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Method for preparing MoS2 microspheres by solvent hot method

A solvothermal method and microsphere technology, applied in the direction of molybdenum sulfide, can solve problems such as unfavorable large-scale production and application, harsh production conditions, high synthesis temperature, etc., and achieve high product yield and purity, low preparation cost, and reaction mild conditions

Inactive Publication Date: 2010-10-06
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above method has disadvantages such as high synthesis temperature, harsh production conditions, complicated process and high cost, which is not conducive to large-scale production and application.

Method used

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  • Method for preparing MoS2 microspheres by solvent hot method
  • Method for preparing MoS2 microspheres by solvent hot method
  • Method for preparing MoS2 microspheres by solvent hot method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 0.002mol of sodium molybdate and 0.0045mol of thiourea and mix them in 50mL of ethylene glycol, fully stir and ultrasonically treat for 3 minutes, transfer the mixture to an autoclave, react at a constant temperature of 160°C for 24 hours, and then cool naturally. Wash twice with deionized water and absolute ethanol, and dry at 90 °C to obtain black MoS 2 Microspheres.

[0021] figure 1 is the resulting MoS 2 The XRD pattern of microspheres, compared with the standard card, it can be seen that the synthesized material is pure phase MoS 2 crystal material.

Embodiment 2

[0023] Weigh 0.005mol of ammonium paramolybdate and 0.07mol of thiourea and mix them in 60mL of glycerol, fully stir and ultrasonically treat for 5 minutes, transfer the mixture to an autoclave, react at a constant temperature of 180°C for 18 hours, and then cool naturally , washed three times with deionized water and absolute ethanol, and dried at 90 °C to obtain black MoS 2 Microspheres.

[0024] figure 2 is the resulting MoS 2 The SEM image of the microsphere, it can be seen from the figure that the obtained material is a uniform microsphere, and its particle size is about 1um.

Embodiment 3

[0026] Weigh 0.002mol of ammonium molybdate and 0.002mol of sodium thiosulfate and mix them in 70mL of n-propanol, fully stir and ultrasonically treat for 5 minutes, transfer the mixture to an autoclave, and react at a constant temperature of 190°C for 12 hours, then naturally Cool, wash twice with deionized water and absolute ethanol, and dry at 90°C to obtain black MoS 2 Microspheres. The detection of SEM images shows that the obtained MoS 2 The material is uniform microspheres.

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Abstract

The invention relates to a method for preparing MoS2 microspheres by a solvent hot method, which comprises the following preparation steps: 1) mixing molybdenum source compounds and sulfur source compounds into an alcohol solvent, sufficiently stirring the mixture, and carrying out ultrasonic processing for sufficiently dispersing the mixture; 2) then, transferring the uniformly dispersed mixture into a reaction kettle for carrying out constant-temperature reaction; and 3) carrying out natural cooling, separation, washing and drying on reacting substances to obtain black MoS2 microspheres. The invention has the advantages of mild reaction condition, good reaction reproduction quality, simple preparation process, low preparation cost and high product yield and purity, and is hopeful to realize mass production. The MoS2 products prepared by the solvent hot method of the invention have very important application prospects in all aspects of energy storage, catalysts, solid lubricating agents and the like.

Description

【Technical field】 [0001] The present invention relates to inorganic material MoS 2 The field of preparation, especially a method of preparing MoS by solvothermal method 2 microsphere method. 【Background technique】 [0002] Molybdenum disulfide (MoS 2 ) is a transition metal layered binary compound, which has diamagnetic and semiconducting properties, and also has good optical, electrical, lubricating, catalytic and other properties, and has always attracted people's attention. Molybdenum disulfide belongs to the hexagonal crystal system. There are quite a lot of Mo-S facets, and the specific surface area is large. There are strong covalent bonds in the layer, and weak van der Waals force between the layers. The layers are easy to peel off and have good properties. anisotropy with a lower friction factor, and due to the strong adhesion of S to metals, MoS 2 Can be well attached to the metal surface and always play a lubricating function, even under high temperature, high ...

Claims

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Application Information

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IPC IPC(8): C01G39/06
Inventor 焦丽芳袁华堂王一菁彭文修高海燕亓瞻王庆红杜红梅孙均利
Owner NANKAI UNIV
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