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Preparation method of nitrogen-doped three-dimensional porous carbon loaded with nano cobalt and application thereof in lithium sulfur batteries

A three-dimensional porous, nano-cobalt technology, applied in battery electrodes, nanotechnology, nanotechnology, etc., can solve the problems of lack of mesoporous, macroporous structure, low yield, unfavorable high energy density and high performance lithium-sulfur battery, etc. The effect of increasing the number of mesopores and increasing the yield

Active Publication Date: 2019-10-15
NAT UNIV OF DEFENSE TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the nano-metal-microporous carbon obtained by simply carbonizing MOFs has the following disadvantages: (1) The yield during the synthesis of ZIF-67 is too low (about 20%), resulting in the final nano-Co-N doped microporous carbon material It is difficult to prepare for large-scale production; (2) the prepared nano-Co-N doped microporous carbon material is mainly a microporous structure, lacking a mesopore and macroporous structure, and it is difficult to accommodate a large amount of sulfur and buffer the sulfur positive electrode in the process of charging and discharging. Volume change is not conducive to the preparation of high energy density and high performance lithium-sulfur batteries

Method used

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  • Preparation method of nitrogen-doped three-dimensional porous carbon loaded with nano cobalt and application thereof in lithium sulfur batteries
  • Preparation method of nitrogen-doped three-dimensional porous carbon loaded with nano cobalt and application thereof in lithium sulfur batteries
  • Preparation method of nitrogen-doped three-dimensional porous carbon loaded with nano cobalt and application thereof in lithium sulfur batteries

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preparation example Construction

[0025] The present invention proposes a preparation method of nitrogen-doped three-dimensional porous carbon supported by nano-cobalt, comprising the following steps:

[0026] (1) adding inorganic nanospheres to methanol for ultrasonic dispersion, then adding cobalt salt and stirring to dissolve, then adding 2-methylimidazole methanol solution to obtain a precursor solution;

[0027] Preferably, the concentration of inorganic nanospheres in the precursor solution is 5-50 g / L; the concentration of cobalt salt in the precursor solution is 0.01-0.1 mol / L; the cobalt salt and 2-methylimidazole The molar ratio of 1: (0.5 ~ 10) to form the ZIF67 precursor. The number of mesopores and macropores is controlled by controlling the amount of cobalt salt and inorganic nanospheres added, and the wall thickness of the three-dimensional porous carbon in the product is controlled by controlling the ratio of cobalt salt and inorganic nanospheres.

[0028] Preferably, the inorganic nanospheres...

Embodiment 1

[0041] This embodiment provides a method for preparing nano-cobalt-supported nitrogen-doped three-dimensional porous carbon, comprising the following steps:

[0042] (1) Add 15ml tetraethyl orthosilicate to a mixed solvent composed of 10ml ammonia water, 200ml ethanol, and 100ml water under magnetic stirring, stir at 30°C for 2h, filter, wash and dry the resulting product to obtain a particle size of 300nm Silica nanosphere powder left and right.

[0043] (2) get the 3.0g white SiO obtained in step (1) 2 The nanosphere powder was ultrasonically dispersed in 100ml methanol for 2h, and then 0.8g Co(NO 3 ) 2 Stir to dissolve, then add 100ml of methanol solution containing 1.0g of 2-methylimidazole to obtain a precursor solution.

[0044] (3) The precursor solution was stirred and reacted at 30°C for 1 hour, and then stirred and evaporated to dryness at 80°C to obtain gray-purple precursor powder;

[0045] (4) Place the gray-purple precursor powder in a tube furnace under high...

Embodiment 2

[0054] This embodiment provides a method for preparing nano-cobalt-supported nitrogen-doped three-dimensional porous carbon, comprising the following steps:

[0055] (1) Add 15ml of tetraethyl orthosilicate to a mixed solvent consisting of 5ml of ammonia water, 200ml of ethanol, and 20ml of water under magnetic stirring, stir at 30°C for 2 hours, filter, wash and dry the resulting product to obtain a particle size of 100nm Silica nanosphere powder left and right.

[0056] (2) get the SiO of 3.0g that step (1) obtains 2 The nanosphere powder was ultrasonically dispersed in 100ml methanol for 2h, and then 0.8g Co(NO 3 ) 2 Stir to dissolve, and then add 100 ml of methanol solution containing 1.0 g of 2-methylimidazole to obtain a precursor reaction solution.

[0057] (3) The precursor reaction solution obtained in step (2) was stirred and reacted at 40°C for 0.5h, and then stirred and evaporated to dryness at 90°C to obtain gray-purple precursor powder;

[0058] (4) Place the...

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Abstract

The invention discloses a preparation method of nitrogen-doped three-dimensional porous carbon loaded with nano cobalt and an application thereof in lithium sulfur batteries. The method includes the following steps: preparing precursor solution containing an inorganic nanosphere template; preparing a precursor by using cobalt salt and 2-methylimidazole as a cobalt source, a carbon source and a nitrogen source and using inorganic nanospheres as a template, and carbonizing and reducing the precursor at high temperature; and finally, removing part of the template and part of metal cobalt to obtain nitrogen-doped three-dimensional porous carbon loaded with nano cobalt. According to the preparation method provided by the invention, the precursor is prepared through a stirring evaporation solvent method by using cobalt salt as a cobalt source, 2-methylimidazole as a carbon source and a nitrogen source and inorganic nanospheres as a template, which makes the yield of the precursor close to 100%, can improve the yield of the final product, namely, the nitrogen-doped three-dimensional porous carbon loaded with nano cobalt, and is beneficial to large-scale production and preparation. The three-dimensional porous carbon prepared by the preparation method can be used in lithium sulfur batteries to improve the sulfur loading capacity and electrochemical performance of lithium sulfur batteries.

Description

technical field [0001] The invention relates to the technical field of nano-carbon materials and their preparation, in particular to a method for preparing nano-cobalt-loaded nitrogen-doped three-dimensional porous carbon and its application in lithium-sulfur batteries. Background technique [0002] Lithium-sulfur batteries have the advantages of high theoretical specific capacity (1672mAh / g) and high energy density (2600Wh / kg), as well as abundant sulfur resources, low price, and environmental friendliness, and are regarded as the most promising next-generation high-energy batteries. Density secondary power. However, the following problems in lithium-sulfur batteries restrict its performance: (1) The conductivity of the sulfur cathode is poor (only 5×10 -30 S / cm), seriously reducing the utilization rate of sulfur and the rate performance of the battery; (2) the long-chain lithium polysulfide (Li 2 S x , x=3~8) dissolved in the ether electrolyte, forming a "shuttle" effec...

Claims

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Application Information

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IPC IPC(8): H01M4/62H01M4/38H01M10/0525B82Y30/00
CPCH01M4/625H01M4/628H01M4/38H01M10/0525B82Y30/00H01M2004/028H01M2004/021Y02E60/10
Inventor 刘双科吴文植洪晓斌王丹琴郑春满
Owner NAT UNIV OF DEFENSE TECH
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