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

A technology of nanotube arrays and metal ions, which is applied in nanotechnology, electrolytic coatings, surface reaction electrolytic coatings, etc., can solve the problems of excessive doping of metal ions in nanotube arrays, small gaps, and difficulty in effectively attaching metal oxides. To achieve the effect of simplifying the preparation process and uniform dispersion

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 metal oxides to the outer wall of the tube
The content of alloy components in titanium alloy is generally high, and the nanotube arrays prepared from it may also have the problem of excessive metal ion doping

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Cut the TA5 alloy sheet with a thickness of 2mm into 2×8cm 2 Long strips, polished by sandpaper and ultrasonically cleaned, used as standby anodes, and Pt sheets of the same size as cathodes and prepared ethylene glycol solution containing 2wt% water and 0.3wt% ammonium fluoride as electrolytes. The electrolysis process adopts a two-electrode DC electrolysis system with a voltage of 50V, a temperature of 20°C, and a time of 30 minutes. After the electrolysis is completed, rinse the residual liquid on the surface of the anode with deionized water, then immerse it in the HCl solution with a pH of 1 at a constant temperature of 20°C, and take it out after ultrasonication at a frequency of 30KHz for 2 hours and rinse it with deionized water to obtain a 1.5wt% Al ion-doped solution. Miscellaneous TiO 2 array of nanotubes. Comparing the nanotube array with conventional TiO 2 Nanotube arrays are applied to ultraviolet light to degrade methylene blue solutions with an initia...

Embodiment 2

[0028] Cut the TA6 alloy rod with a diameter of 2 cm into a short rod with a length of 8 cm, grind it with sandpaper and clean it ultrasonically, and use it as a standby anode, with a size of 2×8 cm 2 The Pt sheet is used as the cathode and a glycerin solution containing 2wt% water and 0.3wt% ammonium fluoride is prepared as the 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 surface of the anode with deionized water, and then soak it in H2O with a pH of 3 at a constant temperature of 30°C 3 PO 4 In the solution, after ultrasonication at 30KHz for 4h, it was taken out and rinsed with deionized water to obtain 2wt% Al ions and 1wt% Sn ions co-doped TiO 2 array of nanotubes. Comparing the nanotube array with conventional TiO 2 The nanotube array is applied to ultraviolet light to degrade the methylene blue s...

Embodiment 3

[0030] Cut the TA10 alloy sheet with a thickness of 2mm into 2×8cm 2Long strips, polished by sandpaper and ultrasonically cleaned, used as standby anodes, and Pt sheets of the same size as cathodes and prepared ethylene glycol solution containing 2wt% water and 0.3wt% ammonium fluoride as electrolytes. The electrolysis process adopts a two-electrode DC electrolysis system with a voltage of 30V, a temperature of 40°C, and a time of 2h. After the electrolysis is completed, rinse the residual liquid on the surface of the anode with deionized water, and then soak it in H2O with a pH of 4 at a constant temperature of 40°C 2 SO 4 In the solution, after ultrasonication at 40KHz for 20min, take it out and rinse it with deionized water to obtain 0.2wt% Mo ions and 0.5wt% Ni ions co-doped TiO 2 array of nanotubes. Comparing the nanotube array with conventional TiO 2 Nanotube arrays are applied to ultraviolet light to degrade methylene blue solution with an initial solubility of 10mg...

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Abstract

The invention relates to a preparation method for a TiO2 nanotube array doped with regulated metal ions in situ. The preparation method comprises the following steps: 1) taking a titanium alloy sheet or a titanium alloy bar as a positive pole and a Pt sheet or Pt bar as a negative pole, preparing a nanotube array sample doped with regulated metal ions in situ through anodic oxidation in a fluorine-containing solution, and cleaning the sample; 2) selecting a proper acid or alkali solution, and partially leaching metal ions out by an ultrasonic-assisted selective acid or alkali dissolving method so as to realize quantitative regulation of the metal ion content of the nanotube array sample; and 3) performing cleaning after finishing the quantitative regulation, and performing drying to obtain the TiO2 nanotube array doped with the regulated metal ions in situ. The preparation method provided by the invention has the advantages and the beneficial effects as follows: a titanium alloy is taken as a base material, so that not only the preparation technique of the TiO2 nanotube array doped with the metal ions is simplified, but also the ions doped in the TiO2 nanotube array are dispersed more uniformly; and the doping content of the metal ions can be conveniently and controllably regulated by adopting the ultrasonic-assisted selective dissolving method so as to provide a reliable method for preparing a high-performance catalyst.

Description

technical field [0001] The invention belongs to the field of nanomaterial preparation, and relates to an in-situ doped TiO with regulated metal ions 2 Preparation method of nanotube arrays. Background technique [0002] TiO 2 Nanotube arrays have excellent photo(electro)catalytic activity and chemical stability, and are widely used in the fields of photo(electro)catalytic hydrogen production, photo(electro)catalytic treatment of environmental pollutants, and solar cells. After metal ion doping, a lower energy doping energy level is formed to absorb visible light and broaden the spectral response range. At the same time, TiO 2 Oxygen vacancies are formed on the surface, promoting the Ti 3 + The formation of oxidation centers is beneficial to charge trapping and inhibits electron-hole recombination, improving photon quantum efficiency. Currently, metal ion doped TiO 2 The nanotube array mainly adopts the conventional post-introduction method, that is, the preparation of ...

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