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A kind of preparation method of sheet-stacked molybdenum disulfide nanotubes

A molybdenum disulfide and nanotube technology, which is applied in the field of transition metal compound material preparation, can solve the problems of large volume expansion, poor electrical conductivity, and limit the practical application of molybdenum disulfide materials, and achieves the effect of simple method and easy operation.

Inactive Publication Date: 2019-06-25
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to its own poor electrical conductivity, large volume expansion during lithium storage, and insufficient electrochemically active sites in hydrogen evolution reaction, the practical application of molybdenum disulfide materials is greatly limited.

Method used

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  • A kind of preparation method of sheet-stacked molybdenum disulfide nanotubes
  • A kind of preparation method of sheet-stacked molybdenum disulfide nanotubes
  • A kind of preparation method of sheet-stacked molybdenum disulfide nanotubes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Add 1.21g sodium molybdate and 0.6g sodium chloride to 60mL deionized water to obtain a solution, continue stirring for 10min to obtain a uniform dispersion, add 3mol / L hydrochloric acid solution to adjust the pH value to 1, and transfer to a hydrothermal kettle The hydrothermal reaction was carried out in an oven, the reaction temperature was 180°C, and the reaction time was 24 hours. After the reaction kettle was cooled to room temperature, the obtained dispersion was subjected to suction filtration to separate the light blue precipitate, and the obtained solid was washed with deionized water. , dried in an oven at 60° C. for 24 hours to obtain molybdenum oxide nanobelts.

[0025] (2) Weigh 20 mg of molybdenum oxide nanobelts and 100 mg of sulfur powder in step (1), grind them in agate, mix them evenly, and add them to a porcelain ark with a length of 6 cm and a width of 3 cm. The tube furnace is vulcanized at high temperature, the protective gas is nitrogen, the ...

Embodiment 2

[0030] (1) Add 1.21g sodium molybdate and 1.21g sodium chloride to 40mL deionized water to obtain a solution, continue stirring for 10min to obtain a uniform dispersion, add 3mol / L hydrochloric acid solution to adjust the pH value to 1.5, and transfer to a hydrothermal kettle The hydrothermal reaction was carried out in an oven, the reaction temperature was 190°C, and the reaction time was 20h. After the reaction kettle was cooled to room temperature, the obtained dispersion liquid was subjected to suction filtration to separate the light blue precipitate, and the obtained solid was washed with deionized water. , dried in an oven at 60° C. for 24 hours to obtain molybdenum oxide nanobelts.

[0031] (2) Weigh 20 mg of molybdenum oxide nanobelts and 80 mg of sulfur powder in step (1), grind them in agate, mix them evenly, and add them to a porcelain ark with a length of 6 cm and a width of 3 cm. The tube furnace is vulcanized at high temperature, the protective gas is argon, the...

Embodiment 3

[0033] (1) Add 0.6g sodium molybdate and 1.2g sodium chloride to 12mL deionized water to obtain a solution, continue stirring for 10min to obtain a uniform dispersion, add 3mol / L hydrochloric acid solution to adjust the pH value to 0.5, and transfer to a hydrothermal kettle The hydrothermal reaction was carried out in an oven, the reaction temperature was 200°C, and the reaction time was 18 hours. After the reaction kettle was cooled to room temperature, the obtained dispersion was subjected to suction filtration to separate the light blue precipitate, and the obtained solid was washed with deionized water. , dried in an oven at 60° C. for 24 hours to obtain molybdenum oxide nanobelts.

[0034] (2) Weigh 20 mg of molybdenum oxide nanobelts and 100 mg of sulfur powder in step (1), grind them in agate, mix them evenly, and add them to a porcelain ark with a length of 6 cm and a width of 3 cm. The tube furnace is vulcanized at high temperature, the protective gas is nitrogen, the...

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Abstract

The invention relates to a preparation method for a sheet-stacked molybdenum disulfide nanotube. The preparation method comprises the following steps: dissolving a molybdenum source and sodium chloride in a solvent, carrying out a hydrothermal reaction under stirring, then carrying out cooling, vacuum filtering, washing and drying so as to obtain a molybdenum oxide nanobelt, mixing the molybdenumoxide nanobelt with a sulfur source, carrying out grinding, then carrying out vulcanizing under protective gas, and carrying out washing, vacuum filtering and drying. The preparation method provided by the invention is simple and highly-efficient, facilitates operation, is an effective and rapid preparation method, and has the prospect of large-scale preparation; and the sheet-stacked molybdenum disulfide nanotube prepared by using the preparation method provided by the invention has a structure that molybdenum disulfide is shown as an ultrathin nanosheet and can be self-assembled into a three-dimensional nanotube, and the structure facilitates complete exposure of active sites of molybdenum disulfide.

Description

technical field [0001] The invention belongs to the field of preparation of transition metal compound materials, in particular to a method for preparing sheet-stacked molybdenum disulfide nanotubes. Background technique [0002] As a typical transition metal sulfide, molybdenum disulfide has a graphene-like layered structure, and its structural unit is composed of three layers of atoms to form a sandwich-like layered structure. Each molybdenum atom is in the center of a triangular prism and is connected with six The sulfur atoms are coordinated in the form of covalent bonds, and the weak van der Waals force between the layers is conducive to the intercalation and deintercalation of Li+. At the same time, molybdenum disulfide also has good electric double layer charge storage capacity, so it has a high theoretical value. Lithium storage capacity, as a lithium-ion battery anode material has a good application prospect. Meanwhile, due to its preferentially exposed active sites...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G39/06B82Y40/00
CPCB82Y40/00C01G39/06C01P2002/72C01P2004/03C01P2004/04C01P2004/13
Inventor 张超刘颖刘天西刘思良王开周俊杨静
Owner DONGHUA UNIV
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