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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: 2014-07-30
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 (referred to 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 solvents (oleylamine accounts for the total solvent volume 5%), the ratio of the total solvent volume to the final moles of CZTS is 20mL: 1mmol, N 2 Exhaust the air and keep it as a protective gas, heat 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. and kept for 1 hour.

[0047] 2. Raise the temperature at 2.5°C / min to 210°C, react at this temperature for 30 to 60 minutes, put the reaction flask in ...

Embodiment 2

[0051] This embodiment provides a pure phase monodisperse Cu 2 ZnSnS 4 The preparation method of nanocrystals (referred to 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 solvents (oleylamine accounts for the total solvent 5% by volume), the ratio of the total solvent volume to the moles of the final CZTS is 20mL: 1mmol, and N 2 Exhaust the air and keep it as a protective gas, heat to 120°C-140°C for 1 hour while stirring.

[0053] 2. Raise the temperature at 2.5°C / min to 210°C, react at this temperature for 30 to 60 minutes, put the reaction flask into the air and cool it below 80°C, transfer the fluid reaction solution into a centrifuge filled with ethanol After mixing evenly, centrifuge at 6...

Embodiment 3

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

[0058] 1. Weigh 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, ethylene glycol, polyethylene glycol and other common solvents) and oleylamine as solvents (oleylamine accounts for The total solvent volume is 10%), the ratio of the total solvent volume to the final molar number of CZTSSe is 30mL: 1mmol, and N 2 Exhaust the air and keep it as a protective gas, heat 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. and kept for 1 hour.

[0059] 2. Raise the temperature at 2.5°C / min to 220°C, react at this temperature for 3...

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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 photoelectric materials, in particular to a monodisperse Cu with adjustable bandgap controlled crystal phase synthesis 2 ZnSn(S 1-x Se x ) 4 nanocrystal approach. Background technique [0002] Cu 2 ZnSnS 4 (referred to as CZTS) solar cell materials are rich in components in the earth's crust and are 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 etc. have 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 adjustable composition was obtained by introducing selenium element. 2 ZnSn(S 1-x Se x ) 4 (CZTSSe for short) battery material is an im...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01L31/0264H01L31/0256C01B19/00B82Y30/00
Inventor 季书林叶长辉邱晓东
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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