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Method for preparing double-layer self peeling nano porous anodised aluminum film

A technology of anodized aluminum and porous anodes, applied in the field of material chemistry, can solve problems such as corrosion, poor effect of membrane through-holes, expensive equipment, etc., achieve regular pore diameters, and avoid the effects of chemical corrosion and pore expansion

Inactive Publication Date: 2011-02-09
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The chemical etching method has chemical reagent pollution and phosphoric acid corrosion of the membrane pores, the electrochemical stripping method is not effective for the membrane through-holes prepared under high voltage, and the equipment required by the ion beam etching method is expensive, which is to a large extent limit the application range of porous anodic aluminum oxide membrane

Method used

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  • Method for preparing double-layer self peeling nano porous anodised aluminum film
  • Method for preparing double-layer self peeling nano porous anodised aluminum film
  • Method for preparing double-layer self peeling nano porous anodised aluminum film

Examples

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Effect test

Embodiment 1

[0030] The steps of preparing double-layer self-stripping porous anodic aluminum oxide membrane provided by the invention are as follows:

[0031] (1) The aluminum sheet is annealed at 500° C. for 5 hours under the protection of nitrogen atmosphere. Electrochemical polishing was performed for 5 minutes in a 1:5 perchloric acid-ethanol mixture solution at a potential of 20V.

[0032] (2) install the aluminum sheet after the pretreatment of step (1) in the U-shaped electrolytic cell system as the anode, add the phosphoric acid that contains 1.0mol / L of 50% polyethylene glycol-400 as the electrolysis Liquid, with a clean large-area aluminum sheet as the cathode to form a two-electrode electrolysis system;

[0033] (3) Adopting a constant temperature water bath to control the temperature of the electrolytic cell to be 15°C;

[0034] (4) Use a potentiostat to control the oxidation potential, and perform electrolysis at 180V, 190V, 200V, 210V, 220V, 230V, 240V, 250V and 260V;

[...

Embodiment 2

[0038] The steps of preparing double-layer self-stripping porous anodic aluminum oxide membrane provided by the invention are as follows:

[0039] (1) The aluminum sheet is annealed at 500° C. for 5 hours under the protection of nitrogen atmosphere. Electrochemical polishing was performed for 5 minutes in a 1:5 perchloric acid-ethanol mixture solution at a potential of 20V.

[0040] (2) install the aluminum sheet after the pretreatment of step (1) in the U-shaped electrolytic cell system as the anode, add the phosphoric acid that contains 1.0mol / L of 50% polyethylene glycol-400 as the electrolysis Liquid, with a clean large-area aluminum sheet as the cathode to form a two-electrode electrolysis system;

[0041] (3) Adopting a constant temperature water bath to control the temperature of the electrolytic cell to be 15°C;

[0042] (4) Adopt potentiostat to control oxidation potential, carry out electrolysis with 190V;

[0043] (5) Connect the power supply in step (4) to the a...

Embodiment 3

[0046] The steps of preparing double-layer self-stripping porous anodic aluminum oxide membrane provided by the invention are as follows:

[0047] (1) The aluminum sheet is annealed at 500° C. for 5 hours under the protection of nitrogen atmosphere. Electrochemical polishing was performed for 5 minutes in a 1:5 perchloric acid-ethanol mixture solution at a potential of 20V.

[0048] (2) install the aluminum sheet after the pretreatment of step (1) in the U-shaped electrolytic cell system as the anode, and add the concentration of 50% polyethylene glycol-400 containing 0.8mol / L, 1.0mol / L, 1.5mol / L and 2.0mol / L phosphoric acid are used as the electrolyte, and a clean large-area aluminum sheet is used as the cathode to form a two-electrode electrolysis system;

[0049] (3) Adopting a constant temperature water bath to control the temperature of the electrolytic cell to be 15°C;

[0050] (4) Adopt potentiostat to control oxidation potential, carry out electrolysis with 190V;

[0...

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Abstract

The invention relates to a preparation method of double-layer self-stripping multi-pore anode alumina film, which comprises the following steps: first, an aluminum sheet receives annealing and electro-chemical polishing treatment; and then, the treated aluminum sheet is put into a constant potential electrolytic cell, high-concentration phosphoric acid solution is added in as electrolyte and polyoxyethylene-400 is added in to be regulator, constant potential anode oxidation is carried out, and the double-layer self-stripping multi-pore anode alumina film is obtained, wherein, the upper layer of the film is a through hole structure and the lower layer of the film is a nano tube array structure. The invention leads the multi-pore alumina film to self strip with local heat produced in the oxidation process under high potential and high phosphoric acid concentration conditions, to form the double-layer film with the upper layer of a through hole structure and the lower layer of a nano tube array structure. The polyoxyethylene-400 can effectively prevent pore expansion produced by chemical corrosion, and the obtained upper layer of through hole film has regular aperture and can be directly used for template preparation with nano separation film or nano material.

Description

technical field [0001] The invention relates to a preparation method of an anodic aluminum oxide film, which belongs to the field of material chemistry. Background technique [0002] At present, the controllable preparation and application of porous alumina membranes as templates for the preparation of nanomaterials and nano-separation membranes has attracted widespread attention. In these applications, porous alumina membranes with through holes are often required. However, the porous alumina film prepared by anodic oxidation is connected to the substrate aluminum sheet, and there is still a closed barrier layer after being separated from the aluminum sheet, so it is impossible to directly obtain the alumina film with through holes. The currently used lift-off via technologies mainly include chemical etching, electrochemical lift-off, and ion beam etching. The chemical etching method has chemical reagent pollution and the corrosion of the membrane pores by phosphoric acid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25D11/04
Inventor 夏兴华陈伟
Owner NANJING UNIV
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