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A preparation method of through-hole anodic aluminum oxide film with controllable pore size and thickness

An anodizing aluminum and anodizing technology, applied in anodizing, electrolytic coating, surface reaction electrolytic coating, etc., can solve the problem of inability to obtain small pore size, ultra-thin, pore size and thickness through-hole anodic aluminum film, etc. High toughness, uniform pore size distribution and good chemical stability

Active Publication Date: 2011-12-14
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a small pore size, ultra-thin, controllable pore size and thickness, uniform pore size, through-hole anodic aluminum oxide film preparation method, the method is simple, the required time is short, environmentally friendly, and does not need to change the anode The nano-channel of alumina solves the technical problem that it is impossible to obtain through-hole anodic aluminum oxide film with small pore size, ultra-thin, pore size and thickness controllable

Method used

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  • A preparation method of through-hole anodic aluminum oxide film with controllable pore size and thickness
  • A preparation method of through-hole anodic aluminum oxide film with controllable pore size and thickness
  • A preparation method of through-hole anodic aluminum oxide film with controllable pore size and thickness

Examples

Experimental program
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Effect test

Embodiment 1

[0033] (1) The high-purity aluminum sheet (purity of 99.99 wt%) was ultrasonically cleaned with acetone for 3 minutes and then immersed in a 2M sodium hydroxide solution for 3 minutes to remove grease and oxides on the surface of the aluminum sheet.

[0034] The aluminum sheet used is strip-shaped, and the anodic aluminum oxide film prepared at one time is the front and back sides of the aluminum sheet (that is, two sheets), and the pore structure of the two sheets is exactly the same.

[0035] (2) The processed aluminum sheet in step (1) is used as an anode, and it is anodized in a 30wt% sulfuric acid solution at -10°C with a constant voltage of 5V direct current for 5 hours.

[0036] (3) The alumina obtained after the treatment in step (2) is immersed in a mixed aqueous solution of 1.8 wt% chromium trioxide and 6 wt% phosphoric acid at 60°C for about 20 minutes to remove the oxide layer.

[0037] (4) After the aluminum sheet treated in step (3) is washed with deionized water, it is a...

Embodiment 2

[0041] (1) Repeat step 1 in Example 1.

[0042] (2) The processed aluminum sheet in step (1) is used as the anode, and it is anodized in a 30wt% sulfuric acid solution at -8°C with a 7.5V direct current constant voltage for 2 hours.

[0043] (3) The aluminum oxide obtained after the treatment in step (2) is immersed in a mixed aqueous solution of 1.8 wt% chromium trioxide and 6 wt% phosphoric acid at 60° C. for about 30 minutes to remove the oxide layer.

[0044] (4) After the aluminum sheet treated in step (3) is washed with deionized water, it is anodized again under the same conditions as in step (2) for 3 hours.

[0045] (5) Step (4) The treated alumina membrane is put into perchloric acid acetone stripping solution (volume ratio is 1:1), 12.5V DC constant voltage is applied, and anodic electrolytic stripping treatment is performed at room temperature for about 5 Within seconds, a through-hole, ultra-thin, independent anodic aluminum oxide film can be obtained. The pore diameter ...

Embodiment 3

[0048] (1) Repeat step 1 in Example 1.

[0049] (2) The processed aluminum sheet in step (1) is an anode, and is anodized in a 15 wt% sulfuric acid solution at 0° C. at a constant voltage of 10V direct current for 2 hours.

[0050] (3) The aluminum oxide obtained after the treatment in step (2) is immersed in a mixed aqueous solution of 1.8 wt% chromium trioxide and 6 wt% phosphoric acid at 60° C. for about 30 minutes to remove the oxide layer.

[0051] (4) After the aluminum sheet treated in step (3) is washed with deionized water, it is anodized again under the same conditions as in step (2) for 3 hours.

[0052] (5) Step (4) The treated alumina membrane is put into perchloric acid acetone stripping solution (volume ratio is 1:1), 15V DC constant voltage is applied, and anodic electrolysis stripping treatment is performed at room temperature for about 5 seconds Clock, through-hole, independent anodic aluminum oxide film can be obtained. The pore diameter at the top of the membrane ...

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Abstract

The invention relates to a technique for preparing an anode alumina film, in particular to a method for preparing the anode alumina film which has small aperture, is ultra thin and is controllable in aperture and thickness. In the method, high-pure aluminum is used as an anode, a certain constant-voltage and direct-current power supply is applied onto a sulfuric acid electrolyte to perform anodicoxidation, proper voltages between the cathode and the anode, electrolyte concentration, electrolyte temperature and anode oxidization time are selected, and after the reaction, anode alumina with analuminum substrate is used as an anode and placed in mixed solution of perchloric acid and acetone, anode electrolysis treatment is performed under a voltage which is 5 to 15V higher than an anode oxidization voltage to make an alumina film separate from the aluminum substrate and to remove a baffle layer, and thus, the small-aperture through-hole anode alumina film with controllable aperture andthickness is obtained. When the method is used, the mass, simple, nondestructive, uniform and large-scale preparation of small-aperture and through-hole anode alumina film is realized, and the technical problem that the small-diameter and ultra-thin through hole anode alumina film is not available at present is solved.

Description

Technical field [0001] The invention relates to a preparation technology of an anodic alumina membrane, in particular to a method for preparing a through-hole anodic alumina membrane with small pore size, ultra-thin, pore size and thickness controllable. Background technique [0002] Due to its highly ordered hexagonal periodic pore structure, uniform pore size, high temperature resistance, good insulation, adjustable pore spacing, pore density, pore length and pore size, etc., anodized aluminum membrane is widely used as a large-area preparation Highly ordered template materials for nanoholes, nanodots, nanorods, nanowires and nanotube array structures of various metals, oxides, and semiconductor materials. At the same time, alumina membrane is also a filter material, surface anticorrosive material, catalyst carrier, bioceramic material and so on with superior performance. [0003] At present, the aluminum oxide films prepared by anodizing method all have aluminum substrates and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/08C25D11/12
Inventor 侯鹏翔石超刘畅成会明
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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