Preparation method of nitrogen-doped graphene

A nitrogen-doped graphene, graphene technology, applied in graphene, chemical instruments and methods, nano-carbon and other directions, can solve the problem of difficult popularization and application of the method

Active Publication Date: 2013-10-23
OCEANS KING LIGHTING SCI&TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The traditional method of preparing nitrogen-doped graphene is mainly by vapor deposition or arc discharge method

Method used

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  • Preparation method of nitrogen-doped graphene

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preparation example Construction

[0018] see figure 1 , The preparation method of nitrogen-doped graphene according to one embodiment includes the following steps.

[0019] Step S101, placing graphite oxide under an inert gas atmosphere, rapidly raising the temperature to 200-400° C., keeping the temperature for 0.5-2 hours, and cooling to room temperature to obtain graphene oxide.

[0020] Preferably, the graphite oxide is placed under an argon atmosphere with a flow rate of 400ml / min, the temperature of the graphite oxide is raised from room temperature to 300°C at a rate of 15°C / min, and kept for 1 hour, and then the flow rate is 200ml / min atmosphere was cooled to room temperature to obtain graphene oxide. It can be understood that the inert gas may also be helium, neon or the like.

[0021] Graphite oxide can be purchased or prepared by the following methods:

[0022] Add graphite into the mixed solution of concentrated sulfuric acid and concentrated nitric acid, stir in an ice-water mixing bath, then ...

Embodiment 1

[0033] Step (1), providing graphite with a purity of 99.5%.

[0034] Step (2), take by weighing the graphite 1g that purity is 99.5% in the step (1), add in the mixed solution that is made up of 92ml vitriol oil (mass fraction is 98%) and 24ml concentrated nitric acid (mass fraction is 65%), the mixture Stir in an ice-water mixed bath environment for 20 minutes, then slowly add 10g of potassium permanganate to the mixture, stir for 1 hour, then heat the mixture to 85°C and keep it for 30 minutes, then add 92ml of deionized water to continue Keep at 85°C for 30 minutes, finally add 10ml hydrogen peroxide solution (mass fraction 30%), stir for 10 minutes, filter the mixture with suction, then wash the solids with 100ml dilute hydrochloric acid and 150ml deionized water successively, Washed three times in total, and finally the solid matter was dried in a vacuum oven at 60° C. for 12 hours to obtain graphite oxide.

[0035] Step (3), place the graphite oxide obtained in step (2)...

Embodiment 2

[0042] Step (1), providing graphite with a purity of 99.5%.

[0043]Step (2), take by weighing the graphite 1g that purity is 99.5% in the step (1), add in the mixed solution that is made up of 90ml vitriol oil (mass fraction is 98%) and 30ml concentrated nitric acid (mass fraction is 65%), the mixture Stir in an ice-water mixed bath environment for 20 minutes, then slowly add 10g of potassium permanganate to the mixture, stir for 1 hour, then heat the mixture to 70°C and keep it for 30 minutes, then add 92ml of deionized water to continue Keep at 85°C for 30 minutes, finally add 10ml hydrogen peroxide solution (mass fraction 30%), stir for 10 minutes, filter the mixture with suction, then wash the solids with 100ml dilute hydrochloric acid and 150ml deionized water successively, Washed three times in total, and finally the solid matter was dried in a vacuum oven at 60° C. for 12 hours to obtain graphite oxide.

[0044] Step (3), place the graphite oxide obtained in step (2) ...

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Abstract

The invention provides a preparation method of nitrogen-doped graphene. The preparation method comprises the following steps of putting graphite oxide in the atmosphere of inert gas, heating the mixture to 200-400 DEG C quickly, preserving heat for 0.5-2 hours, and cooling the product to the room temperature, thus obtaining graphene oxide; and mixing the graphene oxide with urea, putting the mixture in the atmosphere of a mixture of inert gas and ammonia gas, heating the mixture to 800-1100 DEG C at a heating rate of 1-10 DEG C/min, preserving heat for 0.5-2 hours, and cooling the product to the room temperature, thus obtaining the nitrogen-doped graphene. In the preparation method, an oxidative thermal reduction method is utilized to prepare the single-layer nitrogen-doped graphene, so that the preparation is simple in equipment and process, convenient to operate, cheap in raw materials, low in cost and easy in achievement of large-scale industrial production.

Description

【Technical field】 [0001] The invention relates to a preparation method of nitrogen-doped graphene. 【Background technique】 [0002] Due to its two-dimensional monolayer structure and excellent physical properties, such as high theoretical specific surface area, excellent mechanical strength, good flexibility and high electrical conductivity, graphene has attracted great attention from researchers from various industries. Graphene will revolutionize materials in electronics, energy and more. At present, graphene with less than 10 layers can be called graphene. Most of the prepared graphene has more than 1 layer. Since single-layer graphene can maximize its advantages, It is the goal pursued by researchers. At present, the method for preparing single-layer graphene is mainly chemical vapor deposition (CVD method), and the amount of single-layer graphene prepared by this method is very small, and the process is complicated, so it is difficult to realize industrial production. ...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B32/184C01B32/194
Inventor 周明杰钟辉王要兵
Owner OCEANS KING LIGHTING SCI&TECH CO LTD
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