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Micron-sized spherical copper-zinc-tin-sulfur monocrystal particle preparation method

A technology of copper-zinc-tin-sulfur and single-crystal particles, which is applied in the manufacture of final products, sustainable manufacturing/processing, electrical components, etc., can solve the problems of difficult growth of large-size single crystals, large phase differences, and gaps, and achieve easy industrialization The effect of simple production and preparation equipment and low price

Active Publication Date: 2015-09-30
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, it is difficult to grow large-sized single crystals that meet the performance requirements of the solar cell absorber layer by traditional single crystal growth techniques (vapor phase transport technology, melting technology)

Method used

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  • Micron-sized spherical copper-zinc-tin-sulfur monocrystal particle preparation method
  • Micron-sized spherical copper-zinc-tin-sulfur monocrystal particle preparation method
  • Micron-sized spherical copper-zinc-tin-sulfur monocrystal particle preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0045] (1) Preparation of Cu by hydrothermal method 2 ZnSnS 4 Nanoparticles: 2 mmol CuCl 2 2H 2 O, 1 mmol ZnCl 2 , 1 mmol SnCl 4 ·5H 2 O was dissolved in 30mL deionized water and stirred for 10min to obtain clear solution A; 5 mmol 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 The turbid solution was stirred for 10 min to obtain a mixed solution, and the mixed solution was transferred into a 100ml polytetrafluoroethylene autoclave and placed in the autoclave at 180°C for 16 hours, then cooled to room temperature and deionized water and absolute ethanol were used at 8000r / min. Centrifuge and dry at 60°C for 8 hours to obtain a black sample, that is, CZTS nanoparticles.

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

Embodiment 2

[0048] Weigh the reaction raw materials 18 mmol CuS, 12 mmol ZnS, 10 mmol Sn powder, 10 mmol S powder and 50 mmol CsCl as a flux, and add 1 mmol CZTS nanoparticles prepared in step (1) of Example 1 and mix them thoroughly to make them Mix evenly; put the mixed sample after grinding into a quartz bottle, and use the vacuum pump unit to vacuum through the three-way valve to reach 10-10 2 Pa (can also be protected with 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 mixed samples in an ordinary heating furnace to heat from normal temperature to 850 Keep the temperature at ℃ for 72 hours, 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 ...

Embodiment 3

[0050] Weigh the reaction raw materials 18 mmol Cu, 12 mmol Zn, 10 mmol Sn powder, 40 mmol S powder and flux 80 mmol CsCl, and add 2 mmol CZTS nanoparticles prepared in step (1) of Example 1 and mix them thoroughly to make them Mix evenly; put the mixed sample after grinding into a quartz bottle, and use the vacuum pump unit to vacuum through the three-way valve to reach 10-10 2 Pa (can also be protected with 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 mixed samples in an ordinary heating furnace to heat from normal temperature to 850 Keep the temperature at ℃ for 72 hours, 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. It has become the most promising solar cell material at present. At present, 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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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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