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A preparation method of porous anodized aluminum three-dimensional nanostructure

A porous anode and alumina technology, applied in the preparation of alumina/hydroxide, nanotechnology, etc., can solve the problems of difficult realization of three-dimensional micro-nano structure, low efficiency, expensive processing cost, etc.

Active Publication Date: 2016-03-16
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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Problems solved by technology

However, there are generally problems such as low efficiency and difficulty in realizing truly complex three-dimensional micro-nano structures.
The Photonic Professional direct-writing 3D laser processing system that has appeared since 2007 has solved the problem of preparing truly complex 3D micro-nano structures. Low efficiency and high processing cost
However, there are few reports on the rapid and low-cost realization of three-dimensional ordered porous micro-nanostructures with characteristic linewidths below 500 nm, especially below 200 nm.
[0004] Chinese patent CN101598895A publicly reported a method for preparing a phase grating with a three-dimensional structure on a porous anodized aluminum substrate by using periodic anodization of aluminum sheets combined with photolithography and chemical etching, but it is limited by the process conditions that photolithography technology must be used This method is also difficult to quickly manufacture large-area three-dimensional micro-nanoporous structures with characteristic linewidths below 500 nm in three-dimensional directions at low cost.

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  • A preparation method of porous anodized aluminum three-dimensional nanostructure
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[0054] Preparation of Porous Anodized Aluminum Material

[0055] The present invention also provides a method for preparing a porous anodized aluminum material, the method comprising the steps of:

[0056] (1) providing a porous anodic aluminum oxide sheet with a one-dimensional layered periodic structure;

[0057] (2) forming a PS microsphere self-assembled film on at least one major surface of the sheet;

[0058] (3) processing the PS microsphere self-assembled film so that the self-assembled film is bonded to the main surface of the sheet to form an aluminum oxide sheet with a PS microsphere self-assembled film bonded to the surface;

[0059] (4) chemically etching the alumina flakes with the self-assembled film, thereby forming a three-dimensional structure in the alumina flakes;

[0060] (5) Optionally, removing the PS microsphere self-assembled film to obtain a three-dimensional nanostructured porous anodized alumina material.

[0061] The porous anodized aluminum sheet...

Embodiment 1

[0094] High-purity aluminum flakes with a purity of 99.999% are used as raw materials to prepare porous anodized aluminum films with a layered periodic structure. The preparation method is as follows: before anodizing, the high-purity aluminum is first degreased with acetone, and then, at 450 ° C The aluminum foil was annealed for 4 hours, and the annealed aluminum foil was placed in a 1:9 mixture of perchloric acid and ethanol for electrochemical polishing for 3 minutes. Then, under the guidance of preset periodic voltage control, anodic oxidation treatment is carried out. The parameters of oxidation are: the electrolyte is 0.3M oxalic acid, the oxidation temperature is 15°C, the oxidation cycle time is 600S, and the minimum voltage of periodic anodic oxidation is 12V, the highest voltage is 30V, the number of periodic oxidation layers is 10, and the layer spacing is 500nm. After the periodic anodizing treatment, put the sample in 40°C, 5wt% phosphoric acid solution and etch ...

Embodiment 2

[0101]High-purity aluminum flakes with a purity of 99.999% are used as raw materials to prepare porous anodized aluminum films with a layered periodic structure. The preparation method is as follows: before anodizing, the high-purity aluminum is first degreased with acetone, and then, at 450 ° C The aluminum foil was annealed for 4 hours, and the annealed aluminum foil was placed in a 1:9 mixture of perchloric acid and ethanol for electrochemical polishing for 3 minutes. Then, under the guidance of preset periodic voltage control, the anodic oxidation treatment is carried out. The parameters of oxidation are: the electrolyte is 0.3M oxalic acid, the oxidation temperature is 15°C, the oxidation cycle time is 240S, and the minimum voltage of periodic anodic oxidation is 12V, the highest voltage is 30V, the number of periodic oxidation layers is 1000, and the layer spacing is 200nm. After the anodizing treatment, the sample was etched in a 5wt% phosphoric acid solution at 40°C fo...

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Abstract

The invention provides a preparation method of a porous anodic aluminum oxide material, which specifically comprises the following steps: (1) providing a porous anodic aluminum oxide sheet with a one-dimensional layered periodic structure; (2) forming a layer of PS microsphere self-assembled film on the surface of the sheet; (3) treating the PS microsphere self-assembled film so that the self-assembled film is bound with the surface of the sheet to form an aluminum oxide sheet bound with the PS microsphere self-assembled film on the surface; (4) performing chemical etching on the aluminum oxide sheet with the self-assembled film; (5) removing the PS microsphere self-assembled film to obtain the porous anodic aluminum oxide with a three-dimensional nano structure. The method has the characteristics of low cost and fitness with large-scale quick production, and is particularly suitable for preparing a three-dimensional micro-nano structure material of which the characteristic line width in three-dimensional directions is less than 2,000nm.

Description

technical field [0001] The invention relates to the field of preparation of three-dimensional nanomaterials, in particular, the invention relates to a method for preparing three-dimensional ordered porous anodic aluminum oxide nanomaterials. Background technique [0002] With the development of modern industry and high-tech industry, new micro-nano structure devices such as nano-sensors, nano-smart devices and micro-systems continue to appear in laboratories. Based on the important role of nano-devices, nano-manufacturing technology has become a high-tech in developed countries The commanding heights of competition. my country has also listed "nanotechnology and microsystems" as one of the "eight strategic high-tech fields and high-tech industrialization" in the next fifteen years. Three-dimensional porous micro-nanostructures are one of the important directions of nanomaterials and devices, and have been widely used in photonic crystals, metamaterials, distributed laser fe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F7/42B82Y40/00
Inventor 张海青杨伟王彪许高杰
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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