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One-dimensional anatase TiO2 nanotube array thin film preferred oriented crystallization method

A nanotube array and preferred orientation technology, which is applied in the field of preparation of one-dimensional anatase TiO2 nanotube array film, can solve problems such as inability to control crystal plane orientation, and achieve the effects of low equipment requirements, inhibition of recombination, and simple operation

Active Publication Date: 2017-06-30
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the methods used are not comparable and cannot effectively control the crystal plane orientation, it still shows a solution to the problem of recombination of photogenerated electrons and holes at grain boundaries.

Method used

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  • One-dimensional anatase TiO2 nanotube array thin film preferred oriented crystallization method
  • One-dimensional anatase TiO2 nanotube array thin film preferred oriented crystallization method
  • One-dimensional anatase TiO2 nanotube array thin film preferred oriented crystallization method

Examples

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Effect test

Embodiment 1

[0020] 1) Titanium sheet pretreatment and electrolyte configuration: cut the titanium sheet into 8×9cm 2 The rectangular slices were ultrasonically cleaned in soap solution, ethanol and deionized water for 2 hours, and finally dried at 60°C for later use; electrolyte A was prepared, and the composition ratio of the electrolyte was: ethylene glycol: 5v%H 2 O: 0.2wt.%NH 4 F.

[0021] 2) Preparation of amorphous TiO 2 Nanotube Array Thin Films: Preparation of Amorphous TiO by a Two-Step Process 2 Nanotube thin film array, step 1: place the titanium sheet obtained in (1) in the electrolyte solution (260mL) of ethylene glycol, water and ammonium fluoride, take the titanium sheet as the anode and the graphite sheet as the cathode, and the two The distance between them is 3.5cm, and electrolysis is performed at 30V for 90min to obtain anodized TiO 2 Nanotube; Step 2: First, by sonicating to remove the TiO grown on the surface of the titanium sheet in step (1) 2 Nanotubes, to obt...

Embodiment 2

[0024] 1) Titanium sheet pretreatment and electrolyte configuration: cut the titanium sheet into 8×9cm 2 The rectangular slices were ultrasonically cleaned in soap solution, ethanol and deionized water for 2 hours, and finally dried at 80°C for later use; electrolyte A was prepared, and the composition ratio of the electrolyte was: ethylene glycol: 5v%H 2 O: 0.3wt.%NH 4 F.

[0025] 2) Preparation of amorphous TiO 2 Nanotube Array Thin Films: Preparation of Amorphous TiO by a Two-Step Process 2 Nanotube array film, step 1: place the titanium sheet obtained in (1) in the electrolyte solution (260mL) of ethylene glycol, water and ammonium fluoride, take the titanium sheet as the anode and the graphite sheet as the cathode, and the two The distance between them is 3.5cm, and electrolysis is performed at 30V for 90min to obtain anodized amorphous TiO 2 Nanotube array thin film; Step 2: First, by ultrasonic treatment to remove the TiO grown on the surface of the titanium sheet i...

Embodiment 3

[0028] 1) Titanium sheet pretreatment and electrolyte configuration: cut the titanium sheet into 8×9cm 2 The rectangular slices were ultrasonically cleaned in soap solution, ethanol and deionized water for 2 hours, and finally dried at 80°C for later use; electrolyte A was prepared, and the composition ratio of the electrolyte was: ethylene glycol: 5v%H 2 O: 0.4wt.%NH 4 F.

[0029] 2) Preparation of amorphous TiO 2 Nanotube Array Thin Films: Preparation of Amorphous TiO by a Two-Step Process 2 Nanotube array film, step 1: place the titanium sheet obtained in (1) in the electrolyte solution (200mL) of ethylene glycol, water and ammonium fluoride, take the titanium sheet as the anode and the graphite sheet as the cathode, and the two The distance between them is 5cm, and electrolysis is performed at 50V for 70min to obtain anodized amorphous TiO 2 Nanotube array film; Step 2: First, by ultrasonic treatment to remove the amorphous TiO grown on the surface of the titanium shee...

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Abstract

The invention discloses a one-dimensional anatase TiO2 nanotube array thin film preferred oriented crystallization method. The method achieves titanium sheet anodic oxidation combined heat treatment. The method specifically comprises the steps that a titanium sheet is placed into electrolyte containing ethylene glycol, ammonium fluoride and water to be subject to anodic oxidation preparation to obtain an amorphous TiO2 nanotube array thin film; then ethylene glycol washing and ethyl alcohol washing are sequentially carried out, and the concentration of F-ions remaining in the amorphous TiO2 nanotube array thin film is regulated and controlled; and after drying, heat treatment is carried out at the temperature ranging from 350 DEG C to 650 DEG C, heat preservation is carried out for 0.5 hour to 20 hours, and the one-dimensional anatase TiO2 nanotube array preferred oriented crystallization crystal thin film is obtained. By means of the method, through process regulation and control, one-dimensional anatase TiO2 nanotube array thin film preferred oriented crystallization can be achieved. The one-dimensional anatase TiO2 nanotube array thin film preferred oriented crystallization method is expected to be widely applied to the fields of solar cells, lithium ion batteries, photocatalytic hydrogen generation, organic pollutant photocatalytic decomposition and the like.

Description

technical field [0001] The invention belongs to the field of energy and environmental materials, in particular to a one-dimensional anatase TiO which obtains preferential orientations along different crystal planes 2 Preparation method of nanotube array thin film. Background technique [0002] Titanium dioxide (TiO 2 ), especially anatase TiO 2 As an excellent semiconductor catalyst, because of its safety, non-toxicity, excellent chemical stability, and low cost, it is widely used in photocatalytic organic pollutants, dye-sensitized solar cells, lithium-ion batteries, and photo-splitting water to generate hydrogen. It has broad application prospects. Both theory and experiment show that in anatase TiO 2 Among them, the {001} crystal plane has higher catalytic activity than the {101} crystal plane, however, due to the surface energy of the former (0.90J·m -2 ) is greater than the latter (0.44J·m -2 ), so that most of the crystals obtained in the actual preparation proce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/26B82Y40/00
CPCB82Y40/00C25D11/26
Inventor 裘吕超刘芳马朝霞杨杭生
Owner ZHEJIANG UNIV
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