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Method for preparing crystal-phase-controllable monodispersed Cu2ZnSnS4 nanocrystalline

A nanocrystalline, monodisperse technology, applied in nanotechnology, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of solar cell cost reduction, difficulty in cleaning, high cost, etc., to reduce material cost, facilitate recycling, and low cost Effect

Active Publication Date: 2012-08-22
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Abstract
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Problems solved by technology

[0003] The embodiment of the present invention provides a monodisperse Cu with controllable crystal phase 2 ZnSnS 4 The preparation method of nanocrystals can solve the problem of using expensive and difficult-to-clean oleylamine as a solvent in the preparation of CZTS nanocrystal materials by solvothermal method, which has high cost and restricts the cost reduction of solar cells in the later stage

Method used

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  • Method for preparing crystal-phase-controllable monodispersed Cu2ZnSnS4 nanocrystalline
  • Method for preparing crystal-phase-controllable monodispersed Cu2ZnSnS4 nanocrystalline
  • Method for preparing crystal-phase-controllable monodispersed Cu2ZnSnS4 nanocrystalline

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[0027] The embodiment of the present invention provides a crystal phase controllable monodisperse Cu 2 ZnSnS 4 The preparation method of nanocrystals (referred to as CZTS nanocrystals) is a cheap, simple, and scalable solvothermal growth method for preparing CZTS nanocrystals. It does not require expensive equipment and complicated processes. Metal chloride salts in alcohol solvents react with elemental sulfur at a certain temperature and under the protection of an inert gas. By adding a small amount of oleylamine to complex the precursors, react and disperse the products to inhibit their agglomeration and rapid growth, that is, to obtain crystal phases. Controlled monodisperse Cu 2 ZnSnS 4 nanocrystals, the method comprising:

[0028] Precursor complexation: metal chloride salts CuCl (copper chloride), ZnCl 2 (zinc chloride), SnCl 4 (Tin tetrachloride) and elemental sulfur (S) add in the container, add alcoholic solvent and oleylamine in the described container, feed nit...

Embodiment 1

[0046] This embodiment provides a crystal phase controllable monodisperse Cu 2 ZnSnS 4 The preparation method of nanocrystal (being called for short CZTS nanocrystal), the steps are as follows:

[0047] (1) Precursor complexation of CZTS nanocrystals: Weigh CuCl and ZnCl at a molar ratio of 2:1:4 2 , S powder, put into a three-necked flask as a reaction container, pour glycerin (or the mixed solution of glycerin and ethylene glycol, polyethylene glycol and other common solvents) and oleylamine as solvent (oleylamine account for 10% of the total solvent volume), the ratio of the total solvent volume to the moles of the final CZTS is 10mL: 1mmol, and feed N into the three-necked flask 2 The gas exhausts the air in it and has been in N 2 gas as a protective gas, heated to 80°C while stirring, press ZnCl 2 : SnCl 4 =1:1 molar ratio to take SnCl 4 The liquid is injected under the liquid surface of the reaction solution, and the temperature is raised to 120°C to 140°C for 1 ho...

Embodiment 2

[0052] This embodiment provides a crystal phase controllable monodisperse Cu 2 ZnSnS 4 The preparation method of nanocrystal (being called for short CZTS nanocrystal), the steps are as follows:

[0053] (1) Precursor complexation of CZTS nanocrystals: Weigh CuCl and ZnCl at a molar ratio of 2:1:4 2 , S powder, put into a three-necked flask as a reaction container, pour glycerin (or the mixed solution of glycerin and ethylene glycol, polyethylene glycol and other common solvents) and oleylamine as solvent (oleylamine account for 7% of the total solvent volume), the ratio of the total solvent volume to the moles of the final CZTS is 15mL: 1mmol, and feed N into the three-necked flask 2 The gas exhausts the air in it and has been in N 2 gas as a protective gas, heated to 80°C while stirring, press ZnCl 2 : SnCl 4 =1:1 molar ratio to take SnCl 4 The liquid is injected under the liquid surface of the reaction solution, and the temperature is raised to 120°C to 140°C for 1 hou...

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Abstract

The invention discloses a method for preparing crystal-phase-controllable monodispersed Cu2ZnSnS4 nanocrystalline, which belongs to the field of photoelectric material preparation. The method includes: precursor complexation, namely adding metal chloride salt and simple substance sulfur into a container, adding alcohol solvent and oleyl amine, feeding nitrogen or argon as shielding gas, magnetically stirring, heating to a certain temperature and complexing to obtain reaction precursor liquid; solvent thermal preparation, namely stirring while adding the shielding gas nitrogen or argon, heating the reaction precursor liquid to a certain temperature, reacting for a while, cooling and adding ethanol into reaction liquid with liquidity, centrifugally separating for precipitation to obtain Cu2ZnSnS4 nanocrystalline grains; cleaning, namely using cleaning agent to wash off the oleyl amine on the surfaces of the obtained Cu2ZnSnS4 nanocrystalline grains to obtain monodispersed CZTS (copper zinc tin sulfide) nanocrystalline colloid; and post-treatment, namely subjecting the obtained monodispersed CZTS nanocrystalline colloid to vacuum drying to obtain monodispersed Cu2ZnSnS4 nanocrystalline powder. The method is simple and low in cost.

Description

technical field [0001] The invention relates to the field of photoelectric material preparation, in particular to a monodisperse Cu with controllable crystal phase that can be used as a photoelectric material 2 ZnSnS 4 Methods of preparing nanocrystals. Background technique [0002] In recent years, with the rapid development of new energy technology and industry, new solar cells have received widespread attention, especially with the continuous application of nanotechnology in this field, the so-called third-generation solar cells with high cost performance have become the focus of the scientific and industrial circles. hot spot. In order to meet the needs of marketization, further reducing the cost of battery materials is the key. Cu 2 ZnSnS 4 (referred to as CZTS) material is rich in components in the earth's crust and is non-toxic, and its optical and electrical properties fully meet the requirements of batteries. Compared with Si, CdTe, CuIn 1-x Ga x Se 2 etc. h...

Claims

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Application Information

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IPC IPC(8): C01G19/00B82Y40/00
Inventor 季书林叶长辉邱晓东张煜欣
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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