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Preparation process of phosphorus-and-nitrogen-doped graphene porous carbon composite material

A composite material and preparation technology, which is applied in the manufacture of hybrid/electric double layer capacitors, hybrid capacitor electrodes, etc., can solve the problems of unfavorable industrialization development and complicated experimental process, and achieve the improvement of electron transfer rate and electrochemical activity, preparation method Simple, energy-dense effects

Inactive Publication Date: 2019-03-08
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the multi-experimental process of the existing technology is complicated, which is not conducive to the development of industrialization. The energy density of most of the related work is concentrated at 20Wh kg -1 Therefore, it is still a potential challenge to realize the co-doping of carbon materials with phosphorus and nitrogen, especially doped graphene.

Method used

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  • Preparation process of phosphorus-and-nitrogen-doped graphene porous carbon composite material
  • Preparation process of phosphorus-and-nitrogen-doped graphene porous carbon composite material
  • Preparation process of phosphorus-and-nitrogen-doped graphene porous carbon composite material

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Dissolve 300mg o-phenylenediamine in 8.8mL deionized water, add 7mL graphene oxide (GO) solution (4.3mgmL -1 ) And ultrasonic for 30min, add 4.2mL phosphoric acid solution (2M) and continue ultrasonication for 30min, the obtained GO concentration is 1.5mg mL -1 .

[0035] Transfer the above solution to an autoclave and keep it at 90℃ for 6h. When it is cooled to room temperature, take out the reactant, place it in a 35℃ water bath, add 8.9mL of ferric chloride solution (1M), seal it and let it stand for 24h, and freeze-dry it. mixture.

[0036] 3℃min in a nitrogen environment -1 The rate was raised to 800°C and kept for 2h. After the tube furnace was cooled to room temperature, the samples were collected, and then soaked in 1M hydrochloric acid solution, then washed, dried and passed through a 400 mesh sieve for use. The prepared phosphorus-nitrogen-doped graphene porous carbon composite material is washed and dried. After testing, its specific surface area is 1101.6m 2 g -...

Embodiment 2

[0044] The o-phenylenediamine, phosphoric acid and graphene oxide solution are subjected to hydrothermal reaction, ferric chloride polymerization and freeze drying. Weigh 2g of the obtained sample into a tube furnace and roast it at 700°C for 2h in a nitrogen atmosphere, soak and wash it in a 1M hydrochloric acid solution, then dry and pass through a 400 mesh sieve for use.

[0045] The commercial acetylene black, polytetrafluoroethylene, and phosphorus-nitrogen co-doped graphene porous carbon materials in a ratio of 1:1:8 are mixed uniformly, and a mixed solution of alcohol and water is added to make a slurry, and then evenly spread on 1 cm 2 The stainless steel net is dried and compacted at 20Mpa to prepare super capacitor electrodes.

[0046] After testing, the specific capacitance value of the prepared supercapacitor electrode material is 390F g -1 .

Embodiment 3

[0048] The o-phenylenediamine, phosphoric acid and graphene oxide solution are subjected to hydrothermal reaction, ferric chloride polymerization and freeze drying. Weigh 2g of the obtained sample and put it into a tube furnace in a nitrogen atmosphere to roast at 900°C for 2h, then wash with 1M hydrochloric acid, dry and pass through a 400 mesh sieve for use.

[0049] The commercial acetylene black, polytetrafluoroethylene, and phosphorus-nitrogen co-doped graphene porous carbon materials in a ratio of 1:1:8 are mixed uniformly, and a mixed solution of alcohol and water is added to make a slurry, and then evenly spread on 1 cm 2 The stainless steel net is dried and compacted at 20Mpa to prepare super capacitor electrodes.

[0050] After testing, the specific capacitance value of the prepared supercapacitor electrode material is 274F g -1 .

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Abstract

The present invention relates to a preparation process of a phosphorus-and-nitrogen-doped graphene porous carbon composite material. The preparation process comprises the following steps: (1) hydrothermal reaction: dissolving a nitrogen source into deionized water, adding a graphene oxide solution and performing ultrasound for a pre-set time, adding a phosphorus source and performing ultrasound for a pre-set time to obtain a mixed solution, and then transferring the mixed solution to a high pressure reactor and performing the hydrothermal reaction to obtain a hydrogel, wherein the nitrogen source is one or more of aromatic polyamines, and the phosphorus source is phosphoric acid or phosphate; (2) oxidative polymerization: adding the hydrogel in step (1) into a ferric chloride solution after the hydrogel is cooled, and sealing and standing the mixed solution under a predetermined temperature for a pre-set time to obtain a composite hydrogel; and (3) carbonization activation. The preparation method has the advantages of simplicity, low cost and high production efficiency, no pollutants generate, and the prepared phosphorus-and-nitrogen-doped graphene porous carbon composite materialhas excellent specific capacitance value, high cycle stability, high energy density and excellent electrochemical performance when the material is applied to super capacitor electrodes.

Description

Technical field [0001] The invention belongs to the technical field of preparation of carbon materials for supercapacitors, and specifically relates to a preparation process of a phosphorus-nitrogen-doped graphiteene porous carbon composite material. Background technique [0002] The carbon electrode material of supercapacitors has a multi-layered pore structure, a large specific surface area and abundant active sites are the keys to obtain high electrochemical performance. As a two-dimensional ultra-thin honeycomb carbon structure material, graphene has many outstanding physical, chemical and mechanical properties, so it is widely used in the research field of super capacitor electrode materials. However, graphene materials are expensive, low yield, poor ductility, cumbersome preparation process and other shortcomings, coupled with the small energy gap in the electronic energy spectrum of graphene sheets, easy to stack or agglomerate and other factors, which greatly limit its us...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01G11/32H01G11/26H01G11/86
CPCH01G11/26H01G11/32H01G11/86Y02E60/13
Inventor 魏晓林庹怀金黄首吉高铭阮森彪
Owner XIANGTAN UNIV
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