A nitrogen-doped molybdenum disulfide/graphene composite material

A molybdenum disulfide and composite material technology, applied in the direction of active material electrodes, structural parts, electrical components, etc., can solve the problems of low nitrogen doping content of nitrogen doping precursors, complicated equipment, low product utilization rate, etc. The effects of stacking, uniform nitrogen doping and fast heating

Active Publication Date: 2021-11-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problems in the preparation of nitrogen-doped molybdenum disulfide / graphene composite materials in the prior art, the equipment is complicated, the process is cumbersome, the operation is complicated and time-consuming, the product utilization rate is low, the raw material is difficult to obtain, and the nitrogen-doped precursor is large in the process of nitrogen doping. The problem of low nitrogen doping content caused by loss and the aggregation and accumulation of nanoparticles during the long-term heat treatment process of active components and graphene, etc., the present invention provides an efficient, fast, and large-scale synthesis of high nitrogen content doped molybdenum disulfide / graphite The method of olefin composite material, the obtained material has high nitrogen content, and the utilization rate of raw materials is significantly improved. The product does not need washing, separation, drying and other processes, and can be directly used as lithium battery negative electrode material, with good application performance

Method used

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  • A nitrogen-doped molybdenum disulfide/graphene composite material
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  • A nitrogen-doped molybdenum disulfide/graphene composite material

Examples

Experimental program
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Effect test

Embodiment 1

[0039] (1) Weigh 1.0g of graphene oxide and disperse it in 20mL of 37% formaldehyde aqueous solution, place it in an ultrasonic instrument and disperse evenly, record it as dispersion A.

[0040] (2) Weigh 3.0g of melamine, 1.2g of sulfur powder and 5.2g of ammonium paramolybdate and add them into 40mL of deionized water, place them in an ultrasonic instrument and disperse evenly by ultrasonic, and record it as dispersion liquid B.

[0041] (3) Mix Dispersion A and Dispersion B, raise the temperature of the water bath to 60°C and stir for 10 minutes. Then triethanolamine was added to the reaction solution to adjust the pH value of the reaction solution system to 8.0, and the mixture was uniformly mixed by ultrasonic, then the reaction solution was poured into a high-pressure reactor, and the temperature was raised to 120° C. for 12 hours to react. Suction filtration, vacuum drying to obtain a black solid powder.

[0042] (4) Put the black solid powder obtained in step (3) int...

Embodiment 2

[0044] (1) Weigh 1.0g graphene oxide and disperse it in 30mL 37% formaldehyde aqueous solution, place it in an ultrasonic instrument and disperse evenly, record it as dispersion liquid A.

[0045] (2) Weigh 5.0g of melamine, 2.1g of sulfur powder and 10.0g of ammonium paramolybdate and add them into 40mL of deionized water, place them in an ultrasonic instrument and disperse evenly by ultrasonic, and record it as dispersion liquid B.

[0046] (3) Mix Dispersion A and Dispersion B, raise the temperature of the water bath to 60°C and stir for 10 minutes. Then triethanolamine was added to the reaction solution to adjust the pH value of the reaction solution system to 8.0, and the mixture was uniformly mixed by ultrasonic, then the reaction solution was poured into a high-pressure reactor, and the temperature was raised to 120° C. for 12 hours to react. Suction filtration, vacuum drying to obtain a black solid powder.

[0047] (4) Put the black solid powder obtained in step (3) i...

Embodiment 3

[0049] (1) Weigh 1.0g graphene oxide and disperse it in 30mL 37% formaldehyde aqueous solution, place it in an ultrasonic instrument and disperse evenly, record it as dispersion liquid A.

[0050] (2) Weigh 10.0g of melamine, 1.2g of sulfur powder and 5.0g of sodium molybdate into 40mL of deionized water, place it in an ultrasonic instrument and disperse evenly by ultrasonication, and record it as dispersion liquid B.

[0051] (3) Mix Dispersion A and Dispersion B, raise the temperature of the water bath to 70°C and stir for 10 minutes. Then triethanolamine was added to the reaction solution to adjust the pH value of the reaction solution system to 8.0, and the mixture was uniformly mixed by ultrasonic, then the reaction solution was poured into a high-pressure reactor, and the temperature was raised to 120° C. for 12 hours to react. Suction filtration, vacuum drying to obtain a black solid powder.

[0052] (4) Put the black solid powder obtained in step (3) into a microwave ...

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Abstract

A nitrogen-doped molybdenum disulfide / graphene composite material, which uses formaldehyde as a bridge to make it moderately cross-linked with melamine to form a nitrogen-doped precursor, and then undergoes hydrothermal reaction to make the nitrogen-doped precursor, active components and graphite Graphene interaction uniform fusion, and then solvent-free microwave reaction, synthesis of high nitrogen content doped molybdenum disulfide / graphene composites. The composite material of the present invention avoids the loss caused by the sublimation of the nitrogen-doped precursor in the heating process in the traditional nitrogen doping process during the preparation process, improves the nitrogen doping efficiency, and the reaction conditions are progressive from mild to strong, realizing the nitrogen-doped precursor, The active components interact with graphene and fuse uniformly. The prepared nitrogen-doped molybdenum disulfide / graphene composite material has good stability, is not easy to denature in the air, is easy to store, and has a large specific surface area. As a negative electrode material for lithium-ion batteries, it provides a good channel for lithium ion transmission, showing relatively Large specific capacity and good cycle stability.

Description

technical field [0001] The invention relates to a nitrogen-doped molybdenum disulfide / graphene composite material, in particular to a molybdenum disulfide / graphene lithium battery negative electrode material doped with high nitrogen content, and provides a preparation method thereof, belonging to nanocomposite materials and their Field of application technology. Background technique [0002] Graphene is a two-dimensional honeycomb lattice structure carbonaceous material that is tightly packed by a single layer of carbon atoms. Since the discovery by Andre K. Geim of the University of Manchester in 2004, graphite Enenes have received great attention in both experimental and theoretical sciences. Graphene is only one carbon atom thick, making it the thinnest known material, yet extremely strong and hard, stronger than diamond and 100 times stronger than the world's hardest steel. Due to its special nanostructure and excellent performance, it has potential application prospec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/38H01M4/58H01M4/587
CPCH01M4/364H01M4/38H01M4/5815H01M4/587H01M2004/027Y02E60/10
Inventor 郭金廖莎凌凤香张会成王少军
Owner CHINA PETROLEUM & CHEM CORP
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