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An electrochromic wo 3 Controlled Preparation of Thin Films

An electrochromic and thin film technology, applied in ion implantation plating, coating, metal material coating process, etc., can solve the problems of poor controllability, small optical modulation amplitude, and high integral transmittance of film coloring state, and achieve optical The effect of large modulation amplitude, low transmittance, and adjustable oxygen-deficient phase intensity

Active Publication Date: 2017-06-20
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the invention is to solve the current electrochromic WO 3 The film has the disadvantages of high integrated transmittance in colored state, small optical modulation amplitude and poor controllability, etc., thus providing an electrochromic WO that can prepare low integrated transmittance in colored state, large optical modulation amplitude and good controllability 3 thin film method

Method used

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  • An electrochromic wo <sub>3</sub> Controlled Preparation of Thin Films
  • An electrochromic wo <sub>3</sub> Controlled Preparation of Thin Films
  • An electrochromic wo <sub>3</sub> Controlled Preparation of Thin Films

Examples

Experimental program
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Effect test

Embodiment 1

[0021] To clean the ITO conductive glass substrate, first clean the glass pieces in sequence with tap water and deionized water, then soak them in acetone and ethanol solutions successively, clean them with an ultrasonic cleaner for 15 minutes, and then put them in a drying box to dry; Preparation of WO by Beam Sputtering Deposition x Thin films, before sputtering deposition, use the method of "mechanical pump + molecular pump" to pump the basic vacuum of the chamber to 4.5×10 -3 Pa, and then pass high-purity argon gas with a purity of 99.999% and a flow rate of 16 sccm, and a working vacuum of 1.5×10 -2 Pa; in sputtering deposition, the accelerating voltage of sputtering ions is 2000V, the sputtering beam current is 60mA, and the deposition time is 3 hours, the prepared WO x The film thickness is about 280nm. Using 99.999% pure O 2 As an annealing atmosphere, at 500 o C temperature will WO x After the film was annealed for 10 minutes, the film crystallized into WO 3 Mai...

Embodiment 2

[0023]Under the same conditions in Example 1, at 500 o C temperature will WO x After annealing the film for 20 minutes, the film crystallized into WO 3 Main crystalline phase, accompanied by oxygen-deficient phase WO 2.83 and W 10 o 29 polycrystalline film ( figure 1 ); for WO 3 Li + Electrochemical coloring and fading reaction, the coloring time is about 20s; after applying ± 4V voltage coloring and fading treatment, WO 3 The optical modulation value of the film at 632.5nm wavelength is as high as 78% (see Table 1 and figure 2 ); the integral transmittance of the colored state for visible light is only 12%; the highest transmittance of the colored state is located at the wavelength of 414.5nm, and its value is only 34%; in the visible light range, the optical modulation values ​​at each wavelength are greater than 50%, Optical modulation value varies with anoxic phase WO 2.83 and W 10 o 29 The total strength of the monotonically increasing trend ( image 3 ).

Embodiment 3

[0025] Under the same conditions in Example 1, at 500 o C temperature will WO x The film was annealed for 40 minutes, and the film crystallized into WO 3 Main crystalline phase, accompanied by oxygen-deficient phase WO 2.83 and W 10 o 29 polycrystalline film ( figure 1 ); for WO 3 Li + Electrochemical coloring and fading reaction, the coloring time is about 20s; after applying ± 4V voltage coloring and fading treatment, WO 3 The optical modulation value of the film at 632.5nm wavelength is as high as 87% (Table 1 and figure 2 ), in the visible light range, the optical modulation values ​​at each wavelength are greater than 50%, and the optical modulation values ​​increase with the oxygen-deficient phase WO 2.83 and W 10 o 29 The total strength of the monotonically increasing trend ( image 3 ).

[0026] Table 1

[0027]

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Abstract

The invention relates to a preparation method of a WO3 film. An ion-beam sputtering deposition technique and a subsequent annealing treatment technique are combined to prepare the electrochromic WO3 film with favorable optical properties, and the strength of the anaerobic phase in the WO3 film is controlled to regulate the optical modulation properties. By using ITO (indium tin oxide) conducting glass as the substrate, the ion-beam sputtering deposition technique is utilized to prepare the WOx film; and by using 99.999% pure O2 as an annealing atmosphere, the WOx film is subjected to annealing treatment at different temperatures for different time periods to prepare the WO3 film containing anaerobic phase. When the WO3 film is subjected to Li<+> electrochemical coloring / discoloring reaction, after the discoloring voltage is applied, the prepared electrochromic WO3 film has the advantages of low coloring-stage integral transmittivity, adjustable anaerobic phase strength, large optical modulation amplitude and favorable controllability. The WO3 film is simple in preparation technique and is hopeful to be applied to the fields of smart windows, electronic information display devices, no-glare reflectors and the like.

Description

technical field [0001] The present invention relates to a WO 3 The preparation method of the thin film, using the ion beam sputtering deposition technology combined with the subsequent annealing process to prepare electrochromic WO with excellent optical properties 3 thin film, and controlled by WO 3 The intensity of the oxygen-deficient phase in the film is used to control the optical modulation properties. Background technique [0002] WO 3 Thin film is an indirect band semiconductor material with good electronic and optical properties. WO 3 The thin film acts as a cathode, and under the action of an external electric field, cations (Li + , H + ), WO 3 The thin film will exhibit good electrochromic properties, and can return to its original state when the cations are extracted. Therefore, with WO 3 As an electrochromic device made of electrochromic coating, it has the functions of recording (coloring), storage (removing voltage, record preservation), erasing (blea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C14/08C23C14/46
Inventor 蒋美萍薛金鑫苏江滨陈宪锋刘阳
Owner CHANGZHOU UNIV
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