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Method for preparing pore diameter controllable through hole anodized aluminum oxide film

A technology of anodic aluminum and anodic oxidation, which is applied to the preparation of anodic aluminum film, through-hole anodic aluminum film, and the field of controllable pore size, which can solve the problem of nano-pore size containing other impurities, and the process of removing film and removing aluminum is cumbersome and inaccurate. control and other problems, to achieve the effect of regular and orderly pore structure, high toughness and low price

Inactive Publication Date: 2011-02-02
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

[0006] The purpose of the present invention is to provide a simple, efficient, and pollution-free method for preparing anodic aluminum oxide films with controllable apertures and through holes, which solves the cumbersome, time-consuming, fragile, uneven, and time-consuming process of removing aluminum after aluminum oxide preparation. There are many problems such as other impurities and the inability to accurately control the nanopore size in the subsequent opening, and it is the first time that the stripping and opening are carried out simultaneously without destroying the original pore structure.

Method used

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  • Method for preparing pore diameter controllable through hole anodized aluminum oxide film

Examples

Experimental program
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Effect test

Embodiment 1

[0025] (1) High-purity aluminum sheet (99.99wt% purity) is annealed at a constant temperature of 500° C. for 4 hours under the protection of an inert gas (such as argon), so as to eliminate the mechanical stress on the surface of the aluminum sheet.

[0026] (2) The aluminum sheet treated in step (1) was ultrasonically cleaned with acetone for 3 minutes and soaked in 1M sodium hydroxide solution for 5 minutes to further remove the grease and oxides present on the surface of the aluminum sheet.

[0027] (3) After the aluminum sheet after step (2) is cleaned with deionized water, it is electropolished at 12V for 5 minutes in the alcohol polishing solution of perchloric acid (the volume ratio of perchloric acid and alcohol is 1: 4) at 5°C, Get a flat and bright aluminum plane.

[0028] (4) The aluminum sheet treated in step (3) was anodized once at 10° C. with 20 V DC constant voltage for 2 hours in 10 wt % sulfuric acid aqueous solution with the aluminum sheet as the cathode.

...

Embodiment 2

[0034] (1) Repeat (1-3) steps in Example 1.

[0035] (2) The aluminum sheet after the above treatment was anodized in 3 wt % oxalic acid aqueous solution, using the aluminum sheet as a cathode at 20° C. for 2 hours at a constant voltage of 40 V direct current.

[0036](3) The alumina obtained after the treatment in step (2) was immersed in a mixed aqueous solution of 1.8wt% dichromic acid and 6wt% phosphoric acid at 60°C for 40 minutes to remove the oxide layer.

[0037] (4) After the aluminum sheet treated in step (3) was washed with deionized water, it was anodized again under the same conditions as in step (2) for 4 hours.

[0038] (5) After the oxidation in step (4) is completed, step down the voltage by 2V each time until the current is stable until the voltage is 20V, and an anodic aluminum oxide film with an aluminum substrate, regular and orderly pore structure and uniform pore size distribution is obtained. .

[0039] (6) The aluminum oxide film after step (5) is pu...

Embodiment 3

[0041] (1) Repeat (1-3) steps in Example 1.

[0042] (2) The aluminum sheet after the above treatment was anodized in 10 wt% sulfuric acid solution, using the aluminum sheet as the cathode at 10°C for 3 hours at 10° C. with a constant voltage of 20 V direct current.

[0043] (3) The alumina obtained after the treatment in step (2) was immersed in a mixed aqueous solution of 1.8wt% dichromic acid and 6wt% phosphoric acid at 60°C for 50 minutes to remove the oxide layer.

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

[0045] (5) After the oxidation in step (4) is finished, step down the voltage by 2V each time until the current is stable until the current is zero (the voltage is 4V at this time), and the aluminum matrix is ​​obtained and the pore structure is regular and orderly. Uniformly distributed anodized aluminum film.

[0046] (6) The aluminum oxide f...

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Abstract

The invention relates to technology for preparing an anodized aluminum oxide film, in particular to a method for preparing a pore diameter controllable through hole anodized aluminum oxide film. The method comprises the following steps of: performing anode electrolysis treatment on an anodized aluminum oxide film with an aluminum substrate in mixed solution of perchloric acid and acetone to obtain a pore diameter controllable anodized aluminum oxide film with two open ends in short time (2-300 seconds), wherein the pore diameters at the top end and the bottom end fo the anodized aluminum oxide film are accurately controllable in ranges of between 10 and 100nm and between 5 and 25nm; and putting the aluminum oxide film with the aluminum substrate subjected to stage depressurization-method oxidation into acetone solution of perchloric acid, and applying voltage 5-15V higher than film forming voltage for anode electrolysis treatment to obtain the pore diameter controllable through hole anodized aluminum oxide film. In the method, the pore diameters at the top end and the bottom end of the anodized aluminum oxide film can be respectively controlled, holing and removal of the aluminum substrate are completed by one step, and a plurality of problems of complicated process, time consumption, difficult control of pore diameters and the like in the conventional process for preparing the through hole anodized aluminum oxide film.

Description

technical field [0001] The invention relates to the preparation technology of anodic aluminum oxide film, specifically a method for preparing anodic aluminum oxide film with controllable pore size and through holes. Anodic electrolytic treatment in a mixed solution of acetone can directly obtain an anodic aluminum oxide film with open ends and controllable pore size. Background technique [0002] With the rapid development of nanotechnology, nanomaterials have attracted more and more attention as functional materials due to their unique electronic structure and physical properties. Due to the potential application prospects of nanostructure ordered array system materials in information transmission and storage devices such as electronic components, field emission displays, and magnetic memory materials, nanoassembly and its properties have become a very important topic in the field of nanomaterial research. aspect. [0003] Due to its highly ordered hexagonal periodic pore...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/04
Inventor 刘畅喻万景侯鹏翔成会明
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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