A nitrogen-doped molybdenum disulfide/c/3D graphene composite

A molybdenum disulfide and composite material technology, applied in structural parts, electrical components, battery electrodes, etc., can solve the problems of low product utilization, difficulty in obtaining raw materials, loss of nitrogen-doped precursors, etc., and achieve fast heating speed and stability. The effect of improving and simplifying the production process

Active Publication Date: 2021-03-02
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0006] In order to solve the problems in the preparation of nitrogen-doped molybdenum disulfide / C / three-dimensional graphene composite materials in the prior art, the equipment is complex, 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 doping process is difficult. Due to the low nitrogen doping content caused by the loss of precursors and the aggregation and accumulation of nanoparticles during the long-term heat treatment of active components and graphene, the present invention provides an efficient, fast, and large-scale synthesis of high nitrogen content doped disulfide The method of molybdenum / C / three-dimensional graphene 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 a negative electrode material for lithium batteries, with good application performance

Method used

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  • A nitrogen-doped molybdenum disulfide/c/3D graphene composite
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  • A nitrogen-doped molybdenum disulfide/c/3D graphene composite

Examples

Experimental program
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Effect test

Embodiment 1

[0044] (1) Weigh 1.0g of graphene oxide and 3.0g of L-cysteine ​​and disperse them in 20mL of 37% formaldehyde solution, place them in an ultrasonic instrument and disperse evenly, and record it as dispersion A.

[0045] (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.

[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. ...

Embodiment 2

[0049] (1) Weigh 1.0g of graphene oxide and 3.0g of L-cysteine ​​and disperse them in 30mL of 37% formaldehyde solution, place them in an ultrasonic instrument and disperse evenly, and record it as dispersion A.

[0050] (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.

[0051] (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. The resulting soli...

Embodiment 3

[0054] (1) Weigh 1.0g of graphene oxide and 4.0g of L-cysteine ​​and disperse them in 30mL of 37% formaldehyde solution, place them in an ultrasonic instrument and disperse evenly, and record it as dispersion A.

[0055] (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.

[0056] (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. fo...

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Abstract

A nitrogen-doped molybdenum disulfide / C / three-dimensional 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 and active group The precursors and three-dimensional graphene interact and fuse uniformly, and then perform solvent-free microwave reaction to synthesize high nitrogen content doped molybdenum disulfide / C / three-dimensional 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 component precursors interact with graphene and fuse uniformly. The prepared nitrogen-doped molybdenum disulfide / C / 3D 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. Show a larger specific capacity and better cycle stability.

Description

technical field [0001] The invention relates to a nitrogen-doped molybdenum disulfide / C / three-dimensional graphene composite material, in particular to a high-nitrogen-doped molybdenum disulfide / C / three-dimensional graphene lithium battery negative electrode material, and provides a preparation method thereof, The invention belongs to the technical field of nano composite material and its application. 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 and is the thinnest known material, yet it is extremely strong and hard, stronger than diamond and 100 times stronger than the world's hardest steel. Due to its special nanostructure and excellent perform...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/583H01M10/052
CPCH01M4/362H01M4/5815H01M4/583H01M10/052Y02E60/10
Inventor 郭金廖莎张会成王少军凌凤香
Owner CHINA PETROLEUM & CHEM CORP
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