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Preparation method of three-dimensional nitrogen-doped carbon fibers

A nitrogen-doped carbon fiber, acidified carbon fiber technology, applied in the direction of carbon fiber, fiber processing, fiber chemical characteristics, etc., can solve the problems of the internal material being unable to contact the electrolyte, small effective specific surface area, and few active sites, etc., to achieve nitrogen doping The effect of high volume, good structural stability and simple operation

Inactive Publication Date: 2016-09-21
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, carbon fiber is stacked with multilayer graphene flakes, its effective specific surface area is small, and the active sites only exist on the surface of carbon fiber bundles. When used as an electrode material, the internal material cannot be in contact with the electrolyte, and there are few active sites [Adv Mater, 2013, 25,5956-5970]

Method used

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  • Preparation method of three-dimensional nitrogen-doped carbon fibers
  • Preparation method of three-dimensional nitrogen-doped carbon fibers
  • Preparation method of three-dimensional nitrogen-doped carbon fibers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Add 1 g of commercially available chopped carbon fibers into a mixed solution of 30 mL of commercially available concentrated sulfuric acid and 10 mL of commercially available concentrated nitric acid, and react at 60 °C for 2 hours to obtain acidified carbon fibers.

[0018] (2) Put 1 g of the acidified carbon fiber obtained in step (1) into a crucible, and conduct microwave treatment in a microwave oven with a power of 600 W and a treatment time of 8 seconds.

[0019] (3) Mix 200 mg of the product from step (2) with NH 4 Cl is mixed, and the product of step (2) is mixed with NH 4 The mass ratio of Cl is 1:3.

[0020] (4) the mixture obtained in step (3) in N 2 Heat treatment under atmosphere, the heat treatment temperature is 700°C, and the heat treatment time is 3 hours to obtain three-dimensional nitrogen-doped carbon fibers.

Embodiment 2

[0022] (1) Add 1 g of commercially available chopped carbon fibers into a mixed solution of 30 mL of commercially available concentrated sulfuric acid and 10 mL of commercially available concentrated nitric acid, and react at 60 °C for 3 hours to obtain acidified carbon fibers.

[0023] (2) Put 1 g of the acidified carbon fiber obtained in step (1) into a crucible, and conduct microwave treatment in a microwave oven with a power of 700 W and a treatment time of 6 seconds.

[0024] (3) Mix 200 mg of the product from step (2) with (NH 4 ) 2 SO 4 Mix, step (2) gain and (NH 4 ) 2 SO 4 The mass ratio is 2:3.

[0025] (4) the mixture obtained in step (3) in N 2 Heat treatment under atmosphere, the heat treatment temperature is 800°C, and the heat treatment time is 2 hours, to obtain three-dimensional nitrogen-doped carbon fibers.

Embodiment 3

[0027] (1) Add 1 g of commercially available chopped carbon fibers into a mixed solution of 30 mL of commercially available concentrated sulfuric acid and 10 mL of commercially available concentrated nitric acid, and react at 60 °C for 4 hours to obtain acidified carbon fibers.

[0028] (2) Put 1 g of the acidified carbon fiber obtained in step (1) into a crucible, and conduct microwave treatment in a microwave oven with a power of 800 W and a treatment time of 12 seconds.

[0029] (3) Mix 200 mg of the product from step (2) with (NH 4 ) 2 SO 4 Mix, step (2) gain and (NH 4 ) 2 SO 4 The mass ratio is 1:1.

[0030] (4) the mixture obtained in step (3) in N 2 Heat treatment under atmosphere, the heat treatment temperature is 900° C., and the heat treatment time is 3 hours to obtain three-dimensional nitrogen-doped carbon fibers.

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Abstract

The invention discloses a preparation method of three-dimensional nitrogen-doped carbon fibers. The preparation method comprises steps as follows: (1) 1 g of commercially available short carbon fibers are added to a mixed solution of 30 mL of commercially available concentrated sulfuric acid and 10 mL of commercially available concentrated sulfuric acid, the mixture reacts at the temperature of 60 DEG C for 1-4 hours, and acidized carbon fibers are obtained; (2) 1 g of the acidized carbon fibers are put into a crucible and subjected to microwave treatment in a microwave oven; (3) 200 mg of the product obtained in the step (2) is mixed with ammonium salt; (4) the mixture obtained in the step (3) is subjected to thermal treatment in an N2 atmosphere, and the three-dimensional nitrogen-doped carbon fibers are obtained, wherein ammonium salt is one of NH4Cl, (NH4)2SO4 and (NH4)3PO3. The preparation method is simple to operate, the carbon fibers with stable structures are obtained with a microwave expansion method, inorganic salt is taken as a nitrogen source, nitrogen doping treatment is performed in the thermal treatment process, follow-up cleaning and drying processes are not required, and the obtained product has good structural stability and high nitrogen doping content.

Description

technical field [0001] The invention relates to a preparation method of three-dimensional nitrogen-doped carbon fiber. Background technique [0002] Carbon fibers have high mechanical strength, light weight, high electrical conductivity, and stable chemical properties. They can be used as raw materials for wearable electronic devices, solar cells, supercapacitors, and battery electrode materials [ACS Nano, 2013, 7, 5940-5947]. However, carbon fiber is stacked with multilayer graphene flakes, its effective specific surface area is small, and the active sites only exist on the surface of carbon fiber bundles. When used as an electrode material, the internal material cannot be in contact with the electrolyte, and there are few active sites [Adv Mater, 2013, 25, 5956-5970]. [0003] Ji et al first acidified and oxidized carbon fibers, and then used heat treatment to peel off some graphene sheets on the surface of carbon fibers, increasing the specific surface area and active si...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/12D01F1/10D06M11/55D06M10/06D06M101/40
CPCD01F9/12D01F1/10D06M10/06D06M11/55D06M2101/40
Inventor 罗志虹罗鲲朱旻
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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