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Method for preparing aluminum oxide template by step decompression reaming

A technology of alumina template and stepped step-down, which is applied in the direction of electrolytic coating, surface reaction electrolytic coating, coating, etc., and can solve the problems of unfavorable one-dimensional nanomaterial deposition, low density of nanomaterials, and easily damaged template structure, etc. , to achieve the effect of smooth diffusion process, easy structure completion, and uniform distribution of pores

Inactive Publication Date: 2012-08-29
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the currently prepared alumina templates do not undergo subsequent treatment to reduce the barrier layer after the second oxidation is completed, so that although the prepared alumina templates are neatly arranged in appearance, they are not conducive to the deposition of one-dimensional nanomaterials. Moreover, a thicker barrier layer will lead to a higher deposition voltage, which will easily damage the template structure.
In addition, due to the small diameter of the alumina oxalate template prepared by secondary anodization, it is not conducive to the diffusion of the solution during the deposition process, making the deposition process slow and the deposited nanomaterials are not dense, and the deposition efficiency is low.

Method used

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  • Method for preparing aluminum oxide template by step decompression reaming
  • Method for preparing aluminum oxide template by step decompression reaming
  • Method for preparing aluminum oxide template by step decompression reaming

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1 The comparative description of step-down and hole-enlarging treatment on the effect of the prepared template, specifically using the comparison of basic treatment, step-down pressure without hole expansion treatment, and step-down pressure with hole expansion treatment.

[0035] The basic processing described is:

[0036] Anneal high-purity aluminum foil with an area of ​​3×5cm (purity above 99.99%) in the air at 450°C for 2 hours, put the aluminum foil that has been annealed at high temperature into acetone (99.5%) and ultrasonically clean it for 15 minutes, and then soak it in 20% Sodium hydroxide aqueous solution for 10min, put the aluminum foil into the mixed solution of 60wt% phosphoric acid, 6wt% chromic acid, 15wt% sulfuric acid and 19wt% deionized water for electrochemical polishing. During the polishing process, the anode is aluminum foil, and the cathode is For ring electrodes, the polishing temperature is 70°C, the voltage is 14V, and the polishing ...

Embodiment 2

[0047] The method for preparing an alumina template by step-down depressurization and reaming comprises the following steps:

[0048] 1) Pretreatment of aluminum foil and first anodic oxidation

[0049] Anneal high-purity aluminum foil (purity above 99.99%) and anneal at 450°C in air for 2 hours to remove stress and grain defects in the aluminum foil and improve crystallization performance;

[0050] Ultrasonic cleaning of the annealed aluminum foil to remove surface oil: Put it in 99.5% acetone for ultrasonic cleaning for 15 minutes;

[0051] Then put the aluminum foil in 20% sodium hydroxide solution (mass fraction) for 10 minutes to remove surface alumina, and then electrochemically polish the aluminum foil:

[0052] Put the aluminum foil into a mixed solution with a concentration of 60wt% phosphoric acid, 6wt% chromic acid, 15wt% sulfuric acid and 19wt% deionized water for electrochemical polishing. During the polishing process, the anode is aluminum foil, the cathode is a...

Embodiment 3

[0063] The method for preparing an alumina template by step-down depressurization and reaming comprises the following steps:

[0064] 1) Pretreatment of aluminum foil and first anodic oxidation

[0065] Anneal high-purity aluminum foil (purity above 99.99%) and anneal for 3 hours at 480°C in air to remove stress and grain defects in the aluminum foil and improve crystallization performance;

[0066] The annealed aluminum foil is ultrasonically cleaned to remove surface oil stains: put in 99.5% medium and ultrasonically clean for 10 minutes;

[0067] Then put the aluminum foil into 20% sodium hydroxide solution (mass fraction) for 20min to remove surface alumina, and then electrochemically polish the aluminum foil:

[0068] Put the aluminum foil into a mixed solution of 50wt% phosphoric acid, 10wt% chromic acid, 15wt% sulfuric acid and 25wt% deionized water for electrochemical polishing. During the polishing process, the anode is aluminum foil, the cathode is a ring electrode,...

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Abstract

The invention discloses a method for preparing an aluminum oxide template by step decompression reaming. The method comprises the steps as follows: 1) taking a polished aluminum foil as an anode and a platinum electrode as a cathode, placing the anode and the cathode into an acidic electrolytic solution, connecting a power supply, and carrying out anodic oxidation for 1-5 h for the first time; 2) after the anodic oxidation for the first time, removing an aluminum oxide film on the surface of the anode, and carrying out anodic oxidation for 1-5 h for the second time; 3) after the anodic oxidation for the second time, carrying out step decompression treatment by reducing the voltage between the anode and the cathode at a speed of 0.5-3 V / min and disconnecting the power supply until the voltage is reduced to be less than 16 V; and 4) after the step decompression treatment, cleaning the aluminum foil, placing into a reaming solution, and reaming for 10-60 min. According to the method, the baffle layer thickness of the aluminum oxide template and the length and diameter of template holes can be accurately controlled; and the needed equipment is simple, the operation process is convenient, and the parameters are easy to control.

Description

technical field [0001] The invention belongs to the technical field of preparing nanometer mesoporous materials, and relates to a method for preparing an alumina template by step-down pressure expansion and hole expansion. Background technique [0002] The template method is an important method for preparing one-dimensional nanomaterials. In the process of preparing secondary anodized aluminum templates, different geometric parameters and shapes can be obtained by controlling different experimental conditions (such as deposition time, temperature, pH value, etc.). alumina template. The characteristics of the prepared alumina template directly affect the preparation of subsequent one-dimensional nanomaterials (nanowires, nanotubes, etc.), therefore, the preparation of templates is particularly important in the process of synthesizing one-dimensional nanomaterials. [0003] At present, the most commonly used templates are oxalic acid template, sulfuric acid template and phosp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/12C25D11/18C25D11/24C25D11/16
Inventor 杨森高禄梅龚俊峰王洁琼宋晓平
Owner XI AN JIAOTONG UNIV
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