Thin-wall anodic aluminum oxide film with large aperture and preparation method thereof

An anodized aluminum, large pore size technology, used in anodizing, electrolytic coatings, surface reaction electrolytic coatings, etc.

Inactive Publication Date: 2009-12-16
INST OF ELECTRICAL ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Using phosphoric acid as the electrolyte can obtain an aluminum oxide film with a larger pore size. Patent CN 1403632A uses a mixed acid solution of phosphoric acid and oxalic acid as the electrolyte to obtain an anodized aluminum oxide film with a larger pore size through anodic oxidation at a constant voltage, but the pore size Also only 30-70nm

Method used

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  • Thin-wall anodic aluminum oxide film with large aperture and preparation method thereof
  • Thin-wall anodic aluminum oxide film with large aperture and preparation method thereof
  • Thin-wall anodic aluminum oxide film with large aperture and preparation method thereof

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Embodiment 1

[0022] The aluminum sheet is first ultrasonically cleaned with acetone, ethanol, and high-purity water for 10 minutes to remove surface grease and dirt. Anodic oxidation is carried out by putting the cleaned aluminum sheet into a mixed electrolyte with a mass percentage of phosphoric acid of 1% and a mass percentage of phosphoric acid and acetic acid of 1:1. The oxidation voltage was 40 volts, and the first anodizing time was 5 minutes. After taking out the aluminum sheet, clean it with high-purity water, then put the aluminum sheet in a mixed solution of 0.2mol / L chromic acid and 0.4mol / L phosphoric acid, and soak it at 60°C for 20 minutes; Under the same mixed electrolyte and anodic oxidation voltage conditions as the first step, the second anodic oxidation is carried out, and the anodic oxidation time is 10 hours; then the aluminum sheet is washed with high-purity water, and then placed in a phosphoric acid solution with a mass percentage of 10% Soak for 20 minutes.

[00...

Embodiment 2

[0025] The aluminum sheet is first ultrasonically cleaned with acetone, ethanol, and high-purity water for 10 minutes to remove grease and dirt on its surface. The cleaned aluminum sheet is put into a mixed electrolyte with a mass percentage of phosphoric acid of 1% and a mass percentage of phosphoric acid and acetic acid solution of 1:1 for anodic oxidation. The oxidation voltage is 80 volts, and the anodizing time for the first time is 3 minutes; after taking out the aluminum sheet, clean it with high-purity water, then put the aluminum sheet into a mixed solution of 0.2mol / L chromic acid and 0.4mol / L phosphoric acid. Soak at a temperature of 60°C for 20 minutes; then wash it with high-purity water, and then perform a second anodic oxidation under the same mixed electrolyte and anodic oxidation voltage conditions as the first step, and the anodic oxidation time is 1 hour; then use high-purity water to The aluminum sheet is washed clean, and then soaked in a 10% phosphoric ac...

Embodiment 3

[0029] The aluminum sheet is first ultrasonically cleaned with acetone, ethanol, and high-purity water for 10 minutes to remove surface grease and dirt; put the cleaned aluminum sheet into a solution with a mass percentage of 1% phosphoric acid and a 1:1 mass percentage of phosphoric acid and acetic acid solution. In the mixed electrolyte, anodic oxidation is carried out. The oxidation voltage is 160 volts, and the first anodic oxidation time is 1 minute; clean it with high-purity water, then put the aluminum sheet into a mixed solution of 0.2mol / L chromic acid and 0.4mol / L phosphoric acid, and soak it at 60°C 20 minutes; then wash it with high-purity water, and then perform the second anodic oxidation under the same mixed electrolyte and anodic oxidation voltage conditions as the first step, and the anodic oxidation time is 10 minutes; then wash the aluminum sheet with high-purity water, Then put it into a 10% phosphoric acid solution and soak for 20 minutes.

[0030] The pr...

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Abstract

The invention discloses a hexagonal thin-wall anodic aluminum oxide film with large aperture. The aperture of the anodic aluminum oxide is 200 to 300 nanometers, and the thickness of the hole wall is 5 to 20 nanometers. A method for preparing the film comprises the following steps: ultrasonically cleaning an aluminum sheet for 10 minutes by acetone, ethanol and high-purity water in turn, putting the cleaned aluminum sheet into mixed electrolyte in which the mass percentage of phosphoric acid to acetic acid is (10-1):(1-10) percent, and anodically oxidizing the aluminum sheet for 1 to 5 minutes under the voltage of 40 to 160 volts; then, cleaning the obtained anodic aluminum oxide film by the high-purity water, and soaking the cleaned anodic aluminum oxide film in mixed solution of 0.2 mol / L chromic acid and 0.4 mol / L phosphoric acid for 20 minutes at the temperature of 60 DEG C; anodically oxidizing the anodic aluminum oxide film for the second time for 5 minutes to 10 hours under the condition of the same mixed electrolyte and anodic oxidizing voltage as the first anodic oxidization; and soaking the obtained anodic aluminum oxide film into 10 percent phosphoric acid solution in percentage by mass for 20 minutes, finally cleaning the anodic aluminum oxide film by the high-purity water, and drying the anodic aluminum oxide film by nitrogen.

Description

technical field [0001] The invention relates to an anodized aluminum oxide film and a preparation method thereof, in particular to a large-aperture thin-wall anodized aluminum oxide film and a preparation method thereof. Background technique [0002] Anodic oxidation of aluminum and its alloys in sulfuric acid, oxalic acid, phosphoric acid and other electrolytes can form an aluminum oxide film with a porous structure on the surface, and filling different substances in its micropores can obtain various surface composite materials to improve The surface properties of aluminum and aluminum alloy materials; in addition, porous anodic aluminum oxide membranes are also widely used in separation membranes, optical and optoelectronic components, magnetic thin films, selective absorption membranes, catalyst supports, etc., and become ideal for preparing uniform nanostructures. Templates, such as the synthesis of nanowires, nanotubes, etc., using porous alumina as a template. [0003...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/04C25D11/06C25D11/18
Inventor 刘敏赵雷王文静
Owner INST OF ELECTRICAL ENG CHINESE ACAD OF SCI
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