• Bulletin of the Korean Chemical Society
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• 제24권7호
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• pp.975-980
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• 2003

The electrochemical properties and the mechanism of formation of anodic oxide films on Mg alloys containing 0-15 mass% Al, when anodized in NaOH solution, were investigated by focusing on the effects of anodizing potential, Al content, and anodizing time. The intensity ratio of Mg(OH)₂ in the XRD analysis decreased with increasing applied potential, while that of MgO increased. Mg(OH)₂ was barely detected at 80 V, while MgO was readily detected. The anti-corrosion properties of anodized specimens at each constant potential were better than those of non-anodized specimens. The specimen anodized at an applied potential of 3 V had the best anti-corrosion property. The intensity ratio of the β phase increased with aluminum content in Mg-Al alloys. During anodizing, the active dissolution reaction occurred preferentially in β phase until about 4 min, and then the current density increased gradually until 7 min. The dissolution reaction progressed in α phase, which had a lower Al content. In the anodic polarization test in 0.017 mol·$dm^{-3}$ NaCl and 0.1 mol·$dm^{-3}$ Na₂SO₄ at 298 K, the current density of Mg-15 mass% Al alloy anodized for 10 min increased, since the anodic film that forms on the α phase is a non-compacted film. The anodic film on the α phase at 30 min was a compact film as compared with that at 10 min.

• 한국표면공학회지
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• 제56권3호
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• pp.169-179
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• 2023

This work studies dielectric breakdown behavior of AAO (anodic aluminum oxide) films formed on pure aluminum at a constant current density in 5 ~ 20 vol.% sulfuric acid (SA) and 2 ~ 8 wt.% oxalic acid (OA) solutions. It was observed that dielectric breakdown voltage of AAO film with the same thickness increased with increasing concentration of both SA and OA solutions up to 15 vol.% and 6 wt.%, respectively, above which it decreased slightly. The dielectric breakdown resistance of the OA films appeared to be superior to that of SA films. After dielectric breakdown test, cracks and a hole were observed. The crack length increased with increasing SA film thickness but it did not increase with increasing OA film thickness. To explain the reason why shorter cracks formed on the OA films than the SA films after dielectric breakdown test, the generation of tensile stresses at the oxide/metal interface was discussed in relation to porosity of AAO films obtained from cross-sectional morphologies.

• 대한화학회지
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• 제56권5호
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• pp.542-547
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• 2012

Borate 완충용액에서 Fe의 산화 반응 경로와 생성된 산화피막의 전기적 특성을 조사하였다. Fe는 pH에 의존하는 두 가지의 반응 경로에 의하여 산화되었으며 산화된 피막은 Mott-Schottky 식이 적용되는 n-형 반도체 성질을 가지고 있음을 알 수 있었다.

• 한국표면공학회지
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• 제57권1호
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• pp.8-13
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• 2024

Anodizing of Al6061 alloy was conducted in two different electrolytes of 20% sulfuric acid and 8% sulfuric acid + 3 % oxalic acid solutions at a constant current or decreasing current density conditions, and its dielectric breakdown voltage was measured. The surface morphology of anodic oxide films was observed by TEM and thermal treatment was carried out at 400 ℃ for 2 h to evaluate the resistance of the anodic oxide films to crack initiation. The anodic oxide film formed in 8% sulfuric acid + 3 % oxalic acid solution showed higher dielectric breakdown voltage and better resistance to crack initiation at 400 ℃ than that formed in 20% sulfuric acid solution. The dielectric breakdown voltage increased 6 ~12% by applying decreasing current density comparing with a constant current density.

• 한국표면공학회지
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• 제50권1호
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• pp.17-23
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• 2017

This work demonstrates arc generation and anodic film formation behaviors on Al1050 alloy during PEO (plasma electrolytic oxidation) treatment under a constant direct current in an alkaline electrolyte containing silicate, carbonate and borate ions. Only one big arc more than 2 mm diameter was generated first at the edges and it was moving on the fresh surface or staying occasionally at the edges, resulting in the local burning due to generation of an extremely big orange colored arc at the edges. Central region of the flat surface was not fully covered with PEO films even after sufficiently long treatment time because of the local burning problem. The anodic oxides formed on the flat surface by arcing once were found to consist of a number of small oxide nodules with spherical shape of $3{\sim}6{\mu}m$ size and irregular shapes of about $5{\sim}10{\mu}m$ width and $10{\sim}20{\mu}m$ length. The anodic oxide nodules showed uniform thickness of about $3{\mu}m$ and rounded edges. These experimental results suggest that one big arc observed on the specimen surface under the application of a constant direct current is composed of a number of small micro-arcs less than $20{\mu}m$ size.

• Applied Science and Convergence Technology
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• 제27권1호
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• pp.9-13
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• 2018

