Preparation method of graphene

A technology of graphene and graphite, which is applied in the field of new material synthesis, can solve the problems of low yield and high number of graphene layers, and achieve the effects of high yield, strong conductivity and simple equipment

Inactive Publication Date: 2014-03-26
OCEANS KING LIGHTING SCI&TECH CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, this method mainly adopts some solvents (such as methylpyrrolidone) as the liquid phase, and the number of layers of the prepared graphene is high, and the yield is low.

Method used

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Examples

Experimental program
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Embodiment 1

[0024] A kind of preparation method of graphene, comprises the following steps:

[0025] (1) Mix 5g of graphite with a purity of 99.5% and 5g of 1-butyl-3-methylimidazole bistrifluoromethanesulfonimide salt, and use an ultrasonic machine with a power of 1000W to ultrasonicate the mixture for 24 hours. Hour, obtain intercalated graphite;

[0026] (2) Place the above-mentioned intercalated graphite in a reactor with argon (400mL / min) atmosphere, and raise the ambient temperature of the intercalated graphite to 900°C at a heating rate of 30°C / min, and keep it for 0.5 hours, Then it was lowered to room temperature in an argon (400 mL / min) atmosphere, and the reaction product was collected to obtain graphene.

[0027] Adopt atomic force microscope (AFM) to observe 100 parts of graphene prepared in this embodiment, its layer number distribution result is as follows figure 1 shown. figure 1 It is the distribution diagram of the number of layers of graphene prepared in Example 1 of...

Embodiment 2

[0029] A kind of preparation method of graphene, comprises the following steps:

[0030] (1) Mix 10g of graphite with a purity of 99.5% and 15g of 1-butyl-3-methylimidazole bistrifluoromethanesulfonimide salt, and use an ultrasonic machine with a power of 1000W to ultrasonicate the mixture for 36 Hour, obtain intercalated graphite;

[0031] (2) Place the above-mentioned intercalated graphite in a reactor with argon (300mL / min) atmosphere, and raise the ambient temperature of the intercalated graphite to 800°C at a heating rate of 25°C / min, and keep it for 1 hour, Then it was lowered to room temperature in an argon (300 mL / min) atmosphere, and the reaction product was collected to obtain graphene.

[0032] Adopt atomic force microscope (AFM) to observe 100 parts of graphenes prepared in this embodiment, the number of layers of graphene sheets prepared in this embodiment is 1~5 layers, wherein, the number of layers of 85% graphenes It is 1~3 layers.

Embodiment 3

[0034] A kind of preparation method of graphene, comprises the following steps:

[0035] (1) Mix 50g of graphite with a purity of 99.5% and 80g of 1-butyl-3-methylimidazole bistrifluoromethanesulfonimide salt, and use an ultrasonic machine with a power of 1000W to ultrasonicate the mixture for 48 Hour, obtain intercalated graphite;

[0036] (2) Place the above-mentioned intercalated graphite in a reactor with a helium (300mL / min) atmosphere, and raise the ambient temperature of the intercalated graphite to 700°C at a heating rate of 20°C / min, and keep it for 1 hour, Then it was lowered to room temperature in a helium (300 mL / min) atmosphere, and the reaction product was collected to obtain graphene.

[0037]Adopt atomic force microscope (AFM) to observe 100 parts of graphenes prepared in this embodiment, the number of layers of the graphene sheets prepared in this embodiment is 1~5 layers, wherein, the number of layers of 90% graphenes It is 1~3 layers.

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Abstract

The invention provides a preparation method of graphene, which comprises the following steps: (1) mixing graphite and an ionic liquid in a mass ratio of 1:(0.5-5), and carrying out ultrasonic dispersion for 10-48 hours to obtain intercalation graphite of which the intercalation compound is the ionic liquid, wherein the ionic liquid is an imidazole ionic liquid or pyrrolidine ionic liquid; and (2) putting the intercalation graphite in a reactor in an inert gas protective atmosphere, heating to 700-900 DEG C, keeping for 0.5-1 hour, cooling to room temperature in the inert gas protective atmosphere, and collecting the solid product which is the graphene. The method has the advantages of simple equipment and simple and feasible operation, and can easily implement large-scale industrial production; the prepared graphene has the characteristics of high yield, smaller number of layers, favorable mechanical properties and high conductivity; and compared with the common graphene prepared by a redox process, the graphene prepared by the method provided by the invention has the advantages of fewer defects, complete crystal structure and the like.

Description

technical field [0001] The invention relates to the field of new material synthesis, in particular to a method for preparing graphene. Background technique [0002] Graphene is a two-dimensional carbon atom crystal discovered by Andre K. Geim of the University of Manchester in 2004. Due to its unique structure and photoelectric properties, it has become a research hotspot in the fields of carbon materials, nanotechnology, condensed matter physics and functional materials, attracting many scientific and technological workers. Single-layer graphene has excellent electrical and thermal conductivity and low thermal expansion coefficient, and its theoretical specific surface area is as high as 2630m 2 / g (A Peigney, Ch Laurent, et al. Carbon, 2001, 39, 507), can be used in effect transistors, electrode materials, composite materials, liquid crystal display materials, sensors, etc. At present, the methods for preparing graphene mainly include mechanical exfoliation, epitaxial gr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/186
Inventor 周明杰王要兵钟辉袁新生
Owner OCEANS KING LIGHTING SCI&TECH CO LTD
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