A nitrogen-doped molybdenum disulfide/carbon nanotube composite

A technology for acidifying carbon nanotubes and molybdenum disulfide, which is applied in secondary batteries, electrochemical generators, structural parts, etc., can solve the problems of complicated and time-consuming operations, low nitrogen doping content, and low product utilization, and achieve The effect of simplified production process, uniform nitrogen doping, and fast heating speed

Active Publication Date: 2021-11-09
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
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Problems solved by technology

[0007] In order to solve the problems in the preparation of nitrogen-doped molybdenum disulfide / carbon nanotube composites 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, and the nitrogen-doped precursor is lost during the nitrogen-doping process. For problems such as low doping content, the present invention provides an efficient, rapid, and large-scale method for synthesizing molybdenum disulfide / carbon nanotube composite materials doped with high nitrogen content. The nitrogen content of the obtained nitrogen-doped carbon nanotubes is high, and the utilization rate of raw materials is obvious Improvement, 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/carbon nanotube composite
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  • A nitrogen-doped molybdenum disulfide/carbon nanotube composite

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preparation example Construction

[0037] 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

[0040] (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.

[0041] (2) Weigh 3.0g of melamine, 1.2g of sulfur powder and 5.2g of ammonium paramolybdate and add them into 40mL of deionized water, place them in an ultrasonic instrument and disperse evenly by ultrasonic, and record it as dispersion liquid B.

[0042] (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.

[0043] (4) Put the black solid ...

Embodiment 2

[0045] (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.

[0046] (2) Weigh 5.0g of melamine, 2.1g of sulfur powder and 10.0g of ammonium paramolybdate and add them into 40mL of deionized water, place them in an ultrasonic instrument and disperse evenly by ultrasonic, and record it as dispersion liquid B.

[0047] (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.

[0048] (4) Put the black solid...

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Abstract

A nitrogen-doped molybdenum disulfide / carbon nanotube 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 molybdenum disulfide precursor The body and carbon nanotubes interact and fuse uniformly, and then perform solvent-free microwave reaction to synthesize high nitrogen content doped molybdenum disulfide / carbon nanotube materials. The nitrogen-doped molybdenum disulfide / carbon nanotube 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 range from mild to strong. Further, the nitrogen-doped precursor, molybdenum disulfide precursor and carbon nanotubes interact and fuse uniformly. The prepared nitrogen-doped molybdenum disulfide / carbon nanotube 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, showing Larger specific capacity and better cycle 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 Patents(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/583H01M4/62H01M10/0525
CPCH01M4/362H01M4/58H01M4/583H01M4/62H01M10/0525Y02E60/10
Inventor 郭金廖莎张会成王少军凌凤香
Owner CHINA PETROLEUM & CHEM CORP
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