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Method for obtaining large-hole-diameter double-through-hole AAO membrane

A large-pore, single-pass technology, used in electrolytic coatings, surface reaction electrolytic coatings, anodizing and other directions, can solve problems such as easy to cause harm, fast reaction rate, AAO membrane corrosion, etc. order, the effect of ensuring order

Active Publication Date: 2017-12-22
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When copper chloride or copper sulfate is used to remove the aluminum matrix, the reaction rate is slow, and solid substances are precipitated on the surface of the aluminum sheet. These solid products are dense and adhere to the aluminum matrix, which is not easy to remove. It will not only pollute the AAO film, but also prevent the further progress of the stripping reaction. , will also destroy the integrity of the AAO film; when the aluminum matrix is ​​removed with hydrochloric acid, the reaction rate is too fast, and the stripping process is difficult to control, which is easy to corrode the AAO film and destroy the integrity of the AAO film; use tin chloride or mercuric chloride When removing the aluminum matrix, both tin chloride and mercury chloride solutions are toxic and easy to cause harm, so they are rarely used, and the results are rarely reported

Method used

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  • Method for obtaining large-hole-diameter double-through-hole AAO membrane
  • Method for obtaining large-hole-diameter double-through-hole AAO membrane
  • Method for obtaining large-hole-diameter double-through-hole AAO membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Step 1. Pretreatment of aluminum foil

[0047] The preprocessing process is as follows:

[0048] Step1.1: Anneal the aluminum foil with a purity of 99.999% at 500°C for more than 2 hours to eliminate the internal stress generated during the processing of the aluminum foil, reduce microscopic defects such as grain boundaries, and increase the grain size.

[0049] Step1.2: Place the annealed aluminum foil in acetone, absolute ethanol, and distilled water in sequence for ultrasonic cleaning to remove surface contamination.

[0050] Step1.3: Use the cleaned aluminum foil as the anode, and the platinum mesh as the cathode, in a mixed solution of perchloric acid and ethanol (the content of perchloric acid is 3.5M, and the content of absolute ethanol is 14M), the aluminum foil is Electrochemical polishing eliminates mechanical damage on the surface of the aluminum foil and obtains a mirror-smooth and flat aluminum foil.

[0051] Step 2. Prepare a large-aperture single-throug...

Embodiment 2

[0070] Step 1. Pretreatment of aluminum foil

[0071] The pretreatment process is the same as that in Example 1.

[0072] Step 2. Prepare a large-aperture single-through-hole AAO membrane with an aluminum substrate and a barrier layer by secondary anodic oxidation

[0073] The process of preparation is as follows:

[0074] Step2.1: Prepare an anodic oxidation electrolyte, which is a mixed solution of phosphoric acid and sodium oxalate, wherein the content of phosphoric acid is 0.2M, and the content of sodium oxalate is 0.03M.

[0075] Step2.2: Use the pretreated aluminum foil as the anode, immerse in the anodic oxidation electrolyte prepared in Step2.1, use the platinum mesh as the cathode, and perform the first anodic oxidation, the oxidation voltage is 150V, and the oxidation temperature is -1 ℃, the oxidation time is 3h.

[0076] Step2.3: Remove the aluminum oxide layer obtained by the first oxidation in a mixed solution of chromium trioxide and phosphoric acid (the cont...

Embodiment 3

[0087] Step 1. Pretreatment of aluminum foil

[0088] The pretreatment process is the same as that in Example 1.

[0089] Step 2. Prepare a large-aperture single-through-hole AAO membrane with an aluminum substrate and a barrier layer by secondary anodic oxidation

[0090] The process of preparation is as follows:

[0091] Step2.1: Prepare an anodic oxidation electrolyte, which is a mixed solution of phosphoric acid and sodium oxalate, wherein the content of phosphoric acid is 0.05M, and the content of sodium oxalate is 0.02M.

[0092] Step2.2: Use the pretreated aluminum foil as the anode, immerse in the anodic oxidation electrolyte prepared in Step2.1, use the platinum mesh as the cathode, and perform the first anodic oxidation, the oxidation voltage is 200V, and the oxidation temperature is -3 ℃, the oxidation time is 2h.

[0093] Step2.3: Remove the aluminum oxide layer obtained by the first oxidation in a mixed solution of chromium trioxide and phosphoric acid (the con...

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Abstract

The invention discloses a method for obtaining a large-hole-diameter double-through-hole AAO membrane. The method comprises the following steps that 1, aluminum foil is pretreated, and thus aluminum foil with the surface being as smooth and flat as a mirror is obtained; 2, a large-hole-diameter single-through-hole AAO membrane with an aluminum base and a blocking layer is prepared through a secondary anodic oxidation method, wherein an anodic oxidation electrolyte is a mixed solution of phosphoric acid (with the content being 0.05 M-0.2 M) and sodium oxalate (with the content being 0.01 M-0.03 M); and 3, the aluminum base and the blocking layer of the large-hole-diameter single-through-hole AAO membrane are removed through a corrosion stripping method, wherein aluminum base corrosive liquid is a mixed solution of copper chloride (with the content being 0.1 M-0.15 M) and ferric chloride (with the content being 0.15 M-0.18 M). The method has the advantage that the double-through-hole AAO membrane which is large in hole diameter, orderly in hole arrangement, large in area and good in integrality is obtained.

Description

technical field [0001] The invention relates to a method for obtaining an AAO membrane, in particular to a method for obtaining a large-aperture and double-through-hole AAO membrane, and belongs to the technical field of AAO membranes. Background technique [0002] Porous Anodic Aluminum Oxide Membrane, also known as AAO membrane, is a highly ordered nanopore array structure formed by self-assembly on the surface of aluminum foil or aluminum sheet by electrochemical anodic oxidation in a certain electrolyte. , the holes are parallel to each other and perpendicular to the aluminum substrate, and the array structure "cells" are arranged in a hexagonal close-packed arrangement. Due to the unique structure, good thermal stability and chemical stability of the AAO membrane, its pore size, pore spacing and pore wall thickness are controllable, and the preparation process is mature and the production cost is low, making it a good choice for preparing nanomaterials and constructing ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/12C25D11/10C25D11/08
CPCC25D11/045C25D11/08C25D11/10C25D11/12
Inventor 李阳平李莉刘鹏马智达陈一丹韦秋霞
Owner NORTHWESTERN POLYTECHNICAL UNIV
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