A kind of preparation method of copper sulfide nanopowder with multi-stoichiometric ratio

Abstract

A method for preparing a multi-stoichiometric copper sulfide nanopowder relates to a method for preparing a chemical powder material, the method comprising the following steps: uniformly mixing a copper salt and a vulcanization medium according to a certain Cu / S molar ratio Add it into the pressure-resistant reactor. After the reactor is sealed, pump a certain amount of reaction medium into it, so that the concentration of the copper salt precursor in the reaction medium is 0.1~1.0 M, and magnetically stir it, and heat it to 100~ 400°C, the reaction pressure is 0.1~10 MPa, and keep it in this state for 0.05~1.0h, and then the reactor is rapidly cooled, and the reaction system is collected, centrifuged, washed, and vacuum dried to obtain the product CuxS,x =1~2. The preparation method has simple process, short reaction time, cheap and easy-to-obtain raw materials, and is suitable for large-scale production.

Description

technical field [0001] The invention relates to a preparation method of chemical materials, in particular to a preparation method of multi-stoichiometric copper sulfide nanometer powder. Background technique [0002] Copper sulfide is a series of compounds with different stoichiometric ratios of copper and sulfur atoms formed by Cu and S under different conditions, such as: CuS, Cu 9 S 8 、Cu 39 S 28 、Cu 8 S 5 、Cu 7 S 4 、Cu 9 S 5 、Cu 31 S 16 、Cu 2 S et al. As important p-type semiconductors, copper sulfides have shown excellent performance and potential application prospects in the fields of solar cells, photocatalysts, cathode materials for lithium-ion batteries, nano-switches, and biomedicine. So far, scholars at home and abroad have used solvothermal (Crystengcomm 2014, 16, 5290; Eur. J. Inorg. Chem. 2014, 2014, 2368; Crystengcomm 2015, 17, 3452; CN105293560A), ionic liquid-assisted synthesis (CN104386733A; CN101367541A), anion exchange reaction (Dalton trans...

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Problems solved by technology

Although these methods realize the chemical preparation of copper sulfide, there are still some problems, such as the preparation time required by the currently used solvothermal method is too long (about 5~24 h), and usually the solvothermal method needs to add some additional Reagents, such as stabilizers, surfactants, organic ligands, directing agents, etc., make the reaction system and post-treatment more complicated, and these added reagents are usually toxic and expensive; the reaction time required for ionic liquid-assisted synthesis is too long (24~48 h), and the ionic liquid used is not easy to obtain and the price is high; the anion exchange reaction method and the template method first need to synthesize precursors such as cuprous oxide and sodium sulfate, and the reduction is also used in the synthesis of precursors. Agents, surfactants and acid-base reagents; the pyrolysis method does not need to use any solvents and additives, but the Cu-mercaptopropionic acid complex precursor must first be prepared

In addition, there are some other restrictive factors, such as complicated operation, unavailable reaction raw materials, and high cost, which make it difficult to realize industrial scale-up production of these methods

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