Ordered extralarge-hole-pitch alumina film and preparation method thereof

An aluminum oxide film, super-porous technology, applied in anodizing, electrolytic coating, surface reaction electrolytic coating, etc., can solve the problems of high price of ethylphosphoric acid, difficult practical application, poor reproducibility, etc., and achieve obvious results. Photoluminescence performance, good industrial application prospect, simple process effect

Active Publication Date: 2017-03-29
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, how to fabricate self-assembled AlO films with ultra-large pore spacing (>500 nm) remains a great challenge.
[0004] Kikuchi. et al prepared an ordered alumina film with a pore spacing of 530-670 nm using etidronate as the electrolyte at 210-270 V. However, etidronate is expensive and difficult to apply in practice, which limits its use as a new Electrolyte Preparation of Ultra-Large Pore Spacing Membrane
Chinese invention patent CN102839408B discloses a method for ultrasonically assisted anodic oxidation to prepare porous aluminum oxide film with super large pore spacing, using ethanol in citric acid electrolyte to increase the electrolysis voltage, combined with ultrasonic technology to increase the electrolysis rate, to achieve ultra-high voltage (>500V ) stable electrolysis, and obtain ultra-large pore spacing PAA with a pore spacing of more than 1 micron. This preparation method has complex procedures, poor reproducibility, and poor stability

Method used

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  • Ordered extralarge-hole-pitch alumina film and preparation method thereof
  • Ordered extralarge-hole-pitch alumina film and preparation method thereof
  • Ordered extralarge-hole-pitch alumina film and preparation method thereof

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Embodiment 1

[0027] A method for preparing an aluminum oxide film with an ordered ultra-large pore spacing, comprising the following steps:

[0028] Step 1: Prepare polished aluminum sheet: use high-purity aluminum sheet (≥99.999%) as the anode, perform electrochemical polishing in a mixture of perchloric acid and absolute ethanol with a volume ratio of 1:4, and the polishing voltage is 20 V , the polishing temperature is 0 ºC, and the polishing time is 10 minutes to obtain a polished aluminum sheet;

[0029] Step 2: Preparation of aluminum oxide film: use a polished aluminum sheet as the anode, and perform anodic oxidation in a citric acid electrolyte with an oxidation voltage of 560 V, an oxidation temperature of 10 ºC, and an oxidation time of 7 h to form an aluminum oxide film with an aluminum substrate. film, the optical image of the oxide film is shown in the attached figure 1 , the current density-time variation curve of the oxidation process is as follows figure 2 , it can be se...

Embodiment 2

[0035] A method for preparing an aluminum oxide film with an ordered ultra-large pore spacing, comprising the following steps:

[0036]Step 1: Prepare polished aluminum sheet: use high-purity aluminum sheet (≥99.999%) as the anode, perform electrochemical polishing in a mixture of perchloric acid and absolute ethanol with a volume ratio of 1:3, and the polishing voltage is 18 V , the temperature was -5°C, and the polishing time was 11 minutes to obtain a polished aluminum sheet;

[0037] Step 2: Preparation of aluminum oxide film: use the polished aluminum sheet as the anode, perform anodic oxidation in the electrolyte of malic acid and methanol, the oxidation voltage is 800 V, the oxidation temperature is -10 ºC, and the oxidation time is 8 h to form a band Aluminum oxide film with aluminum substrate;

[0038] Step 3: Prepare an aluminum sheet with ordered pits: immerse in a mixture of 6 wt% chromic acid and 7 wt% phosphoric acid to remove the aluminum oxide film. The immers...

Embodiment 3

[0042] A method for preparing an aluminum oxide film with an ordered ultra-large pore spacing, comprising the following steps:

[0043] Step 1: Prepare polished aluminum sheet: use high-purity aluminum sheet (≥99.999%) as the anode, perform electrochemical polishing in a mixture of perchloric acid and absolute ethanol with a volume ratio of 1:3.5, and the polishing voltage is 20 V , the polishing temperature is 20°C, and the polishing time is 9 minutes to obtain a polished aluminum sheet;

[0044] Step 2: Preparation of aluminum oxide film: use the polished aluminum sheet as the anode, and the graphite electrode as the cathode, perform anodic oxidation in the electrolyte of citric acid and methanol, the oxidation voltage is 580 V, the oxidation temperature is 5 ºC, and the oxidation time is 6 h, forming an aluminum oxide film with an aluminum substrate;

[0045] Step 3: Form the aluminum sheet with ordered pits: immerse in a mixture of 4 wt% chromic acid and 8 wt% phosphoric ...

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Abstract

The invention discloses an ordered extralarge-hole-pitch alumina film and a preparation method thereof. The alumina film has high hardness and elastic modulus, low reflectivity and obvious photoluminescence performance. The surface of the film is composed of innumerable holes. The bottoms of the holes are distributed in ordered hexagons. According to the ordered extralarge-hole-pitch alumina film and the preparation method thereof, macromolecular organic acid serves as an electrolyte, the electrolyte and an aluminum base are effectively cooled simultaneously, and the aluminum base is stably oxidized under extra-high voltage. The alumina film can serve as an ideal template for preparing various ordered major-cycle nano array structures of metal, polymer and the like, and can also be used for developing three-dimensional channel alumina films of micro and nano composite structures. The major-cycle alumina film is an excellent bioactivator carrier and has wide application prospects in the aspects of biosensors, medicine transport platforms, solar cells and the like.

Description

technical field [0001] The invention relates to an aluminum oxide film and a preparation method thereof, in particular to an aluminum oxide film with ordered ultra-large pore spacing and a preparation method thereof. Background technique [0002] At present, the aluminum oxide film formed by electrochemical oxidation has attracted great attention in the fields of industrial application and scientific research. The aluminum oxide film formed by electrochemical oxidation has the advantages of low cost, convenient operation, stable production, and technology integration. It is widely used in industry to improve the surface properties of aluminum, such as color, corrosion resistance, and friction resistance. The self-organized alumina film formed through a mild oxidation process is not only an ideal template for the synthesis of various ordered functional nanomaterials with unique optical and electromagnetic properties, but also can be used as a diverse platform to develop chemi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/10C25D11/12C25D11/08
CPCC25D11/045C25D11/08C25D11/10C25D11/12
Inventor 李娟马英俊文一豪孙润广
Owner SHAANXI NORMAL UNIV
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