Method for preparing gradient TiO2 nano-tube arrry thin film by using multistep anodic oxidation process

A nanotube array and anodic oxidation technology is applied in the field of preparing nanotube array thin films, which can solve the problems that nanotube array thin films have not been reported in literature, that it is difficult to synthesize gradient nanotube array thin films, and the electrochemical conditions are fixed. The effect of mass production, simple process and simple operation

Inactive Publication Date: 2008-07-30
TSINGHUA UNIV
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Problems solved by technology

[0004] However, the traditional single-step anodic oxidation method also has the following shortcomings: (1) The morphology of the nanotube array film synthesized in a single electrolyte is affected by the properties of the electrolyte itself, and it is difficult to synthesize a gradient without changing the electrolyte. Nanotube array films; (2) When single-step anodization is used, the applied electrochemical conditions are fixed, and it is difficult to synthesize gradient nanotube array films under fixed electrochemical conditions
So far, there have been no reports in the literature on the preparation of nanotube array films with gradient characteristics on "valve metal" single substrates

Method used

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  • Method for preparing gradient TiO2 nano-tube arrry thin film by using multistep anodic oxidation process

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Embodiment 1

[0023] 1. Polish the titanium foil with 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1200 mesh SiC sandpaper respectively, and then use 0.05μm Al 2 o 3 Polish to mirror brightness, put the polished titanium foil into acetone and deionized water for 10 minutes and ultrasonically clean it, and dry it for later use;

[0024] 2. Add 12 milliliters of phosphoric acid to 136 milliliters of deionized water, and mix evenly under magnetic stirring to prepare a 1 mol / liter phosphoric acid solution, then add 10 milliliters of hydrofluoric acid to the above phosphoric acid solution, and continue stirring under magnetic force and mix evenly, and be prepared into a water-based electrolyte containing 2% hydrofluoric acid by mass percent;

[0025] 3. Add 3.015 grams of ammonium fluoride to 60 grams of glycerin, mix under magnetic stirring until the ammonium fluoride is completely dissolved, and prepare an organic electrolyte solution containing 5% ammonium fluoride by mass;

[0026] 4. At ro...

Embodiment 2

[0030] 1. Polish the titanium foil with 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1200 mesh SiC sandpaper respectively, and then use 0.05μm Al 2 o 3 Polish to mirror brightness, put the polished titanium foil into acetone and deionized water for 10 minutes and ultrasonically clean it, and dry it for later use;

[0031] 2. Add 12 milliliters of phosphoric acid to 136 milliliters of deionized water and mix evenly under magnetic stirring to prepare a 1 mol / liter phosphoric acid solution, then add 25 milliliters of hydrofluoric acid to the above phosphoric acid solution, and continue stirring under magnetic force Mix evenly, and prepare a water-based electrolyte containing 5% hydrofluoric acid by mass;

[0032] 3. Add 0.63 grams of ammonium fluoride to 60 grams of glycerin, mix under magnetic stirring until the ammonium fluoride is completely dissolved, and prepare an organic electrolyte solution containing 1% ammonium fluoride by mass;

[0033] 4. At room temperature, put the...

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Abstract

The invention relates to a method of preparing a gradient TiO2 nanotube array film by utilizing the method of multi-step anodic oxidation. Firstly, phosphoric acid, hydrofluoric acid, ammonium fluoride, glycerin and deionized water are adopted as raw materials and prepared into a water-base electrolyte and an organic electrolyte respectively; secondly, the two electrode systems composed of a titanium foil sheet and a platinum sheet are placed into the water-base electrolyte and the organic electrolyte for a repeated anodic oxidation; and finally, the TiO2 nanotube array film material with a gradient structure is generated on the titanium foil sheet. The method is fit for manufacturing photoelectrochemical apparatuses of various types and has a far-ranging application prospect in the industrial fields of light energy utilization, green energy development, sewage disposal and so on.

Description

technical field [0001] The invention relates to a method for preparing a nanotube array thin film, in particular to a method for preparing gradient TiO by using a multi-step anodic oxidation method 2 A method for nanotube array thin films. Background technique [0002] and other forms of nano-TiO 2 material compared to TiO 2 The nanotube array film has the characteristics of regular shape, large specific surface area, easy recycling and good regeneration, so TiO 2 Nanotube array films are significantly better than their corresponding materials in terms of photocatalysis, photoelectrochemistry and superhydrophilicity, especially in the fields of dye-sensitized solar cells, photocatalysts and self-cleaning materials, which have broad market application prospects. On the other hand, TiO 2 The preparation technology of nanotubes has been developed for a period of time, and various preparation methods have been formed, including hydrothermal synthesis, template synthesis, ele...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/26C30B29/16C30B29/62C30B30/02
Inventor 王晓慧杨阳李龙土
Owner TSINGHUA UNIV
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