Preparation method of one-step hydrothermal synthesis of carbon/molybdenum disulfide composite microsphere

A technology of molybdenum disulfide and composite microspheres, applied in the directions of molybdenum sulfide, vanadium oxide, etc., can solve problems such as no public reports, and achieve the effects of high yield, wide application prospect and mild reaction conditions

Inactive Publication Date: 2007-07-11
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But so far, using glucose or sucrose as the carbon source, molybdate as the molybdenum source, and thioacetamide or thiourea as the sulfur source, there are literatures and patents on direct synthesis of carbon / molybdenum disulfide composite microspheres in one step by hydrothermal reaction. Haven't seen public reports yet

Method used

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  • Preparation method of one-step hydrothermal synthesis of carbon/molybdenum disulfide composite microsphere

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Dissolve 1.2mmol sodium molybdate in 60ml deionized water to form a 0.02M solution, add 5.3mmol of thiourea and stir evenly, then add 15mmol of glucose, wherein the molar ratio of thiourea to sodium molybdate is 4.4:1, glucose and The molar ratio of sodium molybdate was 12.5:1. After fully stirring, the solution was transferred to a hydrothermal reaction kettle, and hydrothermally reacted at 240°C for 24 hours, then cooled naturally, collected and collected after being fully washed with centrifugal separation and deionized water The carbon / molybdenum disulfide composite microspheres can be obtained after drying, and the microspheres have a uniform particle size as observed by SEM, and the average particle size is 0.40 microns (see Figure 1).

Embodiment 2

[0023] Dissolve 1.2mmol sodium molybdate in 60ml deionized water to form a 0.02M solution, add 5.4mmol of thioacetamide and stir evenly, then add 17mmol of glucose, wherein the molar ratio of thioacetamide to sodium molybdate is 4.5: 1. The molar ratio of glucose to sodium molybdate is 14.2:1. After fully stirring, transfer the solution to a hydrothermal reaction kettle, conduct a hydrothermal reaction at 230°C for 23 hours, then cool naturally, wash thoroughly with centrifuge and deionized water, collect and dry to obtain carbon / molybdenum disulfide composite microparticles. Balls with an average particle size of 0.44 microns (see Figure 2).

Embodiment 3

[0025] Dissolve 3.0mmol sodium molybdate in 60ml deionized water to form a 0.05M solution, add 15mmol of thiourea and stir evenly, then add 45mmol of glucose, wherein the molar ratio of thiourea to sodium molybdate is 5:1, glucose and molybdenum The molar ratio of sodium bicarbonate is 15:1. After fully stirring, the solution is transferred to a hydrothermal reaction kettle, hydrothermally reacted at 220°C for 21 hours, then cooled naturally, and then collected and dried with centrifugation and deionized water. The carbon / molybdenum disulfide composite microspheres can be obtained, and the average particle size is 1.3 microns.

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Abstract

The invention discloses a making method of carbon / molybdenum disulfide composite microball through water heat method, which comprises the following steps: dissolving molybdate in the deionized water to form 0.02-0.1m solution; adding thioacetamide or sulfourea as sulfur source with molar rate of thioacetamide or sulfourea and molybdate at 31-51; stirring evenly; adding glucose or sucrose as carbon source with the molar rate of glucose or sucrose and molybdate at 51-251; stirring completely; transmitting solution into water heat reacting autoclave to react under 200-240 deg. c for 20-24h; cooling naturally; separating; washing; drying to obtain the product.

Description

technical field [0001] The invention relates to the preparation of inorganic chemical materials, in particular to a preparation method for synthesizing carbon / molybdenum disulfide composite microspheres by one-step hydrothermal method. Background technique [0002] MoS 2 It belongs to the hexagonal crystal system, in which there are quite a lot of Mo-S facets, the specific surface area is large, the inner layer is a strong covalent bond, and the interlayer is a weaker van der Waals force, and the layers are easy to peel off. It has good anisotropy and low friction coefficient, and S has strong adhesion to metal, making MoS 2 It can be well attached to the metal surface and always play a lubricating function, especially under the conditions of high temperature and high vacuum, it still has a low friction coefficient, so it is an excellent solid lubricant. In addition, MoS with a layered structure 2 As the host lattice, it can react with different guest atoms or molecules, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06C01G31/02
Inventor 马琳陈卫祥李辉赵杰
Owner ZHEJIANG UNIV
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