material. WO$_3$ films have been prepared by a variety of methods including vacuum evaporation, chemical vapor deposition, electrodeposition process, sol-gel synthesis, sputtering, and laser ablation. Sol-gel process is widely used for oxide film at low temperature in atmosphere and requires lower capital investment to deposit large area coating compared to vacuum deposition process.

• Journal of the Korean Vacuum Society
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• v.15 no.1
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• pp.97-102
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• 2006

Anodic alumina with self-organized and ordered nano hole arrays can be a good candidate of an irradiation mask to modify the properties of nano-scale region. In order to try using porous anodic alumina as a mask for ion-beam patterning, ion beam transmittance of anodic alumina was tested. 4 Um thick self-standing AAO templates anodized from Al bulk foil with two different aspect ratio, 200:1 and 100:1, were aligned about incident ion beam with finely controllable goniometer. At the best alignment, the transmittance of the AAO with aspect ratio of 200:1 and 100:1 were $10^{-8}\;and\;10^{-4}$, respectively. However transmittance of the thin film AAO with low aspect ratio, 5:1, were remarkably improved to 0.67. The ion beam transmittance of self-standing porous alumina with a thickness larger than $4{\mu}m$ is extremely low owing to high aspect ratio of nano hole and charging effect, even at a precise beam alignment to the direction of nano hole. $SiO_2$ nano dot array was formed by ion irradiation into thin film AAO on $SiO_2$ film. This was confirmed by scanning electron microscopy that the $SiO_2$ nano dot array is similar to AAO hole array.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2017.05a
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• pp.77-77
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• 2017

Titanium and its alloys offer attractive properties in a variety of applications. These are widely used for the field of biomedical implants because of its good biocompatibility and high corrosion resistance. Titanium anodizing is often used in the metal finishing of products, especially those can be used in the medical devices with dense oxide surface. Based on SAE/AMS (Society of Automotive Engineers/Aerospace Material Specification) 2488D, it has the specification for industrial titanium anodizing that have three different types of titanium anodization as following: Type I is used as a coating for elevated temperature forming; Type II is used as an anti-galling coating without additional lubrication or as a pre-treatment for improving adherence of film lubricants; Type III is used as a treatment to produce a spectrum of surface colours on titanium. In this study, we have focused on Type II anodization for the medical (dental and orthopedic) application, the anodized surface was modified with gray color under alkaline electrolyte. The surface characteristics were analyzed with Focused Ion Beam (FIB), Scanning Electron Microscopy (SEM), surface roughness, Vickers hardness, three point bending test, biocompatibility, and corrosion (potentiodynamic) test. The Ti-6Al-4V alloy was used for specimen, the anodizing procedure was conducted in alkaline solution (NaOH based, pH>13). Applied voltage was range between 20 V to 40 V until the ampere to be zero. As results, the surface characteristics of anodic oxide layer were analyzed with SEM, the dissecting layer was fabricated with FIB method prior to analyze surface. The surface roughness was measured by arithmetic mean deviation of the roughness profile (Ra). The Vickers hardness was obtained with Vickers hardness tester, indentation was repeated for 5 times on each sample, and the three point bending property was verified by yield load values. In order to determine the corrosion resistance for the corrosion rate, the potentiodynamic test was performed for each specimen. The biological safety assessment was analyzed by cytotoxic and pyrogen test. Through FIB feature of anodic surfaces, the thickness of oxide layer was 1.1 um. The surface roughness, Vickers hardness, bending yield, and corrosion resistance of the anodized specimen were shown higher value than those of non-treated specimen. Also we could verify that there was no significant issues from cytotoxicity and pyrogen test.

• Journal of the Korean institute of surface engineering
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• v.51 no.2
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• pp.87-94
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• 2018

Various sealing techniques were applied to the anodized 5083 aluminum alloy for marine environment to reduce corrosion and cavitation erosion damage. Electrochemical experiments and cavitation erosion tests were conducted to evaluate the corrosion resistance and cavitation resistance of the anodic oxide film treated with sealing in natural seawater solution. Then, damaged surface morphology was analyzed by scanning electron microscope(SEM) and 3D microscope. As the results of the electrochemical experiments, it was observed that the surface damage of all the experimental conditions in the anodic polarization experiment was locally grown by the combination of crack and corrosion damage. In the Tafel analysis, the corrosion resistance of all sealing treatment conditions was improved compared to the anodizing. On the other hand, cavitation erosion tests showed that the anodizing and all the sealing treatment conditions generated local pit damage by cavitation erosion attack and grew to crater damage in the observation of damaged surface by SEM. Also, the weight loss and the surface damage depth measured with the experiment time presented that most of the sealing treatment conditions showed better cavitation erosion resistance than the anodizing, and they had an incubation period at the beginning of the experiment.

• Journal of the Korean Chemical Society
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• v.57 no.5
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• pp.547-553
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• 2013

Zirconium oxide ($ZrO_2$) nano porous membranes were fabricated by electrochemical two-step anodization with an electropolished zirconium substrate in inorganic water-based and organic electrolyte systems containing small amounts of fluoride. Using two-step anodization and organic electrolytes, highly regular and ordered nanotubular $ZrO_2$ oxide layers can be compared with aqueous electrolytes. The morphology and size of the nano porous layers were characterized by FE-SEM (field emission scanning electron microscopy), XRD (X-ray diffraction), and EDS (energy dispersive spectroscopy). Luminescence properties were investigated by photoluminescence measurements.

• Journal of the Korean institute of surface engineering
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• v.52 no.5
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• pp.265-274
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• 2019

Formation behavior of PEO (Plasma Electrolytic Oxidation) films on AZ31 Mg alloy was investigated under application of 310 Hz AC as a function of $Na_3PO_4$ concentration from 0.02 M to 0.2 M. Film formation voltage and in-situ observation of arcs generated on the specimen surface were recorded with time, and surface morphologies of the PEO films were investigated using optical microscopy, confocal scanning laser microscopy and scanning electron microscopy. PEO film formation voltage decreased linearly with increasing $Na_3PO_4$ concentration which is attributed to the increase of solution pH. PEO films were grown uniformly over the entire surface in $Na_3PO_4$ solutions between 0.05 M and 0.1 M. However, non-uniform PEO films with white spots were formed in $Na_3PO_4$ solutions containing more than 0.1 M. Thickness and roughness of PEO films on AZ31 Mg alloy increased linearly with increasing $Na_3PO_4$ concentration and their increasing rates appeared to be much higher under 1 M than above 1 M. The experimental results suggest that phosphate ions can contribute to the formation of PEO films but higher $Na_3PO_4$ concentration more than 1 M results in local damages of PEO films due to repeated generation of white arcs at the same surface site of AZ31 Mg alloy.