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Diffusion Couple Method for Determination of Copper-Zinc-Sn-Sulphur Phase Transition in Synthetic Optoelectronic Materials

A technology of copper-zinc-tin-sulfur and optoelectronic materials, which is applied in the preparation of test samples, etc., can solve problems such as phase transition research difficulties, complex ternary systems, etc., and achieve the effects of wide application range, simple process and high efficiency

Active Publication Date: 2018-03-23
NANJING INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the ternary system, it is relatively complicated, and some even have to prepare hundreds or even tens of thousands of alloy samples to accurately determine the phase transition of the system, which brings difficulties to the study of phase transition

Method used

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  • Diffusion Couple Method for Determination of Copper-Zinc-Sn-Sulphur Phase Transition in Synthetic Optoelectronic Materials
  • Diffusion Couple Method for Determination of Copper-Zinc-Sn-Sulphur Phase Transition in Synthetic Optoelectronic Materials
  • Diffusion Couple Method for Determination of Copper-Zinc-Sn-Sulphur Phase Transition in Synthetic Optoelectronic Materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Preparation of diffusion couple for 500°C phase transition of Cu-Zn-S system. like figure 1 Firstly, after polishing off the oxide layer on the surface of 99.99wt% Cu sheet with W50 metallographic sandpaper, the surface is cleaned and dried, then the copper sheet is put into a ceramic boat, and 99.99wt% S powder is covered around the copper sheet, In the OTF-1200X vacuum vulcanization furnace, argon protection was carried out at 600°C for 1 hour to synthesize high-purity Cu 2 S powder.

[0041] Mix 99.9wt% Zn powder and 99.99wt% S powder at a stoichiometric ratio of 1:1, and mix evenly; use a manual desktop powder press to press the mixed powder into a 10mm×10mm×5mm square; put the square sample into a ceramic boat In this method, the sample was covered with 99.99wt% S powder, and reacted at 800 °C under argon protection for 1 h in an OTF-1200X vacuum vulcanization furnace to synthesize high-purity solid block ZnS.

[0042] will synthesize high-purity Cu 2 S powder ...

Embodiment 2

[0046] Preparation of diffusion couple for 500°C phase transition of Cu-Sn-S system. First, after polishing the oxide layer on the surface of the 99.99wt% Cu sheet with W50 metallographic sandpaper, the surface was cleaned and dried, and then the copper sheet was put into a ceramic boat, and 99.99wt% S powder was covered around the copper sheet. In the OTF-1200X vacuum vulcanization furnace, use argon as a protective gas at 600°C for 1 hour to synthesize high-purity Cu 2 S powder.

[0047] Mix 99.9wt% Sn powder and 99.99wt% S powder according to the stoichiometric ratio of 1:2, and mix evenly; use a manual desktop powder tablet press to press the mixed powder into a 10mm×10mm×5mm square; put the tablet sample into In a ceramic boat, the sample is covered with 99.99wt% S powder, and reacted at 550°C for 1h under the protection of argon in an OTF-1200X vacuum vulcanization furnace to synthesize high-purity SnS 2 .

[0048] The synthesized high-purity Cu 2 S powder is pressed...

Embodiment 3

[0053] Preparation of diffusion couple for 500°C phase transition of Sn-Zn-S system. First, mix 99.9wt% Zn powder and 99.99wt% S powder according to the stoichiometric ratio of 1:1, and mix evenly; use a manual desktop powder tablet press to press the mixed powder into a 10mm×10mm×5mm square, and put the square sample into the ceramic In the boat, the sample was covered with 99.99wt% S powder, and reacted at 800°C for 1 hour in an OTF-1200X vacuum vulcanization furnace under the protection of argon to synthesize high-purity ZnS.

[0054] Mix 99.9wt% Sn powder and 99.99wt% S powder according to the stoichiometric ratio of 1:2, and mix evenly; use a manual desktop powder tablet press to press the mixed powder into a 10mm×10mm×5mm square; put the tablet sample into In a ceramic boat, the sample is covered with 99.99wt% S powder, and reacted at 550°C under argon protection in an OTF-1200X vacuum vulcanization furnace for 1 hour to synthesize high-purity SnS 2 .

[0055] Synthesi...

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Abstract

The invention provides a diffusion couple method for the determination of the copper-zinc-tin-sulfur phase transition of synthetic photoelectric materials. High-purity Cu, Zn, and Sn are vulcanized at different temperatures in a sulfur atmosphere to obtain sulfide powders; the sulfides are respectively loaded into tantalum The mold is sintered into solid massive binary sulfides in a vacuum diffusion welding furnace, pressurized at 20MPa, and the sintering temperature is 100-200°C below the melting point of each compound; the surface of solid massive Cu2S, ZnS, SnS2 is ground, and the metallographic The sandpaper is further polished, then polished, and the polished surface is placed in contact with a high-temperature-resistant tantalum mold for vacuum diffusion welding to form a diffusion couple. During welding, the pressure is 20MPa, and the pressed diffusion couple is placed in a vacuum-sealed quartz tube. Diffusion annealing was carried out at ℃ for 480 hours, followed by water quenching. This method can be used to determine the phase transition of Cu-Zn-Sn-S system at 500 °C. Moreover, the process is simple, the cost is low, the operation is easy, and the application range is wide.

Description

technical field [0001] The invention relates to a diffusion couple method for measuring the copper-zinc-tin-sulfur phase transition of a synthesized photoelectric material. Background technique [0002] At present, in the face of serious problems such as energy shortage and environmental pollution, energy saving and emission reduction, and the development of new environmentally friendly solar cells are current research hotspots. Cu 2 ZnSnS 4 (CZTS) is a direct bandgap semiconductor with a large light absorption coefficient. A thin film of a few microns can be used as the absorbing layer. The band gap is 1.45-1.6eV, which matches the solar spectrum very well. The theoretical conversion efficiency of CZTS solar cells is about 32%. The element reserves are abundant without any environmental hazards. In the CZTS film, the ratio of Cu / (Zn+Sn) and Zn / Sn directly affects the existence of the intermediate compound phase in the CZTS film, and the existence of defects such as the i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/28
Inventor 贺显聪王章忠皮锦红位浩邹高鹏
Owner NANJING INST OF TECH