Samples of anodic oxide film used in semiconductor and display manufacturing processes were prepared at different electrolyte temperatures to investigate the corrosion resistance. The anodic oxide film was grown on aluminum alloy 6061 by using a sulfuric acid ($H_2SO_4$) electrolyte of 1.5 M at $0^{\circ}C$, $5^{\circ}C$, $10^{\circ}C$, $15^{\circ}C$, and $20^{\circ}C$. The insulating properties of the samples were evaluated by measuring the breakdown voltage, which gradually increased from 0.43 kV ($0^{\circ}C$) to 0.52 kV ($5^{\circ}C$), 1.02 kV ($10^{\circ}C$), and 1.46 kV ($15^{\circ}C$) as the electrolyte temperature was increased from $0^{\circ}C$ to $15^{\circ}C$, but then decreased to 1.24 kV ($20^{\circ}C$). To evaluate the erosion of the film by fluorine plasma, the plasma erosion and the contamination particles were measured. The plasma erosion was evaluated by measuring the breakdown voltage after exposing the film to $CF_4/O_2/Ar$ and $NF_3/O_2/Ar$ plasmas. With exposure to $CF_4/O_2/Ar$ plasma, the breakdown voltage of the film slightly decreased at $0^{\circ}C$, by 0.41 kV; however, the breakdown voltage significantly decreased at $20^{\circ}C$, by 0.83 kV. With exposure to $NF_3/O_2/Ar$ plasma, the breakdown voltage of the film slightly decreased at $0^{\circ}C$, by 0.38 kV; however, the breakdown voltage significantly decreased at $20^{\circ}C$, by 0. 77 kV. In addition, for the entire temperature range, the breakdown voltage decreased more when sample was exposed to $NF_3/O_2/Ar$ plasma than to $CF_4/O_2/Ar$ plasma. The decrease of the breakdown voltage was lower in the anodic oxide film samples that were grown slowly at lower temperatures. The rate of breakdown voltage decrease after exposure to fluorine plasma was highest at $20^{\circ}C$, indicating that the anodic oxide film was most vulnerable to erosion by fluorine plasma at that temperature. Contamination particles generated by exposure to the $CF_4/O_2/Ar$ and $NF_3/O_2/Ar$ plasmas were measured on a real-time basis. The number of contamination particles generated after the exposure to the respective plasmas was lower at $5^{\circ}C$ and higher at $0^{\circ}C$. In particular, for the entire temperature range, about five times more contamination particles were generated with exposure to $NF_3/O_2/Ar$ plasma than for exposure to $CF_4/O_2/Ar$ plasma. Observation of the surface of the anodic oxide film showed that the pore size and density of the non-treated film sample increased with the increase of the temperature. The change of the surface after exposure to fluorine plasma was greatest at $0^{\circ}C$. The generation of contamination particles by fluorine plasma exposure for the anodic oxide film prepared in the present study was different from that of previous aluminum anodic oxide films.

• 한국표면공학회지
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• 제42권6호
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• pp.260-266
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• 2009

The anodic oxidation behaviour of a cast component of AC2A Al alloy with machined surface and ascast surface was investigated in sulfuric acid solution. The anodized specimen showed relatively uniform and thick anodic oxide films on the as-cast surface, while non-uniform and very thin oxide films were formed on the machined surface. Non-anodized as-cast surface was observed to be covered with thick oxide scales and showed a number of second-phase particles containing Si, while non-anodized machined surface showed no oxide scales and relatively very small number of Si particles. Thus, the very limited growth of anodic oxide films on the as-cast surface was attributed to the presence of thick oxide scales and Si-containing second-phase particles on its surface.

• 한국표면공학회지
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• 제53권1호
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• pp.15-21
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• 2020

In this study, growth and burning behavior of 6061 aluminum alloy was studied under constant anodic voltages at various temperatures and magnetic stirring rates in 20% sulfuric acid solution by analysing I-t curves, measuring thickness and hardness of aluminum anodic oxide (AAO) films, observations of surface and cross-sectional images of AAO films. AAO films were grown continuously at lower voltages than 18.5V but burning occurred when a voltage more than 19V was applied in 20% H₂SO₄ solution at 20±0.5℃ and 200 rpm of magnetic stirring. The burning was always related with an extremely large increase of anodic current density with anodizing time, suggesting that high heat generation during anodizing causes deteriorations of AAO films by chemical reaction with acidic solutions. The burning resulted in decreases of film thickness and hardness, surface color brightened and formation of porous defects in the AAO films. The burning voltage was found to decrease with increasing solution temperature and decreasing magnetic stirring rate. The decreased burning voltages seem to be closely related with increased chemical reactions between AAO films and hydrogen ions.

• Corrosion Science and Technology
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• 제7권3호
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• pp.168-172
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• 2008

A new type of electrochemical random signal (electrochemical noise) analysis technique was applied to localized corrosion of anodic oxide film formed 1100 aluminum alloy in $0.5kmol/m^3$ $H_3BO_4/0.05kmol/m^3$ $Na_2B_4O_7$ with $0.01kmol/m^3$ NaCl. The effect of anodic oxide film structure, barrier type, porous type, and composite type on galvanic corrosion resistance was also examined. Before localized corrosion started, incubation period for pitting corrosion, both current and potential slightly change as initial value with time. The incubation period of porous type anodic oxide specimens are longer than that of barrier type anodic oxide specimens. While pitting corrosion, the current and potential were changed with fluctuations and the potential and the current fluctuations show a good correlation. The records of the current and potential were processed by calculating the power spectrum density (PSD) by the Fast Fourier Transform (FFT) method. The potential and current PSD decrease with increasing frequency, and the slopes are steeper than or equal to minus one (-1). This technique allows observation of electrochemical impedance changes during localized corrosion.

• 한국표면공학회지
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• 제32권3호
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• pp.235-238
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• 1999

Silicon dioxide films were prepared by anodizing silicon wafers in an ethylene $glycol+HNO_3(0.04{\;}N)$ at 20 to $70^{\circ}C$. The voltage between silicon anode and platinum cathode was measured during this process. Under the constant current electrolysis, the voltage increased with oxide film growth. The transition time at which the voltage reached the predetermined value depended on the temperature of the electrolyte. After the time of electrolysis reached the transition time, the anodization was changed the constant voltage mode. The depth profile of oxide film/Si substrate was confirmed by XPS analysis to study the influence of the electrolyte temperature on the anodization. Usually, the oxide-silicon peaks disappear in the silicon substrate, however, this peak was not small at $45^{\circ}C$ in this region.