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

A technology of molybdenum disulfide and composite materials, which is applied in the direction of structural parts, electrical components, battery electrodes, etc., can solve the problems of low nitrogen doping content, difficulty in obtaining raw materials, low product utilization rate, etc., and achieve large specific surface area and stability Good, fast heating effect

Active Publication Date: 2021-03-05
CHINA PETROLEUM & CHEM CORP +1
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  • Description
  • Claims
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Problems solved by technology

[0004] In order to solve the problems in the preparation of nitrogen-doped molybdenum disulfide / C / 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, and the raw material is difficult to obtain. The problem of low nitrogen doping content caused by a large amount of bulk loss and the aggregation and accumulation of nanoparticles during the long-term heat treatment process of active components and graphene, the present invention provides an efficient, fast, large-scale synthesis of high nitrogen content doped molybdenum disulfide / C / graphene composite material method, 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 a negative electrode material for lithium batteries, with good application performance

Method used

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Effect test

Embodiment 1

[0041] (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.

[0042] (2) Take 0.5g ammonium paramolybdate and 20mL concentrated ammonia water (NH 3 ·H 2 O) Mix, heat up, add 3.0g ammonium sulfide ((NH 4 ) 2 S), reacted for 0.5 h under the state of magnetic stirring, and then respectively added 0.1 g of tetramethylammonium bromide and 0.6 g of melamine to the solution, and ultrasonically mixed them uniformly to obtain dispersion B.

[0043] (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. S...

Embodiment 2

[0046] (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.

[0047] (2) Take 0.5g ammonium paramolybdate and 20mL concentrated ammonia water (NH 3 ·H 2 O) Mix, heat up, add 9.0g ammonium sulfide ((NH 4 ) 2 S), reacting for 1 h under magnetic stirring, then adding 2.0 g of tetramethylammonium bromide and 2.0 g of melamine to the solution, and ultrasonically mixing to obtain a dispersion B.

[0048] (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...

Embodiment 3

[0051] (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.

[0052] (2) Take 0.9g ammonium paramolybdate and 20mL concentrated ammonia water (NH 3 ·H 2 O) Mix, heat up, add 10.0g ammonium sulfide ((NH 4 ) 2 S), reacted for 1 h under the state of magnetic stirring, and then respectively added 2.5 g of tetraethylammonium bromide and 2.0 g of melamine to the solution, and ultrasonically mixed them uniformly to obtain dispersion B.

[0053] (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. Su...

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Abstract

A nitrogen-doped molybdenum disulfide / C / 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 a hydrothermal reaction to make the nitrogen-doped precursor and active component The precursor and graphene interact and fuse uniformly, and then perform a solvent-free microwave reaction to synthesize a high nitrogen content doped molybdenum disulfide / C / graphene composite. 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 component precursors interact with graphene and fuse uniformly. The prepared nitrogen-doped molybdenum disulfide / C / graphene composite material has good stability, is not easily denatured 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. It has a larger specific capacity and better cycle stability.

Description

technical field [0001] The invention relates to a nitrogen-doped molybdenum disulfide / C / graphene composite material, in particular to a molybdenum disulfide / C / graphene lithium battery negative electrode material doped with high nitrogen content, and provides a preparation method thereof, which belongs to nano Composite materials and their application technologies. 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 prosp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/38H01M4/58H01M4/583
CPCH01M4/364H01M4/38H01M4/5815H01M4/583Y02E60/10
Inventor 郭金王少军凌凤香张会成廖莎
Owner CHINA PETROLEUM & CHEM CORP
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