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Preparation method of graphene

A graphene and fluorinated graphite technology, applied in the field of nanomaterial preparation, can solve the problems of low atomic ratio of C and O in graphene, and achieve the effects of large sheet area, easy mass production, and pure product

Inactive Publication Date: 2014-02-19
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition to the chemical reduction method, graphite oxide can also be reduced to graphene by electrochemical methods, but the ratio of C and O atoms in the graphene prepared by this method is low

Method used

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  • Preparation method of graphene
  • Preparation method of graphene

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Mix sodium chloride, potassium chloride, and zinc chloride in a mass ratio of 1:1:3, heat at 250°C for 30 minutes to melt, then mix 100mg of graphite fluoride with 5g of the above molten salt, and heat at 300°C Heat for 10 hours to carry out thermal intercalation reaction. After the heating time is over, add the above-mentioned intercalation complex to 200mL N-methylpyrrolidone, and then ultrasonicate the resulting suspension at 200W power for 12 hours. After the ultrasonic time is over, the ultrasonicated suspension Centrifuge at a speed of 2000r / min for 20min to remove the solid in the lower layer, suction filter the obtained solution, wash with deionized water three times, and then dry the obtained filter cake at 60°C to obtain a graphene material.

Embodiment 2

[0019] Mix sodium chloride, potassium chloride, and zinc chloride in a mass ratio of 1:1:3, heat at 250°C for 30 minutes to melt, then mix 200mg of graphite fluoride with 5g of the above molten salt, and heat at 280°C Heated for 12 hours to perform thermal intercalation reaction. After the heating time was over, the above intercalation complex was added to 200 mL of dimethylformamide, and then the resulting suspension was ultrasonicated at 200 W for 10 hours. After the ultrasonic time was over, the ultrasonic suspension was The solution was centrifuged at a speed of 1000r / min for 20min to remove the solid in the lower layer, the obtained solution was suction-filtered, washed three times with deionized water, and then the obtained filter cake was dried at 60°C to obtain a graphene material.

Embodiment 3

[0021] Mix sodium chloride, potassium chloride, and zinc chloride in a mass ratio of 1:1:3, heat at 250°C for 30 minutes to melt, then mix 100mg of graphite fluoride with 5g of the above molten salt, and heat at 200°C Heated for 12 hours to carry out thermal intercalation reaction. After the heating time was over, the above intercalation complex was added to 200 mL of isopropanol, and then the resulting suspension was ultrasonicated for 12 hours at a power of 200 W. After the ultrasonic time was over, the ultrasonicated suspension was placed in Centrifuge at a speed of 3000r / min for 15min to remove the solids in the lower layer, suction filter the obtained solution, wash with deionized water three times, and then dry the obtained filter cake at 60°C to obtain a graphene material.

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Abstract

The invention discloses a preparation method of graphene. The preparation method is implemented according to the following steps: mixing evenly sodium chloride, potassium chloride and zinc chloride, to prepare a molten salt with a low melting point, carrying out thermal intercalation of graphite fluoride by using the molten salt, and carrying out the intercalation process and a reaction process atthe same time to obtain better intercalation effect; carrying out ultrasonic stripping of the intercalation composite; centrifuging to remove the intercalation composite which is not stripped, carrying out suction filtration of the centrifuged upper solution, and washing to obtain graphene. The preparation method does not require high temperature and high vacuum conditions and special reaction instruments; and compared with other preparation methods of the graphene material, the preparation method has simple preparation process and low preparation cost, and allows the obtained graphene to have large sheet area, fewer sheet layers, and high regularity.

Description

technical field [0001] The invention relates to a preparation method of graphene, which belongs to the field of nanometer material preparation. Background technique [0002] In 2004, British scientists first prepared graphene, a two-dimensional atomic crystal composed of a single atomic layer of carbon atoms, with a thickness of only 0.3354nm, which is the thinnest material found in the world so far. Graphene has a special monoatomic layer structure and novel physical properties: the strength reaches 130GPa, the thermal conductivity is about 5000J / (m·K·s), and the carrier mobility reaches 2×10 5 cm 2 / (V s), the theoretical calculation value of the specific surface area is 2630m 2 / g, high transparency (about 97.7%), and almost zero bandgap, it also has a series of properties such as fractional quantum Hall effect, quantum Hall ferromagnetism, and minimum quantum conductivity at the limit of zero carrier concentration. In the past few years, graphene has become a research...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/19
Inventor 封伟孙传彬冯奕钰李瑀
Owner TIANJIN UNIV
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