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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 problems of decreasing specific surface area and limiting the application prospects of graphene

Active Publication Date: 2016-08-03
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

However, since supercapacitors and lithium-ion batteries have certain requirements for energy storage electrode materials, especially for supercapacitor electrode materials, the higher the specific surface area, the better the energy storage performance; for lithium-ion battery materials, although a high specific surface area is not required surface area, but has a certain specific surface area (such as 700m 2 / g~1000m 2 / g) Its energy storage performance is also greatly improved
Although the theoretical specific surface area of ​​graphene reaches 2630m 2 / g, but due to the stacking of graphene sheets in graphene materials, the specific surface area is greatly reduced. The highest specific surface area reported in the literature is 600m 2 / g, which greatly limits the application prospects of graphene in supercapacitors and lithium-ion battery electrode materials

Method used

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preparation example Construction

[0023] see figure 1 , The preparation method of nitrogen-doped graphene according to one embodiment includes the following steps.

[0024] Step S101, preparing graphite oxide.

[0025] Using graphite as a raw material, preferably, graphite with a purity of 99.5% can be used as a raw material, adding graphite to a mixed solution of concentrated sulfuric acid and concentrated nitric acid, stirring in an ice-water mixed bath, and then adding permanganate to the mixed solution Potassium, to oxidize the graphite, then heat the mixed solution to 70-95°C and keep it warm, further oxidize the graphite, finally add hydrogen peroxide to remove potassium permanganate, filter with suction, and use dilute hydrochloric acid and deionized water to treat the solid Repeated washing and drying to obtain graphite oxide. The volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 90-95:20-30; the mass ratio of the graphite to potassium permanganate is 1:3-10.

[0026]...

Embodiment 1

[0038] Step (1), providing graphite with a purity of 99.5%.

[0039] Step (2), with the graphite that purity is 99.5% in (1) as raw material, take by weighing the graphite 1g that purity is 99.5% in step (1), add by 92ml vitriol oil (massfraction is 98%) and 24ml concentrated nitric acid ( Mass fraction is 65%) in the mixed solution that forms), the mixture is placed in the ice-water mixing bath environment and stirred for 20 minutes, then slowly adds 10g potassium permanganate to the mixture, stirs for 1 hour, then the mixture is heated to 85°C and keep it for 30 minutes, then add 92ml of deionized water and continue to keep it at 85°C for 30 minutes, finally add 10ml of hydrogen peroxide solution (mass fraction 30%), stir for 10 minutes, filter the mixture with suction, and then use 100ml of dilute hydrochloric acid and 150ml of deionized water were used to wash the solid matter three times in total, and finally the solid matter was dried in a vacuum oven at 60°C for 12 hour...

Embodiment 2

[0049] Step (1), providing graphite with a purity of 99.5%.

[0050] Step (2), with the graphite that purity is 99.5% in (1) as raw material, take by weighing the graphite 1g that purity is 99.5% in step (1), add by 90ml vitriol oil (massfraction is 98%) and 28ml concentrated nitric acid ( Mass fraction is 65%) in the mixed solution that forms), the mixture is placed in the ice-water mixing bath environment and stirred for 20 minutes, then slowly adds 8g potassium permanganate to the mixture, stirs for 1 hour, then the mixture is heated to 85°C and keep it for 30 minutes, then add 92ml of deionized water and continue to keep it at 85°C for 30 minutes, finally add 10ml of hydrogen peroxide solution (mass fraction 30%), stir for 10 minutes, filter the mixture with suction, and then use 100ml of dilute hydrochloric acid and 150ml of deionized water were used to wash the solid matter for three times, and finally the solid matter was dried in a vacuum oven at 60°C for 12 hours to o...

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Abstract

The invention provides a preparation method of nitrogen-doped graphene. The preparation method comprises the following steps of dispersing graphite oxide in deionized water, carrying out ultrasonic processing, and then leaching and drying the product to obtain graphene oxide; adding the graphene oxide and silicon dioxide to the deionized water in sequence, stirring the materials for 2-4 hours, filtering the solution, and drying the product to obtain a graphene oxide / silicon dioxide mixture; putting the graphene oxide / silicon dioxide mixture in the atmosphere of a mixture of inert gas and ammonia gas, heating the mixture to 800-1000 DEG C at a heating rate of 5-20 DEG C / min, preserving heat for 30-120 minutes, and cooling the product to the room temperature, thus obtaining a nitrogen-doped graphene / silicon dioxide mixture; and adding the nitrogen-doped graphene / silicon dioxide mixture to a hydrofluoric acid solution, stirring the mixture for 12-24 hours, leaching in vacuum, washing and drying, thus obtaining the nitrogen-doped graphene.

Description

【Technical field】 [0001] The invention relates to a preparation method of nitrogen-doped graphene. 【Background technique】 [0002] Graphene has a two-dimensional monolayer structure (thickness is only 0.335nm), and has excellent electrical conductivity, high theoretical specific surface area, good mechanical properties and flexibility. with broadly application foreground. The use of graphene in the field of energy storage is a focus of current development, such as graphene used in supercapacitors and lithium-ion battery electrode materials. However, since supercapacitors and lithium-ion batteries have certain requirements for energy storage electrode materials, especially for supercapacitor electrode materials, the higher the specific surface area, the better the energy storage performance; for lithium-ion battery materials, although a high specific surface area is not required surface area, but has a certain specific surface area (such as 700m 2 / g~1000m 2 / g) has also ...

Claims

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Application Information

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