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Method for preparing CuInS2 nanocrystals by using mother liquor through solvothermal process

A technology of solvothermal method and mother liquor, which is applied in the direction of nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, can solve the problems of large solvent discharge, unfavorable low-carbon environmental protection, etc., and reduce waste liquid discharge and treatment, high solid relative yield, and suitable band gap width

Inactive Publication Date: 2013-10-16
JIANGSU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, CuInS with high purity and good crystal form is prepared by a single solvent system. 2 It is still not easy to control; the amount of solvent emitted during the preparation process is large, which is not conducive to low-carbon environmental protection

Method used

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  • Method for preparing CuInS2 nanocrystals by using mother liquor through solvothermal process
  • Method for preparing CuInS2 nanocrystals by using mother liquor through solvothermal process
  • Method for preparing CuInS2 nanocrystals by using mother liquor through solvothermal process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1) Weigh 0.4651g CuCl with an analytical balance 2 2H 2 O, 0.8000g InCl 3 4H 2 O, 0.5192gCH 4 N 2 S, successively placed in 40ml N,N-dimethylformamide (DMF), stirred to fully dissolve it, and a yellow clear solution was obtained. where n(CuCl 2 2H 2 O):n(InCl 3 4H 2 O):n(CH 4 N 2 S)=1︰1︰2.5.

[0023] 2) Measure 40ml of ethylene glycol (EG) and slowly pour it into the solution in step 1), stir to disperse it evenly, and obtain a colorless and clear solution. Add concentrated hydrochloric acid to adjust the pH of the system to 2-3.

[0024] 3) Transfer the mixed solution in step 2) into a polytetrafluoroethylene-lined autoclave with a volume of 100mL and seal it, react at 190°C for 12h, and then cool down to room temperature naturally.

[0025] 4) Centrifuge the reaction feed liquid in step 3) in an electric centrifuge for 15 minutes at a speed of 3000 r / min, then pour out the upper layer and clear it for later use. The samples were washed several times with...

Embodiment 2

[0027] 1) Weigh 0.4651g CuCl with an analytical balance 2 2H 2 O, 0.8000g InCl 3 4H 2 O, 0.5192gCH 4 N 2 S, sequentially placed in the first solid-liquid separation mother liquor in Example 1, stirred to make it evenly dispersed.

[0028] 2) Add concentrated hydrochloric acid to the mixed solution in step 1) to adjust the pH of the system to 2-3.

[0029] 3) Transfer the mixed solution in step 2) into a polytetrafluoroethylene-lined autoclave with a volume of 100mL and seal it, react at 190°C for 12h, and then cool down to room temperature naturally.

[0030] 4) Centrifuge the reaction feed liquid in step 3) in an electric centrifuge for 15 minutes at a speed of 3000 r / min, then pour out the upper layer and clear it for later use. The samples were washed several times with absolute ethanol and deionized water. The obtained product was dried in a vacuum oven at 60° C. for 6 hours, and a sample was taken out to obtain a black solid powder, which was weighed and packaged. ...

Embodiment 3

[0032] 1) Weigh 0.4651g CuCl with an analytical balance 2 2H 2 O, 0.8000g InCl 3 4H 2 O, 0.5192gCH 4 N 2 S, sequentially placed in the first solid-liquid separation mother liquor in Example 2, stirred to make it evenly dispersed.

[0033] 2) Add concentrated hydrochloric acid to the mixed solution in step 1) to adjust the pH of the system to 2-3.

[0034] 3) Transfer the mixed solution in step 2) into a polytetrafluoroethylene-lined autoclave with a volume of 100mL and seal it, react at 190°C for 12h, and then cool down to room temperature naturally.

[0035] 4) Centrifuge the reaction feed liquid in step 3) in an electric centrifuge for 15 minutes at a speed of 3000 r / min, then pour out the upper layer and clear it for later use. The samples were washed several times with absolute ethanol and deionized water. The obtained product was dried in a vacuum oven at 60° C. for 6 hours, and a sample was taken out to obtain a black solid powder, which was weighed and packaged. ...

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Abstract

The invention discloses a method for preparing CuInS2 nanocrystals by using a mother liquor through a solvothermal process. The method comprises the following steps: 1, sequentially dissolving a Cu element source, an In element source and an S element source in a solvent, and stirring to obtain a clear solution; 2, transferring the clear solution to a pressure container for a reaction, and naturally cooling to room temperature after reaction ending; and 3, centrifuging products obtained in step 2, washing, and carrying out vacuum drying to obtain target products, wherein the solvent is one of or a mixture of N,N-dimethyl formamide and glycol. The method adopting the solvothermal process is cheap and convenient; the prepared nanocrystals have a uniform nanosheet structure, a high solid yield and a good optical absorption property; and the prepared CuInS2 nanocrystals have a highest optical absorption coefficient of 10<5> order of magnitude and a forbidden band width reaching 1.41eV, and the atom stoichiometric ratio of Cu:In:S is 1:0.89:1.93 and tends to a standard stoichiometric ratio of 1:1:2.

Description

technical field [0001] The invention belongs to the field of photovoltaic materials, in particular to ternary compound semiconductor nanopowder CuInS 2 Preparation methods of nanocrystalline materials. Background technique [0002] I-III-VI 2 Type semiconductor compounds are key materials for photovoltaic cells, especially CuInS 2 It has attracted widespread attention because of its excellent comprehensive performance. Its advantages are: the band gap is 1.5eV, which is close to the optimal band gap of solar cells (1.45eV); the absorption coefficient is large (10 5 ), as the light absorbing layer of solar cells, the thickness is only 1-2 μm, which reduces the amount of raw materials; it has good stability to heat and electricity; it is compatible with CdTe, PbS, CuInSe 2 Compared with other solar cell materials such as CuInS 2 Does not contain any toxic ingredients, environmentally friendly and safe. But currently CuInS 2 The laboratory photoelectric conversion effici...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G15/00B82Y30/00B82Y40/00
Inventor 高延敏赵琴
Owner JIANGSU UNIV OF SCI & TECH
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