Preparation method of graphene

A graphene and solvent technology, applied in the field of synthesis of inorganic chemical materials, can solve the problems of low cost, complex process conditions, and low yield, and achieve good reproducibility, mild reaction conditions, and simple process

Active Publication Date: 2012-01-18
TIANJIN UNIV
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  • Claims
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Problems solved by technology

[0004] However, the yield of graphene prepared based on the micromechanical exfoliation method is very low, and a small amount of exfoliation is doped with many multilayer graphite sheets
The biggest advantage of the chemical vapor deposition method is the formation of graphene on the conductive substrate, which provides the possibility for the next step in the application of electronics, but the process conditions are complex
The graphene oxide reduction method is a feasible method for large-scale synthesis of graphene. Although this method is simple and low-cost, it can produce a large amount of graphene, but because graphite oxide cannot be completely reduced, some physical problems are caused. , chemical and other performance loss

Method used

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  • Preparation method of graphene
  • Preparation method of graphene

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Embodiment 1

[0043] Put 20mL of diethylene glycol dimethyl ether in a 50mL round bottom flask, then add 0.04g of hexabromobenzene (equivalent to 2mg / mL) and 0.01g of CuBr (equivalent to 0.5mg / mL), stir, and After 30 minutes of pure Ar gas, the oil bath was heated at 140° C., and the reaction was carried out for 14 hours. The Ar gas atmosphere of the reaction system was maintained until the reaction system was naturally cooled to room temperature to obtain graphene. See figure 1 and figure 2 .

Embodiment 2

[0045] Put 20mL of toluene in a 50mL round bottom flask, then add 0.002g of hexabromobenzene (equivalent to 0.1mg / mL), 0.001g of CuCl (equivalent to 0.05mg / mL), stir, and heat in an oil bath under air conditions, the temperature is 100°C, reflux for 4 hours, and then naturally cool to room temperature to obtain graphene.

Embodiment 3

[0047] Put 20mL of diethylene glycol dimethyl ether in a 50mL round bottom flask, then add 1g of hexabromobenzene (equivalent to 50mg / mL), and 10g of Cu powder (equivalent to 500mg / mL) in a 50mL round bottom flask, stir , after passing Ar gas for 30 min, the oil bath was heated to 160° C., and the reaction time was 6 hours. The Ar gas atmosphere of the reaction system was kept until the reaction system was naturally cooled to room temperature to obtain graphene.

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Abstract

The invention discloses a preparation method of graphene, which comprises the following steps that: hexabromobenzene and substances A are added into solvents, are stirred into a mixed solution and are heated to take reaction for 2 to 48 hours at 100 to 200 DEG C, and a reaction system is oxygen-free or aerobic environment and the normal pressure or pressurized environment in the pressure aspect; the proportion of the hexabromobenzene to the substances A to the solvents is 0.1 to 50mg/0.05 to 500mg/1mL; the solvents are Bis(2-methoxy ethyl)ether, diphenyl ether, diethyl ether, tetrahydrofuran, toluene or benzene; the substances A are CuBr, CuI, CuCl, Cu or Ni. The preparation method has the advantages that the reaction condition is mild, the process is simple, and in addition, good reproducibility is realized. The prepared graphene is single-layer graphene. The graphene is used as chemical reaction raw materials, catalyst carriers and battery electrode materials and has wide application prospects in the aspects of physics and microtronics.

Description

technical field [0001] The invention relates to the synthesis of inorganic chemical materials, and relates to a preparation method of graphene. Background technique [0002] Graphene, as a new type of carbon material, is currently a hot research topic due to its large specific surface area and good electrical conductivity. The theoretical specific surface area of ​​graphene material is as high as 2600m 2 .g -1 , with outstanding thermal conductivity (3000W.m -1 .K -1 ), high conductivity (2×10 2 S.m -1 ). [0003] The synthesis of graphene generally has the following several methods. Micromechanical exfoliation method: Novoselov et al. 2004 [1] Single-layer graphene was successfully exfoliated from highly oriented pyrolytic graphite by micromechanical exfoliation. This is the first reported method to obtain graphene. Graphene oxide reduction method: Horiuchi et al. [2] The natural graphite was oxidized, followed by a series of purification, and then the graphite o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04B82Y40/00
Inventor 秦学王丽刘厚彬
Owner TIANJIN UNIV
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