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Method for synthesis of band gap-adjustable monodispersed Cu2ZnSn(S1-xSex)4 nano-crystals by crystal phase control

A nanocrystalline, monodisperse technology, applied in the direction of nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, can solve the problems of high cost of oleylamine, impact on environmental protection, high cost of battery materials, etc., and achieve the purpose of inhibiting rapid growth Large, easy to operate, and the effect of inhibiting agglomeration

Active Publication Date: 2013-01-02
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The cost of oleylamine is expensive. CZTSSe is prepared entirely by oleylamine. The product cost is more than 10,000 yuan / kg, and the cost of battery materials is too high; a large amount of oleylamine is coated on the surface of nano-grains, which affects the photoelectric performance of the grains in solar cell applications. , general solvents are difficult to clean and remove oleylamine thoroughly, unless toxic alkanes (such as cyclohexane, n-hexane) and halogenated alkanes (such as methyl chloride) are used for repeated cleaning, which will affect environmental protection

Method used

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  • Method for synthesis of band gap-adjustable monodispersed Cu2ZnSn(S1-xSex)4 nano-crystals by crystal phase control
  • Method for synthesis of band gap-adjustable monodispersed Cu2ZnSn(S1-xSex)4 nano-crystals by crystal phase control
  • Method for synthesis of band gap-adjustable monodispersed Cu2ZnSn(S1-xSex)4 nano-crystals by crystal phase control

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Experimental program
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Effect test

Embodiment 1

[0045] This embodiment provides a pure-phase monodisperse Cu 2 ZnSnS 4 The preparation method of nanocrystals (abbreviated as CZTS nanocrystals), the steps are as follows:

[0046] 1. Weigh CuCl powder and ZnCl according to the molar ratio of 2:1:4 2 Powder, S powder, put into a three-necked flask, pour glycerol (or a mixture of glycerol and ethylene glycol, polyethylene glycol and other common solvents) and oleylamine as a solvent (oleylamine accounts for the total solvent volume 5%), the ratio of the total solvent volume to the moles of the final CZTS was 20 mL: 1 mmol, and the flask was filled with N 2 Exhaust air and use it as protective gas all the time, heat to 80°C while stirring, press ZnCl 2 : SnCl 4 =1:1 molar ratio to take SnCl 4 The liquid was injected under the liquid surface of the reaction liquid, and the temperature was raised to 120°C to 140°C for 1 hour.

[0047] 2. Raise the temperature to 210°C at 2.5°C / min, react at this temperature for 30 to 60 minu...

Embodiment 2

[0051] This embodiment provides a pure-phase monodisperse Cu 2 ZnSnS 4 The preparation method of nanocrystals (abbreviated as CZTS nanocrystals), the steps are as follows:

[0052] 1. Weigh CuCl powder and ZnCl according to the molar ratio of 2:1:1:4 2 Powder, SnCl 4 ·5H 2 Put O powder and S powder into a three-necked flask, pour glycerol (or a mixture of glycerol and ethylene glycol, polyethylene glycol and other common solvents) and oleylamine as a solvent (oleylamine accounts for the total solvent 5% by volume), the ratio of the total solvent volume to the molar number of the final CZTS was 20 mL: 1 mmol, and the flask was filled with N 2 The air was exhausted and kept as protective gas, and heated to 120°C to 140°C for 1 hour while stirring.

[0053] 2. Raise the temperature to 210°C at 2.5°C / min, react at this temperature for 30 to 60 minutes, put the reaction flask in the air and cool it to below 80°C, and transfer the fluid reaction solution to a centrifuge filled ...

Embodiment 3

[0057] This embodiment provides a pure-phase monodisperse Cu 2 ZnSn(S 0.8 Se 0.2 ) 4 The preparation method of nanocrystals (abbreviated as CZTSSe nanocrystals), the steps are as follows:

[0058] 1. Weigh the CuCl powder and ZnCl according to the molar ratio of 2:1:3.2:0.8 2 Powder, S powder, Se powder, put into a three-necked flask, pour glycerol (or a mixture of glycerol and ethylene glycol, polyethylene glycol and other common solvents) and oleylamine as a solvent (oleylamine accounts for The total solvent volume is 10%), the ratio of the total solvent volume to the moles of the final CZTSSe is 30 mL: 1 mmol, and the flask is filled with N 2 Exhaust air and use it as protective gas all the time, heat to 80°C while stirring, press ZnCl 2 : SnCl 4 =1:1 molar ratio to take SnCl 4 The liquid was injected under the liquid surface of the reaction liquid, and the temperature was raised to 120°C to 140°C for 1 hour.

[0059] 2. Raise the temperature to 220°C at 2.5°C / min, re...

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Abstract

The invention discloses a method for synthesis of band gap-adjustable monodispersed Cu2ZnSn(S1-xSex)4 nano-crystals by crystal phase control. The method comprises the following steps of mixing a metal chloride, elemental sulfur and elemental selenium in a three-necked flask, pouring an alcohol solvent and a less amount of oleylamine into the three-necked flask, putting the three-necked flask in a magnetic stirring electric jacket, stirring with heating in a nitrogen or argon protective atmosphere for a complex reaction, then cooling, adding ethanol into reaction products, carrying out centrifugal separation precipitation, cleaning oleylamine on surfaces of crystal particles by a cleaning agent, and carrying out vacuum drying to obtain the band gap-adjustable monodispersed Cu2ZnSn(S1-xSex)4 nano-crystals. The method provided by the invention has simple processes, a low cost and no pollution on the environment and is suitable for large scale production.

Description

technical field [0001] The invention relates to a preparation technology of optoelectronic materials, in particular to a monodisperse Cu controlled crystal phase synthesis band gap adjustable 2 ZnSn(S 1-x Se x ) 4 Nanocrystalline method. Background technique [0002] Cu 2 ZnSnS 4 (CZTS for short) solar cell materials are rich in content in the earth's crust and non-toxic, and their optical and electrical properties fully meet the requirements of batteries. Compared with Si, CdTe, Culn 1-x Ga x Se 2 It has obvious promotion prospects, and the third-generation CZTS solar cells combined with nanotechnology are expected to occupy a large share of the non-toxic, cheap and high-efficiency solar cell market in the future. In order to further improve the photoelectric efficiency of CZTS solar cells, the so-called Cu with tunable composition was obtained by introducing selenium element. 2 ZnSn(S 1-x Se x ) 4 (CZTSSe for short) battery materials are an important means to o...

Claims

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Application Information

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IPC IPC(8): C01B19/00B82Y30/00
Inventor 季书林叶长辉邱晓东
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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