Method for preparing large-hole-interval porous anodic alumina membrane at high voltage

A technology of porous anode and aluminum oxide film, which is applied in the field of high-voltage preparation of porous anodic aluminum oxide film with large pore spacing, can solve the problems of complicated equipment and process, difficult to obtain raw materials, high cost, etc., and achieves fast film forming speed and convenient operation. , the effect of low cost

Inactive Publication Date: 2016-02-03
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The sub-micron and micro-porous templates currently used are mainly derived from natural materials or photolithography preparation processes, and there are disadvantages such as difficulty in obtaining raw materials, complex equipment and processes, and high cost. These problems have not been solved well.
However, increasing the anodizing voltage is likely to cause breakdown and burning of the film

Method used

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  • Method for preparing large-hole-interval porous anodic alumina membrane at high voltage
  • Method for preparing large-hole-interval porous anodic alumina membrane at high voltage
  • Method for preparing large-hole-interval porous anodic alumina membrane at high voltage

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Embodiment 1

[0026] A method for preparing a porous anodic aluminum oxide film with a large-pore spacing at high voltage, the large-pore spacing is generally considered to exceed 300nm, comprising the following steps:

[0027] (1) Cleaning high-purity aluminum sheets with a mass fraction ≥ 99.99% in absolute ethanol and deionized water in sequence to obtain clean aluminum sheets.

[0028] (2) With the clean aluminum sheet obtained in step (1) as the anode and the graphite as the cathode, perform electrochemical polishing at 20V in a mixed solution of perchloric acid and absolute ethanol with a volume ratio of 1:4 at 0°C to obtain Polished aluminum sheet.

[0029] (3) the polished aluminum flake obtained in step (2) is an anode, and graphite is a cathode, and the voltage is 1000V, and the current density is set to 40mA / cm 2 , solution A (absolute ethanol) and solution B (0.25mol / L oxalic acid aqueous solution) volume ratio is A: B = 2 mixed solution to carry out anodic oxidation process, t...

Embodiment 2

[0032] A method for preparing a porous anodic aluminum oxide membrane with large pore spacing at high voltage, comprising the steps of:

[0033] (1) Cleaning high-purity aluminum sheets with a mass fraction ≥ 99.99% in absolute ethanol and deionized water in sequence to obtain clean aluminum sheets.

[0034] (2) With the clean aluminum sheet obtained in step (1) as the anode and the graphite as the cathode, perform electrochemical polishing at 25V in a mixed solution of perchloric acid and absolute ethanol with a volume ratio of 1:5 at 3°C ​​to obtain Polished aluminum sheet.

[0035] (3) the polished aluminum flake obtained in step (2) is an anode, and graphite is a cathode, and at a voltage of 700V, the current density is set to 50mA / cm 2 , solution A (absolute ethanol) and solution C (0.3mol / L oxalic acid aqueous solution) volume ratio is A:C=1 mixed solution to carry out anodic oxidation process, the temperature is 4 ° C: first under constant flow conditions Adapt to the...

Embodiment 3

[0038]A method for preparing a porous anodic aluminum oxide membrane with large pore spacing at high voltage, comprising the steps of:

[0039] (1) Cleaning high-purity aluminum sheets with a mass fraction ≥ 99.99% in absolute ethanol and deionized water in sequence to obtain clean aluminum sheets.

[0040] (2) With the clean aluminum sheet obtained in step (1) as the anode and the graphite as the cathode, perform electrochemical polishing at 15V in a mixed solution of perchloric acid and absolute ethanol with a volume ratio of 1:4 at 5°C to obtain Polished aluminum sheet.

[0041] (3) the polished aluminum sheet obtained in step (2) is an anode, and graphite is a cathode, and at a voltage of 900V, the current density is set to 20mA / cm 2 , the volume ratio of solution A (absolute ethanol) and solution D (0.35mol / L oxalic acid aqueous solution) is A: D = 4 mixed solution conditions to carry out anodic oxidation process, the temperature is 2 ° C: first under constant flow condi...

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Abstract

The invention discloses a method for preparing a large-hole-interval porous anodic alumina membrane at high voltage. The method includes the steps that a high pure aluminum sheet is subjected to electrochemical polishing after being washed; the polished aluminum sheet serves as an anode, graphite serves as a cathode, the anode oxidation process is performed while an oxalic acid-ethanol-water mixed solution serves as an electrolyte, and high anode oxidization voltage is obtained by performing self-adaption boosting under constant current density; a sample obtained through anode oxidization is soaked in a saturated copper chloride solution, then the large-hole-interval porous anodic alumina membrane is obtained, and the average hole interval of the prepared porous anodic alumina membrane is regulated and controlled by adjusting the ethanol adding proportion, the anode oxidization voltage and the current density. The large hole interval size of the prepared porous anodic alumina membrane is adjustable so that the porous anodic alumina membrane can serve as a template to synthesize various functional submicron and micron materials. Meanwhile, the large-hole-interval porous anodic alumina membrane has the advantages that raw materials are easy to obtain, operation is easy, cost is low, and repeatability is good, and feasibility is improved when the large-hole-interval porous anodic alumina membrane is applied to production.

Description

technical field [0001] The invention relates to the technical field of material preparation, in particular to a method for preparing a porous anodic aluminum oxide film with large pore spacing at high voltage. Background technique [0002] In recent years, due to the rapid development of industry, a large number of functional materials are required, and the natural functional materials in nature are far from meeting the needs of industrial development. Therefore, more and more attention has been paid to the artificial synthesis technology of materials. The commonly used methods for synthetic materials mainly include template method and direct synthesis method, among which the template method is widely used to synthesize various nano functional materials, such as nanodots, nanowires, nanotubes, etc. Compared with the direct synthesis method, the template method has the advantages of simple manufacturing process, high controllability, and good repeatability. Considering that ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/10
Inventor 李屹金世遇覃玉燕
Owner SOUTH CHINA UNIV OF TECH
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