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Microwave-assisted solvothermal synthesis method of I-III-VI semiconductor material nano-powder

An auxiliary solvent, thermal synthesis technology, applied in nanotechnology, chemical instruments and methods, selenium/tellurium compounds, etc., can solve the problems of difficult to control product stoichiometric ratio, high reaction temperature, and high equipment requirements, and achieve strong reaction activation ability. , Reduce the reaction temperature, the effect of precise control of the stoichiometric ratio

Inactive Publication Date: 2011-11-23
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

The traditional solvothermal synthesis method has problems such as high equipment requirements, high reaction temperature, long time consumption, and difficult control of product stoichiometric ratio ([6] SeJin Ahn, KiHyun Kim, KyungHoon Yoon. Nanoparticle derived Cu(In, Ga)Se 2 absorberlayer for thin film solar cells,Colloids and Surfaces A[J].2008(313-314):171-174.)

Method used

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  • Microwave-assisted solvothermal synthesis method of I-III-VI semiconductor material nano-powder

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Experimental program
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Effect test

Embodiment 1

[0018] Embodiment 1: (CuIn 0.5 Ga 0.5 Se 2 Synthesis of powder)

[0019] with CuCl 2 2H 2 O, InCl 3 4H 2 O, GaCl 3 , Se powder as raw material, respectively weighed 0.17045g CuCl in molar ratio 1:0.5:0.5:2 2 2H 2 O, 0.146575 g InCl 3 4H 2 O, 0.08804 g GaCl 3 , 0.15792g Se powder, put into the microwave reactor, add ethylenediamine 20ml; close the reactor and put it into the microwave instrument, set the microwave parameters: heating power 400W, heating time 15min, reaction temperature 230℃, The reaction time is 120min. After the reaction is over, cool naturally to below 100°C, transfer the reaction solution from the microwave reactor to a centrifuge tube, carry out centrifugal washing and separation of the product, and wash it several times with distilled water and absolute ethanol. Dry in a vacuum oven at 80°C for 8 hours to obtain CuIn 0.5 Ga 0.5 Se 2 Nano powder. The sample was analyzed by XRD as pure CuIn 0.5 Ga 0.5 Se 2 , by SEM analysis, the powder pr...

Embodiment 2

[0020] Embodiment 2: (CuIn 0.7 Ga 0.3 Se 2 Synthesis of powder)

[0021] with CuCl 2 2H 2 O, InCl 3 4H 2 O, GaCl 3 , Se powder as raw material, respectively weighed 0.17045g CuCl according to the molar ratio of 1:0.3:0.7:2 2 2H 2 O, 0.087945 g InCl 3 4H 2 O, 0.123256 g GaCl 3, 0.15792g Se powder, put into the microwave reactor, add ethylenediamine 20ml; close the reactor and put it into the microwave instrument, set the microwave parameters: heating power 400W, heating time 15min, reaction temperature 230℃, The reaction time is 60min. After the reaction is over, cool naturally to below 100°C, transfer the reaction solution from the microwave reactor to a centrifuge tube, carry out centrifugal washing and separation of the product, and wash it several times with distilled water and absolute ethanol. Dry in a vacuum oven at 80°C for 8 hours to obtain CuIn 0.7 Ga 0.3 Se 2 Nano powder. The sample was analyzed by XRD as pure CuIn 0.3 Ga 0.7 Se 2 , by SEM analysi...

Embodiment 3

[0022] Embodiment 3: (CuInS 2 Synthesis of powder)

[0023] with CuCl 2 2H 2 O, InCl 3 4H 2 O, thiourea (CH 4 N 2 S) is raw material, weigh 0.17045g CuCl by molar ratio 1:1:2 2 2H 2 O, 0.29318g InCl 3 4H 2 O, 0.15224g thiourea, put into the microwave reactor, add 20ml of ethylene glycol; close the reactor and put it into the microwave instrument, set the microwave parameters: heating power 400W, heating time 10min, reaction temperature 190°C , The reaction time is 60min. After the reaction is over, cool naturally to below 100°C, transfer the reaction solution from the microwave reactor to a centrifuge tube, carry out centrifugal washing and separation of the product, and wash it several times with distilled water and absolute ethanol. Vacuum dry at 80°C for 8 hours in a vacuum oven to obtain CuInS 2 Nano powder. The sample was analyzed as CuInS by XRD 2 , according to SEM analysis, the powder particles are mainly composed of spherical and flake, and the particle ...

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Abstract

The invention discloses a microwave-assisted solvothermal synthesis method of I-III-VI semiconductor material nano-powder. The method comprises the following steps: adding metal salt and a sulfur source or selenium source into a beaker based on the mole ratio of an expected product, adding a solvent, evenly mixing and then transferring the obtained mixed solution to a microwave reaction kettle; after the reaction kettle is closed, heating the mixed solution to rated temperature in a microwave field, and performing heat preservation for rated time; and centrifugally washing the final product to obtain the target powder. In the method, the solvent is one or more of water, ethylenediamine, ethylene glycol, diamine and ethanol; the metal salt is the metal salt of Cu, In, Ga and Al; the sulfur source is thiourea or sulfur powder; and the selenium source is selenium powder or seleninic acid. The microwave-assisted solvothermal synthesis method has the beneficial effects that based on the heating and activation effect of the microwave field, reaction temperature is lowered and reaction time is shortened; and part of reaction that can not be made in the traditional high-pressure solvothermal synthesis process can be performed smoothly. The obtained semiconductor material nano-powder has the advantages of smaller grain size, pure phases, accurately controlled stoichiometric ratio of the phases and the like.

Description

technical field [0001] The invention relates to a microwave-assisted solvothermal synthesis method of I-III-VI semiconductor materials. The synthesized semiconductor materials can be used in solar cells, photoelectric sensors and other technical fields, especially widely used in CIS / CIGS thin films Solar cell absorber material. Background technique [0002] In recent years, the research and development of solar cells has been paid more and more attention, especially the development of thin-film solar cells with direct bandgap materials has become a new research hotspot. Because thin-film solar cells have the characteristics of less consumable materials and high photoelectric conversion, the cost of battery devices is greatly reduced. In the study of thin-film solar cells, Cu(In,Ga)Se 2 、CuInS 2 、CuInSe 2 , Cu(In, Ga)(Se, S) 2 、CuAlSe 2 、Cu(In,Al)Se 2 , Cu(In, Ga, Al)Se 2 Semiconductor materials such as semiconductors have very high light absorption coefficients and a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/00B82Y40/00
Inventor 龙飞邹正光谢春艳高洁
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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