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Preparation method of metal chalcogen compound thin film

A technology of compound and metal sulfur, which is applied in the direction of electrolytic inorganic material coating, etc., can solve the problems of easy cracking of the film, difficult control of film composition and thickness, etc., and achieve the effect of ensuring the shape and thickness, solving the problem of easy expansion, and precise control

Active Publication Date: 2013-12-25
CENT SOUTH UNIV
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Problems solved by technology

[0005] Aiming at the deficiencies of the prior art, the present invention provides an environmentally friendly and low-cost metal chalcogen compound thin film preparation method, which solves the problems in the prior art that the film composition and thickness are not easy to control, and the film is easy to crack when it is dried and annealed

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  • Preparation method of metal chalcogen compound thin film

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Embodiment 1

[0037] This embodiment illustrates the preparation method of a kind of metal chalcogen compound film provided by the present invention, adopts this method to prepare ferrous disulfide (chemical formula FeS 2 ) compound film.

[0038] A. The conductive substrate is used as a working electrode in the electrolyte solution, and the required single-component metal or alloy gold film is prepared by electrodeposition, and then the substrate is cleaned with deionized water;

[0039] A titanium sheet of 20×20×0.2 mm was selected as the conductive substrate, cleaned with degreasing agent, high-temperature lye, ethanol and deionized water, and then dried for later use.

[0040] Use constant potential deposition, use graphite electrode as counter electrode, saturated calomel electrode as reference electrode, electrolyte formula is 9.50mol / L FeSO 4 Main salt, 8.5mol / L NaCl supporting electrolyte, 10.0mol / L KSCN complexing agent, solution pH=3.0, deposition potential is -6.0V vs. SCE, elec...

Embodiment 2

[0047] This embodiment illustrates the preparation method of a kind of metal chalcogen compound film provided by the present invention, adopts this method to prepare ferrous disulfide (chemical formula FeS 2 ) compound film.

[0048] A. The conductive substrate is used as a working electrode in the electrolyte solution, and the required single-component metal or alloy gold film is prepared by electrodeposition, and then the substrate is cleaned with deionized water;

[0049] Select a 20×20×0.2mm stainless steel sheet as the conductive substrate, wash it with degreasing agent, high temperature lye, ethanol and deionized water, and then dry it for later use.

[0050] Using constant potential deposition, graphite electrode is used as the counter electrode, saturated calomel electrode is used as the reference electrode, and the electrolyte formula is 0.001mol / L FeSO 4 Main salt, 0.001mol / L NaCl supporting electrolyte, 0.001mol / L KSCN complexing agent, solution pH=1, deposition po...

Embodiment 3

[0057] This embodiment illustrates the preparation method of a kind of metal chalcogen compound film provided by the present invention, adopts this method to prepare copper indium gallium selenide (chemical formula Cu(In,Ga)Se 2 ) compound film.

[0058] A. The conductive substrate is used as a working electrode in the electrolyte solution, and the required single-component metal or alloy film is prepared by electrodeposition, and then the substrate is cleaned with deionized water;

[0059] Select 35×25×5mm Mo conductive glass as the conductive substrate, wash it with degreasing agent, high temperature lye, ethanol and deionized water, and dry it for later use.

[0060] Using constant current deposition, using a Pt electrode as the counter electrode, the electrolyte formula contains 0.50mol / L InCl 3 , 0.05mol / L GaCl 2 , 0.002mol / L CuCl 2 and 0.006mol / L of SeO 2 aqueous solution, the supporting electrolyte is 0.1mol / L LiCl and 0.6mol / L NH 4 Cl, the complexing agent is 0.08...

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Abstract

The invention relates to a preparation method of a metal chalcogen compound thin film and belongs to the technical field of optoelectronic film material preparation. The preparation method of combining electric deposition with chemical reaction is adopted comprises the following steps: firstly, putting a conductive substrate as a working electrode into an electrolyte solution, preparing desired single-component metal or an alloy thin-layer film by an electric deposition method, and then soaking the substrate into a precursor solution containing chalcogen anions so that the thin film reacts in the solution to generate a layer of target compound thin film, and then performing pre-annealing treatment on the obtained thin film; repeating the steps and controlling the times of circulation to obtain a prefabricated layer of the compound thin film of the desired thickness; finally, carrying out heat treatment on the prefabricated layer to form the metal chalcogen compound thin film. According to the preparation method, the problems that thin film components and thickness are not easy to control, and the flim is easy to crack when being subjected to drying and annealing process in the prior art are solved. Besides, the preparation method provided by the invention has the advantages of simple needed equipment, low preparation cost, and excellent performance of the obtained product and the like, and is convenient for industrial production.

Description

technical field [0001] The invention relates to a method for preparing a metal chalcogen compound thin film, belonging to the technical field of photoelectric thin film material preparation. Background technique [0002] Metal chalcogenide thin film materials have been widely used in photovoltaic, photothermal and semiconductor fields due to their unique photoelectric and chemical properties. At present, more and more attention has been paid to the research on the method of preparing metal chalcogenide thin film materials. [0003] Traditional methods for preparing metal chalcogenide thin film materials include vacuum and non-vacuum preparation methods. Vacuum methods include sputtering, thermal evaporation, molecular epitaxy, etc. Non-vacuum methods include electrodeposition, chemical solution method, spray thermal decomposition, sol-gel, coating method, etc. Compared with the vacuum method, the non-vacuum method, especially the electrodeposition method and the chemical so...

Claims

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Application Information

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IPC IPC(8): C25D9/04C25D5/50
Inventor 刘芳洋孙凯文苏正华蒋良兴韩自力赖延清李劼刘业翔
Owner CENT SOUTH UNIV
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