• 한국표면공학회지
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• 제54권1호
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• pp.30-36
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• 2021

In this study, double-layered anodizing films were formed on Al 5052 and Al 6061 alloys consecutively first in sulfuric acid and then in oxalic acid, and hardness, withstand voltage, surface roughness and acid resistance of the anodizing films were compared with single-layered anodizing films in sulfuric acid and oxalic acid electrolytes. Hardness of the double-layered anodizing film decreased with increasing ratio of inner layer to outer layer for both Al 5052 and Al 6061 alloys, suggesting that outer anodizing film formed in sulfuric acid electrolyte is damaged during the second anodizing in oxalic acid electrolyte. Withstand voltage of the double-layered anodizing films increased with increasing the thickness ratio of inner layer to outer layer. Surface roughness of the double-layered anodizing films were comparable with that of single-layered anodizing film formed in sulfuric acid but higher than that of single layer anodizing film formed in oxalic acid electrolyte. In acid resistance test, all of the double-layered and single-layered anodizing films showed good acid resistance more than 3 h without any visible gas evolution, which is attributable to sealing of pores. Based on the experimental results obtained in this work, it is possible to design a double-layered anodizing film with cost-effectiveness and improved physical and electrical properties by combining two consecutive anodizing processes of sulfuric acid anodizing and oxalic acid anodizing methods.

• 한국융합학회논문지
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• 제7권5호
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• pp.169-173
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• 2016

알루미늄의 양극산화는 황산법, 수산법과 황산과 수산을 활용한 혼산법 등이 있다. 산업체에서 만들어지는 양극산화는 황산법으로 전해액속의 황산농도가 15~20 wt %이다. 연질 양극산화피막을 생성할 경우는 전해액의 온도가 $20{\sim}30^{\circ}C$ 범위에서 생산되고 있으며, 생산 전압은 직류전압으로 13~15 V 이내가 가장 많이 사용된다. 경질 양극산화피막을 생성할 경우는 전해액의 온도가 $0{\sim}-5^{\circ}C$에서 생산되어지고 있다. 본 연구에서는 황산법과 수산법을 이용하여 $50{\mu}m$ 두께의 양극산화피막(알루미나)를 제작하였다. 황산법과 수산법에 의해 시편을 제조하여 열 피로시험을 수행하였다. 황산법과 수산법의 균열발생온도는 $500^{\circ}C$와 $600^{\circ}C$이었다. 황산법의 균열발생온도는 수산법의 균열발생온도보다 낮았다. 시험결과 수산법의 열 피로는 황산법의 열 피로 특성보다 좋았다. 그 이유를 알루미늄과 알루미나의 열팽창계수와 제조온도로 설명하였다. 고온에서 사용되는 양극산화제품의 제조방법을 여기서의 융합 연구를 통해 제안 가능하게 되었다.

• 한국표면공학회지
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• 제51권6호
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• pp.393-399
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• 2018

Formation behavior of aluminum anodic oxide (AAO) films on Al6061 alloy was studied in view of thickness, morphology and defects in the anodic films in 20 vol.% sulfuric acid solution at a constant current density of $40mA/cm^2$, using voltage-time curve, observation of anodized specimen colors and surface and cross-sectional morphologies of anodic films with anodization time. With increasing anodizing time, voltage for film formation increased exponentially after about 12 min and its increasing rate decreased after 25 min, followed by a rapid decrease of the voltage after about 28 min. Surface color of anodized specimen became darker with increasing anodizing time up to about 20 min, while it appeared to be brighter with increasing anodizing time after 20 min. The darkened and brightened surfaces with anodizing time are attributed to an increase in thickness of porous anodic oxide film and a chemical damage of the films due to heat generated by increased resistance of the film, respectively. Cross-sectional observation of AAO films revealed the formation of defects of crack shape at the metal/oxide interface after 15 min which prevents the growth of AAO films. Width and length of the crack-like defect increased with anodizing time up to 25 min of anodizing, and finally the outer part of AAO films was partly dissolved or detached after 30 min of anodizing, resulting in non-uniform surface structures of the AAO films.

