Method for preparing surface hydroxylated WO3 film photoelectrode material through plasma treatment

A plasma and hydroxylation technology, applied in the field of materials, can solve the problems of increasing the danger of the experimental process, being unfavorable to mass production, increasing the preparation cost, etc., and achieving a wide range of applications, excellent photoelectric catalytic water splitting performance, and increased electrical conductivity. Effect

Active Publication Date: 2019-09-17
TAIZHOU UNIV
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these modification methods all involve a high-temperature calcination process, which consumes a large amount of electric energy and increases the preparation cost.
Moreover, the use of flammable and explosive gases such as hydrogen increases the danger of the experimental process, which is not conducive to industrial mass production.

Method used

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  • Method for preparing surface hydroxylated WO3 film photoelectrode material through plasma treatment
  • Method for preparing surface hydroxylated WO3 film photoelectrode material through plasma treatment
  • Method for preparing surface hydroxylated WO3 film photoelectrode material through plasma treatment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Preparation of Surface Hydroxylated WO by Plasma Treatment 3 The method for thin film photoelectrode material, concrete steps are as follows: take 1.25g of H 2 WO 4 and 0.5g polyvinyl alcohol (PVA) dissolved in 17ml of H 2 o 2 (30wt%), pipette 200uL above-mentioned solution and spin-coat on FTO, spin coater parameter is set to low-speed 500 rev / s, time 10 seconds, high-speed 1500 revs / sec, time 30 seconds; After the FTO thin film is dried at room temperature, Calcined at 500°C in air for 2h, the heating rate was 180°C / h, to obtain WO 3 / FTO seed crystal; 1.25gH 2 WO 4 Dissolve in 30mL H 2 O, add 17 mL of 30 wt% H 2 o 2 , heated at 95°C for 2h to obtain a clear solution, and dilute it to a 100ml volumetric flask to obtain 0.05mol / L of H 2 WO 4 solution; add 3mL H in 10mL acetonitrile 2 WO 4 (0.05mol / L) solution, 0.2g oxalic acid, 0.5mL hydrochloric acid solution with a concentration of 6mol / l and 2.5ml deionized water, stir for 15min to fully stir the solutio...

Embodiment 2

[0024] Preparation of Surface Hydroxylated WO by Plasma Treatment 3 The method for thin film photoelectrode material, concrete steps are as follows: take by weighing 1.5g of H 2 WO 4 and 0.6g of polyvinyl alcohol (PVA) dissolved in 20ml of H 2 o 2 (30wt%), pipette 200uL above-mentioned solution and spin-coat on FTO, spin coater parameter is set to low speed 600 revs / sec, time 15 seconds, high speed 1800 revs / sec, time 20 seconds; After the FTO thin film is dried at room temperature, Calcined at 500°C in air for 2h, the heating rate was 180°C / h, to obtain WO 3 / FTO seed crystal; 1.5gH 2 WO 4 Dissolve in 30mL H 2 O, add 20 mL of 30 wt% H 2 o 2 , heated at 95°C for 2 hours to obtain a clear solution, and dilute it to a 100ml volumetric flask to obtain 0.06mol / L of H 2 WO 4 solution; add 3mL H in 10mL acetonitrile 2 WO 4 (0.06mol / L) solution, 0.2g oxalic acid, 0.5mL hydrochloric acid solution with a concentration of 6mol / l and 2.5ml deionized water, stir for 15min to f...

Embodiment 3

[0026] Preparation of Surface Hydroxylated WO by Plasma Treatment 3 The method for thin film photoelectrode material, concrete steps are as follows: take 2g of H 2 WO 4 and 0.8g polyvinyl alcohol (PVA) dissolved in 25ml of H 2 o 2 (30wt%), pipette 200uL above-mentioned solution and spin-coat on FTO, spin coater parameter is set to low speed 800 rev / s, time 10 seconds, high speed 2000 revs / sec, time 20 seconds; After the FTO film room temperature drying, Calcined at 500°C in air for 2h, the heating rate was 180°C / h, to obtain WO 3 / FTO seed; 1.25g H 2 WO 4 Dissolve in 30mL H 2 O, add 17 mL of 30 wt% H 2 o 2 , heated at 95°C for 2h to obtain a clear solution, and dilute it to a 100ml volumetric flask to obtain 0.05mol / L of H 2 WO 4 solution; add 3mL H in 10mL acetonitrile 2 WO 4 (0.05mol / L) solution, 0.2g oxalic acid, 0.5mL hydrochloric acid solution with a concentration of 6mol / l and 2.5ml deionized water, stir for 15min to fully stir the solution evenly, with the c...

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Abstract

The invention relates to a method for preparing a surface hydroxylated WO3 film photoelectrode material through plasma treatment. The specific steps comprise: preparing a WO3 seed crystal on the surface of a FTO electric-conduction glass, and hydrothermally growing nano-sheet-like WO3 on the surface of the WO3 seed crystal by using the H2O2 solution of H2WO4, acetonitrile, oxalic acid and a hydrochloric acid solution as raw materials; and treating the surface of the WO3 film electrode by using a low temperature plasma technology to obtain the surface hydroxylated WO3 film. According to the present invention, the prepared surface hydroxylated WO3 film has characteristics of good wettability with water, increased bulk phase carrier concentration and accelerated interface charge transfer, and can effectively promote the photoelectrocatalytic water decomposition performance; and the process for the plasma treatment of the WO3 film has characteristics of simpleness, energy saving, environmental protection, no pollution, high efficiency and short time, and provides the important way for the large-scale treatment of the WO3 photoelectrode.

Description

technical field [0001] The invention relates to the field of materials, in particular to a method for preparing surface hydroxylated WO by plasma treatment. 3 The method of thin-film photoelectrode materials is mainly used as photoanode materials for photocatalytic water splitting to produce hydrogen. Background technique [0002] Photoelectrochemical water splitting is an efficient and green way to produce renewable hydrogen, which has attracted more and more researchers' attention in recent years. Among them, the design and selection of semiconductor photoelectrode materials is the key to realize efficient photocatalytic water splitting. Semiconductor photocatalytic water splitting mainly involves three steps: light absorption, carrier separation and transfer, and chemical reaction at the semiconductor / solution interface, and inefficiency in any one step will inhibit the quantum efficiency of the photocatalytic process. Therefore, the development of high-efficiency photo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B11/06C25B1/04C23C18/12
CPCC23C18/1216C25B1/04C25B1/55C25B11/051C25B11/077Y02E60/36
Inventor 熊贤强梅优阳李江山范利亚武承林付帅
Owner TAIZHOU UNIV
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