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Preparation method of porous alumina membrane with two layers communicated with each other

A technology of porous alumina and alumina film, applied in the field of material science, can solve problems such as the destruction of alumina film, and achieve the effects of easy control of reaction, simplified preparation process and simple process

Inactive Publication Date: 2013-04-10
HEBEI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above preparation method requires some special devices, and the whole process of removing the aluminum base needs to be very careful, otherwise the aluminum oxide film is easily damaged

Method used

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  • Preparation method of porous alumina membrane with two layers communicated with each other
  • Preparation method of porous alumina membrane with two layers communicated with each other
  • Preparation method of porous alumina membrane with two layers communicated with each other

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Under the condition of ice-water bath (~0°C), immerse 99.999% high-purity aluminum foil in a mixture of perchloric acid and ethanol with a volume ratio of 1:4 for electrochemical polishing, with a current of 200mA and a polishing time of 1 min;

[0020] (2) Under stirring, pre-oxidize the polished high-purity aluminum foil in 0.3mol / L oxalic acid electrolyte at a voltage of 10-20V and a current of 7mA for 0.5h, then fine-tune the aluminum foil (oxidized film) position, lift up the aluminum foil so that the top of the aluminum foil is slightly exposed to the electrolyte surface by 1 mm, and continue to oxidize for 3 hours under the conditions of a voltage of 30V and a current of 5-8mA;

[0021] (3) The aluminum foil obtained in step (2) is heated in 0.6mol / L H at a temperature of 50°C 3 PO 4 and 0.18mol / L H 2 CrO 4 Immerse in the mixed solution mixed in equal volume for 1 hour to remove the oxide film on the surface of the aluminum foil;

...

Embodiment 2

[0026] (1) Under the condition of ice-water bath (~0°C), immerse 99.999% high-purity aluminum foil in a mixture of perchloric acid and ethanol with a volume ratio of 1:4 for electrochemical polishing, with a current of 200mA and a polishing time of 1 min;

[0027] (2) Under stirring, pre-oxidize the polished high-purity aluminum foil in 0.3mol / L oxalic acid electrolyte at a voltage of 10-20V and a current of 5mA for 1h, then fine-tune the position of the aluminum foil (oxidation film) , lift the aluminum foil up, so that the top of the aluminum foil is slightly exposed to the electrolyte surface by 2mm, and continue to operate at a voltage of 40V and a current of 10-15mA

[0028] Oxidation under the condition of 1.5h;

[0029] (3) The aluminum foil obtained in step (2) is heated in 0.6mol / L H at a temperature of 50°C 3 PO 4 and

[0030] 0.18mol / L H 2 CrO 4 Immerse in the mixed solution mixed in equal volume for 1 hour to remove the oxide film on...

Embodiment 3

[0036] (1) Under the condition of ice-water bath (~0℃), immerse 99.999% high-purity aluminum foil in a mixture of perchloric acid and ethanol with a volume ratio of 1:4 for electrochemical polishing, with a current of 150mA and a polishing time of 2 min;

[0037] (2) Under stirring, pre-oxidize the polished high-purity aluminum foil in 0.3mol / L oxalic acid electrolyte for 0.5h at a voltage of 10-20V and a current of 3.5mA, then fine-tune the aluminum foil (oxidation film) Lift the aluminum foil upwards, so that the top of the aluminum foil is slightly exposed to the electrolyte surface by 3 mm, and continue to oxidize for 2 hours under the conditions of voltage 35V and current 8-10mA;

[0038] (3) The aluminum foil obtained in step (2) is heated in 0.6mol / L H at a temperature of 50°C 3 PO 4 and 0.18mol / L H 2 CrO 4 Immerse in the mixed solution mixed in equal volume for 1 hour to remove the oxide film on the surface of the aluminum foil;

[0039] (4...

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Abstract

The invention discloses a preparation method of a porous alumina membrane with two-sided communicated with each other. The method comprises carrying out a electrochemical polishing process for an aluminium foil, then carrying out a preoxidation process for the polished aluminium foil for a certain time under a condition of low current and a continued oxidation process under a certain voltage for the polished aluminium foil, then removing an alumina membrane of the oxidized aluminium foil by a mixed liquor of phosphoric acid and chromic acid, then carrying out a secondary oxidation process for the aluminium foil processed by the above processes, and carrying out a aperture reaming process finally to obtain a highly ordered aluminum substrate-free porous alumina membrane with two-sided communicated with each other. Through a position adjustment for an aluminium foil and a preoxidation process under a condition of low current, the aluminium foil can be oxidized stably without being broken down under a condition of a high voltage, and a highly ordered aluminum substrate-free porous alumina membrane with two-sided communicated with each other can be obtained in a short time. The preparation method provided by the invention has the advantages of simple processes, low cost and high yield, and can be utilized for the preparations of nanometer materials and devices.

Description

technical field [0001] The invention relates to a method for preparing a double-sided through-hole porous aluminum oxide film, which belongs to the technical field of material science. Background technique [0002] Porous alumina thin films have been widely used in the preparation of one-dimensional nanomaterials, nanoarrays, and nanodevices due to their regular and ordered fine hexagonal pore structure and stable physical and chemical properties. At present, the preparation method of porous alumina film is relatively mature. In the prior art, many patents have disclosed the preparation method of aluminum oxide thin film, such as CN03136606.6, CN200310111834.1, CN200510007195.3, CN200710039634.8, CN200910089254.4 and so on. Usually, the preparation method of porous alumina film is: the aluminum foil is first annealed in an argon or nitrogen atmosphere; then, using oxalic acid, sulfuric acid or phosphoric acid, etc. Aluminum film. Usually CuCl 2 , SnCl 4 , HgCl 2...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25D11/12C25D11/16
Inventor 柴玉俊刘增彦闫小龙王宁
Owner HEBEI NORMAL UNIV
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