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Preparation method of three-dimensional nano structure of porous anodic aluminum oxide

A porous anode and three-dimensional nanotechnology, which is applied in the preparation of alumina/hydroxide and nanotechnology, can solve the problems of high processing cost, difficulty in realizing three-dimensional micro-nano structure, and low efficiency.

Active Publication Date: 2014-05-21
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. Still inefficient and expensive to process
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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  • Preparation method of three-dimensional nano structure of porous anodic aluminum oxide
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  • Preparation method of three-dimensional nano structure of porous anodic aluminum oxide

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[0054] Preparation of Porous Anodic Aluminum Oxide

[0055] The present invention also provides a method for preparing porous anodic aluminum oxide material. The method includes the steps:

[0056] (1) Provide 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 main surface of the sheet;

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

[0059] (4) Chemically etch the aluminum oxide sheet with self-assembled film, thereby forming a three-dimensional structure in the aluminum oxide sheet;

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

[0061] The porous anodic aluminum oxide flakes can be prepared ...

Embodiment 1

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

Embodiment 2

[0101] High-purity aluminum sheets with a purity of 99.999% are used as raw materials to prepare porous anodic aluminum oxide films with a layered periodic structure. The preparation method is as follows: before anodizing, the high-purity aluminum is degreasing with acetone, and then at 450°C The aluminum foil is annealed for 4 hours, and the annealed aluminum foil is electrochemically polished for 3 minutes in a mixture of perchloric acid and ethanol at a ratio of 1:9. Then, the anodic oxidation treatment is carried out under the guidance of the preset periodic voltage control. The oxidation parameters 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 periodically oxidized layers is 1000, and the layer spacing is 200nm. After the anodizing treatment, put the sample in a 5wt% phosphoric acid solution at 40°C and etch...

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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 present invention relates to the field of preparation of three-dimensional nanomaterials. Specifically, the present invention relates to a method for preparing three-dimensional ordered porous anodic alumina nanomaterials. Background technique [0002] With the development of modern industry and high-tech industries, new micro-nano structure devices such as nano-sensors, nano-smart devices and micro-systems continue to appear in the laboratory. Based on the important role of nano-devices, nano-manufacturing technology has become a high-tech in developed countries in the world The commanding heights of competition. my country also lists "nanotechnology and microsystems" as one of the "8 strategic high-tech fields and high-tech industrialization" in the next 15 years. Three-dimensional porous micro-nano structure is one of the important directions of nanomaterials and devices. It has a wide range of applications in the fields of photonic crystals, metama...

Claims

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Application Information

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Patent Type & Authority Applications(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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