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Preparation method of three-dimensional nitrogen-doped graphene

A nitrogen-doped graphene, three-dimensional technology, applied in the field of preparation of three-dimensional nitrogen-doped graphene, can solve the problems of complex preparation process, and achieve the effect of simple operation, accelerated reaction and easy control

Active Publication Date: 2015-07-22
QINGDAO UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the nitrogen-doped graphene prepared by electrochemical method, the nitrogen element exists at the edge of the graphene sheet and does not enter the graphene sheet. In addition, the preparation process of this method is relatively complicated.

Method used

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  • Preparation method of three-dimensional nitrogen-doped graphene

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Embodiment 1 3

[0030] The preparation of embodiment 1 three-dimensional nitrogen-doped graphene

[0031]Utilize the improved Hummer method to prepare graphene oxide (GO), first add 2.5g expanded graphite and 5g sodium nitrate in 500mL beaker, then add 120mL mass concentration to it to be the concentrated sulfuric acid of 98% then, the mixture that obtains is in ice bath condition Stir for 120min under high temperature; then under the condition of vigorous stirring, slowly add 15g of potassium permanganate to the obtained mixture for reaction, the temperature of the reaction is controlled below 20°C; remove the ice bath after completing the addition of potassium permanganate equipment, the resulting reaction product was stirred overnight at room temperature. Finally, 150 mL of secondary water was added dropwise to the beaker under vigorous stirring, and the reaction temperature rose rapidly to 98° C., and foam generation was observed, and the color of the reaction product in the beaker turned...

Embodiment 2

[0040] The ratio of the addition of thioacetamide and graphene oxide is 3:1, and other conditions are with embodiment 1. The obtained nitrogen-doped three-dimensional graphene has a nitrogen content as high as 6.7%, and the capacity retention rate is as high as 94.5% after charging and discharging 10,000 times.

Embodiment 3

[0042] The ratio of the addition of thioacetamide and graphene oxide is 8:1, and other conditions are with embodiment 1. The obtained nitrogen-doped three-dimensional graphene has a nitrogen content as high as 8.5%, and the capacity retention rate is as high as 96.1% after charging and discharging 10,000 times.

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Abstract

The invention discloses a preparation method of three-dimensional nitrogen-doped graphene, which adopts a dual-function reagent thioacetamide solution process to synthesize the three-dimensional nitrogen-doped graphene (3D G-N). The method comprises the following steps: thioacetamide is decomposed into NH3 and H2S during hydrolysis, and the NH3 is used as a nitrogenous component to implement nitrogen doping of the graphene (G-N); when Zn<2+> exists in the solution, S<2-> and the Zn<2+> form a ZnS particle precipitate which is dispersed among the nitrogen-doped graphene lamellae; and dilute hydrochloric acid is utilized to dissolve out the ZnS to obtain the porous three-dimensional nitrogen-doped graphene. The preparation method is simple and environment-friendly, and can greatly widen the application of the graphene in the fields of optics, electricity, magnetics and the like.

Description

technical field [0001] The invention belongs to the technical field of carbon materials, and in particular relates to a preparation method of three-dimensional nitrogen-doped graphene. Background technique [0002] Graphene (G), due to its unparalleled specific surface area and electrical conductivity, has led a new wave of research on carbon nanomaterials. However, graphene sheets are easy to agglomerate under the action of van der Waals force, which reduces its active surface area and application stability. The porous three-dimensional graphene greatly reduces the agglomeration effect of graphene due to its special spatial structure, thereby maintaining a high catalytically active surface area. However, based on current research, the controllable preparation of high-performance 3D graphene composites is still a challenging topic. Theoretical studies have shown that the energy band structure of graphene will be adjusted after nitrogen doping, which can greatly expand the ...

Claims

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Application Information

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IPC IPC(8): C01B31/00
Inventor 王宗花赵凯赵春芹杨敏张菲菲夏建飞桂日军毕赛
Owner QINGDAO UNIV
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