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Method for producing titanium dioxide nano tube array with molybdenum tungsten doped anodizing method

An anodic oxidation method, nanotube array technology, applied in the direction of final product manufacturing, sustainable manufacturing/processing, electrolytic coating, etc., can solve the problems of only absorption, insufficient specific surface area, easy damage, etc.

Inactive Publication Date: 2008-01-23
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the applied anodic oxidation voltage is generally only in the range of 10-25V, beyond this voltage range, the nanotube-like structure cannot be formed, which limits the diameter of the nanotube to a certain extent, and the nanotubes prepared in the aqueous solution system The tube wall is thin and easy to break
200410021589.X discloses a preparation method of titanium dioxide nanotube arrays with a high aspect ratio. The solute of the electrolyte is fluoride and supporting electrolyte, the solvent is water, and alcohol additives are added. This kind of nanotube is still relatively short, only 250 nanometers long, the specific surface area is not large enough, and it can only absorb light in the ultraviolet region, so it cannot make full use of natural sunlight.
At present, there is no report on the preparation of titanium dioxide nanotube arrays by anodic oxidation method doped with metal elements at home and abroad.

Method used

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  • Method for producing titanium dioxide nano tube array with molybdenum tungsten doped anodizing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Grinding the surface of the base material, cleaning it for later use;

[0020] (2) Preparation of organic electrolyte:

[0021] Measure 1.47mL of 40% hydrofluoric acid (HF) solution by mass, mix it evenly with 28.53mL of anhydrous dimethyl sulfoxide (DMSO), and prepare a DMSO solution with 2% by mass of HF ;

[0022] (3) Preparation of titanium oxide nanotube arrays: use a titanium sheet (0.3*1.8cm) with a purity of more than 99.9% as an anode, and a platinum sheet (0.5*1cm) as a cathode, and electrolyze it for 24 hours under a DC voltage of 60V to produce Nanotubes with a length of 35 microns were obtained;

[0023] (4) Preparation of titanium dioxide nanotube arrays doped with tungsten and molybdenum:

[0024] (a). Dissolve 1g of tungsten powder or molybdenum powder in 15mL of 30% H 2 o 2 , stirred in ice bath for 10h, to obtain WO 3 or MoO 3 with O 2 2- It is the clear solution of chelating agent, then add 15mL absolute ethanol solution to the above clea...

Embodiment 2

[0028] (1) Grinding the surface of the base material, cleaning it for later use;

[0029] (2) Preparation of organic electrolyte:

[0030] (a). Measure 2.21mL of 40% hydrofluoric acid (HF) solution by mass, mix it with 27.79mL of anhydrous dimethyl sulfoxide (DMSO), and prepare 3% by mass of HF % DMSO solution;

[0031] (3) Preparation of titanium oxide nanotube arrays: use a titanium sheet (0.3*1.8cm) with a purity of more than 99.9% as an anode, and a platinum sheet (0.5*1cm) as a cathode, and electrolyze it for 24 hours under a DC voltage of 40V to produce Nanotubes with a length of 8 microns were obtained.

[0032] (4) Preparation of titanium dioxide nanotube arrays doped with tungsten and molybdenum:

[0033] (a). Dissolve 1g of tungsten powder or molybdenum powder in 15mL of 30% H 2 o 2 , stirred in ice bath for 10h, to obtain WO 3 or MoO 3 with O 2 2- It is the clear solution of chelating agent, then add 15mL absolute ethanol solution to the above clear solutio...

Embodiment 3

[0037] (1) Grinding the surface of the base material, cleaning it for later use;

[0038] (2) Preparation of organic electrolyte:

[0039] (a). Measure 0.375mL of 40% hydrofluoric acid (HF) solution by mass, mix it with 29.625mL of anhydrous dimethyl sulfoxide (DMSO), and prepare 0.5% by mass of HF % DMSO solution;

[0040] (3) Preparation of titanium oxide nanotube arrays: use a titanium sheet (0.3*1.8cm) with a purity of more than 99.9% as an anode, and a platinum sheet (0.5*1cm) as a cathode, and electrolyze it for 12 hours under a DC voltage of 30V to produce nanotubes with a length of 2 microns.

[0041] (4) Preparation of titanium dioxide nanotube arrays doped with tungsten and molybdenum:

[0042] (a). Dissolve 1g of tungsten powder or molybdenum powder in 15mL of 30% H 2 o 2 , stirred in ice bath for 10h, to obtain WO 3 or MoO 3 with O 2 2- It is the clear solution of chelating agent, then add 15mL absolute ethanol solution to the above clear solution;

[004...

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Abstract

The invention discloses a method for preparing titanium dioxide nanometer tube array by molybdenum-tungsten mixture anode oxidation. Wherein, an electrolyte is an organic electrolyte system of hydrofluoric acid with HF content by mass of 0.5 swung dash 3% and dimethyl sulfoxide; under a DC voltage of 25 swung dash 100 V, some pure titanium or titanium alloy is taken as an anode, a platinum sheet as a cathode, and the nanometer tube is prepared by electrolyzing in the electrolyte; then the prepared TiO2 nanometer tube array is immersed in clearing solution of WO3 or MoO3 taking O22- as chelant for 10 swung dash 90 min., then TiO2 nanometer tube array mixed with tungsten and molybdenum is prepared. The invention increases the length of TiO2 nanometer tube, enlarges the specific surface area of the light-pole material, and widens the absorption spectrum of the TiO2 nanometer tube array in visible light area.

Description

technical field [0001] The invention relates to a method for preparing a titanium dioxide nanotube array by a molybdenum-tungsten doped anodic oxidation method. Background technique [0002] The preparation of titanium dioxide nanotube arrays by anodic oxidation has the advantages of large specific surface area and adjustable pore size. Its special nanotube structure is conducive to the separation of photogenerated electrons and photogenerated holes, which can effectively improve the photoelectric conversion efficiency of solar cells. Research hotspots in the field of science in various countries. The electrolyte solution for the preparation of titanium dioxide nanotube arrays by the current anodic oxidation method is usually an inorganic aqueous solution system. Since the migration speed of various ions in the aqueous solution is relatively fast, the speed of electrochemical anodic oxidation is also fast, and it can be formed in a relatively short time. array of nanotubes....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/26H01L31/18
CPCY02P70/50
Inventor 蔡青云杨丽霞邝淑云
Owner HUNAN UNIV
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