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Preparation method of ternary copper-based sulfide semiconductor semiconductor nanomaterial

A technology of nano-materials and sulfides, applied in chemical instruments and methods, antimony compounds, inorganic chemistry, etc., can solve the problems of uncontrollable preparation process, difficult multi-phase coexistence, poor production stability, etc., to overcome long-term high-temperature treatment , Good production stability and less impurities

Inactive Publication Date: 2019-08-06
CHONGQING UNIV OF ARTS & SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are still several problems to be solved in the above synthesis method: (1) the operation is relatively complicated, and multiple steps are required to realize the recovery of particles; (2) the yield is very low; (3) the problem of multiphase coexistence is difficult to solve, and eventually Multi-step processing is required; (4) The preparation process is uncontrollable, making the grains easy to grow; (5) The reaction process is prone to explosion and the preparation fails; (6) The product has many impurities and low purity; (7) The process is unstable and the production is stable poor sex

Method used

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  • Preparation method of ternary copper-based sulfide semiconductor semiconductor nanomaterial
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  • Preparation method of ternary copper-based sulfide semiconductor semiconductor nanomaterial

Examples

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Effect test

Embodiment 1

[0032] A preparation of nanometer ternary copper antimony sulfide (Cu 12 Sb 4 S 13 ) particle method, comprising the steps of:

[0033] (1) Pour 3 mmol of antimony acetate powder as the antimony source into 15 ml of glacial acetic acid solvent, and complete the dissolution of the antimony acetate powder by ultrasonication for 30 minutes to obtain a 0.2 mol / L antimony acetate solution.

[0034] (2) Pour 0.6 mmol of copper acetate dihydrate powder into 70 ml of ethylene glycol methyl ether solution, and dissolve it completely by stirring. Then 0.5 mL of diethanolamine is poured into the above solution, and the color of the solution changes from blue-green to blue-purple; then 0.68 mmol of thiourea is poured into the above solution, and the color of the solution becomes light yellow; then 1 mL of antimony acetate solution (1 ) was poured into the above solution, and the solution became transparent and colorless. Put the prepared solution above into a hydrothermal reaction ket...

Embodiment 2

[0038] A preparation of nanometer ternary copper antimony sulfide (Cu 3 Sb 4 ) particle method, comprising the steps of:

[0039] (1) Pour 3 mmol of antimony acetate powder as the antimony source into 15 ml of glacial acetic acid solvent, and complete the dissolution of the antimony acetate powder by ultrasonication for 30 minutes to obtain a 0.2 mol / L antimony acetate solution.

[0040] (2) Pour 9 mmol of copper acetate dihydrate powder into 250 ml of ethylene glycol methyl ether solution, and dissolve it completely by stirring. Then pour 1mL of diethanolamine into the above solution, and the color of the solution changes from blue-green to blue-purple; then pour 105 mmoles of thiourea into the above solution, and the color of the solution turns into light yellow; then add 15mL of antimony acetate solution (1) Pour into the above solution, the solution becomes transparent and colorless. Put the prepared solution above into a hydrothermal reaction kettle, and the hydrotherm...

Embodiment 3

[0042] A preparation of nanometer ternary copper antimony sulfide (CuSbS 2 ) particle method, comprising the steps of:

[0043] (1) Pour 3 mmol of antimony acetate powder as the antimony source into 15 ml of glacial acetic acid solvent, and complete the dissolution of the antimony acetate powder by ultrasonication for 30 minutes to obtain a 0.2 mol / L antimony acetate solution.

[0044] (2) Pour 0.6 mmol of copper acetate dihydrate powder into 70 ml of ethylene glycol methyl ether solution, and dissolve it completely by stirring. Then 0.5 milliliters of diethanolamine is poured into the above-mentioned solution, and the color of the solution changes from blue-green to blue-purple; then 1.5 mmoles of thiourea are poured into the above-mentioned solution, and the color of the solution becomes pale yellow; then 3 milliliters of antimony acetate solution ( 1) Pour into the above solution, the solution becomes transparent and colorless. Pour the above prepared solution into the hy...

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Abstract

The invention discloses a preparation method of a ternary copper-based sulfide semiconductor semiconductor nanomaterial. The preparation method of the ternary copper-based sulfide semiconductor semiconductor nanomaterial comprises following steps: solvothermal method is adopted to prepare a nanometer scale ternary copper antimony sulfides of different stoichiometric ratios, an inorganic copper salt, an inorganic antimony salt, and a sulfur source are taken as raw material, middle temperature pressurization one-step reaction is adopted to prepare the ternary sulfide powder. The operation is simple; few steps are needed; the raw materials are cheap and easily available; the applicability on selection of different raw materials is high; in the preparation process, the product is easily prepared; product particle size is small; crystal grain growth is avoided; in the reaction process, preparation failure caused by explosive is avoided; the preparation method is beneficial for industrial large scale production; yield is as high as 86.2%; product phase purity is high; impurities are few; purity can be as high as 97.8%; the universality is high; technology is stable; production stabilityis high; a defect in the prior art that long time high temperature treatment is needed is avoided; and the prepared nanometer ternary sulfur antimony copper material can be widely used in the energy fields of lithium battery, thermoelectricity, and photoelectricity.

Description

technical field [0001] The invention belongs to the technical field of nanomaterials, and in particular relates to a preparation method of a ternary copper-based sulfide semiconductor nanomaterial. Background technique [0002] Facing the shortage of ore energy and the environmental pollution it brings, it is urgent and necessary to develop and use new energy technologies. Among them, photoelectric, thermoelectric and lithium battery technologies have extremely excellent performance and low prices, making them have great potential for popularization in the energy market. The basis for the improvement of energy conversion and storage performance is materials and suitable preparation technologies. The elements contained in ternary copper-based antimony sulfide (Cu-Sb-S, denoted as CAS) are cheap, stable, abundant, and non-toxic. At the same time, there are four stable ternary phases in the CAS system, CuSbS 2 (Stimbite structure), Cu 12 Sb 4 S 13 (tetrahedrite structure),...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G30/00
CPCC01G30/002C01P2002/72C01P2004/03C01P2006/80
Inventor 孟祥程江唐华李璐
Owner CHONGQING UNIV OF ARTS & SCI
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