Preparation method of nitrogen-doped graphene

A nitrogen-doped graphene and graphite technology, applied in capacitors, structural parts, electrical components, etc., can solve problems such as complex process, high cost, and limitations on the application of nitrogen-doped graphene

Active Publication Date: 2012-10-31
OCEANS KING LIGHTING SCI&TECH CO LTD +1
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  • Abstract
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  • Application Information

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Problems solved by technology

However, the traditional preparation method of nitrogen-doped graphene is complex and costly, which limits the further application of nitrogen-doped graphene.

Method used

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preparation example Construction

[0021] Such as figure 1 Shown, the preparation method of the nitrogen-doped graphene of one embodiment, comprises the steps:

[0022] Step S110: Oxidize the graphite raw material to prepare graphite oxide.

[0023] The above-mentioned graphite raw materials can be various forms of graphite powder, such as flake graphite, crystalline graphite and the like. In this embodiment, natural flake graphite with a purity of not less than 99.5% is preferred.

[0024] Among them, the following method can be used to prepare graphite oxide by oxidizing graphite raw materials: adding graphite raw materials, potassium persulfate and phosphorus pentoxide to concentrated sulfuric acid at 80°C, stirring evenly, cooling for more than 6 hours, suction filtration, and washing to Neutral, dry, get a mixed sample;

[0025] Add the mixed sample to concentrated sulfuric acid at 0°C, then add potassium permanganate, keep the temperature of the system below 20°C, then keep it in an oil bath at 35°C fo...

Embodiment 1

[0038] Graphite raw material→graphite oxide→graphene oxide solution→graphene oxide and urea mixed solution→nitrogen-doped graphene

[0039] (1) Graphite raw material: 50 meshes of natural flake graphite with a purity of 99.5%.

[0040] (2) Graphite oxide: Add 20g of graphite raw material, 10g of potassium persulfate and 10g of phosphorus pentoxide into concentrated sulfuric acid at 80°C, stir evenly, cool for more than 6 hours, filter with suction, wash until neutral, and dry to obtain a mixed sample ;

[0041] Add the dried mixed sample to 230mL of concentrated sulfuric acid at 0°C, then add 60g of potassium permanganate, keep the temperature of the system below 20°C, then keep it in an oil bath at 35°C for 2 hours, then slowly add 920mL Deionized water;

[0042] After 15 minutes, add 2.8L of deionized water to the system until the color of the mixture turns bright yellow, filter while hot, then wash with 5L of 10% hydrochloric acid, filter with suction, and dry in vacuum a...

Embodiment 2

[0051] Step (1) and step (2) are the same as embodiment 1.

[0052] (3) Graphene oxide solution: Add the graphite oxide prepared in step (2) into water and ultrasonically disperse for 1 hour to form a graphene oxide solution with a concentration of 0.1 mg / mL uniformly dispersed in a monolithic layer.

[0053] (4) graphene oxide and urea mixed solution: adding mass fraction in the graphene oxide solution of step (3) is 20% urea solution, the volume ratio of graphene oxide solution and urea solution is 10: 1, stirs 10 minutes , so that the two are evenly mixed to obtain a mixed solution of graphene oxide and urea.

[0054] (5) Nitrogen-doped graphene: put the mixed solution obtained in step (4) into a hydrothermal kettle, and perform a hydrothermal reaction at 80° C. to obtain nitrogen-doped graphene.

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Abstract

The invention relates to a preparation method of nitrogen-doped graphene. According to the invention, urea is adopted as a reducing agent, and is subjected to a hydro-thermal reaction with graphene, such that the nitrogen-doped graphene is obtained. According to the invention, the hydro-thermal method is adopted, a relatively high temperature is not required, requirements on equipment are low, and energy can be saved. During the preparation process, urea is adopted as the reducing agent. Urea is advantaged in non-toxicity and low environment pollution. The preparation method is advantaged in simple process, short reaction time, and relatively high efficiency. With the method, the prepared nitrogen-doped graphene is advantaged in good performance.

Description

【Technical field】 [0001] The invention relates to the field of synthesis of nano-carbon materials, in particular to a preparation method of nitrogen-doped graphene. 【Background technique】 [0002] Andre K. Geim (Andre K.Geim) of the University of Manchester in the United Kingdom prepared graphene materials in 2004, and it has received widespread attention due to its unique structure and photoelectric properties. Single-layer graphite has a large specific surface area, excellent electrical and thermal conductivity and low thermal expansion coefficient. In particular, its high conductivity, large specific surface properties and its monolayer two-dimensional nanoscale structural properties can be used as electrode materials in supercapacitors and lithium-ion batteries. There are many traditional methods for preparing graphene, such as: (1) micromechanical exfoliation method, which can only produce a very limited number of graphene sheets, and can only be used as a basic resear...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/1393H01G9/042
CPCY02E60/122Y02E60/10
Inventor 周明杰钟玲珑王要兵
Owner OCEANS KING LIGHTING SCI&TECH CO LTD
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