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A preparation method of micron-scale spherical copper-zinc-tin-sulfur single crystal particles and its single crystal particles and application

A copper-zinc-tin-sulfur, single crystal particle technology, applied in the direction of final product manufacturing, sustainable manufacturing/processing, electrical components, etc. The effect of simple production and preparation equipment and low price

Active Publication Date: 2016-09-14
LINGNAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the highest efficiency of CZTS-based solar cells can reach 12.7%, but according to theoretical calculations, the limit conversion efficiency of single-junction CZTS thin-film cells can reach 30%, which is quite different, even compared with the current highest conversion efficiency of CIGS of 21.7%. , there is also a big difference
This shows that the efficiency of CZTS thin-film batteries still has a very large room for improvement; at the same time, compared with binary and ternary compound semiconductors, CZTS and other quaternary compound semiconductors have more complex physical properties due to the increase in constituent elements, making them The preparation and performance optimization of quaternary compound high-efficiency thin-film batteries have become more difficult; at the same time, the thermodynamically stable region of the CZTS phase is very small, and various impurity phases and metastable phases compete with CZTS. Therefore, during the preparation of CZTS thin films, if there is no To achieve effective component control, due to the volatilization of some elements, the deviation from the stoichiometric ratio is easily accompanied by various binary and ternary heterophases and some metastable phases, which will eventually have an adverse effect on the performance of CZTS batteries; in the preparation of solar energy For solar cells, single crystal CZTS has better performance than thin film CZTS. However, traditional single crystal growth techniques (vapor phase transport technology, melting technology) are difficult to grow large-sized single crystals that meet the performance requirements of the solar cell absorber layer.

Method used

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  • A preparation method of micron-scale spherical copper-zinc-tin-sulfur single crystal particles and its single crystal particles and application
  • A preparation method of micron-scale spherical copper-zinc-tin-sulfur single crystal particles and its single crystal particles and application
  • A preparation method of micron-scale spherical copper-zinc-tin-sulfur single crystal particles and its single crystal particles and application

Examples

Experimental program
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Effect test

Embodiment 1

[0045] (1) Preparation of Cu by hydrothermal method 2 ZnSnS 4 Nanoparticles: 2mmol CuCl 2 2H 2 O, 1mmol ZnCl 2 , 1mmol SnCl 4 ·5H 2 O was dissolved in 30mL deionized water and stirred for 10min to obtain clear solution A; 5mmol thiourea was dissolved in 20ml deionized water and stirred for 10min to obtain clear solution B; solution B was slowly added to solution A under stirring to obtain white turbidity solution, stirred for 10min to obtain a mixed solution, moved the mixed solution into a 100ml polytetrafluoroethylene autoclave and placed the autoclave at 180°C for 16h, cooled to room temperature and centrifuged at 8000r / min with deionized water and absolute ethanol respectively Separate and dry at 60°C for 8 hours to obtain a black sample, namely CZTS nanoparticles.

[0046] (2) Preparation of Cu by molten salt method 2 ZnSnS 4 Micron single crystal particles: Weigh 18mmol of CuS, 12mmol of ZnS, 10mmol of SnS and 50mmol of CsCl as the flux, add 1mmol of CZTS nanopar...

Embodiment 2

[0048] Weigh the reaction raw materials 18mmol CuS, 12mmol ZnS, 10mmol Sn powder, 10mmol S powder and fluxing agent 50mmol CsCl, and add 1mmol of the CZTS nanoparticles prepared in the step (1) of Example 1 and mix them thoroughly to make them mix uniformly; The homogeneous mixed sample is put into a quartz bottle, and the vacuum is evacuated by a vacuum pump unit through a three-way valve to reach 10-10 2 Pa (can also be protected with an inert gas), so as to eliminate the influence of air on the molten salt reaction, seal the quartz bottle with an oxyhydrogen flame; place the sealed quartz bottle with the mixed sample in an ordinary heating furnace and heat it from normal temperature to 850 Keep the temperature at ℃ for 72h, then cool down to about 600℃, take out the quartz bottle and quickly cool it down to room temperature (put it in water); finally take out the sample in the quartz bottle, wash it with ultrasonic water several times to remove the flux CsCl, and then put th...

Embodiment 3

[0050] Weigh the reaction raw materials 18mmol Cu, 12mmol Zn, 10mmol Sn powder, 40mmol S powder and flux 80mmol CsCl, and add 2mmol embodiment 1 step (1) to prepare CZTS nanoparticles and mix them thoroughly to make them mix evenly; The final mixed sample is put into a quartz bottle, and the vacuum is evacuated by a vacuum pump unit through a three-way valve to reach 10-10 2 Pa (can also be protected with an inert gas), so as to eliminate the influence of air on the molten salt reaction, seal the quartz bottle with an oxyhydrogen flame; place the sealed quartz bottle with the mixed sample in an ordinary heating furnace and heat it from normal temperature to 850 Keep the temperature at ℃ for 72h, then cool down to about 600℃, take out the quartz bottle and quickly cool it down to room temperature (put it in water); finally take out the sample in the quartz bottle, wash it with ultrasonic water several times to remove the flux CsCl, and then put the sample in a drying oven for 80...

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Abstract

The invention relates to the technical field of semiconductor photoelectric materials and devices and discloses a micron-sized spherical copper-zinc-tin-sulfur monocrystal particle preparation method. The method includes: grinding and mixing different combinations of metal powder, sulfides, elemental sulfur powder, fluxing agents, copper-zinc-tin-sulfur nano particles and the like according to designed proportions, packaging mixed powder in a quartz reaction vessel in a vacuum manner, keeping the quartz reaction vessel at the temperature of 750-1000 DEG C for 48-120h, and quickly cooling the quartz reaction vessel to the room temperature; taking out a sample, and washing and drying to obtain copper-zinc-tin-sulfur monocrystal particles; the prepared monocrystal particles are adjustable in size by means of recrystallization temperature and time, and ingredients of the particles can be effectively regulated within a certain range through a molar ratio of elements in a precursor. The prepared monocrystal particles are uniform in ingredient and controllable in size so as to be superior to those prepared according to traditional methods.

Description

technical field [0001] The invention relates to the technical field of semiconductor optoelectronic materials and devices, more specifically, to a method for preparing micron-sized spherical copper-zinc-tin-sulfur single crystal particles. Background technique [0002] Multi-component CuInGaSe 2 (CIGS) thin-film solar cell has high conversion efficiency and is easy to mass-produce, and has become the most promising solar cell material at present. Currently, CIGS cell is the thin-film solar cell with the highest photoelectric conversion efficiency in the world, and its highest conversion efficiency has been up to 21.7%. However, its constituent elements In and Ga are scarce on the earth, making it difficult for CIGS thin-film batteries to achieve TW (10 9 kW) level of large-scale applications. [0003] Copper-zinc-tin-sulfur (CZTS) quaternary compound semiconductors are considered to be the most promising alternatives to Cu(In,Ga)Se 2 Novel compound semiconductors for the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01L31/18H01L31/0296
CPCH01L31/0296H01L31/18Y02P70/50
Inventor 张军王闪闪邵乐喜黄春茂
Owner LINGNAN NORMAL UNIV
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