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A kind of preparation method of ultra-thin through-hole anodic aluminum oxide film

An anodic aluminum and anodic oxidation technology, which is applied in vacuum evaporation plating, coating, sputtering plating and other directions, can solve the problems of difficult to precisely control the thickness of nanopores, complicated steps, etc., and achieves easy mass production and simple control. , the method is easy to repeat the effect

Inactive Publication Date: 2019-03-05
HUAZHONG UNIV OF SCI & TECH
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Problems solved by technology

[0003] In recent years, the preparation of ultra-thin through-hole anodized aluminum nanoporous templates has attracted more and more attention from researchers. For example, patent CN104726920 discloses a preparation and transfer method of ultra-thin through-hole anodized aluminum. And its transfer method uses two times of anodic oxidation to generate an ordered alumina nanoporous structure. Under the protection of polystyrene PS, the aluminum substrate and barrier layer are removed to obtain an ultra-thin through-hole alumina nanoporous structure. This method obtains The alumina templates are evenly distributed and the pore size is consistent, but the steps are cumbersome, and the thickness of the prepared nanopores is not easy to precisely control

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  • A kind of preparation method of ultra-thin through-hole anodic aluminum oxide film
  • A kind of preparation method of ultra-thin through-hole anodic aluminum oxide film
  • A kind of preparation method of ultra-thin through-hole anodic aluminum oxide film

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preparation example Construction

[0031] The preparation method of the ultra-thin through-hole anodic aluminum oxide film mainly includes the following steps:

[0032] In step 1, an aluminum substrate is provided, and after the surface of the aluminum substrate is electrochemically polished, cleaned and dried in sequence, an aluminum film is deposited on the surface of the aluminum substrate by magnetron sputtering coating method. In this embodiment, the sputtering time is 347-3472s, the aluminum film thickness is 100-1000nm; the sputtering power is 200W, the sputtering gas mass flow rate is 35sccm, and the sputtering rate is 0.288nm / s.

[0033] In step 2, the aluminum substrate is subjected to an anodic oxidation reaction by an anodic oxidation method to obtain an aluminum oxide nanotube film, and the anodic oxidation time is 30 minutes. In this embodiment, the thickness of the obtained alumina nanotubes is 2.696 μm, the diameter of the alumina nanotube film is 1-3 cm, the control voltage is 40-60 V, and the ...

no. 1 approach

[0038] (1) The pure aluminum sheet (purity is 99.99%, size is 2cm×2cm×1mm) is electrochemically polished in a mixture of perchloric acid and ethanol (volume ratio 1:4), and the polishing voltage is 15-18V, The current is 1A, and the polishing time is 3min; the polished aluminum sheet is ultrasonically cleaned with deionized water and dried.

[0039] (2) Utilize the magnetron sputtering coating method to deposit a uniform aluminum film on the surface of the polished aluminum sheet, the sputtering power is 200W, the sputtering gas mass flow rate is 35sccm, and the sputtering rate obtained through regulation is 0.288nm / s, the sputtering time is 694s.

[0040] (3) The coated aluminum sheet is used as an anode, and the graphite sheet is used as a cathode, and an anodic oxidation reaction is carried out in an oxalic acid solution with a mass percentage of 3%. The anodizing temperature is 20°C, the voltage is 40V, the current is 20mA, and the oxidation time is 30min. After the rea...

no. 2 approach

[0044] The second embodiment is basically the same as the first embodiment, except that the sputtering time in step (2) of the second embodiment is 1041s, and a 300nm thick aluminum film is deposited on the surface of the aluminum sheet.

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Abstract

The invention belongs to the related technical field of nanometer material preparing, and discloses a preparing method of an ultra-thin through hole anode aluminum oxide film. The method comprises following steps: firstly, the surface of an aluminum substrate is sequentially subject to treatment, and an aluminum film is deposited on the surface of the aluminum substrate; secondly, the aluminum substrate is subject to an anode oxidizing reaction, and an aluminum oxide nanotube film is obtained; thirdly, the aluminum oxide nanotube film is protected, the aluminum substrate is placed in a saturated CuC12 solution to be subject to the reaction, and the aluminum oxide nanotube film with one end closed is obtained; fourthly, a phosphoric acid solution is dripped to the surface, away from a carrier, of the aluminum oxide nanotube film, and the phosphoric acid solution and the aluminum oxide nanotube film close to a blocking layer have the reaction; fifthly, the surface of the aluminum oxide nanotube film is washed, and the ultra-thin through hole anode aluminum oxide film is obtained. The preparing method is simple and easy to repeat, the experiment cost is reduced, and large-scale production is facilitated.

Description

technical field [0001] The invention belongs to the technical field related to the preparation of nanometer materials, and more specifically relates to a method for preparing an ultrathin through-hole anodic aluminum oxide film. Background technique [0002] Pure aluminum sheet can prepare a regular nanoporous alumina structure through anodic oxidation reaction, and the structural parameters of nanotubes include: anodic oxidation voltage, time, electrolyte type and concentration. The nanotube has electrical insulation, light permeability, chemical stability, biological inertness and biocompatibility, and has potential applications in optics, electrochemistry, biology and the like. For the anodic oxidation method, a highly ordered nanoporous structure can be prepared through a simple preparation process under low-cost and simple equipment conditions. It is precisely because of this highly ordered and porous nanopore structure and the controllability of the structure that alu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C14/35C23C14/16C25D11/16C25D11/24C25D11/10
CPCC23C14/165C23C14/35C25D11/10C25D11/16C25D11/24
Inventor 李佳红张文军徐鸣
Owner HUAZHONG UNIV OF SCI & TECH
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