Large-scale preparation method for wurtzite Cu2ZnSnS4 nanocrystal

A technology of nanocrystals and wurtzite, applied in nanotechnology, chemical instruments and methods, inorganic chemistry, etc., can solve the inherent limitations of product yield, which is difficult to increase, unfavorable for high-efficiency, rapid preparation, and difficult to expand the scale of the reaction. The preparation process is intuitive and controllable, the photoelectric conversion efficiency is improved, and the cost is low

Active Publication Date: 2017-02-15
KUNMING UNIV OF SCI & TECH
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Problems solved by technology

The literature Phys. Chem. Chem. Phys., 2015, 17, 19777~19788 and Cryst. Eng. Comm., 2015, 17, 174~182 have successfully prepared wurtzite CZTS nanocrystals, but they all use the hot injection method, the whole reaction The process requires inert gas protection, and the product yield is limited by the inherent limitations of the thermal injection method, which is difficult to improve
The literature Chem. Phys. Lett., 2014, 592, 144–148 uses direct heating to synthesize spindle-shaped wurtzite CZTS. This structure is conducive to increasing the carrier concentration and improving electron transport. However, this method requires the preparation of acetyl The synthesis of CZTS from acetonate is complicated, and the solvent used is expensive and highly toxic
Patent 105197985A discloses a method for preparing ultra-long wurtzite Cu2ZnSnS4 nanorods in one step by solvothermal method, but this reaction needs to be carried out under high temperature and high pressure environment, which makes the equipment complicated and the reaction time is long (more than 12h), which is not conducive to For efficient and fast preparation
And above-mentioned these methods, each wurtzite CZTS particle production all is in milligram level, and it is difficult to expand reaction scale, is unfavorable for realizing large-scale production

Method used

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  • Large-scale preparation method for wurtzite Cu2ZnSnS4 nanocrystal

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Experimental program
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Effect test

Embodiment 1

[0028] (1) Add 14mmol of cuprous iodide, 10mmol of zinc chloride and 8mmol of tin chloride pentahydrate into 48ml of oleylamine solvent, slowly heat the solution to 120°C under vacuum, and keep it warm for 30 minutes to completely remove the Water and oxygen are then cooled to room temperature to obtain a precursor solution;

[0029] (2) Add 16ml of n-dodecanemercaptan to the precursor solution to obtain a mixed solvent, then add 20mmol of carbon disulfide, heat to 140°C for 30 minutes, then heat to 300°C for 30 minutes, during the heating process, pass through a magnetic stirrer The reaction solution is stirred, and the stirring speed is 1000r / min;

[0030] (3) Stop heating, and after the reaction system is cooled to 60°C, add 30 ml each of n-hexane, methanol and ethanol to the reaction liquid at a time, centrifuge at 12000 r / min for 5 min, discard the supernatant, and repeat the above centrifugation operation for 3 times, the cleaned product was dried in a drying oven at 60...

Embodiment 2

[0033] (1) Add 18mmol of cuprous iodide, 10mmol of zinc chloride and 5mmol of tin chloride pentahydrate into 48ml of oleylamine solvent, slowly heat the solution to 120°C under vacuum, keep it warm for 30 minutes, and completely remove the The water and oxygen are cooled to room temperature to obtain the precursor solution;

[0034] (2) Add 16ml of n-dodecanemercaptan to the precursor solution to obtain a mixed solvent, then add 30mmol of carbon disulfide, heat to 160°C for 50 minutes, then heat to 280°C for 45 minutes, during the heating process, use a magnetic stirrer to The reaction solution is stirred, and the stirring speed is 800r / min;

[0035] (3) Stop heating, and after the reaction system is cooled to 60°C, add 30 ml each of n-hexane, methanol and ethanol to the reaction liquid at a time, centrifuge at 11000 r / min for 5 min, discard the supernatant, and repeat the above centrifugation operation 3 times, the cleaned product was dried in a drying oven at 70°C for 10 h ...

Embodiment 3

[0038](1) Add 20mmol of cuprous iodide, 10mmol of zinc chloride and 8mmol of tin chloride pentahydrate into 48 ml of oleylamine solvent, slowly heat the solution to 120°C under vacuum, keep it warm for 30 minutes, and completely remove the The water and oxygen are cooled to room temperature to obtain the precursor solution;

[0039] (2) Add 16ml of n-dodecanethiol to the precursor solution to obtain a mixed solvent, then add 40mmol of carbon disulfide, heat to 180°C for 20 minutes, and then heat to 250°C for 60 minutes. During the heating process, use a magnetic stirrer to The reaction solution is stirred, and the stirring speed is 700r / min;

[0040] (3) Stop heating, and after the reaction system is cooled to 60°C, add 30 ml each of n-hexane, methanol and ethanol to the reaction liquid at a time, centrifuge at 10,000 r / min for 5 min, discard the supernatant, and repeat the above centrifugation operation for 3 times, the cleaned product was dried in a drying oven at 80°C for ...

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Abstract

The invention discloses a large-scale preparation method for a wurtzite Cu2ZnSnS4 nanocrystal, belonging to the field of photoelectric material new-energy technology. The method comprises the following steps: weighing a monovalent copper salt, a zinc salt and a tin salt, adding the monovalent copper salt, the zinc salt and the tin salt into a three-neck flask, adding oleylamine as a solvent and successively carrying out heating and cooling to room temperature; adding 1-dodecanethiol and carbon disulfide as sulfur sources, carrying out a reaction under heating and then carrying out cooling to room temperature; carrying out centrifugation and discarding supernatant; carrying out cleaning with a mixed solution of hexane, methanol and ethanol a plurality of times and collecting a precipitate; and drying the precipitate so as to obtain the wurtzite Cu2ZnSnS4 nanocrystal. The method provided by the invention is simple, great in output and high in yield and can produce plural grams of the wurtzite Cu2ZnSnS4 nanocrystal at a time; the output of the method at a time is one magnitude order higher than the output of conventional methods; and the prepared nanocrystal has an easily regulable atomic ratio, and an ideal wurtzite Cu2ZnSnS4 nanocrystal can be obtained by simply changing the ratio of a precursor.

Description

technical field [0001] The present invention relates to a kind of wurtzite Cu 2 ZnSnS 4 The invention relates to a method for preparing nanocrystals, which belongs to the technical field of photoelectric materials and new energy sources. Background technique [0002] Direct bandgap semiconductor material Cu 2 ZnSnS 4 (CZTS) has a bandgap width (about 1.5 eV) that matches the solar spectrum, a high light absorption coefficient (greater than 10 4 cm -1 ), the composition is non-toxic, and the earth’s crust is relatively rich in reserves, etc., and it is a material for the absorbing layer of thin-film solar cells with great development potential. CZTS mainly exists in three crystal structures of kesterite, kesterite and wurtzite. Compared with CZTS with kesterite and kesterite structures, CZTS with wurtzite structure has higher charge carriers. Concentration, low resistivity, and strong photoelectric response, thus attracting more and more attention from researchers. At ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G19/00B82Y40/00
CPCC01G19/006C01P2002/72C01P2002/78C01P2002/84C01P2004/04C01P2004/64C01P2006/40
Inventor 甘国友邹屏翰沈韬朱艳胡永茂
Owner KUNMING UNIV OF SCI & TECH
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