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Preparation method of graphene

A technology of graphene and thin-layer graphene, which is applied in the direction of graphene, chemical instruments and methods, bulk chemical production, etc., can solve the problems of halide intercalation graphene, etc. The effect of extremely high degree and easy access to equipment

Pending Publication Date: 2018-12-07
AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there have been related methods of exfoliating graphene using halide-intercalated graphite as products, and research on intercalating halides in multi-layer graphene, there has been no direct exfoliation of halide-intercalated graphite composites to prepare halide-intercalated Invention of Graphene Announced

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

[0029] Using aluminum chloride as intercalation agent and 300 mesh flake graphite as precursor, metal chloride-graphite intercalation compound was prepared by molten salt intercalation method. Add 1g of metal chloride-graphite intercalation compound into 100mL of acetone solvent, soak for 72 hours, pour off the supernatant, place the precipitate in a vacuum oven, and keep it in a vacuum environment at 150°C for 6 hours to obtain expanded graphite. Disperse expanded graphite in N,N-dimethylformamide solvent, ultrasonically treat it for 1 hour (dispersion), obtain a suspension of graphene, filter with a 0.2 micron organic filter membrane, wash with ethanol, and suction filter Finally, deionized water was added for washing, and the slurry after suction filtration was freeze-dried to obtain graphene with a yield of about 95%.

[0030] Such as figure 1 As shown, in Example 1, the expanded graphite treated with solvent and vacuum low temperature forms an accordion-like loose struct...

Embodiment 2

[0034] Using aluminum chloride as intercalation agent and graphite as precursor, the metal chloride-graphite intercalation compound was prepared by electrochemical intercalation method. Add 1 g of metal chloride-graphite intercalation compound into 150 mL of aqueous solution, soak for 72 hours, pour off the supernatant, place the precipitate in a vacuum oven, and keep it warm in a vacuum environment at 200°C for 6 hours to obtain expanded graphite. Disperse expanded graphite in N,N-dimethylformamide solvent, and ultrasonically treat it for 1 hour to obtain a suspension of graphene, filter it with a 0.2 micron organic filter membrane, wash it with ethanol, and filter it with suction. Add deionized water to wash, and freeze-dry the slurry after suction filtration to obtain graphene.

Embodiment 3

[0036] Using aluminum chloride as intercalation agent and flake graphite as precursor, metal chloride-graphite intercalation compound was prepared by molten salt intercalation method. Add 10g of metal chloride-graphite interlayer compound into 500mL of ethanol solvent, soak for 72 hours, pour off the supernatant, place the precipitate in a vacuum oven, and keep it in a vacuum environment at 150°C for 12 hours to obtain expanded graphite. Disperse expanded graphite in N-methylpyrrolidone solvent, ultrasonically treat it for 1 hour to obtain a suspension of graphene, filter it with a 0.2 micron organic filter membrane, wash it with ethanol, and add deionized water after suction filtration After cleaning, the slurry after suction filtration is freeze-dried to obtain graphene.

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Abstract

The invention relates to a preparation method of graphene. A graphene precursor is prepared by taking a metal chloride-graphite interlaminar compound as a raw material at a vacuum low heating temperature. The efficiency is improved, the redox step in a conventional method is also avoided, the integrity of a graphene structure is improved greatly, the defect degree is reduced, and the problem of preparing high quality graphene is solved. The preparation method has the advantages of being short in time, high in efficiency, high in safety, low in cost, common in equipment and the like, and can bewidely applied to the fields of energy source materials, conducting materials, heat conducting materials, semi-conductor materials and the like.

Description

technical field [0001] The invention relates to a method for preparing a graphene material, in particular to a vacuum-assisted low-temperature preparation of a high-quality graphene material. Background technique [0002] Graphene, two-dimensional sp2 hybridized carbon, is the most studied material today. It is a monoatomic layer of carbon atoms arranged in a honeycomb shape, becoming the thinnest, hardest and toughest material in the world, and an excellent conductor of heat and electricity. After being isolated as early as 2004, many studies have shown that this single atomic layer carbon material uniquely combines superior mechanical strength, exhibits high electronic and thermal conductivity, high surface area and impermeability to gases, besides There are many other desirable characteristics, all of which make it an attractive application. It is considered to be the basic structural unit of fullerene, carbon nanotube (CNT) and graphite. Because of its special mechanic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/19
CPCC01B32/19C01B2204/04C01B2204/22Y02P20/54
Inventor 齐新燕绍九彭思侃王晨王继贤
Owner AVIC BEIJING INST OF AERONAUTICAL MATERIALS