• 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.

• 한국재료학회지
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• 제12권5호
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• pp.353-358
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• 2002

The microstructure and growth behaviors of anodic oxide layers on titanium were investigated. $TiO_2$ oxide films were prepared by anodizing at constant voltages of 180 and 200V in sulfuric acid electrolyte. The anodic $TiO_2$ layer formed at 200V showed a cell structure with more irregular pore shapes around the interface between the anodic oxide layer and the substrate titanium compared with that formed at 180V. Irregular shape of pores at the initial stage of anodization seemed to be attributed to spark discharge phenomena which heavily occurred during increasing voltages. The thickness of the anodic oxide film increased linearly at a rate of $1.9{\times}10^{ -1}\mu\textrm{m}$/min. The oxide layers formed at 180 and 200V were composed mainly of anatase structure, and the anodizing process could be suggested as one of fabrication methods of photocatalytic $TiO_2$.

• 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.

• 한국재료학회지
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• 제12권2호
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• pp.121-128
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• 2002

Anodic alumina layer can be used as templates for preparation of nano-structured materials, because porous oxide layer on aluminum shows a uniform pore size and a high pore density. In order to find out possibility for template material to prepare nano wire, the effects of the anodic applied potential, anodic time and the temperature of electrolyte on pore diameter of anodic alumina layer were studied using SEM and AFM. The pore diameter of anodic alumina layer increased with applied anodic potential and electrolytic temperature. Especially, the pore diameter of anodic oxide layers formed in chromic acid can be well replicated by widening process in $H_3$$PO_4$solution.

• 한국표면공학회지
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• 제47권4호
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• pp.155-161
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• 2014

The present work is concerned with the formation behavior of anodic oxide films on Al7075 alloy under a galvanostatic condition in 20 vol.% sulfuric acid solution. The formation behaviour of anodic oxide films was studied by the analyses of voltage-time curves and observations of colors, morphologies and thicknesses of anodic films with anodization time. Hardness of the anodic oxide films was also measured with anodization time and at different positions in the anodic films. Six different stages were observed with anodiziation time : barrier layer formation (stage I), pore formation (stage II), growth of porous films (stage III), abnormal rapid oxide growth (stage IV), growth of non-uniform oxide films (stage V) and breakdown of the thick oxide films under high anodic voltages (stage VI). Hardness of the anodic oxide films appeared to decrease with increasing anodization time and with the position towards the outer surface. This work provides useful information about the thickness, uniformity, imperfections and hardness distribution of the anodic oxide films formed on Al7075 alloy in sulfuric acid solution.

• Corrosion Science and Technology
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• 제20권3호
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• pp.152-157
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• 2021

Stainless steel is a metal that does not generate rust. Due to its excellent workability, economic feasibility, and corrosion resistance, it is used in various industrial fields such as ships, piping, nuclear power, and machinery. However, stainless steel is vulnerable to corrosion in harsh environments. To solve this problem, its corrosion resistance could be improved by electrochemically forming an anodized film on its surface. In this study, 316L stainless steel was anodized at room temperature with ethylene glycol-based 0.1 M NH₄F and 0.1M H₂O electrolyte to adjust the thickness of the oxide film using different anodic oxidation voltages (30 V, 50 V, and 70 V) with time control. The anodic oxidation experiment was performed by increasing the time from 1 hour to 7 hours at 2-hour intervals. Corrosion resistance according to the thickness of the anodic oxide film was observed. Electrochemical corrosion behavior of oxide films was investigated through polarization experiments.

• 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.

• 한국세라믹학회지
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• 제28권6호
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• pp.443-450
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• 1991

Microstructures of tantalum oxide, anodic-oxidized in oxalic acid, are shown to be related to voltage-time characteristics during formation reaction. It is observed that a crystalline phase transformed from an amorphous phase is recrystallized in the presence of the high electric field within the film, and this recrystallized film has a very porous microstructure. From the results of the XRD, the nonlinearity observed after the first spark voltage is recognized to be due to the local crystallization.

• 한국표면공학회지
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• 제21권2호
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• pp.68-75
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• 1988

To know the growth behavior of Conductive polyaniline file, the anodic oxidation of anilien on a platiunm in aqueous sulfuric acid solution has been studied. Cyclic votammetry and currenttime transisents method used to investigate the anodic oxidation of aniline to polyaniline films on a platinum. The oxidation of aniline is shown to occur in several steps dependent on the potential. it the phase growth resembles the deposition of a metal film.

• 한국표면공학회지
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• 제22권3호
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• pp.145-153
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• 1989

양극산화 피막의 형성 반응에 대한 연구는 1930년대부터 되어 왔으며, 특히 High Field Conduction에 대한 물리학자들의 관심도는 아주 높아었다. 1960년대 이르러 비정질 구조에 대한 심도 있는 연구가 진행되면서, 여러 가지 이론적으로 풀지 못하는 실험실적 결과들에 대한 제한들이 나오게 되었고, Ionic Migration Process에 대한 Kinetics는 많은 발전을 보게 되었다. 최근까지의 연구결과, Ioinc Conduction Mechanism은 Anodic Film의 미세 결정 구조와 밀접한 연관성을 가진다는 결론에 도달하였고, 비정질 구조의 High Field하에서의 거동에 대한 새로운 분야의 연구가 진행되고 있다. 본 고에서는 반응 Mechanism에 관한 연구결과들을 1930년대 이후 어떻게 진행되어 설명 되었는가를 조명하므로서 실제 실험 결과의 해석게 도움이 되었으면 하는 바램이다.