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Method for rapid preparation of large-area highly ordered porous anodic aluminum oxide membrane with large pore spacing

A highly ordered and large-area technology, applied in the field of electrochemistry, can solve problems such as complex and cumbersome pretreatment processes and long preparation times

Inactive Publication Date: 2019-02-22
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantage is that it requires complex and cumbersome pretreatment processes (such as annealing, polishing, embossing, deoxidation film, etc.) and long preparation time (even up to several days)

Method used

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  • Method for rapid preparation of large-area highly ordered porous anodic aluminum oxide membrane with large pore spacing

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] First, immerse an aluminum foil strip with a purity of 99.99%, a thickness of 200 μm, and a width of 20 mm in a 2 wt % sodium hydroxide solution at a temperature of 70 ° C for 1 minute to remove the natural oxide film on the aluminum surface. Then rinse it with deionized water, put it into the electrolytic cell as the anode, and use another aluminum foil strip of the same size that has not been treated to remove the natural oxide film as the cathode. Use 30wt% ethyl phosphate aqueous solution as the electrolyte, constant voltage 200V, and carry out constant voltage anodic oxidation under the condition of vigorously stirring the electrolyte. The temperature of the electrolyte is kept at about 60°C by a water bath, the oxidation time is determined by the thickness of the PAA template, and the growth rate of the oxide film is about 3 μm·min -1 . The average hole spacing of PAA nanoholes is about 460nm.

Embodiment 2

[0026] First, immerse an aluminum foil strip with a purity of 99.99%, a thickness of 200 μm, and a width of 20 mm in a 2 wt % sodium hydroxide solution at a temperature of 70 ° C for 1 minute to remove the natural oxide film on the aluminum surface. Then rinse it with deionized water, put it into the electrolytic cell as the anode, and use another aluminum foil strip of the same size that has not been treated to remove the natural oxide film as the cathode. Use 30wt% ethyl phosphate aqueous solution as the electrolyte, constant voltage 230V, and carry out constant voltage anodic oxidation under the condition of vigorously stirring the electrolyte. The temperature of the electrolyte is maintained at about 10°C by a water bath. The oxidation time is determined by the thickness of the PAA template, and the growth rate of the oxide film is about 2.8 μm min -1 . The average hole spacing of PAA nanoholes is about 530nm.

Embodiment 3

[0028] First, immerse an aluminum foil strip with a purity of 99.99%, a thickness of 200 μm, and a width of 20 mm in a 2 wt % sodium hydroxide solution at a temperature of 70 ° C for 1 minute to remove the natural oxide film on the aluminum surface. Then rinse it with deionized water, put it into the electrolytic cell as the anode, and use another aluminum foil strip of the same size that has not been treated to remove the natural oxide film as the cathode. Using 20wt% phosphate monoester aqueous solution as the electrolyte, constant voltage 270V, under the condition of vigorously stirring the electrolyte, the constant voltage anodic oxidation is carried out. The temperature of the electrolyte is maintained at about 25°C by a water bath. The oxidation time is determined by the thickness of the PAA template, and the growth rate of the oxide film is about 2.5 μm min -1 . The average hole spacing of PAA nanoholes is about 620nm.

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Abstract

The invention discloses a method for preparing a large-area highly-ordered large-hole-pitch porous anodic aluminum oxide membrane. Aluminum foil which is subjected to oxidation membrane removing treatment serves as an anode, a phosphomonoester solution with the concentration, by weight, being 2-30% serves as an electrolyte, constant-pressure anodic oxidation treatment is conducted under the electrolyte temperature of 10-60 DEG C, and a large-area large-hole-pitch highly-ordered PAA membrane is obtained. By adoption of the method, it is ensured that the oxide membrane can grow evenly, stably and quickly and the electric breakdown phenomenon does not occur, the aluminum oxide membrane does not need to be subjected to complex pretreatment processes, a strong cooling system is not needed, quick and stable growing of the large-area highly-ordered large-hole-pitch porous anodic aluminum oxide membrane is achieved, and the growing speed of the membrane can reach 2 [mu]m / min or above under the voltage within 200-530V.

Description

technical field [0001] The invention belongs to the technical field of electrochemistry, and relates to a method for preparing a porous anodic aluminum oxide film, in particular to a simple and fast electrolytic process for an anodic aluminum oxide film with a nano-hole array structure with a large area and highly ordered large pore spacing. Chemical preparation method. Background technique [0002] Porous anodized aluminum (PAA) membrane is a self-assembled hexagonal close-packed nano-hole array structure, which has the advantages of simple preparation process, low cost, adjustable pore size, high pore density, and easy chemical dissolution by acid or alkali. . Using PAA as a template has a very wide range of applications in the synthesis of nanomaterials and devices of different sizes. Among them, in some application fields such as the preparation of nanostructured photovoltaic devices (Fan Z, et al., Nature materials, 2009, 8(8): 648), PAA templates with large apertures...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25D11/06C25D11/10
CPCC25D11/045C25D11/06C25D11/10
Inventor 宋晔刘仪朱绪飞张贺陈群王晶
Owner NANJING UNIV OF SCI & TECH