• Journal of the Korean institute of surface 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.

• Korean Journal of Materials Research
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• v.29 no.2
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• pp.65-72
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• 2019

Dual porous structures are observed for the first time on a metallic Cu surface underneath anodic Cu oxide by the application of an anodizing voltage to Cu in oxalic acid. The as-prepared porous Cu surface contains macropores of less than $1{\mu}m$ diameter and mesopores of about tens of nanometers diameter with circular shapes. The size and density (number of pores/area) of the macropores are dependent on the applied voltage. It is likely that the localized dissolution (corrosion) of Cu in oxalic acid under the anodizing voltages is responsible for the formation of the mesopores, and the combination of a number of the mesopores might create the macropores, especially under a relatively high anodizing voltages or a prolonged anodizing time. The variations of pore structure (especailly macropores) with applied voltage and time are reasonably explained on the basis of the proposed mechanism of pore formation.

• 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.

• Applied Science and Convergence Technology
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• v.25 no.1
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• pp.15-18
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• 2016

Study investigated the optimal anodizing conditions for fabricating an oxide film that produces less contamination in a corrosive plasma environment, using oxalic acid and tartaric acid. Oxide films were produced using sulfuric acid, oxalic acid, and tartaric acid electrolyte mixtures with various mole ratios. The oxide film made by adding 0.05M tartaric acid to 0.3M oxalic acid showed higher breakdown voltage and lower leakage current. Additionally, contamination particles were reduced during plasma etching, thus demonstrates that this mixture presented optimal conditions. However, higher tartaric acid content (0.1 M, 0.15 M) led to lower breakdown voltages and higher leakage currents. Also, it resulted in more cracking during thermal shock tests as well as the generation of more contamination particles during plasma processing.

• Journal of the Korean institute of surface engineering
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• v.47 no.3
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• pp.121-127
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• 2014

In this study, in order to improve corrosion resistance and wear resistance of aluminum, surface treatment was made by anodizing with oxalic acid solution and sealing with nano-diamond powder. Average size of nano-diamond powder was 30nm. Anodizing with oxalic acid made many pores in the aluminum oxide layer. Pore size and oxide thickness were investigated by scanning electron microscope (SEM). Pore size increased as temperature increased and voltage increased. It was possible to make oxide layer with pore diameter more than 50 nm. Oxide thickness increased as temperature and voltage and treatment time increased. Oxide layer with above $10{\mu}m$ thickness was made. Aluminum oxide layer with many pores was sealed by water with nano-diamond powder. Surface morphology was investigated by SEM. After sealing treatment with nano-diamond powder, corrosion resistance, wear resistance and hardness increased.

• Journal of the Korean institute of surface engineering
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• v.17 no.3
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• pp.78-86
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• 1984

Hard anodic oxide film was investigated formed on pure aluminium with various temperature (30$^{\circ}-60^{\circ}C$), current densities (1.5-3.0A/$dm^2$) and concentrations(3-15g/l) of oxalic acid in 0.5M malic acid bath. The resulting characteristic of the anodic oxide film obtained were summarized as follows in the view point of physical and mechanical properties in relation with the above process variables. 1. The film thickness increased with oxalic acid concentration and bath temperature, while the reversed phenomena were obtained at a high concentration of oxalic acid and high temperature due to the severe dissolution of the anodic oxide film. 2. The hardness and the abrasion resistance were improved by lowering the addition of oxalic acid and the bath temperature. This feature was directly dependent on the porosity formed on the anodic oxide film. 3. The maximum hardness of anodic oxide film showed Hv 579 in the temperature of 30$^{\circ}C$ with the current density, 2.5A/$dm^2$ in the 0.5M malic acid bath mixed with 5g/l oxalic acid.

• Journal of the Korean institute of surface engineering
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• v.53 no.5
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• pp.249-256
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• 2020

As the size of manufacturing equipment for LCD and OLED displays increases, replacement of existing heavy stainless steel components with light metals, such as aluminum alloys, is being more important in semiconducting and display manufacturing industries. To use aluminum alloys for components in semiconducting and display industries, it is important to develop a new anodization method for improved performance of anodic oxide films than conventional anodization method based on sulfuric acid. In this work, optimum applied current density and the best sealing methods for anodic oxide films in 3% oxalic acid were explored. Experimental results showed 2.5 A/dm2 is the best applied current density for improved hardness and dielectric breakdown voltage. Sealing of the anodic oxide films further improved their hardness, dielectric breakdown voltage and resistance to HCl, by which application of anodic oxide films become applicable for components in semiconducting and display industries.

• Journal of the Korean institute of surface 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.

• Korean Journal of Materials Research
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• v.16 no.8
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• pp.503-510
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• 2006

The measurement of specific gases is based on the reversible conductivity change of sensing materials in semiconductor type gas sensors. For an application as gas sensors of high sensitivity, porous $SnO_2$ films have been fabricated by anodizing of pure Sn foil in oxalic acid and characteristics of anodic tin oxide films have been investigated. Pore diameter and distribution were dependent on process conditions such as electrolyte concentration, applied voltage, anodizing temperature, and time. Characteristics of anodic films were explained with current density-time curves.

• Corrosion Science and Technology
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• v.21 no.6
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• pp.476-486
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• 2022

Recently, aluminum 6061 instead of copper alloy is used for cooling heat exchangers used in the internal combustion of engines due to its economic feasibility, lightweight, and excellent thermal conductivity. In this study, aluminum 6061 alloy was anodized with oxalic acid, phosphoric acid, or chromic acid as an anodizing electrolyte at the same concentration of 0.3 M. After the third anodization, FDTS, a material with low surface energy, was coated to compare hydrophobic properties and anti-icing characteristics. Aluminum was converted into an anodization film after anodization on the surface, which was confirmed through Energy Dispersive X-ray Spectroscopy (EDS). Pore distance, interpore distance, anodization film thickness, and solid fraction were measured with a Field Emission Scanning Electron Microscope (FESEM). For anti-icing, hydrophobic surfaces were anodized with oxalic acid, phosphoric acid, or chromic acid solution. The sample anodized in oxalic acid had the lowest solid fraction. It had the highest contact angle for water droplets and the lowest contact hysteresis angle. The anti-icing contact angle showed a tendency to decrease for specimens in all solutions.