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Preparation method of high-performance nitrogen-doped three-dimensional graphene

A graphene and nitrogen doping technology, which is applied in graphene, chemical instruments and methods, hybrid/electric double layer capacitor manufacturing, etc., can solve the problems of limiting the application of nitrogen-doped three-dimensional graphene and the limited amount of nitrogen doping, etc. Achieving the effect of excellent electrochemical performance and simple preparation method

Active Publication Date: 2016-06-08
NANJING UNIV OF POSTS & TELECOMM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the amount of nitrogen doping on 3D graphene is currently limited, which greatly limits the application of nitrogen doped 3D graphene.

Method used

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  • Preparation method of high-performance nitrogen-doped three-dimensional graphene
  • Preparation method of high-performance nitrogen-doped three-dimensional graphene
  • Preparation method of high-performance nitrogen-doped three-dimensional graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] The preparation of the nitrogen-doped three-dimensional graphene of the present embodiment is as follows:

[0047] Step S1: using graphite to prepare graphene oxide; it is prepared by improving the Hummers method, and the specific steps include:

[0048] (1) Take 5g of 300 mesh expandable graphite, add 150ml of concentrated sulfuric acid and 50ml of fuming nitric acid each, stir at room temperature for 24h pre-expansion, dilute the mixed solution with 1L of deionized water, filter and wash the diluted solution 3 times, and collect the product Dry it in the air, and then heat it with microwave 1800W for 60s to completely expand the graphite.

[0049] (2) Take 5g of expanded graphite and add 300ml of concentrated sulfuric acid, 4.2g of potassium persulfate, 6.2g of phosphorus pentoxide and stir at 60°C for 5h. After the reaction, wash with deionized water and filter, dry for one day to obtain pre-oxidized graphite .

[0050] (3) Add 200ml of concentrated sulfuric acid a...

Embodiment 2

[0056] The preparation of the nitrogen-doped three-dimensional graphene of the present embodiment is as follows:

[0057] Step S1: using graphite to prepare graphene oxide; it is prepared by improving the Hummers method, and the specific steps include:

[0058] (1) Take 5g of 300 mesh expandable graphite, add 150ml of concentrated sulfuric acid and 50ml of fuming nitric acid each, stir at room temperature for 24h pre-expansion, dilute the mixed solution with 1L of deionized water, filter and wash the diluted solution 3 times, and collect the product Dry it in the air, and then heat it with microwave 1800W for 40s to fully expand the graphite.

[0059] (2) Add 5 g of expanded graphite to 300 ml of concentrated sulfuric acid, 4.2 g of potassium persulfate, and 6.2 g of phosphorus pentoxide and stir at 80° C. for 3 h. After the reaction, wash with deionized water and filter, dry for one day, and collect pre-oxidized graphite.

[0060] (3) Add 200ml of concentrated sulfuric acid ...

Embodiment 3

[0066] The preparation of the nitrogen-doped three-dimensional graphene of the present embodiment is as follows:

[0067] Step S1: using graphite to prepare graphene oxide; it is prepared by improving the Hummers method, and the specific steps include:

[0068] (1) Take 5g of 300 mesh expandable graphite, add 150ml of concentrated sulfuric acid and 50ml of fuming nitric acid each, stir at room temperature for 24h pre-expansion, dilute the mixed solution with 1L of deionized water, filter and wash the diluted solution 3 times, and collect the product Dry it in the air, and then heat it with microwave 1800W for 40s to fully expand the graphite.

[0069] (2) Add 5 g of expanded graphite to 300 ml of concentrated sulfuric acid, 4.2 g of potassium persulfate, and 6.2 g of phosphorus pentoxide and stir at 80° C. for 5 h. After the reaction, wash with deionized water and suction filter, and dry for one day to obtain pre-oxidized graphite.

[0070] (3) Add 200ml of concentrated sulfu...

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Abstract

The invention relates to the technical field of synthesizing of graphene materials and provides a preparation method of nitrogen-doped graphene. The preparation method includes: using an improved Hummers method to prepare continuous large-piece graphene oxide; using a hydrothermal method to prepare the graphene oxide into graphene of a porous three-dimensional structure; ultrasonically dispersing the graphene of the porous three-dimensional structure into an acid solution with the pH being 1-5, adding aniline, well mixing, adding ammonium persulfate, well mixing, and transferring the obtained mixed liquid into a teflon container for hydrothermal reaction so as to obtain a porous three-dimensional graphene-polyaniline compound; performing high-temperature treatment under nitrogen protection to allow polyaniline to decompose out nitrogen sources so as to obtain the nitrogen-doped porous three-dimensional graphene. The method has the advantages that the nitrogen-doped graphene with high nitrogen content can be prepared, the structure of the three-dimensional graphene can be kept, the obtained nitrogen-doped porous three-dimensional graphene is good in electrochemical performance and quite suitable for being used for producing a super capacitor, and the method is convenient to operate and beneficial to industrial popularization.

Description

technical field [0001] The invention relates to the technical field of synthesis of graphene materials, in particular to a preparation method of high-performance nitrogen-doped graphene. Background technique [0002] Graphene is a two-dimensional honeycomb network structure composed of single atomic layers of carbon, which is the basic unit of other graphite materials. The basic structural unit of graphene is a benzene six-membered ring, which is currently the most ideal two-dimensional nanomaterial. Graphene is close to a perfect material, but in order to expand its practical application in the fields of energy, environment and biology, it is necessary to self-assemble two-dimensional graphene into a three-dimensional graphene structure. Such a three-dimensional structure not only has some properties of graphene itself, but also has its own unique characteristics. [0003] Three-dimensional graphene is stacked by single atomic layers of carbon, which has better electrical...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04H01G11/32H01G11/86
CPCY02E60/13H01G11/32C01B2204/22C01B2204/32C01P2004/03C01P2004/30H01G11/86
Inventor 闵永刚肖壮青申佳欣冯亚飞
Owner NANJING UNIV OF POSTS & TELECOMM
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