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Preparation method of copper zinc tin sulfide nanocrystal with custerite structure

A copper-zinc-tin-sulfur and kesterite technology, which is applied in the fields of nanotechnology, nanotechnology, and nanotechnology for materials and surface science, can solve the problem of fast reaction speed, nanocrystal agglomeration, and difficulty in controlling nanocrystal nucleation. and growth problems, to achieve high production efficiency, reduce agglomeration, reduce the formation of binary and ternary compound chalcogenide heterophase

Inactive Publication Date: 2016-01-20
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It has been reported that the high-temperature reaction of metal salts with elemental sulfur (S) usually leads to the formation of thermodynamically stable kesterite CZTS nanocrystals, however, it is difficult to control the nucleation of nanocrystals due to the fast reaction rate of sulfur with oleylamine precursors. and growth, easily lead to the aggregation of nanocrystals, and the formation of binary and ternary compounds chalcogenide heterogeneous compounds

Method used

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  • Preparation method of copper zinc tin sulfide nanocrystal with custerite structure
  • Preparation method of copper zinc tin sulfide nanocrystal with custerite structure
  • Preparation method of copper zinc tin sulfide nanocrystal with custerite structure

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Embodiment 1

[0026] In this embodiment, the method for preparing copper-zinc-tin-sulfur nanocrystals with kesterite structure, the steps are as follows:

[0027] 1) Weigh 0.523g (2mmol) of copper acetylacetonate, 0.220g (1mmol) of zinc acetate and 0.225g (1mmol) of tin dichloride, put them into a three-necked flask, then add 8mL of oleylamine solvent, press 10 Raise the temperature to 100°C at a heating rate of ℃ / min, stir magnetically at a speed of 500rpm and vacuumize to remove water and oxygen for 30 minutes to obtain a stable metal-ligand complex solution;

[0028] 2) Add 0.128g (4mmol) of sulfur powder into 4mL of oleylamine solvent and ultrasonically disperse to form a transparent S-OLA solution, then add 0.32mL of DDT to prepare the S-OLA-DDT sulfur source precursor;

[0029] 3) Heat the metal-ligand complex solution prepared in step 1) to 150°C under argon, and then quickly inject the S-OLA-DDT sulfur source precursor obtained in step 2) into the metal In the ligand complex soluti...

Embodiment 2

[0033] In this embodiment, the method for preparing copper-zinc-tin-sulfur nanocrystals with kesterite structure, the steps are as follows:

[0034] 1) Weigh 0.523g (2mmol) of copper acetylacetonate, 0.220g (1mmol) of zinc acetate and 0.225g (1mmol) of tin dichloride, put them into a three-necked flask, then add 10mL of oleylamine (OLA) solvent , the temperature was raised to 120°C at a heating rate of 20°C / min, magnetically stirred at a speed of 700rpm and vacuumed to remove water and oxygen for 30min to obtain a stable metal-ligand complex solution;

[0035] 2) Add 0.128g (5mmol) of sulfur powder into 4mL of oleylamine solvent and ultrasonically disperse to form a transparent S-OLA solution, then add 0.4mL of dodecanethiol (DDT) to prepare the sulfur source precursor;

[0036] 3) Heating the metal-ligand complex solution prepared in step 1) to 160°C under argon gas, and then quickly injecting the sulfur source precursor obtained in step 2) into the metal-ligand complex solut...

Embodiment 3

[0040] In this embodiment, the method for preparing copper-zinc-tin-sulfur nanocrystals with kesterite structure, the steps are as follows:

[0041] 1) Weigh 0.523g (2mmol) of copper acetylacetonate, 0.220g (1mmol) of zinc acetate and 0.225g (1mmol) of tin dichloride, put them into a three-necked flask, then add 12mL of oleylamine (OLA) solvent , the temperature was raised to 130°C at a heating rate of 30°C / min, magnetically stirred at a speed of 800rpm and vacuumed to remove water and oxygen for 30min to obtain a stable metal-ligand complex solution;

[0042] 2) Add 0.128g (6mmol) of sulfur powder into 4mL of oleylamine solvent and ultrasonically disperse to form a transparent S-OLA solution, then add 0.5mL of dodecanethiol (DDT) to prepare the sulfur source precursor;

[0043] 3) Add the metal-ligand complex solution prepared in step 1) to 170°C under argon, and then quickly inject the sulfur source precursor obtained in step 2) into the metal-ligand complex solution prepare...

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Abstract

The invention relates to a preparation method of a copper zinc tin sulfide nanocrystal with a custerite structure. The method includes the following steps: 1) adding copper salt, zinc salt and tin salt into a reactor after weigh the salts, adding oleylamine solvent and stirring the mixture fully to obtain a metal ligand complex solution; 2) adding sulfur powder into the oleylamine solvent, performing ultrasonic dispersion to form a sulfur-oleylamine solution, and then adding 1-dodecanethiol to obtain a sulfur-source precursor; 3) heating the metal ligand complex solution to the temperature of 150-200 DEG C in the presence of argon, injecting the sulfur-source precursor rapidly, mixing the mixture to obtain a sulfur-based metal complex solution, heating the complex solution to the temperature of 240-280 DEG C and reacting for 0.5-1 hour to obtain a copper zinc tin sulfide nanocrystal; and 4) adding the copper zinc tin sulfide nanocrystal into ethanol, performing centrifugal separation to obtain a precipitate, washing the prepared precipitate with the mixed liquor containing n-hexane and ethanol in a centrifugal manner, drying the prepared solid to obtain the copper zinc tin sulfide nanocrystal with the custerite structure.

Description

technical field [0001] The invention belongs to the technical field of solar photovoltaic material preparation, and in particular relates to a method for preparing copper-zinc-tin-sulfur nanocrystals with a kesterite structure. Background technique [0002] In recent years, the application of solar energy has entered a period of rapid development and has become the most dynamic research field. Among many solar cells, thin-film solar cells are the first of the three key funding projects for new energy photovoltaic power generation in the country's "Twelfth Five-Year Plan". At present, compound thin film solar cells have been greatly developed, and the fastest growing one is Cu(In,Ga)Se 2 (CIGS) battery, but encountered problems such as high cost, rare metal raw materials and environmental pollution in the development process, and Cu 2 ZnSnS 4 Quaternary semiconductors are very likely to become the next generation of absorbing layer materials for thin-film solar cells with ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G19/00B82Y30/00B82Y40/00
CPCC01G19/006C01P2002/72C01P2002/80C01P2004/04C01P2004/64
Inventor 夏冬林周斌王友法
Owner WUHAN UNIV OF TECH
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