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Nitrogen-doped molybdenum disulfide/carbon nanotube composite material

A technology of acidifying carbon nanotubes and molybdenum disulfide, which is applied to electrical components, battery electrodes, circuits, etc., can solve the problems of complicated and time-consuming operations, low nitrogen doping content, and low product utilization, and achieve simplified production processes, The effect of large specific surface area and large specific capacity

Active Publication Date: 2020-05-05
CHINA PETROLEUM & CHEM CORP +1
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the problems in the preparation of nitrogen-doped carbon nanotube materials in the prior art, such as complex equipment, cumbersome process, complicated and time-consuming operation, low product utilization rate and low nitrogen doping content caused by a large amount of nitrogen-doped precursor loss during the nitrogen doping process , the present invention provides a kind of efficient, fast, the method for synthesizing high nitrogen content doped molybdenum disulfide / carbon nanotube composite material in large quantities, the nitrogen content of the obtained material is high, the raw material utilization rate is obviously improved, and the product does not need washing, separation, drying and other processes , can be directly used as lithium battery anode material, with good application performance

Method used

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preparation example Construction

[0036] Preparation of acidified carbon nanotubes: put 1g of carbon nanotubes and 200mL of concentrated sulfuric acid into a three-necked flask, ultrasonically disperse evenly, slowly add 60mL of 70% concentrated nitric acid dropwise, reflux and stir at 60°C for 1h, cool naturally to room temperature, add Dilute with a large amount of deionized water, let it stand for stratification, remove the supernatant, and dialyze the black precipitate at the bottom with deionized water to replace the small molecules in it, so that the surface can be balanced, and a long-term stable and uniform dispersion of carbon nanotubes can be obtained. liquid. The carbon nanotube aqueous dispersion is freeze-dried to obtain acidified carbon nanotube powder, which is placed in a desiccator for subsequent use. Its SEM picture is as follows figure 1 As shown, the structure of one-dimensional carbon nanotubes can be clearly seen, and the walls of carbon nanotubes after acidification treatment are relati...

Embodiment 1

[0039] (1) Weigh 1.0 g of acidified carbon nanotubes and disperse them in 20 mL of 37% formaldehyde aqueous solution, place them in an ultrasonic instrument and disperse evenly, and record them as dispersion liquid A.

[0040] (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.

[0041] (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.

[0042] (4) Put the black solid powder obtained i...

Embodiment 2

[0044] (1) Weigh 1.0 g of acidified carbon nanotubes and disperse them in 30 mL of 37% formaldehyde aqueous solution, place them in an ultrasonic instrument and disperse evenly, and record them as dispersion liquid A.

[0045] (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.

[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. for 12 hours to react. Suction filtration, vacuum drying to obtain a black solid powder.

[0047] (4) Put the black solid powder obtained i...

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Abstract

The invention relates to a nitrogen-doped molybdenum disulfide / carbon nanotube composite material, which is prepared by adopting formaldehyde as a bridge, and enabling the formaldehyde and melamine tobe subjected to moderate crosslinking to form a nitrogen-doped precursor, then performing hydrothermal reaction to enable the nitrogen-doped precursor, an active component single-source precursor andcarbon nanotubes to be interacted and uniformly fused, and then performing solvent-free microwave reaction to synthesize the high-nitrogen-content doped carbon nanotube. According to the nitrogen-doped molybdenum disulfide / carbon nanotube composite material, in the preparation process, 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 interaction of the nitrogen-doped precursor, the active component single-source precursor and the carbon nanotubes is achieved. The prepared nitrogen-doped molybdenum disulfide / carbon nanotube 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 / carbon nanotube composite material is used as a lithium ion battery negative electrode material; and the nitrogen-doped molybdenum disulfide / carbon nanotube composite material has large specific capacity andgood cycling stability.

Description

technical field [0001] The invention relates to a nitrogen-doped molybdenum disulfide / carbon nanotube composite material, in particular to a molybdenum disulfide / carbon nanotube lithium battery negative electrode material doped with high nitrogen content, and provides a preparation method thereof, belonging to nanocomposite materials and its technical fields of application. Background technique [0002] Carbon nanotubes are hollow cylinders formed by curling graphite layers, and its bonding method is mainly deformed Sp2 orbitals. When the graphite layer is rolled into carbon nanotubes, the Sp2 hybridization will be partially deformed, so Sp2 tends to form re-hybridization with Sp3. This re-hybridization structure and two-orbital confinement characteristics can endow carbon nanotubes with excellent mechanical, thermal, and thermal properties. Electrical, optical, magnetic and chemical properties. Therefore, carbon nanotubes have higher mechanical strength, better electrical...

Claims

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Application Information

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