Preparation method for micron-sized spherical CZTSSe monocrystalline particles

A technology of copper-zinc-tin-sulfur-selenium and single crystal particles, which can be used in final product manufacturing, sustainable manufacturing/processing, photovoltaic power generation, etc. and performance optimization difficulties, unfavorable performance of CZTSSe batteries, etc., to achieve the effects of easy industrial production, low price, and low pollution

Active Publication Date: 2015-10-14
LINGNAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This shows that the efficiency of CZTSSe thin film batteries still has a very large room for improvement; at the same time, compared with binary and ternary compound semiconductors, compound semiconductors such as CZTSSe have more complex physical properties due to the increase of constituent elements, so this kind of The preparation and performance optimization of high-efficiency thin film batteries of compounds have become more difficult; at the same time, the thermodynamically stable region of the CZTSSe phase is very small, and various impurity phases and metastable phases compete with CZTSSe. Therefore, in the preparation process of CZTSSe thin films, if the 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 CZTSSe cells; in the preparation of solar cells , the performance of single crystal CZTSSe is better than that of thin film CZTSSe. 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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  • Preparation method for micron-sized spherical CZTSSe monocrystalline particles
  • Preparation method for micron-sized spherical CZTSSe monocrystalline particles
  • Preparation method for micron-sized spherical CZTSSe monocrystalline particles

Examples

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Embodiment 1

[0043] (1) Preparation of Cu by hydrothermal method 2 ZnSnS 4 Nanoparticles: add 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 a clear solution A; 5 mmol thiourea was dissolved in 20ml deionized water and stirred for 10min to obtain a clear solution B; solution B was slowly added to solution A under stirring to obtain a white Turbid solution, stir for 10 min to obtain a mixed solution, transfer the mixed solution into a 100ml polytetrafluoroethylene autoclave and place the reaction kettle at 180℃ for 16h, cool to room temperature with deionized water and absolute ethanol at 8000r / min. Centrifugal separation at 60°C for 8 hours to obtain a black sample, namely CZTS nanoparticles.

[0044] (2) Preparation of copper zinc tin sulfur selenium single crystal particles by molten salt method: weigh 18 mmol CuS, 12 mmol ZnS, 10 mmol SnS, 10 mmol Se, 30 mmol CsCl and 20 mmol KI, and add 1 mmol step (1) ...

Embodiment 2

[0046] Weigh 18 mmol CuS, 12 mmol ZnS, 10 mmol Sn, 6 mmol S, 4 mmol Se, 50 mmol CsCl, and add 1 mmol of the CZTS nanoparticles prepared in step (1) of Example 1 and mix them thoroughly and mix them. Uniformity; the uniformly ground mixed sample is put into a quartz bottle, and the vacuum pump unit is used to vacuum through the three-way valve to reach 10-10 2 Pa (can also be protected by inert gas) to eliminate the influence of air on the molten salt reaction. Seal the quartz bottle with a hydrogen-oxygen flame; place the sealed quartz bottle with mixed samples in an ordinary heating furnace and heat it from room temperature to 800 Keep the temperature for 48 hours, then cool to about 600°C, take out the quartz bottle and quickly cool to room temperature (put it in water); take the sample out of the quartz bottle, remove the flux CsCl after repeated ultrasonic washing, and place the sample in a drying oven at 80°C After drying for 2 h, particles with crystal luster on the surfac...

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Abstract

The invention relates to the technical field of semiconductor photovoltaic materials and semiconductor devices, and discloses a preparation method for micron-sized spherical CZTSSe monocrystalline particles. Metal simple substance powder, sulfide powder, selenide powder, elemental sulfur powder, elemental selenium powder, flux, Cu2ZnSnS4 nanoparticles and as the like are combined as reaction raw materials, and are ground and mixed according to the designed formula. The powder mixture is vacuum-encapsulated into a quartz reactor; the quartz reactor is kept at the temperature of 750 DEG C to 1000 DEG C for 48-120 hours, and then is quickly cooled to the room temperature; and samples are taken out, cleaned and dried to obtain the CZTSSe monocrystalline particles. The size of the prepared monocrystalline particles can be regulated and controlled by utilizing recrystallization temperature and time, and the components of the particles can be effectively regulated within a certain range through the molar ratio of the elements in a precursor. The prepared monocrystalline particles are uniform and controllable in size, and are better than the monocrystalline particles prepared by the traditional method in performance.

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-selenide 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 sulfide selenide (CZTSSe) is considered to be the most promising replacement for copper indium gallium selenide Cu(In,Ga)Se 2 Novel compound semic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01L31/18H01L31/032
CPCH01L31/0326H01L31/18Y02E10/50Y02P70/50
Inventor 张军王闪闪邵乐喜黄春茂
Owner LINGNAN NORMAL UNIV
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