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Method for thinning porous anodized aluminum template barrier layer at normal temperature

A technology of alumina template and porous anode, which is applied in the direction of anodic oxidation, coating, surface reaction electrolytic coating, etc., can solve the problems of restricting popularization, destroying porous structure, and inability to prepare nanomaterials, so as to reduce processing time and improve preparation Efficiency, avoiding the effect of V-shaped channel structure

Inactive Publication Date: 2015-03-25
HUAZHONG UNIV OF SCI & TECH RES INST SHENZHEN
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Problems solved by technology

The chemical corrosion method mainly uses acid solution to corrode the whole template to thin the barrier layer, but this will corrode the pores or channels at the same time, resulting in larger pore diameters and even destroying the porous structure; the step-down method is mainly used at zero degrees Celsius. The purpose of thinning the barrier layer is achieved by gradually reducing the anodic oxidation voltage, but this method is currently limited to mild oxidation under low temperature conditions, which generally takes 3-5 hours, which seriously restricts the popularization of this technical method, and due to If the anodizing time of each voltage platform is too long, a "V"-shaped channel structure will be formed at the bottom of the channel, causing the deposited material to fail to reach the bottom of the "V"-shaped channel, the deposition process cannot be completed, and nanomaterials cannot be prepared.

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  • Method for thinning porous anodized aluminum template barrier layer at normal temperature
  • Method for thinning porous anodized aluminum template barrier layer at normal temperature
  • Method for thinning porous anodized aluminum template barrier layer at normal temperature

Examples

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Embodiment 1

[0032] S1: Preparation of a porous anodized alumina primary template comprising an aluminum layer and an aluminum oxide layer. There are multiple holes in the aluminum oxide layer, the holes penetrate the aluminum oxide layer and form pits on the surface of the aluminum layer, and then remove the aluminum oxide layer on the porous anodized aluminum primary template to obtain the aluminum oxide layer with pits on the surface aluminum layer. The detailed process is as follows:

[0033]First cut the aluminum sheet with a thickness of 100 μm into regular rectangular pieces of 10mm×100mm, and then anneal at 500°C in a muffle furnace. The annealing treatment is used to reduce lattice defects and prevent subsequent irregular nanopores. After annealing The aluminum sheet was ultrasonically cleaned by acetone, alcohol, and distilled water for 15 minutes each to remove surface oil, and finally with N 2 Blow dry to obtain aluminum flakes with clean surface.

[0034] Then electrochemic...

Embodiment 2

[0047] S1: same as step S1 of embodiment 1;

[0048] S2: same as step S2 of embodiment 1;

[0049] S3: Other processes are the same as step S3 of Example 1, except that oxalic acid with a hydrogen ion concentration of 0.2 mol / L is used to thin the barrier layer at a water bath temperature of 25°C. In the step-down current method, the maximum current is 0.07A, the minimum current is 0, and the gradient of each reduction of the current is 0.01A. A porous anodized aluminum template that can be directly prepared for nanomaterials is also obtained.

Embodiment 3

[0051] S1: same as step S1 of embodiment 1;

[0052] S2: same as step S2 of embodiment 1;

[0053] S3: Other processes are the same as step S3 of Example 1, the only difference is that the barrier layer is thinned by using a mixed acid solution of phosphoric acid and citric acid with a hydrogen ion concentration of 0.4 mol / L at a water bath temperature of 20°C processing. In the step-down current method, the maximum current is 0.05A, the minimum current is 0, and the gradient of each reduction of the current is 0.01A. A porous anodized aluminum template that can be directly prepared for nanomaterials is also obtained.

[0054] In the present invention, the acid solution in step S3, the hydrogen ion concentration of the acid solution, the water bath temperature in step S3, etc. are not limited to the specific values ​​of the above examples, and are not limited to the combination of the above specific values. When the water bath temperature is When the temperature is 20-30°C ...

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Abstract

The invention discloses a method for thinning a porous anodized aluminum template barrier layer at normal temperature, belonging to the field of porous anodized aluminum templates. The method comprises the following steps: S1, preparing a primary porous anodized aluminum template and removing an aluminum oxide layer on the template to obtain an aluminum layer with pits on the surface; S2, preparing a secondary porous anodized aluminum template containing the aluminum layer and the aluminum oxide layer by taking the aluminum layer obtained in the step S1 as an anode and an inert metal as a cathode; and S3, thinning a barrier layer in the porous anodized aluminum template in the S2 in acid liquor by using a step-down current method to thin the barrier layer at the bottom of a hole to below 10nm, thus realizing thinning treatment, wherein the step-down current method is an electrochemical treatment method which gradually reduces the current from the maximum current to zero with same gradient each time. According to the method disclosed by the invention, the barrier layer can be quickly and efficiently thinned, the shape of the template can be effectively remained, and a broaching phenomenon that the bore diameter is enlarged does not exist.

Description

technical field [0001] The invention belongs to the field of porous anodized aluminum oxide templates, and more specifically relates to a method for thinning the barrier layer of porous anodized aluminum oxide templates at normal temperature. Background technique [0002] Porous alumina has continuous and straight channels, and the depth of the channels can be adjusted according to the length of oxidation time, and because alumina has good chemical and thermal stability, high hardness, and large specific surface area, Therefore, it has become a widely used template for the preparation of nanomaterials, and has extremely important applications in the fields of preparation of nanomaterials, biosensing materials, spectral materials, magnetic materials, and solar cell materials. At present, the porous anodized alumina template is mainly prepared by anodizing aluminum sheets in oxalic acid, sulfuric acid, phosphoric acid and other solutions to prepare a preliminary porous anodize...

Claims

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Application Information

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IPC IPC(8): C25D11/06C25D11/18B82Y40/00
CPCC25D11/045B82Y40/00C25D11/18
Inventor 朱文曹国宝崇保和
Owner HUAZHONG UNIV OF SCI & TECH RES INST SHENZHEN
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