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Method for preparing graphene by solution phase

A graphene and solution phase technology, applied in the field of solution phase preparation of graphene, can solve the problems of difficult large-scale preparation, harsh process conditions, complex process, etc., and achieve easy industrial production, low energy consumption of the preparation process, and simple preparation process Effect

Active Publication Date: 2013-04-24
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The graphene prepared by this method has a large area, but it often requires complex equipment, and the process conditions are harsh, making it difficult to prepare on a large scale
In addition to the above methods, silicon carbide epitaxial growth method (Berger C et al., Science, 312, 1191-1196), organic synthesis method (Zhi L J et al., J.Mater.Chem.18, 1472-1484) etc. are also applied The preparation of graphene, but these methods have their own disadvantages, such as complicated process, difficult to control, low output, high cost, etc.

Method used

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  • Method for preparing graphene by solution phase
  • Method for preparing graphene by solution phase
  • Method for preparing graphene by solution phase

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 100mg of graphite powder to 150mL of freshly dried tetrahydrofuran solution, ultrasonically disperse for 3min under nitrogen protection, then add 0.36g of metal lithium and 4.9g of naphthalene to the dispersion, and keep stirring for 35min. 12.5 g of 1-bromododecane was gradually added to the above mixture, and the reaction was continued for 12 h under nitrogen protection.

[0028] Add ethanol to the above reaction product to remove unreacted metal lithium. The resulting solid product was washed successively with ethanol, toluene, water and ethanol, and dried under vacuum at 60°C to obtain graphene powder.

[0029] figure 1 B is the macroscopic morphology figure of the graphene powder obtained in the present invention, and figure 1 Compared with the commercially available graphite powder of a, it is obviously fluffy. Graphene gained in the present invention is observed with a scanning electron microscope and a transmission electron microscope, and the obtained re...

Embodiment 2

[0031] Add 100mg of graphite powder to the freshly dried tetrahydrofuran solution, ultrasonically disperse for 3min under nitrogen protection, then add 0.36g of metal lithium and 4.9g of naphthalene to the mixture, and keep stirring for 35min. Gradually added 9.7g of 6-bromohexanoic acid to the above mixture, and reacted for 12h under nitrogen protection.

[0032] Add ethanol to the above reaction product to remove unreacted metal lithium. The resulting solid product was washed successively with ethanol, toluene, water and ethanol, and dried under vacuum at 60°C to obtain graphene powder. The obtained graphene powder can be dispersed in ethanol or aqueous solution by ultrasonic treatment.

Embodiment 3

[0034]Add 100mg of graphite powder to the freshly dried tetrahydrofuran solution, ultrasonically disperse for 3min under nitrogen protection, then add 0.36g of metal lithium and 4.9g of naphthalene to the mixed solution, and keep stirring for 35min. 11.6 g of methyl 6-bromohexanoate was gradually added to the above mixture, and reacted for 12 h under nitrogen protection.

[0035] Add ethanol to the above reaction product to remove unreacted lithium metal. The resulting solid product was washed successively with ethanol, toluene, water, and ethanol, and dried under vacuum at 60°C to obtain graphene powder.

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Abstract

The invention discloses a method for preparing graphene by a solution phase, and relates to grephene. The invention provide a method for preparing graphene by the solution phase, which is low in cost, simple and easy to implement, low in device requirements, and beneficial to large-scale industrial production. The method comprises the following steps: (1) adding graphite powder to a tetrahydrofuran solution and obtaining graphite-powder tetrahydrofuran dispersion liquid by carrying out ultrasonic dispersion under the protection of nitrogen gas; (2) adding alkali metal and naphthalene to the graphite-powder tetrahydrofuran dispersion liquid obtained in the step (1), stirring under the protection of the nitrogen gas to obtain the mixed solution; (3) adding halogenated organic reagent to the mixed solution obtained in the step (2), and reacting under the protection of the nitrogen gas to obtain a solid product; and (4) washing and drying the solid product obtained in the step (3) to obtain the graphene powder. According to the method disclosed by the invention, liquid-phase chemical intercalation is carried out to the graphite by using the graphite powder as material; and then, the chemical modification of the halogenated organic reagent to the graphite is utilized for further opening the graphite, so that the graphene can be prepared by peeling the graphite under the non-ultrasonic action or the light ultrasonic action.

Description

technical field [0001] The invention relates to graphene, in particular to a method for preparing graphene in a solution phase. Background technique [0002] Graphene is a completely sp 2 A new type of two-dimensional carbon material with a thickness of only one atom composed of hybrid carbon atoms. Since it was first prepared in 2004, graphene has attracted widespread attention due to its unique structure and excellent properties, such as high specific surface area, high charge mobility, high strength and flexibility, high thermal conductivity, etc., and is expected to be used in energy materials. , nanoelectronic devices, composite materials, optoelectronic devices, sensors and other fields have been widely used. [0003] Graphene was originally isolated from highly oriented pyrolytic graphite by micromechanical exfoliation (Novoselov K S et al., Science, 2004, 306:666-669), but the yield of this method is small and it is only suitable for basic research. The low-cost a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/19
Inventor 邓顺柳冯蓝刘跃文谢素原黄荣彬郑兰荪
Owner XIAMEN UNIV
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