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Method for preparing neat porous anodic alumina film

A porous anode and aluminum oxide film technology, applied in the field of electrochemistry, can solve the problems of irregular surface pores, different pore sizes, and discontinuous spacing between aluminum oxide template pores, so as to improve the adjustment range, improve stability, and avoid shocks. effect of wear

Inactive Publication Date: 2015-11-11
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the hole spacing of the alumina template is discontinuous, which limits the application range of the alumina film to a large extent.
Patent CN101603191A discloses a method of adding acetic acid to phosphoric acid solution, so that the pore size of the prepared alumina membrane is between 200-300nm, but the surface pores are very irregular and the pore sizes are different
Patent CN103147108A discloses a porous aluminum oxide membrane prepared in citric acid and oxalic acid solution with an adjustable pore spacing of 150-650nm, but the existing problem is still that the order of the pores is not good

Method used

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  • Method for preparing neat porous anodic alumina film
  • Method for preparing neat porous anodic alumina film
  • Method for preparing neat porous anodic alumina film

Examples

Experimental program
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Effect test

Embodiment 1

[0030] The high-purity aluminum sheet with a purity of 99.999% was ultrasonically cleaned in acetone for 5 minutes to remove the grease on the surface, then cleaned with deionized water, and then placed in a 1mol / L NaOH solution for 10 minutes to remove the natural oxide layer on the surface, and finally used Wash and dry with ionic water; take the pretreated aluminum sheet as the anode and the titanium plate as the cathode, in perchloric acid and absolute ethanol with a solution volume ratio of 1:4, at a voltage of 21V, at a temperature of 0-5°C, for 5min Electrochemical polishing to obtain an aluminum sheet with a smooth surface; the polished aluminum sheet is used as the anode, the titanium plate is used as the cathode, and a 1wt% phosphoric acid solution with 0.03M oxalic acid is used as the electrolyte for primary oxidation. The oxidation voltage is 200V and the temperature is 0 ~3°C, the oxidation time is 2h; the aluminum oxide film with aluminum substrate after primary o...

Embodiment 2

[0032] The high-purity aluminum sheet with a purity of 99.999% was ultrasonically cleaned in acetone for 5 minutes to remove the grease on the surface, then cleaned with deionized water, and then placed in a 1mol / L NaOH solution for 10 minutes to remove the natural oxide layer on the surface, and finally used Wash and dry with ionic water; take the pretreated aluminum sheet as the anode and the titanium plate as the cathode, in perchloric acid and absolute ethanol with a solution volume ratio of 1:4, at a voltage of 21V, at a temperature of 0-5°C, for 5min Electrochemical polishing to obtain an aluminum sheet with a smooth surface; the polished aluminum sheet is used as the anode, the titanium plate is used as the cathode, and a 1wt% phosphoric acid solution with 0.05M oxalic acid is used as the electrolyte for primary oxidation. The oxidation voltage is 190V and the temperature is 0 ~3°C, the oxidation time is 2h; the aluminum oxide film with aluminum substrate after primary o...

Embodiment 3

[0034] The high-purity aluminum sheet with a purity of 99.999% was ultrasonically cleaned in acetone for 5 minutes to remove the grease on the surface, then cleaned with deionized water, and then placed in a 1mol / L NaOH solution for 10 minutes to remove the natural oxide layer on the surface, and finally used Wash and dry with ionic water; take the pretreated aluminum sheet as the anode and the titanium plate as the cathode, in perchloric acid and absolute ethanol with a solution volume ratio of 1:4, at a voltage of 21V, at a temperature of 0-5°C, for 5min Electrochemical polishing to obtain an aluminum sheet with a smooth surface; the polished aluminum sheet is used as the anode, the titanium plate is used as the cathode, and a 1wt% phosphoric acid solution with 0.07M oxalic acid is used as the electrolyte for primary oxidation. The oxidation voltage is 180V and the temperature is 0 ~3°C, the oxidation time is 2h; the aluminum oxide film with aluminum substrate after primary o...

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Abstract

The invention discloses a method for preparing a neat porous anodic alumina film. The method comprises the steps that firstly, a pretreated aluminum piece is placed in a mixed solution of phosphoric acid and oxalic acid, then first-time anodic oxidation is carried out to obtain an alumina film, and the alumina film is removed; second-time oxidation completely identical to the first-time oxidation in condition is carried out; the obtained alumina film is placed into a phosphoric acid solution, and pore-enlarging at different times is carried out; and through adjustment of oxidation voltage and pore-enlarging time, the highly-neat porous anodic alumina film with the pore pitch ranging from 348 nm to 500 nm and the pore diameter ranging from 72 nm to 400 nm is prepared. The oxalic acid content in the dilute phosphoric acid solution is adjusted, so that the anodic oxidation voltage value is improved, the regularity of alumina film pores is improved, and the range of the pore pitch is widened. The application of the alumina film to the field of preparation of neat micro-nano materials can be greatly expanded.

Description

technical field [0001] The invention belongs to the field of electrochemical technology, and relates to a method for preparing a regular porous anodic aluminum oxide film, in particular to the preparation of pore spacing and pore diameters with a wide range of adjustable heights using a mixed solution of dilute phosphoric acid added with oxalic acid as the electrolyte Method for Ordered Anodized Aluminum Films. Background technique [0002] The porous anodized aluminum film is a hexagonal continuous structure with columnar holes perpendicular to the aluminum substrate and arranged parallel to each other. It has the advantages of large specific surface area, adjustable pore size, and simple preparation process. In recent years, porous anodized aluminum oxide films have received more and more attention and have potential applications in many fields, such as filtration, catalysis, sensing, bionics, etc. Masuda and Satoh first proposed the secondary oxidation technology in 1996...

Claims

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Application Information

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IPC IPC(8): C25D11/12C25D11/06C25D11/24
Inventor 徐艳芳刘皓李晓久吴健杨桂林许艳张耗
Owner TIANJIN POLYTECHNIC UNIV
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