A method to improve the quality of copper-zinc-tin-sulfur thin film of photoelectrochemical water splitting photocathode

A copper-zinc-tin-sulfur, photoelectrochemical technology, applied in electrodes, electrolysis components, electrolysis process, etc., can solve problems such as adsorption of dense impurity particle layers, and achieve the effects of low cost, inhibition of high-temperature decomposition reaction, and simple and easy method.

Active Publication Date: 2020-03-10
NORTHEAST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The invention provides a method for improving the quality of photoelectrochemical water photocathode copper-zinc-tin-sulfur thin film, so as to solve the common problem of adsorbing dense heterogeneous particle layer on the surface of the thin film

Method used

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  • A method to improve the quality of copper-zinc-tin-sulfur thin film of photoelectrochemical water splitting photocathode
  • A method to improve the quality of copper-zinc-tin-sulfur thin film of photoelectrochemical water splitting photocathode
  • A method to improve the quality of copper-zinc-tin-sulfur thin film of photoelectrochemical water splitting photocathode

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1: the preparation of copper-zinc-tin-sulfur film

[0042] (1) Weigh 0.002mol of copper chloride, 0.001mol of zinc chloride, 0.001mol of stannous chloride and 0.007mol of thiourea into 10ml of dimethylformamide solution, stir and dissolve to form copper zinc tin sulfur Precursor solution;

[0043] (2) Drop the copper-zinc-tin-sulfur precursor solution onto the molybdenum glass substrate for spin-coating, the spin-coating speed is set to 3000 rpm, the spin-coating time is 30 seconds, and 4 layers are spin-coated;

[0044] (3) Add 0.2mmol tin acetate and 0.002mmol sodium fluoride to a mixed solution of 1.9ml ethylene glycol methyl ether and 0.1ml ethanolamine, stir and dissolve to form a fluorine-doped tin-rich solution, and spin-coat this solution onto copper-zinc-tin-sulfur For the upper layer of the prefabricated film, the spin-coating speed is set to 2000 rpm, the spin-coating time is 20 seconds, and one layer is spin-coated;

[0045] (4) Place the above ...

Embodiment 2

[0048] Embodiment 2: the preparation of copper-zinc-tin-sulfur film

[0049] (1) Weigh 0.006 mole of copper acetate, 0.004 mole of zinc acetate, 0.033 mole of stannous acetate and 0.026 mole of thiourea and join in 10ml dimethylformamide, stir and dissolve to form a copper zinc tin sulfur precursor solution;

[0050] (2) Drop the copper-zinc-tin-sulfur precursor solution onto the molybdenum glass substrate, set the spin-coating speed to 3500 rpm, spin-coating time is 40 seconds, and spin-coat 6 layers;

[0051] (3) Add 0.4mmol tin nitrate and 0.008mmol sodium fluoride to 1.9ml ethylene glycol methyl ether and 0.1ml ethanolamine mixed solution, stir and dissolve to form a fluorine-doped tin-rich solution, and spin-coat this solution onto copper-zinc-tin-sulfur For the upper layer of the prefabricated film, the spin-coating speed is set to 3000 rpm, the spin-coating time is 30 seconds, and 2 layers are spin-coated.

[0052] (4) Place the above film on a hot plate at 300°C for p...

Embodiment 3

[0055] Embodiment 3: the preparation of copper-zinc-tin-sulfur film

[0056] (1) Weigh 0.008 mole of copper acetate, 0.005 mole of zinc acetate, 0.006 mole of stannous acetate and 0.025 mole of thiourea into 10ml dimethylformamide, stir and dissolve to form a copper zinc tin sulfur precursor solution;

[0057] (2) Drop the copper-zinc-tin-sulfur precursor solution onto the molybdenum glass substrate, set the spin-coating speed to 4000 rpm, spin-coating time is 40 seconds, and spin-coat 8 layers;

[0058] (3) Add 0.8mmol of tin nitrate and 0.024mmol of sodium fluoride to 1.9ml of ethylene glycol methyl ether and 0.1ml of ethanolamine mixed solution, stir and dissolve to form a fluorine-doped tin-rich solution, and spin-coat this solution onto copper-zinc-tin-sulfur The upper layer of the prefabricated film, the spin-coating speed is set to 3500 rpm, the spin-coating time is 35 seconds, and three layers are spin-coated;

[0059] (4) Place the above film on a hot plate at 400°C ...

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Abstract

The invention relates to a method for improving the quality of a CZTS film for a photo-electrochemical water decomposition photocathode and belongs to the technical field of preparation of photo-electrochemical water decomposition photocathode materials. The method comprises the steps of preparing a CZTS prefabricated film through a solution spin-coating method, inserting a fluoride-doped tin-richmodifying layer on the upper surface of the prefabricated film, carrying out high-temperature sulfurizing treatment in a quick anneal oven, controlling the flow of blowing nitrogen in the heating orcooling process, modifying the sulfurized CZTS film with CdS and Pt cocatalyst, preparing the photo-electrochemical water decomposition photocathode, and testing the photo-electrochemical water decomposition performance of the photo-electrochemical water decomposition photocathode. By means of the method, the nonporous high-quality CZTS film material with the large-grain vertical penetration and firm adhesion properties is obtained, adsorption of impurity phases such as cuprous sulfide, zinc sulfide and excessive sulfur on the surface of the film can be effectively restrained, damage of a common solvent etching impurity disposal method to the film is avoided, the film is applied to a photo-electrochemical water decomposition system, and the photo-electrochemical water decomposition capacity of the film is remarkably improved.

Description

technical field [0001] The invention belongs to the technical field of photoelectrochemical water splitting photocathode material preparation, and in particular relates to a method for improving the quality of a copper-zinc-tin-sulfur thin film used for photoelectrochemical splitting water photocathode. Background technique [0002] kesterite copper zinc tin sulfur (Cu 2 ZnSnS 4 , CZTS) material due to its suitable band structure and bandgap width (about 1.5eV), high absorption coefficient (>10 4 cm -1 ), rich earth element composition, low material cost, and non-toxic constituent elements make it have important applications in the field of photoelectrochemistry. At present, the preparation method of CZTS film basically adopts physical or chemical methods to pre-prepare the precursor film, and then promotes crystal crystallization through high-temperature vulcanization treatment, so as to obtain high-quality crystalline film materials. However, as a quaternary compoun...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B11/08C25B1/04
CPCC25B1/04C25B1/55C25B11/051C25B11/091Y02E60/36Y02P20/133
Inventor 王玲玲赵桂莺滕丽芳陈丽萍张昕彤
Owner NORTHEAST NORMAL UNIVERSITY
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