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Preparation method of crystallized TiO2 nanotube array

A nanotube array, crystallization technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., to achieve the effect of short time, low energy consumption and high crystallization success rate

Inactive Publication Date: 2010-09-29
SOUTHWEST JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

TiO obtained in this way 2 Usually contains two crystal forms of anatase and rutile, with many defects

Method used

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  • Preparation method of crystallized TiO2 nanotube array
  • Preparation method of crystallized TiO2 nanotube array
  • Preparation method of crystallized TiO2 nanotube array

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A specific embodiment of the present invention is a low temperature crystallized TiO 2 The method for the nanotube array, its specific practice is:

[0020] a. TiO 2 Fabrication of nanotube arrays

[0021] Put the titanium sheet in acetone for 30 minutes of ultrasonic cleaning. After air drying, put the titanium sheet into an aqueous solution containing 25ml / L of concentrated sulfuric acid, 15ml / L of hydrofluoric acid, and 60ml / L of glacial acetic acid; Electrochemical polishing was carried out by direct current at room temperature for 8 minutes; then the polished titanium sheet was put into an ethylene glycol solution of ammonium fluoride with a weight volume concentration of 0.05% for anodic oxidation, and the cathode used for anodic oxidation was platinum Chip, voltage 60v, reaction time 12 hours;

[0022] b. TiO 2 Crystallization of nanotube arrays

[0023] The resulting TiO 2 The nanotube array is placed in water, and kept in a hydrothermal reaction kettle at...

Embodiment 2

[0028] This example is basically the same as Example 1, the difference is:

[0029] a. TiO 2 Fabrication of nanotube arrays

[0030] Put the titanium sheet in acetone for 35 minutes of ultrasonic cleaning. After air drying, put the titanium sheet into an aqueous solution containing 26ml / L of concentrated sulfuric acid, 14ml / L of hydrofluoric acid, and 50ml / L of glacial acetic acid; Electrochemical polishing was carried out by direct current at room temperature for 15 minutes; then the polished titanium sheet was put into an ethylene glycol solution of ammonium fluoride with a weight volume concentration of 0.07% for anodic oxidation, and the cathode used for anodic oxidation was platinum Chip, voltage 60v, reaction time 10 hours;

[0031] b. TiO 2 Crystallization of nanotube arrays

[0032] The resulting TiO 2 The nanotube array is placed in water, and kept in a hydrothermal reaction kettle at 50° C. for 12 hours to obtain it.

Embodiment 3

[0034] This example is basically the same as Example 1, the difference is:

[0035] a. TiO 2 Fabrication of nanotube arrays

[0036] Put the titanium sheet in acetone for 40 minutes of ultrasonic cleaning. After air drying, put the titanium sheet into an aqueous solution containing 28ml / L of concentrated sulfuric acid, 12ml / L of hydrofluoric acid, and 65ml / L of glacial acetic acid; Direct current electrochemical polishing at room temperature, polishing for 20 minutes; then put the polished titanium sheet into an ethylene glycol solution of ammonium fluoride with a weight volume concentration of 1% for anodic oxidation, and the cathode used for anodic oxidation is platinum Chip, voltage 60v, reaction time 8 hours;

[0037] b. TiO 2 Crystallization of nanotube arrays

[0038] The resulting TiO 2 The nanotube array is placed in water, and kept in a hydrothermal reaction kettle at 50° C. for 14 hours to obtain it.

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Abstract

The invention discloses a preparation method of a crystallized TiO2 nanotube array. The specific steps are as follows: titanium pieces are placed into acetone to conduct ultrasonic cleaning for 30-40 minutes, after air-drying, the titanium pieces are placed into aqueous solution containing 25-28ml / L of concentrated sulfuric acid, 12-15ml / L of hydrofluoric acid and 50-65ml / L glacial acetic acid, conducting electrochemical polishing at 10-15v constant-current direct current under the room temperature for 8-20 minutes, then the polished titanium pieces are placed into ethylene glycol solution of ammonium fluoride with 0.05-1% of the bulking value concentration to conduct anodic oxidation, when conducting the anodic oxidation, the used negative pole is a platinum piece, the voltage is 60v and the reaction time is 8-12 hours, the obtained TiO2 nanotube array is placed into the water and insulation is conducted for 12-16 hours in a hydro-thermal reaction kettle with the temperature of 50 DEG C, and the crystallized TiO2 nanotube array is obtained. The preparation method has simple devices and low energy consumption, and is applicable to large-scale production; and simultaneously, the TiO2 nanotube array prepared by the method has a pure anatase phase.

Description

technical field [0001] The invention relates to a crystallized TiO 2 Preparation method of nanotube arrays. Background technique [0002] TiO 2 It is an important inorganic functional material. It has broad application prospects in solar cells, photoelectric conversion, photochromism, and photocatalytic degradation of pollutants in the atmosphere and water, and has become one of the key research objects. In 2001, American scientist Grimes prepared TiO by electrochemical anodic oxidation. 2 Nano-array materials have attracted great attention. TiO 2 Due to their excellent photoelectric, catalytic, and sensing properties, nanotube arrays have been widely used in many fields such as gas sensors, photocatalysis, and dye-sensitized solar cells. [0003] TiO 2 The characteristic of nanotube array as an ordered structure is that it not only reflects the collective effect of nanostructure units, but also reflects the synergistic effect and coupling effect that a single nanostru...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/053
Inventor 杨峰柯川蔡芳共赵勇
Owner SOUTHWEST JIAOTONG UNIV
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