• 한국표면공학회지
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• 제52권4호
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• pp.203-210
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• 2019

In this work, anodizing behavior of 6xxx series aluminum alloys was studied under constant current density and constant voltage conditions in 20% sulfuric acid solution by V-t curves, I-t curves, thickness measurement, observations of surface appearance and cross-sectional observation of anodizing films. The film growth rate of the anodizing films on Al6063, Al6061 and Al6082 obtained at 20 V were $0.63{\mu}m/min$. $0.46{\mu}m/min$ and $0.38{\mu}m/min$, respectively. Time to the initiation of imperfections at the oxide/substrate interface under constant current condition was shortened and colors of anodizing films became darker with the amount of alloying elements in 6xxx series aluminum alloys. Based upon the experimental results obtained in this work, it is concluded that maximum anodizing film thickness without interfacial defects is reduced with increasing amount of alloying elements and brighter anodizing films can be obtained by decreasing amount of alloying elements in the aluminum alloys.

• 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.

• 반도체디스플레이기술학회지
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• 제20권1호
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• pp.37-41
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• 2021

We report on the formation of anodic aluminum oxide (AAO) film using sulfuric acid containing cerium salt. When the temperature of the sulfuric acid containing cerium salt changes from 5 ℃ to 20 ℃, the current density and the thickness growth rate increase. The surface morphology of the AAO film change according to the temperature of the electrolytes. And that affected the breakdown voltage and the plasma etch rate. The breakdown voltage per unit thickness was the highest at 15 ℃, and the plasma etch rate was the lowest at 10 ℃ at 2.80 ㎛/h.

• 공업화학
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• 제8권5호
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• pp.756-762
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• 1997

본 실험에서는 황산용액에서 전기화학적으로 금속 알루미늄판을 양극산화하여 원통형 세공구조를 갖고 있는 alumina막을 형성시켰다. 양극화에 사용된 알루미늄 시료는 전해연마, 화학연마 및 열산화와 같은 전처리 공정을 거쳐서 준비하였으며, 형성된 알루미나막의 세공분포와 두께 등을 SEM과 BET를 사용하여 조사하였다. 그 결과 산화피막이 Keller모델과 같은 기하 구조로 이루어져 있으며. 균일한 세공 분포를 지니고 있음을 볼 수 있었다. 그리고 산화막의 세공크기와 두께는 황산전해질의 농도, 반응온도 그리고 전류밀도와 같은 양극산화 공정변수에 의존함을 알수 있었다.

• 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.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2016년도 추계학술대회 논문집
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• pp.153-153
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• 2016

Aluminum alloys have poor corrosion resistance compared to the pure aluminum due to the additive elements. Thus, anodizing technology artificially generating thick oxide films are widely applied nowadays in order to improve corrosion resistance. Anodizing is one of the surface modification techniques, which is commercially applicable to a large surface at a low price. However, most studies up to now have focused on its commercialization with hardly any research on the assessment and improvement of the physical characteristics of the anodized films. Therefore, this study aims to select the optimum temperature of sulfuric electrolyte to perform excellent corrosion resistance in the harsh marine environment through electrochemical experiment in the sea water upon generating porous films by variating the temperatures of sulfuric electrolyte. To fabricate uniform porous film of 5083 aluminum alloy, we conducted electro-polishing under the 25 V at $5^{\circ}C$ condition for three minutes using mixed solution of ethanol (95 %) and perchloric (70 %) acid with volume ratio of 4:1. Afterward, the first step surface modification was performed using sulfuric acid as an electrolyte where the electrolyte concentration was maintained at 10 vol.% by using a jacketed beaker. For anode, 5083 aluminum alloy with thickness of 5 mm and size of $2cm{\times}2cm$ was used, while platinum electrode was used for cathode. The distance between the two was maintained at 3 cm. Afterward, the irregular oxide film that was created in the first step surface modification was removed. For the second step surface modification process (identical to the step 1), etching was performed using mixture of chromic acid (1.8 wt.%) and phosphoric acid (6 wt.%) at $60^{\circ}C$ temperature for 30 minutes. Anodic polarization test was performed at scan rate of 2 mV/s up to +3.0 V vs open circuit potential in natural seawater. Surface morphology was compared using 3D analysis microscope to observe the damage behavior. As a result, the case of surface modification presented a significantly lower corrosion current density than that without modification, indicating excellent corrosion resistance.

• 한국조명전기설비학회:학술대회논문집
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• 한국조명전기설비학회 2002년도 학술대회논문집
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• pp.207-211
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• 2002

Anodizing film was prepared by anodic oxidation of pure aluminum(purity > 99.50) using DC power supply for constant current mode in an electrolytic solution of surface of sulfuric acid. Effects of pre-treatment process such as chemical polishing, acid cleaning, alkali etching before anodic oxidation, were studied to microstructures and surface morphologies. A roughness on surface of anodizing film had to be decreased for amorphous phase by anodic oxidation. A roughness on surface of anodizing film decrease as annealing temperature increased in chemical polishing.