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Preparation method of wurtzite CMTS nano-crystal

A nanocrystal and wurtzite technology, which is applied in chemical instruments and methods, inorganic chemistry, manganese compounds, etc., can solve the problems of inaccurate temperature control of heating equipment, general powder properties, and difficult temperature control, and achieves an intuitive preparation process. Control, low cost, short time effect

Active Publication Date: 2018-06-29
KUNMING UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CMTS compounds have also been synthesized by various methods such as thermal injection, microwave irradiation, dip coating, and electrospinning. In the article RSC Advances, 2012, 2, 5044-5046, the author used thermal injection to prepare CMTS powder, however The process is complicated, and the diameter of the prepared powder is large and uneven, which is caused by inaccurate temperature control of the heating equipment. In the article J. Mater. Chem., 2012, 22, 23136, the author used solvothermal method to prepare samples, the test time is very long, and the equipment is complicated, and it also has the defect that the temperature is not easy to control, so that the properties of the obtained powder are also average

Method used

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  • Preparation method of wurtzite CMTS nano-crystal
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  • Preparation method of wurtzite CMTS nano-crystal

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Effect test

Embodiment 1

[0023] Embodiment 1: a kind of preparation method of wurtzite CMTS nanocrystal, concrete steps are as follows:

[0024] (1) According to the molar ratio of copper source, manganese source and tin source as 1.4:1:0.6, 14mmol cuprous iodide, 10mmol manganese acetate tetrahydrate, 6mmol tin chloride pentahydrate, 10mmol dodecylbenzene Sodium bicarbonate was added to 48mL organic solvent (the organic solvent was oleylamine) and dissolved, then placed in an oil bath and heated at a constant speed to 100°C to obtain a precursor solution;

[0025] (2) Under stirring conditions, add 16mL of n-dodecanemercaptan and carbon disulfide to the precursor solution obtained in step (1) and mix evenly, raise the temperature to 140°C for 60 minutes at a uniform rate, and then raise the temperature to 250°C for 60 minutes min to obtain the reaction system, cooled to room temperature, centrifuged to separate the solid and liquid, washed the solid three times with organic washing liquid, and dried ...

Embodiment 2

[0027] Embodiment 2: a kind of preparation method of wurtzite CMTS nanocrystal, concrete steps are as follows:

[0028] (1) According to the molar ratio of copper source, manganese source and tin source as 1.8:1:0.8, 18mmol cuprous chloride, 10mmol manganese acetate tetrahydrate, 8mmol tin iodide pentahydrate, 15mmol dodecylbenzene Na2O4 was added to 48mL of organic solvent (the organic solvent was oleic acid) and dissolved, then placed in an oil bath and heated at a constant speed to 120°C to obtain a precursor solution;

[0029] (2) Under stirring conditions, add 16mL of n-dodecanemercaptan and carbon disulfide in turn to the precursor solution obtained in step (1) and mix evenly, raise the temperature at a uniform rate to 160°C for 30 minutes, then raise the temperature to 280°C for 40 minutes min to obtain the reaction system, cooled to room temperature, centrifuged to separate the solid and liquid, washed the solid 4 times with an organic washing liquid, and dried at a te...

Embodiment 3

[0030] Embodiment 3: a kind of preparation method of wurtzite CMTS nanocrystal, concrete steps are as follows:

[0031](1) According to the molar ratio of copper source, manganese source and tin source as 2:1:1, add 20mmol cuprous iodide, 10mmol manganese sulfate, 10mmol tin disulfide and 18mmol sodium dodecylbenzoate to Dissolve in 48mL of organic solvent (the organic solvent is oleylamine), and then place it in an oil bath and raise the temperature to 110°C at a constant speed to obtain the precursor solution;

[0032] (2) Under stirring conditions, add 16 mL of n-dodecyl mercaptan and carbon disulfide in turn to the precursor solution obtained in step (1) and mix evenly, raise the temperature to 180°C for 15 minutes at a uniform rate, and then raise the temperature to 300°C for 30 minutes min to obtain the reaction system, cooled to room temperature, centrifuged to separate the solid and liquid, washed the solid 4 times with an organic washing liquid, and dried at a tempera...

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Abstract

The invention relates to a preparation method of a wurtzite CMTS nano-crystal and belongs to the new energy source technical field of photovoltaic materials and devices. The preparation method comprises the following steps: adding a copper source, a manganese source, a tin source and sodium dodecyl benzoate into an organic solvent and dissolving; then raising the temperature to 100 to 120 DEG C ata constant speed to obtain a precursor solution; sequentially adding n-dodecyl mercaptan and carbon disulfide into the precursor solution and uniformly mixing; raising the temperature to 140 to 180 DEG C at a constant speed and reacting for 15 to 60min; then raising the temperature to 250 to 300 DEG C at a constant speed and reacting for 30 to 60min to obtain a reaction system; cooling to room temperature; centrifuging to separate a solid and liquid; washing the solid for 3 to 5 times by adopting an organic washing solution and drying to obtain the wurtzite Cu2MnSnS4 nano-crystal. The wurtzite Cu2MnSnS4 nano-crystal prepared by the invention has the advantages of great production and high yield; the atom ratio of the nano-crystal is easy to regulate and control and the average grain diameter of the wurtzite Cu2MnSnS4 nano-crystal is a nano-grade.

Description

technical field [0001] The invention relates to a preparation method of wurtzite CMTS nanocrystals, belonging to the technical field of new energy sources of photovoltaic materials and devices. Background technique [0002] In recent years, energy crisis and environmental pollution have forced people to develop green and efficient technologies. Sulfide materials such as CuInSe, Cu 2 InGa(Se,S) 4 , CdTe, Bi 2 Te 3 , PbTe, etc. have been widely used in photoelectric, photocatalytic and thermoelectric fields. However, due to the limitations of the rarity of indium (In) and tellurium (Te) and the toxicity of cadmium (Cd), more and more attention has been paid to the development of rare-earth, cheap and environmentally friendly chalcogenide materials. As a new energy conversion material, Cu 2 ZnSnS 4 (CZTS) is very popular among researchers. Cu 2 MnSnS 4 (CMTS) has also been considered as a possible energy conversion material due to its structural similarity to CZTS. O...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/00
CPCC01G45/006C01P2002/72C01P2002/85C01P2002/84C01P2004/04
Inventor 沈韬李继强朱艳孙淑红
Owner KUNMING UNIV OF SCI & TECH
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