Nitrogen-doped molybdenum disulfide/graphene composite material

A technology of molybdenum disulfide and composite materials, applied in electrical components, battery electrodes, circuits, etc., can solve the problems of low nitrogen doping content of nitrogen-doped precursors, difficulty in obtaining raw materials, complicated and time-consuming operations, etc., and achieve large specific surface area , good stability, and the effect of simplifying the production process

Active Publication Date: 2020-05-05
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 lost in a large amount during the nitrogen doping process. Due to the low nitrogen doping content 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 molybdenum disulfide / graphene The method of composite materials, 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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  • Nitrogen-doped molybdenum disulfide/graphene composite material

Examples

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Effect test

Embodiment 1

[0038] (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.

[0039] (2) Weigh 3.0g of melamine and 5.0g of ammonium tetrathiomolybdate and add them into 40mL of deionized water, place them in an ultrasonic instrument and ultrasonically disperse evenly, and record it as dispersion liquid B.

[0040] (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.

[0041] (4) Put the black solid powder obtained in step (3) into a microwave rea...

Embodiment 2

[0043] (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.

[0044] (2) Weigh 5.0g of melamine and 8.0g of ammonium tetrathiomolybdate and add them into 40mL of deionized water, place them in an ultrasonic instrument and ultrasonically disperse evenly, and record it as dispersion liquid B.

[0045] (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.

[0046] (4) Put the black solid powder obtained in step (3) into a microwave re...

Embodiment 3

[0048] (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.

[0049] (2) Weigh 10.0g of melamine and 10.0g of ammonium tetrathiomolybdate and add them into 40mL of deionized water, place them in an ultrasonic apparatus and ultrasonically disperse evenly, and record it as dispersion liquid B.

[0050] (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.

[0051] (4) Put the black solid powder obtained in step (3) into a microwave r...

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Abstract

The invention discloses a nitrogen-doped molybdenum disulfide / graphene composite material. The preparation method comprises the following steps: taking formaldehyde as a bridge, and carrying out moderate crosslinking on the formaldehyde and melamine to form a nitrogen-doped precursor; then, carrying out hydrothermal reaction to make the nitrogen-doped precursor, an active component and graphene interacted and uniformly fused; and carrying out solvent-free microwave reaction to synthesize the high-nitrogen-content-doped molybdenum disulfide / graphene composite material. In the preparation process of the composite material, the loss caused by sublimation of the nitrogen-doped precursor in the heating process in the traditional nitrogen doping process is avoided, and the nitrogen doping efficiency is improved; and the reaction conditions are progressively increased from mild to intense, and uniform fusion of the nitrogen-doped precursor, the active component and the graphene through interaction is realized. The prepared nitrogen-doped molybdenum disulfide / graphene composite material is good in stability, not prone to denaturation in air, easy to store and large in specific surface area; a good channel is provided for lithium ion transmission when the nitrogen-doped molybdenum disulfide / graphene composite material is used as a lithium ion battery negative electrode material; and thenitrogen-doped molybdenum disulfide / graphene composite material has large specific capacity and good cycling 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 applications thereof technology field. 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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IPC IPC(8): H01M4/36H01M4/38H01M4/58H01M4/583
CPCH01M4/36H01M4/38H01M4/58H01M4/583Y02E60/10
Inventor 郭金廖莎凌凤香张会成王少军
Owner CHINA PETROLEUM & CHEM CORP
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