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Bipass large-area aluminum oxide, titanium dioxide or zirconium dioxide nanotube array film and preparation method thereof

A technology of aluminum oxide and nanotube arrays, applied in the direction of surface reaction electrolytic coatings, coatings, electrolytic coatings, etc., can solve problems such as unstable results, complicated processes, and unsafe operations, and achieve easy control of preparation parameters, The preparation process is simple and the effect is good

Pending Publication Date: 2022-04-26
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods have many problems, such as complicated process, unstable results, difficult to control bottom corrosion and unsafe operation, etc.

Method used

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  • Bipass large-area aluminum oxide, titanium dioxide or zirconium dioxide nanotube array film and preparation method thereof
  • Bipass large-area aluminum oxide, titanium dioxide or zirconium dioxide nanotube array film and preparation method thereof
  • Bipass large-area aluminum oxide, titanium dioxide or zirconium dioxide nanotube array film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Double-pass aluminum oxide nanotube array membrane based on oxalic acid small-aperture template

[0029] A square aluminum sheet with a length of 5 cm (purity greater than or equal to 99.9%, and a thickness of 0.2 mm) was removed by conventional mechanical processing to remove the oxide layer on the surface. The electrolyte is prepared from oxalic acid and water, and the content of oxalic acid is 0.3M. Put the processed aluminum sheet into the reaction device, and the diameter of the aluminum sheet exposed to the electrolyte is 4 cm. A refrigerator was used to fix the temperature of the electrolyte at 5° C., and a platinum foil was used as a cathode, and anodized at an anode voltage of 40 V for 2 hours to obtain a nanotube array film with an average pore diameter of 60 nm. Immediately after the reaction, the sample was taken out from the electrolyte and washed with deionized water, then put into a methanol solution of liquid bromine, the volume ratio of liquid bromine ...

Embodiment 2

[0031] Based on NH 4 F-Ethylene Glycol Small Pore Template Double Pass Titanium Dioxide Nanotube Array Membrane

[0032] A circular titanium sheet with a diameter of 2 cm (purity greater than or equal to 99.9%, and a thickness of 0.2 mm) was removed by conventional mechanical processing to remove the oxide layer on the surface. The electrolyte consists of NH 4 F, prepared from ethylene glycol, NH 4 The content of F is 0.5 wt.%. Put the processed titanium sheet into the reaction device, and the diameter of the titanium sheet exposed to the electrolyte is 1 cm. A refrigerator was used to fix the temperature of the electrolyte at 5° C., and a graphite electrode was used as a cathode for anodic oxidation at an anode voltage of 60 V for 12 hours to obtain a nanotube array film with an average pore diameter of 80 nm. Immediately after the reaction, the sample was taken out from the electrolyte and washed with deionized water, then put into a methanol solution of liquid bromine, ...

Embodiment 3

[0034] Based on NH 4 F-Glycerol-Glycerol Small Pore Template Double Pass Zirconia Nanotube Array Membrane

[0035] A square zirconium sheet with a length of 4 cm (purity greater than or equal to 99.9%, and a thickness of 0.3 mm) is removed by conventional mechanical processing to remove the oxide layer on the surface. The electrolyte consists of NH 4 F. Glycerin and glycerol are formulated, glycerin and glycerol are mixed at a ratio of 1:1, NH 4 The content of F is 1 wt.%. Put the processed zirconium sheet into the reaction device, and the diameter of the titanium sheet exposed to the electrolyte is 3 cm. At room temperature, using a graphite electrode as a cathode, anodized at an anode voltage of 50V for 3 hours to obtain a nanotube array film with an average pore size of 100 nm. Immediately after the reaction, the sample was taken out from the electrolyte and washed with deionized water, then put into a methanol solution of liquid bromine, the volume ratio of liquid brom...

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Abstract

The invention discloses a bi-pass large-area aluminum oxide, titanium dioxide or zirconium dioxide nanotube array film and a preparation method thereof. The method comprises the following steps: carrying out anodic oxidation on a pretreated pure aluminum sheet, a pretreated titanium sheet and a pretreated zirconium sheet to prepare a first-grade primary product; dissolving by using a mixed solution of liquid bromine and methanol to remove aluminum, titanium and zirconium metal matrixes, so as to obtain aluminum oxide, titanium dioxide and zirconium dioxide nanotube array films and obtain a secondary preliminary product; after cleaning with absolute ethyl alcohol, putting into a critical CO2 atmosphere drying box for drying, so as to obtain a third-stage preliminary product with a barrier layer at the bottom; and putting into a plasma cleaning instrument containing fluoride gas, and removing the barrier layer at the bottom to obtain the bi-pass nanotube array film. The preparation process is reasonable in design and simple and convenient to operate, and the prepared bi-pass nanotube array film has high regularity and flatness and can be effectively applied to the fields of gas separation, drug delivery, nano templates and the like.

Description

technical field [0001] The invention relates to the preparation of aluminum oxide, titanium dioxide and zirconium dioxide nanotube arrays, in particular to a preparation method for double-pass aluminum oxide, titanium dioxide and zirconium dioxide nanotube arrays. Background technique [0002] Porous nanotube array films are widely used in nanomaterial templates, catalytic synthesis, photovoltaic energy, biosensing and other fields. Electrochemical anodic oxidation is an important method for preparing aluminum oxide, titanium dioxide or zirconium dioxide nanotube array films. In this context, a lot of work has been done and important progress has been made in the preparation of Al2O3, TiO2 or ZrO2 nanotube arrays in recent years. For example, titanium dioxide nanotube arrays can be obtained by anodizing titanium metal sheets in an organic solvent containing fluoride ions. The length of the titanium dioxide nanotube array prepared by the method can reach hundreds of microns...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/10C25D11/16C25D11/26
CPCC25D11/10C25D11/16C25D11/26
Inventor 方东索军陈俊俊
Owner KUNMING UNIV OF SCI & TECH
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