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A nitrogen-doped molybdenum disulfide/three-dimensional graphene composite material

A molybdenum disulfide and composite material technology, applied in secondary batteries, electrochemical generators, active material electrodes, etc., can solve the problems of complicated and time-consuming operation, low product utilization rate, difficulty in obtaining raw materials, etc. The effect of fast heating and not easy particle accumulation

Active Publication Date: 2021-07-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problems in the preparation of nitrogen-doped graphene materials in the prior art, such as complex equipment, cumbersome process, complicated and time-consuming operation, low product utilization rate, difficulty in obtaining raw materials, and nitrogen doping caused by a large amount of nitrogen-doped precursor loss during the nitrogen-doping process Low content 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, and large-scale synthesis of high nitrogen content doped molybdenum disulfide / three-dimensional graphene composite materials. , the nitrogen content of the obtained material is high, 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/three-dimensional graphene composite material
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  • A nitrogen-doped molybdenum disulfide/three-dimensional graphene composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Weigh 1.0 g of oxide oxide and 3.0 g of L-cysteine ​​dispersion in a 20 ml of 37% formaldehyde aqueous solution, placed in the ultrasound gauge is uniformly molved as dispersion A.

[0041] (2) Weighing 3.0 g of melamine and 5.0 g of tetramethyl molybdate addition to 40 ml of deionized water, placed in ultrasound dispersion as a dispersion B.

[0042] (3) Mix the dispersion A and dispersion B, and the water bath was warmed to 60 ° C for 10 min. Subsequently, triethanolamine was added to the reaction solution, and the reaction liquid system was adjusted to be 8.0, and the ultrasonic mix was uniform, and then the reaction solution was poured into the high pressure reactor, and the temperature was tapered to 120 ° C for 12 hours. The obtained solid was frozen.

[0043] (4) Place the product in step (3) in a microwave reaction chamber, 100 ml / min of argon purge 1 h. It was heated at 600 W of microwave power to 10 min to obtain the blended ditzimide / 3-dimensional graphen...

Embodiment 2

[0045] (1) Weigh 1.0 g of oxide oxide and 3.0 g of L-cysteine ​​dispersion in a water solution of 30 ml of 37% formaldehyde, placed in the ultrasound meter as a dispersion A.

[0046] (2) Weigh 5.0 g of melamine and 8.0 g of tetramethyl molybdate to be added to 40 ml of deionized water, and the ultrasonic dispersion is placed in the ultrasound dispersion as dispersion B.

[0047] (3) Mix the dispersion A and dispersion B, and the water bath was warmed to 60 ° C for 10 min. Subsequently, triethanolamine was added to the reaction solution, and the reaction liquid system was adjusted to be 8.0, and the ultrasonic mix was uniform, and then the reaction solution was poured into the high pressure reactor, and the temperature was tapered to 120 ° C for 12 hours. The obtained solid was frozen.

[0048] (4) Place the product in step (3) in a microwave reaction chamber, 100 ml / min of argon purge 1 h. It was heated at 600 W of microwave power to 10 min to obtain the blended ditzimide / 3-d...

Embodiment 3

[0050] (1) Weighing 1.0 g of oxide oxide and 4.0 g of L-cysteine ​​dispersed in a water solution of 30 ml of 37% formaldehyde, placed in the ultrasound meter as a dispersion A.

[0051] (2) Weigh 10.0 g of melamine and 10.0 g of tetramethyl molybdate to be added to 40 ml of deionized water, and the ultrasonic dispersion is placed in the ultrasound dispersion as dispersion B.

[0052] (3) Mix the dispersion A and dispersion B, and the water bath was warmed to 70 ° C for 10 min. Subsequently, triethanolamine was added to the reaction solution, and the reaction liquid system was adjusted to be 8.0, and the ultrasonic mix was uniform, and then the reaction solution was poured into the high pressure reactor, and the temperature was tapered to 120 ° C for 12 hours. The obtained solid was frozen.

[0053] (4) Place the product in step (3) in a microwave reaction chamber, 100 ml / min of argon purge 1 h. It was heated at 600 W of microwave power heating for 20 min to obtain a nitrogen-don...

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Abstract

A nitrogen-doped molybdenum disulfide / 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 component precursor Interact with graphene for uniform fusion, and then perform solvent-free microwave reaction to synthesize high-nitrogen-doped molybdenum disulfide / 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 efficiency of nitrogen doping, and the reaction conditions are progressive from mild to strong, and realizes the nitrogen-doped precursor and the active group. Part precursors interact with graphene and fuse uniformly. The prepared nitrogen-doped molybdenum disulfide / three-dimensional 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. Large specific capacity and good cycle stability.

Description

Technical field [0001] The present invention relates to a blend of boss-donated diomide / 3-dimensional graphene composite, and more particularly to a high nitrate-doped doped doped doped doped molybdenum / 3-dimensional graphene lithium battery negative electrode material, and provides the preparation method, which belongs to the nanocomposite and Its application technology areas. Background technique [0002] Graphie is a two-dimensional honeycomb-like lattice carbonaceous material that is closely stacked by a single layer of carbon atom, and the graphite has been found from Andre K. Geim, the University of Manchester, England. Ethylene has been greatly concerned about experimental science and theory. The graphene has only one carbon atom thickness, which is the thinnest in the material, but it is very firm and hard, which is more hard than the diamond, and its strength is 100 times higher than the world's hardest steel. Because of its special nanostructure and excellent proper...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/0525
CPCH01M4/366H01M4/5815H01M4/625H01M10/0525H01M2004/021H01M2004/027Y02E60/10
Inventor 郭金廖莎张会成王少军凌凤香
Owner CHINA PETROLEUM & CHEM CORP
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