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Electrochemical method for preparing mesoporous tungsten trioxide film

A tungsten trioxide, electrochemical technology, applied in the direction of electrolytic coating, surface reaction electrolytic coating, coating, etc., to achieve the effect of large specific surface area, low cost and simple preparation process

Active Publication Date: 2018-03-30
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Studies have shown that when ionic liquids are mixed with water, PF 6 - Anion containing F will generate HF, and HF plays a key role in the formation of porous tungsten oxide film. However, ionic liquid is used as an additive of ethylene glycol solvent and applied to anodic oxidation to prepare mesoporous tungsten trioxide film. , there are no such reports

Method used

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  • Electrochemical method for preparing mesoporous tungsten trioxide film
  • Electrochemical method for preparing mesoporous tungsten trioxide film
  • Electrochemical method for preparing mesoporous tungsten trioxide film

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Cut the tungsten sheet with a thickness of 0.8mm into 1×1cm 2 The specifications were ultrasonically cleaned in acetone, ethanol and deionized water for 15 minutes, rinsed with deionized water and dried to obtain a metal tungsten electrode after degreasing; the ionic liquid 1-ethyl-3 methylimidazolium tetrafluoroboron Salt ([EMim]BF 4 ) 0.6mL and 9mL of deionized water were added to 51mL of ethylene glycol, wherein the volume fraction of ionic liquid was 1%, and the volume fraction of deionized water was 15%. Use tungsten sheet as anode, titanium sheet (thickness 0.2mm, specification 2×2cm 2 ) as the cathode, put it into the electrolyte, keep the electrode distance at 1.5cm, control the temperature of the electrolyte at 25°C, and oxidize at 10V for 3h; rinse the oxidized metal tungsten sheet with deionized water, and dry it.

[0031] The phase composition of the prepared mesoporous tungsten trioxide thin film is as follows: figure 1 It can be seen from the scanning e...

Embodiment 2

[0033] Cut the tungsten sheet with a thickness of 0.8mm into 1×1cm 2 The specifications were ultrasonically cleaned in acetone, ethanol and deionized water for 15 minutes, rinsed with deionized water and dried to obtain a metal tungsten electrode after degreasing; the ionic liquid 1-ethyl-3 methylimidazolium tetrafluoroboron Salt ([EMim]BF 4 ) 0.6mL and 9mL of deionized water were added to 51mL of ethylene glycol, wherein the volume fraction of ionic liquid was 1%, and the volume fraction of deionized water was 15%. Use tungsten sheet as anode, titanium sheet (thickness 0.2mm, specification 2×2cm 2 ) as the cathode, put it into the electrolyte, keep the distance between the electrodes at 1.5cm, control the temperature of the electrolyte at 25°C, and oxidize it at a voltage of 10V for 1h; wash the oxidized metal tungsten sheet with deionized water, and dry it to obtain Mesoporous tungsten trioxide thin films, such as Figure 4 shown.

Embodiment 3

[0035] Cut the tungsten sheet with a thickness of 0.8mm into 1×1cm 2 The specifications were ultrasonically cleaned in acetone, ethanol and deionized water for 15 minutes, rinsed with deionized water and dried to obtain a metal tungsten electrode after degreasing; the ionic liquid 1-ethyl-3 methylimidazolium tetrafluoroboron Salt ([EMim]BF 4 ) 0.6mL and 9mL of deionized water were added to 51mL of ethylene glycol, wherein the volume fraction of ionic liquid was 1%, and the volume fraction of deionized water was 15%. Use tungsten sheet as anode, titanium sheet (thickness 0.2mm, specification 2×2cm 2 ) as the cathode, put it into the electrolyte, keep the distance between the electrodes at 1.5cm, control the temperature of the electrolyte at 25°C, and oxidize it at a voltage of 10V for 7h; rinse the oxidized metal tungsten sheet with deionized water, and dry it to obtain Mesoporous tungsten trioxide thin films, such as Figure 5 shown.

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Abstract

The invention discloses an electrochemical method for preparing a mesoporous tungsten trioxide film. The method comprises the steps that metal tungsten subjected to pretreatment is taken as an anode,a titanium sheet or a platinum sheet serves as a cathode, in an electrolyte, constant-potential anodic oxidation is performed for 1-7 hours under the condition that the temperature ranges from 5 DEG Cto 40 DEG C and the voltage ranges from 3 V to 15 V, and then the metal tungsten is taken out to be cleaned and dried to obtain the mesoporous tungsten trioxide film on the surface of the metal tungsten. According to the electrochemical method, the tungsten trioxide films with different pore diameters can be obtained on the surface of the metal tungsten by controlling the electrolyte component, the anodic oxidation voltage and the oxidation time; the prepared tungsten trioxide film has a remarkable mesoporous structure, the specific surface area is large, and the prepared tungsten trioxide film is firmly combined with a metal tungsten substrate and is not prone to fall off; and the electrochemical method is simple in preparation process, low in cost, simple and convenient to operate, highin efficiency and wide in application prospect in the aspect of industrial application.

Description

(1) Technical field [0001] The invention relates to an electrochemical method for preparing a mesoporous tungsten trioxide film, in particular to a method for preparing a mesoporous tungsten trioxide film through anodic oxidation in an organic solvent electrolyte containing ionic liquid. (2) Background technology [0002] Tungsten trioxide is a semiconductor nanomaterial with indirect bandgap transition, which has the characteristics of electrochromism and gas sensitivity, and can be applied to smart windows, displays, H 2 sensors and other fields. The tungsten trioxide thin film with mesoporous structure can enhance the gas sensitivity and electrochromic sensitivity due to its high specific surface area and special spectral response. In recent years, the preparation of mesoporous tungsten trioxide thin film has become a research hotspot. [0003] Electrochemical anodization is a low-cost method that can construct porous nanomaterials with adjustable pore size and regular s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/26
CPCC25D11/26
Inventor 李国华吴世照马超胜周浩刘书杰
Owner ZHEJIANG UNIV OF TECH
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