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Method for preparing vertically aligned tungsten oxide nano structural electrochromic film

A nanostructure and electrochromic technology is applied in the field of preparation of tungsten oxide nanostructure electrochromic thin films, which can solve the problems of affecting coloring efficiency, unable to use fast-response devices, and low cycle times, and achieves improved electrochemical stability, Beneficial to electron conduction and simple preparation method

Inactive Publication Date: 2013-01-30
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the electrochromic properties of these nanostructured tungsten oxide films have been greatly improved, there are still many problems in practical applications, such as: (1) the number of cycles is small, and it is difficult to meet the requirements of practical applications; (2) ) The coloring and fading time is long, and it cannot be used for fast response devices; (3) The modulation amplitude of visible light transmittance is low, which cannot meet the needs of practical applications
[0004] The reason is mainly in the following two aspects: First, these nanostructures are randomly attached to the surface of the glass substrate, so the bonding force between the tungsten oxide of these nanostructures and the transparent conductive substrate is relatively poor, especially at the top of the film. Tungsten oxide nanostructures, which will inevitably affect the contact between the ions in the electrolyte and the tungsten oxide nanostructures and the substrate, thereby affecting its electrochromic response speed; secondly, it is precisely because these randomly attached nanostructures are on the transparent conductive substrate The close packing of these nanostructures leads to the underutilization of the active surface of these nanostructures, which affects its coloring efficiency.

Method used

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  • Method for preparing vertically aligned tungsten oxide nano structural electrochromic film
  • Method for preparing vertically aligned tungsten oxide nano structural electrochromic film
  • Method for preparing vertically aligned tungsten oxide nano structural electrochromic film

Examples

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Effect test

Embodiment 1

[0033] The FTO conductive glass was sequentially immersed in deionized water, acetone and ethanol for ultrasonic cleaning for 20 minutes, and dried for later use. Weigh 5g of tungstic acid and dissolve it in a mixed solution of 60mL of hydrogen peroxide and 140mL of water, heat to 95°C, cool down after the tungstic acid is completely dissolved to obtain a transparent sol; then spin-coat the transparent sol on the surface of FTO conductive glass cleaned by ultrasonic , and calcined at 500° C. for 0.5 hour to obtain a tungsten oxide seed layer. Prepare a reaction solution containing 10.5mL of transparent sol, 3.5mL of hydrochloric acid (3mol / L), 1.2mmol of urea, and 42mL of water, and then immerse the FTO conductive glass with the tungsten oxide seed layer obtained above into a hydrothermal solution containing the reaction solution. In the kettle, keep warm at 180°C for 12 hours, and finally cool down to room temperature naturally, take out the FTO conductive glass, wash it with...

Embodiment 2

[0036]The FTO conductive glass was sequentially immersed in deionized water, acetone and ethanol for ultrasonic cleaning for 20 minutes, and dried for later use. Weigh 2.5g of tungstic acid and dissolve it in a mixed solution of 60mL of hydrogen peroxide and 140mL of water, heat to 80°C, cool down after the tungstic acid is completely dissolved to obtain a transparent sol; then spin-coat the transparent sol on the ultrasonically cleaned FTO conductive glass The surface was calcined at 350°C for 2 hours to obtain a tungsten oxide seed layer. Prepare a reaction solution containing 10.5mL of transparent sol, 3.5mL of hydrochloric acid (3mol / L), 3.6mmol of urea, and 42mL of water, and then immerse the FTO conductive glass with the tungsten oxide seed layer obtained above into a hydrothermal solution containing the reaction solution. In the kettle, keep warm at 180°C for 12 hours, and finally cool down to room temperature naturally, take out the FTO conductive glass, wash it with w...

Embodiment 3

[0038] The FTO conductive glass was sequentially immersed in deionized water, acetone and ethanol for ultrasonic cleaning for 30 minutes, and dried for later use. Weigh 5g of tungstic acid and dissolve it in a mixed solution of 60mL of hydrogen peroxide and 140mL of water, heat to 95°C, cool down after the tungstic acid is completely dissolved to obtain a transparent sol; then spin-coat the transparent sol on the surface of FTO conductive glass cleaned by ultrasonic , and calcined at 400° C. for 0.5 hour to obtain a tungsten oxide seed layer. Prepare a reaction solution containing 10.5mL transparent sol, 3.5mL hydrochloric acid (6mol / L), 1.2mmol urea, 21mL water, and 21mL acetonitrile, and then immerse the FTO conductive glass with the tungsten oxide seed layer obtained above into the reaction solution In a hydrothermal kettle, keep warm at 180°C for 6 hours, and finally cool down to room temperature naturally, take out the FTO conductive glass, wash it with water and ethanol ...

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Abstract

The invention relates to a method for preparing a vertically aligned tungsten oxide nano structural electrochromic film. The method comprises the following steps of: 1) dissolving tungstic acid in a mixed solution of hydrogen peroxide and water, heating until tungstic acid is fully dissolved, and cooling to obtain transparent sol; 2) coating the obtained transparent sol on the surface of fluorine-doped tin oxide (FTO) conducting glass which is subjected to ultrasonic washing in a spinning way, and calcining to obtain the FTO conducting glass with a tungsten oxide crystal seed layer; and 3) preparing a reaction solution containing the transparent sol, hydrochloric acid, urea and solvent, immersing the obtained FTO conducting glass with the tungsten oxide crystal seed layer in a hydrothermal kettle in which the reaction solution is filled, preserving heat at the temperature of between 150 and 180 DEG C for 6 to 12 hours, naturally cooling to room temperature, washing and drying to obtain the vertically aligned tungsten oxide nano structural electrochromic film. A preparation process is simple and low in cost; by the method, the electrochromic properties such as color change speed, coloration efficiency, cycling stability and the like of the film are effectively improved; and the method has the industrial application prospect in the aspect of preparing the film on the surface of the glass.

Description

technical field [0001] The invention belongs to the field of preparation of electrochromic thin films, in particular to a preparation method of vertically aligned tungsten oxide nanostructure electrochromic thin films. Background technique [0002] Electrochromism refers to the phenomenon that materials produce stable and reversible changes under the action of electric field. When the material undergoes electrochemical injection and extraction of electrons and ions, its valence and chemical composition change, thereby changing the reflection and transmission properties of the material, and the appearance performance is manifested as a reversible change in color and transparency. . Electrochromic materials have been paid attention to because of their broad application prospects in display devices, smart windows, glare-free mirrors, and military anti-counterfeiting. Since S.K.Deb first reported the electrochromic effect of amorphous tungsten oxide film in 1969, electrochromi...

Claims

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Application Information

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IPC IPC(8): C03C17/34
Inventor 王宏志马董云李耀刚张青红
Owner DONGHUA UNIV
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