Preparation method of three-dimensional nitrogen doped graphene

A technology of nitrogen-doped graphene and graphene, which is applied in the field of preparation of three-dimensional nitrogen-doped graphene, can solve problems such as collapse, high cost, and low output, and achieve simple operation, good structural stability, and low nitrogen doping amount high effect

Inactive Publication Date: 2016-07-06
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Abstract
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  • Application Information

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Problems solved by technology

[0004] Leng Xuanye et al. (Chinese invention patent, CN104777207A) used the foam material as the substrate, and used the CVD method to deposit nitrogen-doped graphene under the condition of a nitrogen source, and obtained three-dimensional unsupported nitrogen-doped graphene after acid etching. However, CVD The cost of the method is hi

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0015] Example 1:

[0016] 1. Put 1 g of commercially available expandable graphite in a crucible, place it in a microwave oven, and treat it with 800W microwave for 8 seconds to obtain three-dimensional graphene.

[0017] 2. Combine 200mg of three-dimensional graphene obtained in step (1) with NH 4 Cl mixing, three-dimensional graphene and NH 4 The mass ratio of Cl is 2:4.

[0018] 3. Put the mixture obtained in step (2) in N 2 In the atmosphere, heat treatment at 800°C for 3 hours to obtain three-dimensional nitrogen-doped graphene.

Example Embodiment

[0019] Example 2:

[0020] 1. Put 1 g of commercially available expandable graphite in a crucible, place it in a microwave oven, and treat it with microwaves at a power of 700W for 6 seconds to obtain three-dimensional graphene.

[0021] 2. Combine 200 mg of three-dimensional graphene obtained in step (1) with NH 4 Cl mixing, three-dimensional graphene and NH 4 NO 3 The mass ratio is 2:1.

[0022] 3. Put the mixture obtained in step (2) in N 2 In the atmosphere, heat treatment at 700°C for 2 hours to obtain three-dimensional nitrogen-doped graphene.

Example Embodiment

[0023] Embodiment 3:

[0024] 1. Put 1 g of commercially available expandable graphite in a crucible, place it in a microwave oven, and treat it with microwaves at a power of 700W for 8 seconds to obtain three-dimensional graphene.

[0025] 2. Combine 200 mg of three-dimensional graphene obtained in step (1) with (NH 4 ) 2 SO 4 Hybrid, three-dimensional graphene and (NH 4 ) 2 SO 4 The mass ratio is 2:3.

[0026] 3. Put the mixture obtained in step (2) in N 2 In the atmosphere, heat treatment at 900°C for 3 hours to obtain three-dimensional nitrogen-doped graphene.

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Abstract

The invention discloses a preparation method of three-dimensional nitrogen doped graphene. The preparation method comprises: (1) putting 1g of commercially-available expandable graphite into a crucible, and putting the crucible in a microwave oven for microwave treatment to obtain three-dimensional graphene, wherein in the process of microwave treatment, the power is 600-800W, and the treatment time is 5-15 seconds; (2) mixing 200mg of the three-dimensional graphene with an ammonium salt, wherein the mass ratio of the three-dimensional graphene to the ammonium salt is 2:(0.5-6); and (3) performing heating treatment on the mixture obtained in the step (2) in a N2 atmosphere to obtain three-dimensional nitrogen doped graphene, wherein the heat treatment temperature is 600-900 DEG C, and the heat treatment time is 2-5 hours; the ammonium salt is one of NH4Cl, (NH4)2SO4 and (NH4)3PO3. The preparation method disclosed by the invention is easy to operate, the three-dimensional graphene with a stable structure is obtained by adopting a microwave expansion method, an inorganic salt is used as a nitrogen source, nitrogen doping treatment is performed in the process of heat treatment, and subsequent cleaning and drying processes are not needed; and the obtained product is good in structural stability and high in nitrogen doping amount.

Description

technical field [0001] The invention relates to a preparation method of three-dimensional nitrogen-doped graphene. Background technique [0002] Graphene is an emerging two-dimensional carbon material, which has the advantages of high electrical conductivity, large specific surface area, and good chemical stability. Doping graphene with nitrogen can adjust its electronic structure, change surface properties, and introduce active groups. . Nitrogen-doped graphene has been widely used in supercapacitors, lithium-air batteries, lithium-ion batteries, and oxygen reduction catalysis. (ACS Appl. Mater. Interfaces, 2014, 6, 6361-6368. Energy Environ. Sci., 2012, 5, 6928-6932; NanoLett., 2014, 14, 1164, 1171.) [0003] Graphene has a planar structure, and single-layer graphene is easy to agglomerate, which will greatly reduce the specific surface area of ​​graphene, thereby reducing its battery capacity and catalytic activity. The construction of a three-dimensional structure can...

Claims

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Application Information

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IPC IPC(8): C01B31/04
CPCC01P2002/85C01P2004/03
Inventor 罗志虹罗鲲朱旻
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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