a kind of wo 3 Electrochromic thin film and preparation method thereof

An electrochromic and thin-film technology, applied in the direction of coating, etc., can solve the problems that the discoloration performance of amorphous tungsten oxide thin film cannot be fully utilized, the cost of precursor and solvent is high, and the electrochromic performance is affected, and the electrochromic performance can be achieved. Good performance, saving annealing time, high solution stability

Active Publication Date: 2022-05-24
SOUTH CHINA UNIV OF TECH
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Problems solved by technology

However, the current sol-gel method has problems such as poor solution stability, high cost of precursors and solvents, and volatilization of toxic components during the preparation process.
Moreover, the amorphous tungsten oxide film prepared by the conventional sol-gel method has the following problems: 1) the organic component cannot be removed under annealing at 25°C to 300°C, which affects the electrochromic performance; ℃~300℃ annealing can only partially transform into amorphous tungsten oxide, which cannot give full play to the excellent discoloration performance of amorphous tungsten oxide thin film; Tungsten oxide begins to change from amorphous state to crystalline state, and the electrochromic performance decreases

Method used

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  • a kind of wo <sub>3</sub> Electrochromic thin film and preparation method thereof
  • a kind of wo <sub>3</sub> Electrochromic thin film and preparation method thereof
  • a kind of wo <sub>3</sub> Electrochromic thin film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Mix nano-tungsten oxide (purity: 99.8%, McLean) and concentrated ammonia (mass fraction: 25%, Guangzhou Chemical) in a mass ratio of 1:4;

[0031] (2) placing the solution obtained in step (1) on a magnetic stirring table and stirring for 24h;

[0032] (3) the solution obtained in step (2) is treated by ultrasonic vibration for 10min;

[0033] (4) the solution obtained in step (3) is adjusted to pH 12 with concentrated ammonia to obtain a precursor solution;

[0034] (5) In the glove box, spin-coating the prepared thin film on the cleaned ITO glass substrate. First rotate the substrate at 1500 rpm, and then drop the precursor solution onto the surface of the rotating substrate at a drop rate of 10 μL / s until the solution completely covers the entire substrate, stop dripping the solution, and then adjust the spin coating speed to 3000rpm, continuous spin coating for 60s;

[0035] (6) pre-annealing the film obtained in step (5) at a temperature of 120° C. for 10 mi...

Embodiment 2

[0041] The steps of (1)-(4) solution treatment and (6)-(7) annealing treatment in Example 1 are the same, except that in step (5): in the glove box, spin on the cleaned ITO glass substrate. Coating to prepare thin films. First rotate the substrate at 2000 rpm, then drop the precursor solution onto the surface of the rotating substrate at a drop rate of 10 μL / s until the solution completely covers the entire substrate, stop dripping the solution, and then adjust the spin coating speed to 4000rpm, continuous spin coating for 90s.

[0042] The resulting film thickness was 52.5±5 nm. The film obtained in Example 2 was subjected to an electrochromic test. 3 The photo of film discoloration is similar to Example 1. The transmittance modulation curve relative to air is as Figure 4 shown. Figure 4The transmittance curves of the initial state, colored state and faded state of the film obtained in Example 2. Taking the wavelength of 550 nm as the reference wavelength, the initial...

Embodiment 3

[0044] The steps of (1) to (6) solution treatment and pre-annealing treatment in Example 1 are the same, except that in step (7): the film after pre-annealing in step (6) is rapidly annealed in a rapid annealing furnace in an air atmosphere , firstly heated at a heating rate of 40°C / s, maintained at 200°C for 60s, then heated at 10°C / s, maintained at 300°C for 60s, and finally lowered to room temperature at a cooling rate of 10°C / s.

[0045] Compared with Examples 1 and 2, this example adopts a lower heating rate, and the obtained film thickness is 86.2±5 nm. The electrochromic test was carried out on the film obtained in Example 3. The electrolyte was 0.5 mol / L lithium perchlorate-propylene carbonate-UV curing glue solid electrolyte, the driving voltage was 2.5 V, and the electrification time was 30 s. Taking the wavelength of 550 nm as the reference wavelength, the initial state transmittance of the film is 78.9%, the color state transmittance is 41.6% and the faded state tr...

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Abstract

The invention belongs to the technical field of electrochromic thin films, and discloses a WO 3 Electrochromic thin film and its preparation method. The method: 1) using concentrated ammonia water to make nano-tungsten oxide into a precursor solution; 2) adding the precursor solution dropwise onto a rotating substrate, and after the dropping, increase the speed of the substrate and continue to rotate to obtain a thin film ; 3) the film is pre-annealed; 4) the pre-annealed film is rapidly annealed in an air atmosphere to obtain WO 3 Electrochromic film. The method of the invention is simple, the raw material cost is low, the solution stability is high, the prepared thin film is uniform and smooth, and the electrochromic performance of the thin film is good.

Description

technical field [0001] The invention belongs to the technical field of electrochromic films, and in particular relates to a WO 3 Electrochromic film and preparation method thereof. Background technique [0002] Tungsten oxide (WO 3 ) is considered to be the electrochromic material with the most commercial application value at present, and has obtained preliminary application in foreign markets. Its preparation techniques include magnetron sputtering, thermal evaporation and sol-gel method. Among them, the magnetron sputtering method is currently a commercially applied production process, and there is a problem of high production cost. The film prepared by the thermal evaporation method has poor stability and large-scale production cost. The sol-gel method has the advantages of simple equipment, convenient operation, high cost performance, no vacuum environment, and large-area film formation. It is expected to replace the magnetron sputtering method and become the mainstre...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C03C17/34
CPCC03C17/3417C03C17/002C03C2217/948C03C2217/70C03C2218/116C03C2218/32
Inventor 宁洪龙张观广姚日晖陈俊龙符晓张旭梁志豪梁宏富史沐杨彭俊彪
Owner SOUTH CHINA UNIV OF TECH
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