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Molybdenum disulfide/three-dimensional graphene composite material

A technology of molybdenum disulfide and composite materials, which is applied in the field of nanocomposite materials and its applications, can solve the problems of electrode damage, unstable combination, long reaction time, etc., and achieve difficult re-stacking and agglomeration, good cycle stability, and heating speed fast effect

Inactive Publication Date: 2019-06-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problem of molybdenum disulfide / graphene nanocomposites in the prior art, most of them use hydrothermal method, or solvents are needed in the synthesis process, the reaction time is generally long, and the products require complicated separation and post-treatment processes. MoS2 in synthetic materials 2 The combination with graphene is unstable, and charging and discharging easily lead to electrode damage. The present invention provides a method for synthesizing molybdenum disulfide / three-dimensional graphene composite materials by a solventless method. The obtained product does not need washing, separation, drying and other processes, and can be used directly For lithium battery anode materials, good application performance

Method used

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  • Molybdenum disulfide/three-dimensional graphene composite material
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  • Molybdenum disulfide/three-dimensional graphene composite material

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Preparation of graphene oxide: slowly add 100mL of 98% concentrated sulfuric acid into a 500mL dry three-necked flask, and place the three-necked flask on a magnetic stirrer for ice bath cooling. Add 2.0 g of natural graphite flakes (180 mesh) under rapid stirring, and when the temperature of the reaction solution drops to about 0° C., slowly add 4.0 g of sodium nitrate, and continue stirring for 2 h. Then slowly add 10 g of potassium permanganate in batches within 1 h, keep stirring for 2 h, and control the reaction temperature below 10°C. Then the three-neck flask was moved into a water bath at 40° C., and the stirring reaction was continued for 2 h. Subsequently, 200 mL of warm deionized water was slowly added, and the temperature of the reaction solution was kept within 100 °C. React at a constant temperature of 98°C until the reaction solution turns bright yellow. Add 20 mL of 30% hydrogen peroxide to the reaction liquid, and keep stirring to make it fully react....

Embodiment 2

[0033] The preparation method of graphene oxide and three-dimensional graphene airgel is the same as embodiment 1

[0034] Preparation of molybdenum disulfide / three-dimensional graphene composite material: mix ammonium tetrathiomolybdate and three-dimensional graphene airgel at a mass ratio of 2:1, place the mixture in an agate tank filled with nitrogen, and use a ball mill to grind, The mass ratio of the ball to the material is 3:1, the rotation speed is 400rpm, after ball milling for 1 hour, the product is naturally cooled to room temperature and collected. The ball-milled material was put into a reaction tube, placed in a microwave reaction chamber, and purged with argon gas at 100 mL / min for 1 h. Microwave with 400W power for 6min. Cool to room temperature under an Ar atmosphere to obtain a molybdenum disulfide / three-dimensional graphene composite material.

Embodiment 3

[0036] The preparation method of graphene oxide and three-dimensional graphene airgel is the same as embodiment 1

[0037] Preparation of molybdenum disulfide / three-dimensional graphene composite material: mix ammonium tetrathiomolybdate and three-dimensional graphene airgel at a mass ratio of 3:1, place the mixture in an agate tank filled with nitrogen, and use a ball mill to grind, The mass ratio of the ball to the material is 3:1, the rotation speed is 400rpm, after ball milling for 1 hour, the product is naturally cooled to room temperature and collected. The ball-milled material was put into a reaction tube, placed in a microwave reaction chamber, and purged with argon gas at 100 mL / min for 1 h. Microwave with 600W power for 9min. Cool to room temperature under an Ar atmosphere to obtain a molybdenum disulfide / three-dimensional graphene composite material.

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Abstract

The invention relates to a molybdenum disulfide / three-dimensional graphene composite material which is prepared by the following method: utilizing graphene oxide and L-cysteine to prepare three-dimensional graphite alkene aerogel, placing four ammonium thiomolybdate and three-dimensional graphite alkene aerogel in a microwave reaction cavity after grinding, heating for 1-20 minutes at the microwave power of 300-1000W to obtain the molybdenum disulfide / three-dimensional graphite alkene composite material. The molybdenum disulfide / three-dimensional graphite alkene composite material is obtainedunder the microwave heating condition, graphene oxide is thermally reduced into graphene, and in the meantime, the single-source precursor is heated and rapidly decomposed to generate MoS2, so that MoS2 directly grows in situ on the surface of the graphene, the microwave heating speed is high, the heating is uniform, the MoS2 nanosheets and the graphene are firmly combined, which is not easy to cause particle accumulation, the time required for synthesizing the material is greatly shortened, and the problem of agglomeration of the graphene and the MoS2 under the long-term heating condition issolved; compared with a two-dimensional structure, the graphene with the three-dimensional structure is not easy to be re-stacked and agglomerated in the compounding process, so that the excellent properties of the graphene are guaranteed; and the composite material mentioned above serving as the cathode material of the lithium ion battery demonstrates good cycling stability and rate capability.

Description

technical field [0001] The invention relates to a molybdenum disulfide / three-dimensional graphene structure lithium battery negative electrode material, and provides a preparation method thereof, belonging to the technical field of nanocomposite materials and their applications. Background technique [0002] Lithium-ion batteries are widely used in modern electric energy storage systems such as mobile phones and electric vehicles due to their high energy density, high operating voltage and long service life. The electrochemical properties of negative electrode materials directly affect the overall performance of lithium-ion batteries. Graphite is widely used as a negative electrode material for lithium-ion batteries due to its high Coulombic efficiency, good cycle stability, and abundant reserves in nature. However, its low specific capacity (372mAh g -1 ) and poor rate performance cannot meet the needs of future portable devices and electric vehicles. Therefore, there is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/583H01M10/0525B82Y30/00
CPCY02E60/10
Inventor 郭金张会成王少军凌凤香
Owner CHINA PETROLEUM & CHEM CORP
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