WO3 electrochromic thin film preparation method

A thin film preparation and electrochromic technology, applied in optics, instruments, nonlinear optics, etc., can solve the problems of difficult to enlarge the area of ​​the thin film, expensive preparation cost, and high preparation requirements, and achieves good coloring efficiency, simple equipment, and easy preparation. Effect

Inactive Publication Date: 2009-11-11
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0007] The above-mentioned electrochromic material preparation methods are mainly magnetron sputtering and spin coating. The advantages are that the prepared film particles are relatively uniform, the light transmittance is good, and the discoloration efficiency is good. However, its defects are also obvious, and the preparation cost of the material is expensive. The area of ​​the produced film is not easy to enlarge, the preparation requirements are high, and the equipment is expensive, etc.

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  • WO3 electrochromic thin film preparation method
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  • WO3 electrochromic thin film preparation method

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preparation example Construction

[0041] The preparation method of the above-mentioned tungsten trioxide film is basically characterized in that it comprises the following specific processes:

[0042] (1) Clean the substrate, ultrasonically clean it in lye and acetone, clean it with deionized water, dry it, and set it aside.

[0043] (2) React tungsten powder with hydrogen peroxide for 5-7 hours, filter, then add absolute ethanol and glacial acetic acid to the filtrate, and stir evenly.

[0044] (3) Reflux at 50-60°C for 5-6 hours through a cooling reflux device to obtain uniform and transparent WO 3 Sol.

[0045] (4) the WO obtained above 3 The sol was distilled under reduced pressure in a rotary evaporator at 50-60°C to concentrate the sol concentration.

[0046] (5) Immerse the substrate in (1) in the above-mentioned sol for about 3 minutes, and the film pulls the substrate vertically upward at a speed of 2-3 cm / min.

[0047] (6) Repeat step (5) twice at an interval of 5 minutes, and then air dry natura...

Embodiment 1

[0050] (1) Clean the FTO conductive glass. (2) React 6.5g of 99.9% tungsten powder with a particle size below 1000nm and 40ml of 30% analytically pure hydrogen peroxide for 5-7 hours, filter, and then add 10.0ml of analytically pure anhydrous ethanol and analytically pure Glacial acetic acid 40.0ml, stir evenly. (3) The peroxypolytungstic acid generated in step (2) is more fully acetylated by cooling and refluxing. The reflux time is an important factor affecting the sol concentration. The reflux time is 6-10 hours to obtain tungsten trioxide sol. (4) Use a rotary evaporator to distill and concentrate the sol under reduced pressure to increase the concentration of the sol, and the vacuum degree of the decompression device is 0.07-0.09Mpa. (5) Place the substrate vertically on the WO obtained in (4) 3 In the sol, the immersion time is about 3 minutes, so that it is fully in contact with the sol, and the substrate is pulled up at a speed of 2-3cm / min evenly and vertically. Aft...

Embodiment 2

[0052] The difference from Example 1 is that 1 g of analytically pure OAD is added in step (3), and the rest of the steps are similar to Example 1.

[0053] To the WO made by the present invention 3 The thin film is tested for light transmittance characteristics and cyclic voltammetry characteristics in the visible light band 400-750nm. with WO 3 As the working electrode, the counter electrode is Pt, Ag / AgCl is the reference electrode, 1.5mol / L LiClO 4 / Ethylene glycol solution is used as the electrolyte, and the cyclic voltammetry characteristics of the film are observed at the electrochemical workstation by using the three-electrode method. The scanning speed is 100mV / s, and the potential scanning range is -2-+2V, and the cycle test is performed continuously for 20 times.

[0054] WO prepared by the present invention 3 The film has a light transmittance adjustment effect on the visible light band 400-750nm, according to figure 1 , figure 2 By changing the polarity of t...

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Abstract

A WO3 electrochromic thin film preparation method belongs to electrochromism technology and comprises the following steps of (1) washing a substrate; (2) conducting filtration after tungsten powder reacts with hydrogen peroxide for 5-7 hours in ice-water bath, then adding absolute ethyl alcohol and glacial acetic acid in the filtrate and stirring evenly; (3) using a reflux device for reflux at temperature of 50-60 DEG C for 5-6 hours to obtain uniform and transparent WO3 sol; (4) dipping the substrate of the step (1) in the sol obtained from the step (3) and pulling and drawing the substrate upwards with speed of 2-3cm / min; (5) repeating the step (4) for a plurality of times and then naturally drying the substrate in the air; and (6) heat treating the substrate obtained from the step (5) to obtain the WO3 thin film. The method adopts a sol-gel method to prepare the electrochromic thin film of tungsten trioxide, has simple device, low cost, easy preparation and good coloration efficiency, and is conducive to industrial large-area practical application and popularization.

Description

technical field [0001] The invention belongs to the technical field of electrochromism, and relates to a tungsten trioxide electrochromic material prepared by a sol-gel method and a film preparation method by a pulling technique. Background technique [0002] Electrochromism (EC) refers to the phenomenon that the optical properties of materials produce stable and reversible changes under the action of an external electric field. With the injection / extraction of external ions or electrons, reversible changes (coloring / fading) occur in the visible light range through wavelengths. . WO 3 The electrochromic film is composed of a layer of transition metal oxide WO 3 The composition is a typical cathode inorganic electrochromic material, the standard stoichiometric ratio of WO 3 With perovskite-like ABO 3 The structure of the cation site A is empty, while the B site is occupied by W, each W 6+ Surrounded by 6 oxygen atoms into an octahedron, each oxygen atom is shared by 2 re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G02F1/15C03C17/23
Inventor 唐武刘贵发翁小龙陈良邓龙江
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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