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A controllable cu ion in situ doping tio 2 Preparation method of nanotube array

A nanotube array and in-situ doping technology, applied in nanotechnology, electrolytic coatings, surface reaction electrolytic coatings, etc., can solve the problems of excessive Cu ion doping, small gaps, and difficulty in effectively attaching Cu oxides, etc., to achieve The effect of uniform dispersion of doping ions and simplified preparation process

Active Publication Date: 2017-12-12
CHANGJIANG RIVER SCI RES INST CHANGJIANG WATER RESOURCES COMMISSION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 2. TiO 2 The structure of the nanotube array is dense, the gap between the tubes is very small, and it is difficult to effectively attach Cu oxide to the outer wall of the tube.
The content of Cu in the TA13 alloy is relatively high, and the nanotube arrays prepared from it may also have the problem of excessive Cu ion doping

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Cut TA13 alloy sheet with a thickness of 2mm into 2×8cm 2 A long strip, polished with sandpaper and ultrasonically cleaned as a standby anode, a Pt sheet of the same size is used as a cathode, and an ethylene glycol solution containing 2 wt% water and 0.3 wt% ammonium fluoride is prepared as an electrolyte. The electrolysis process adopts a two-electrode DC electrolysis system with a voltage of 50V, a temperature of 20°C, and a time of 30min. After the electrolysis is completed, rinse the residual liquid on the anode surface with deionized water, and then immerse it in a 0.1M HCl solution at a constant temperature of 20°C. After ultrasonic 4h at 30KHz, take it out and rinse with deionized water to obtain a Cu ion doping amount of 0 TiO 2 Nanotube array. Combine the nanotube array with conventional TiO 2 The initial solubility of the nanotube array used in ultraviolet light degradation is 10mg / L methyl blue solution. Due to the complete leaching of Cu ions, it is found th...

Embodiment 2

[0027] The TA13 alloy rod with a diameter of 2cm is cut into a short rod shape with a length of 8cm, sanded with sandpaper and ultrasonically cleaned as a standby anode. The size is 2×8cm 2 The Pt sheet is the cathode, and a glycerol solution containing 2wt% water and 0.3wt% ammonium fluoride is prepared as an electrolyte. The electrolysis process adopts a two-electrode DC electrolysis system with a voltage of 40V, a temperature of 30°C, and a time of 1h. After the electrolysis is completed, rinse the residual liquid on the anode surface with deionized water, and then immerse it in 0.01M H at a constant temperature of 30℃ 3 PO 4 In the solution, ultrasonic for 3h at 30KHz frequency, take it out and rinse with deionized water to obtain TiO doped with Cu ions of 0.2wt% 2 Nanotube array. Combine the nanotube array with conventional TiO 2 The nanotube array is used to degrade 10mg / L methyl blue solution by ultraviolet light. Due to the 0.2wt% Cu ion doping, it is found that the phot...

Embodiment 3

[0029] Cut TA13 alloy sheet with a thickness of 2mm into 2×8cm 2 A long strip, polished with sandpaper and ultrasonically cleaned as a standby anode, a Pt sheet of the same size is used as a cathode, and an ethylene glycol solution containing 2 wt% water and 0.3 wt% ammonium fluoride is prepared as an electrolyte. The electrolysis process adopts a two-electrode DC electrolysis system, the voltage is 30V, the temperature is 40℃, and the time is 2h. After the electrolysis is completed, rinse the residual liquid on the anode surface with deionized water, and then immerse it in 0.001M H at a constant temperature of 40℃ 2 SO 4 In the solution, ultrasonic for 2h at 40KHz frequency, take it out and rinse with deionized water to obtain TiO doped with Cu ions of 0.5wt% 2 Nanotube array. Combine the nanotube array with conventional TiO 2 The nanotube array is used to degrade 10mg / L methyl blue solution under ultraviolet light. Due to the 0.5wt% Cu ion doping, it is found that the photocat...

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PUM

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Abstract

The invention relates to a preparation method for a control type Cu ion in-situ doped TiO2 nanotube array. The preparation method comprises the following steps that 1) a TA13 alloy plate or a TA13 alloy bar is taken as an anode, a Pt plate or a Pt bar is taken as a cathode, the Cu ion in-situ doped TiO2 nanotube array is prepared through anodic oxidation in a fluoride solution, and a sample, that is, the Cu ion in-situ doped TiO2 nanotube array is cleaned; 2) a part of Cu ions are leached by adopting an ultrasonic assisted selective acid dissolution method, and quantitative regulation of the content of the Cu ions in the nanotube array is realized; and 3) cleaning and drying are conducted after controlling to obtain the control type Cu ion in-situ doped TiO2 nanotube array. The preparation method has the advantages and beneficial effects that 1, TA13 alloy is taken as a base material, so that the preparation technology for the Cu ion doped TiO2 nanotube array is simplified, and the doped ions are dispersed more uniformly; 2, the Cu ion doping amount can be conveniently and controllably adjusted by adopting the ultrasonic assisted selective acid dissolution method, so that a reliable method is provided for preparing a catalyst with high performance.

Description

Technical field [0001] The invention belongs to the field of nano material preparation, and relates to a regulated Cu ion in-situ doped TiO 2 Preparation method of nanotube array. Background technique [0002] TiO 2 Nanotube arrays have excellent light (electric) catalytic activity and chemical stability, and are widely used in light (electric) catalytic hydrogen production, light (electric) catalytic treatment of environmental pollutants and solar cells. After Cu ion doping, a lower energy doping energy level is formed to absorb visible light and broaden the spectral response range. At the same time, it can be used in TiO 2 Oxygen vacancies are formed on the surface to promote Ti 3+ The formation of the oxidation center is conducive to charge trapping and inhibits electron-hole recombination, and improves the light quantum efficiency. Currently, Cu ion doped TiO 2 Nanotube arrays mainly adopt the conventional late introduction method, that is, prepare TiO first 2 Nanotube array,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25D11/26B82Y40/00
CPCB82Y40/00C25D11/26
Inventor 汤丁丁史德亮李亚龙刘凤丽
Owner CHANGJIANG RIVER SCI RES INST CHANGJIANG WATER RESOURCES COMMISSION