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A preparation method of wurtzite copper-zinc-tin-sulfur particles with micro-nano composite structure

A micro-nano composite structure, copper-zinc-tin-sulfur technology, applied in chemical instruments and methods, tin compounds, inorganic chemistry, etc. The product yield needs to be improved, etc., to achieve the effects of intuitive and controllable preparation process, improved photoelectric conversion efficiency, and controllable components

Active Publication Date: 2017-09-22
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 both prepared wurtzite copper zinc tin sulfur nanocrystals by hot injection method, but the whole reaction The process needs inert gas protection, and the product yield needs to be improved
The literature Chem. Phys. Lett., 2014, 592, 144–148 uses direct heating to synthesize spindle-shaped wurtzite copper zinc tin sulfur. This structure is conducive to increasing the carrier concentration and improving electron transport, but this method requires First prepare acetylacetonate and then synthesize copper zinc tin sulfur, the process is complicated, and the solvent oleylamine used is expensive and highly toxic
Patent 105197985A discloses a method for the one-step synthesis of ultra-long wurtzite copper-zinc-tin-sulfur nanorods 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 the realization of efficient and rapid preparation
Moreover, the above-mentioned methods have failed to further construct a nanoscale structure on the surface of the copper-zinc-tin-sulfur particles, that is, the micro-nano composite structure of copper-zinc-tin-sulfur has not been formed.

Method used

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  • A preparation method of wurtzite copper-zinc-tin-sulfur particles with micro-nano composite structure
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  • A preparation method of wurtzite copper-zinc-tin-sulfur particles with micro-nano composite structure

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Embodiment 1

[0027] (1) Add 2mmol of copper chloride dihydrate, 1mmol of zinc acetate dihydrate, 1mmol of stannous chloride dihydrate and 4mmol of thiourea into 40ml of a mixed solvent of ethylene glycol and triethylenetetramine (volume ratio: 1:6), Use an ultrasonic cleaning machine with a frequency of 40KHz to sonicate for 1 hour to obtain the precursor solution;

[0028] (2) Heat the precursor solution to 120°C for 30 minutes, and then heat to 180°C for 4 hours. During the heating process, stir the reaction solution with a magnetic stirrer at a stirring speed of 500 rpm;

[0029] (3) Stop heating, and after the reaction system is cooled to room temperature, centrifuge the reaction solution at 10,000 rpm for 10 min, discard the upper layer, and centrifuge with absolute ethanol and distilled water at 8,000 rpm for 5 min, discard the upper layer, and repeat the centrifugation operation 5 times, and the cleaned product was dried in a drying oven at 60°C for 12 hours to obtain wurtzite coppe...

Embodiment 2

[0031] (1) Add 2mmol of copper chloride dihydrate, 1mmol of zinc acetate dihydrate, 1mmol of stannous chloride dihydrate and 5mmol of thiourea into 40ml of a mixed solvent of ethylene glycol and triethylenetetramine (volume ratio: 1:6), Use an ultrasonic cleaning machine with a frequency of 40KHz to sonicate for 2 h to obtain the precursor solution;

[0032] (2) Heat the precursor solution to 140°C for 30 minutes, and then heat to 190°C for 2 hours. During the heating process, stir the reaction solution with a magnetic stirrer at a stirring speed of 600rpm;

[0033] (3) Stop heating, and after the reaction system is cooled to room temperature, centrifuge the reaction solution at 10,000 rpm for 15 min, discard the upper layer, centrifuge with absolute ethanol and distilled water at 8,000 rpm for 5 min, discard the upper layer, and repeat centrifugation The operation was performed 4 times, and the cleaned product was dried in a drying oven at 80° C. for 8 hours to obtain wurtzit...

Embodiment 3

[0035] (1) Add 2mmol of copper chloride dihydrate, 1mmol of zinc acetate dihydrate, 1mmol of stannous chloride dihydrate and 6mmol of thiourea into 40ml of a mixed solvent of ethylene glycol and triethylenetetramine (volume ratio: 1:6), Obtain the precursor solution by ultrasonic cleaning with a frequency of 40KHz for 2h;

[0036] (2) Heat the precursor solution to 130°C for 30 minutes, and then heat to 200°C for 1 hour. During the heating process, stir the reaction solution with a magnetic stirrer at a stirring speed of 600 rpm;

[0037] (3) Stop heating, and after the reaction system is cooled to room temperature, centrifuge the reaction solution at 12000rpm for 10min, discard the upper layer, centrifuge with absolute ethanol and distilled water at 10000rpm for 10min, discard the upper layer, and repeat the centrifugation operation for 5 The second time, the cleaned product was dried in a drying oven at 70°C for 10 hours to obtain wurtzite copper-zinc-tin-sulfur particles wi...

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Abstract

The invention discloses a preparation method of wurtzite copper-zinc-tin-sulfur particles with a micro-nano composite structure, and belongs to the technical field of photoelectric material new energy. The method disclosed by the invention comprises the following steps of weighing divalent copper salt, zinc salt, tin salt and thiourea, and putting the weighed divalent copper salt, the weighed zinc salt, the weighed tin salt and the weighed thiourea to the bottom of a three-neck flask; adding a mixed solvent of ethylene glycol and triethylene tetramine, performing a two-step heating reaction, and performing cooling to room temperature; and performing centrifugal separation, abandoning a supernatant, then performing cleaning with anhydrous ethanol and distilled water many times, collecting precipitate, finally performing drying so as to obtain the wurtzite copper-zinc-tin-sulfur particles with the micro-nano composite structure. The preparation method of the wurtzite copper-zinc-tin-sulfur particles with the micro-nano composite structure disclosed by the invention is simple, the synthesis temperature is low, the cost of used precursor materials is low, the crystallinity of products is excellent, and the preparation method is suitable for batch synthesis.

Description

technical field [0001] The invention relates to a preparation method of wurtzite copper-zinc-tin-sulfur particles with a micro-nano composite structure, and belongs to the technical field of photoelectric materials and new energy sources. Background technique [0002] The direct bandgap semiconductor material CuZnSnS has a bandgap width matching the solar spectrum (about 1.5 eV), 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; copper-zinc-tin-sulfur mainly exists in three crystal structures of kesterite, kesterite and wurtzite Compared with kesterite and kesterite-structured copper-zinc-tin-sulfur, wurtzite-structured copper-zinc-tin-sulfur has higher carrier concentration, low resistivity, and strong photoelectric response, so the more increasingly attracted the att...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G19/00
CPCC01G19/00C01P2002/72C01P2002/84C01P2004/03C01P2004/50C01P2004/61C01P2004/62C01P2006/12
Inventor 朱艳青红梅沈韬黎振华胡永茂
Owner KUNMING UNIV OF SCI & TECH