• Journal of Surface Science and Engineering
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• v.54 no.1
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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.

• Journal of the Korea Convergence Society
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• v.7 no.5
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• pp.169-173
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• 2016

Anodic oxidation of aluminum has a sulfuric acid method and a oxalic acid method. Sulfuric acid concentration of the sulfuric acid method is 15~20 wt%. In the case of soft anodizing used in the $20{\sim}30^{\circ}C$ range, and voltage is the most used within a DC voltage 13~15V. In the case of hard anodizing used in the $0{\sim}-5^{\circ}C$ range. An aluminum oxide layer is made using sulfuric acid and oxalic acid. In this study, thermal fatigue of aluminum oxide layer which is made using sulfuric acid and oxalic acid is compared. Crack generating temperature of a sulfuric acid method and a oxalic acid method is $500^{\circ}C$ and $600^{\circ}C$. Thermal fatigue of aluminum oxide layer which is made using oxalic acid is better than thermal fatigue of aluminum oxide layer which is made using sulfuric acid. The characteristic of thermal fatigue can be explained by using thermal expansion coefficient of Al and Al2O3 and manufacturing temperature on Al anodizing. It was made possible through the convergent study to propose the manufacturing method of the anodic oxidation product used at a high temperature.

• Journal of Surface Science and Engineering
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• v.51 no.6
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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.

• Journal of Surface Science and Engineering
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• v.52 no.4
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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.

• Journal of Surface Science and Engineering
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• v.57 no.1
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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.

• Journal of the Semiconductor & Display Technology
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• v.20 no.1
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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.

• Applied Chemistry for Engineering
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• v.8 no.5
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• pp.756-762
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• 1997

The experiment was carried out to fabricate alumina membrane which has a cylindrical pore structure by anodizing aluminium plate in sulfuric acid solution with the electrochemical technique. The aluminium plate for anodizing was prepared by the pretreatment process such as chemical, electro-polishing and thermal treatment. The pore size distribution and the film thickness of alumina membrane were investigated by the implementation of scanning electron microscope(SEM) and BET method. The results show that the oxide film has a geometrical structures like a Keller model and that the membrane has a uniform pore distribution. The pore size and the oxide film thickness are dependent on the anodizing process variables such as the electrolyte concentration, the reation temperature and the anodizing current density.

• Journal of Surface Science and Engineering
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• v.53 no.1
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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.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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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.

• Proceedings of the Korean Institute of IIIuminating and Electrical Installation Engineers Conference
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• 2002.11a
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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.