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Process for preparing porous anode aluminium oxide mould of height ordered by mixed acid electrolyzing liquid

A technology of electrolyte preparation and alumina template, which is applied in the direction of electrolytic coating, surface reaction electrolytic coating, coating, etc., can solve the problems of thin PAA film layer and small nanopore diameter of porous alumina film, and reduce the barrier layer Thickness, effect of improving orderliness

Inactive Publication Date: 2008-11-12
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The invention not only solves the problem that the nanopore diameter of the porous alumina membrane prepared by sulfuric acid electrolyte is small, but adds a certain amount of oxalic acid to the sulfuric acid to increase the nanopore diameter of the porous alumina membrane from 20nm to 45-55nm; The problem of the thin film layer of the PAA film prepared by the electrolyte is that a certain amount of oxalic acid is added to the sulfuric acid to increase the thickness of the porous alumina film from 30 μm to 50-80 μm

Method used

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  • Process for preparing porous anode aluminium oxide mould of height ordered by mixed acid electrolyzing liquid
  • Process for preparing porous anode aluminium oxide mould of height ordered by mixed acid electrolyzing liquid
  • Process for preparing porous anode aluminium oxide mould of height ordered by mixed acid electrolyzing liquid

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specific Embodiment approach 1

[0012] Specific Embodiment 1: In this embodiment, a highly ordered porous anodized aluminum template is prepared according to the following steps: 1. Preparation of electrolyte: use a mixed acid of sulfuric acid and oxalic acid as the electrolyte, and the concentration of sulfuric acid in the electrolyte is 100-200g / L 1. The concentration of oxalic acid is 50-150g / L; 2. Aluminum sample pretreatment: the aluminum sample is degreased, deoxidized, and electrochemically polished in sequence; 3. Two-step anodizing: use a mixed acid of sulfuric acid and oxalic acid as electrolysis liquid, control the area ratio of cathode and anode to 2~1:1, the distance between cathode and anode is between 3~5cm, the oxidation temperature is -5~10℃, the oxidation voltage is 20~30V, and the oxidation time of the first step is 3~6h, the second oxidation time is 3~8h.

[0013] In this embodiment, after the first step of anodic oxidation, wet etching is used to remove the oxide film formed in the first...

specific Embodiment approach 2

[0015] Specific embodiment two: In this embodiment, a highly ordered porous anodized aluminum template is prepared according to the following steps:

[0016] 1. Electrolyte preparation: a mixed acid of sulfuric acid and oxalic acid is used as the electrolyte, and the electrolyte is composed of 100-200 g / L sulfuric acid and 50-150 g / L oxalic acid, and the solvents are all aqueous solutions.

[0017] 2. Aluminum sample pretreatment: Before anodizing, the sample needs to be degreased in acetone, then in NaOH solution, remove the natural oxide layer formed on the aluminum surface, and rinse with distilled water. Electrochemical polishing was carried out in a 1:4 (volume ratio) perchloric acid ethanol solution with a voltage of 10 V and a time of 5 min. The purpose of electrochemical polishing is to eliminate the surface scratches left by the aluminum sample during production and transportation, and to improve the order of the porous alumina film.

[0018] 3. Anodizing: In this em...

specific Embodiment approach 3

[0019] Specific embodiment three: In this embodiment, a highly ordered porous anodized aluminum template is prepared in this way: the mixed acid of sulfuric acid and oxalic acid is used as the electrolyte, and the electrolyte contains 100g / L sulfuric acid and 50g / L oxalic acid; the purity is 99.99% % of the aluminum sheet is subjected to two-step anodic oxidation after degreasing, deoxidizing layer, and electrochemical polishing. Use an aluminum sheet as the anode, graphite as the cathode, control the area ratio of the cathode and the anode to 2:1, the distance between the cathode and the anode is 3cm, the oxidation voltage is 22V, the first oxidation time is 5h, and the second anodic oxidation time is 4h. The prepared porous alumina membrane has a thickness of 53 μm, a nanopore diameter of 45-48 nm, and a barrier layer thickness of 23 nm. The cross-sectional view of the porous alumina template is shown in figure 1 , the order of nanopore size and arrangement see figure 2 ....

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Abstract

The invention relates to a method used mixed acid electrolyte to manufacture high ordered multi-hole anodic alumina die plate. In order to further reduce oxidation voltage, barrier layer thickness, and increase nanometer hole array orderliness, the alumina die plate is manufactured as follows: using the mixed acid of sulfuric acid and oxalic acid as electrolyte; their content are 100-200g / L and 50-150g / L; de-oiling; oxide layer removing; electro polishing; double steps anodic oxidation manufacturing multi-hole anodic alumina die plate. The invention reduces reduce oxidation voltage and barrier layer thickness to make nanometer hole diameter rise from 20nm to 45-55nm. This is good for the further application of multi-hole alumina die plate.

Description

technical field [0001] The invention relates to a method for preparing a porous anodized aluminum template. Background technique [0002] High-purity aluminum is anodized in a suitable acidic electrolyte to obtain a porous anodized aluminum film, which is a typical self-organized nanomaterial. Porous anodized aluminum film has a unique structure, close to the surface of metal aluminum is a thin and dense barrier layer, on which a thicker and loose porous layer is formed. The membranous cells of the porous layer are arranged in hexagonal close packing, and each membranous cell has a nanoscale micropore in the center. By selecting the anodizing parameters, a porous aluminum oxide film with highly ordered nanopore arrays can be obtained. Due to the unique structure and good chemical stability of porous alumina film, it is an ideal template material. If various metals, alloys, semiconductors, conductive polymers, etc. are deposited into nanopores, various nanostructure materi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25D11/10
Inventor 安茂忠杨培霞郭洪飞
Owner HARBIN INST OF TECH
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