Method for preparing high-quality graphene with controllable layer number

A high-quality, graphene technology, applied in the field of macro-production of high-quality graphene with a controllable number of layers, can solve problems such as restricting physical property research and further application, many graphene defects, and difficult to control the number of layers, and achieves low cost. , good dispersion, easy to operate

Inactive Publication Date: 2011-03-30
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of the products prepared by chemical cleavage methods are mixtures of single-layer, double-layer and multi-layer graphene, and the number of layers is difficult to control.
In addition, the use of oxidation, expansion, and ultrasonic treatment in the chemical cleavage method leads to more defects and poor quality of the prepared graphene, which also restricts its in-depth physical property research and further application.

Method used

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  • Method for preparing high-quality graphene with controllable layer number
  • Method for preparing high-quality graphene with controllable layer number
  • Method for preparing high-quality graphene with controllable layer number

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The artificial graphite powder of size<10 μ m is raw material, and graphite powder average particle size is 8 μ m in the present embodiment; Adopt Hummer method [" Hummer method " please refer to literature: Hummers W, Offman R.Journal of The American Chemical Society 1958,80: 1339 .] Oxidation for 10 hours; rapid heating to the expansion temperature of 1100°C at a heating rate of 50°C / s, rapid expansion in an atmosphere of argon (flow rate 200ml / min), and a residence time of 10s; at 450°C, hydrogen (100ml / min) ) + argon (100 liters / min) in a reducing atmosphere for 2 hours; ultrasonically dispersed in NMP for 2 hours at 40°C, with an ultrasonic dispersion power of 300W; 20,000 rpm high-speed centrifugation was used to remove graphite and Thick graphite flakes.

[0026] Observation under an electron microscope shows that the obtained graphene has a smooth surface and a thickness of about 1nm-1.8nm, of which 1 layer accounts for 90%, and 2 layers account for 10%. In thi...

Embodiment 2

[0028] The difference from Example 1 is:

[0029] The artificial graphite powder of size<30 μ m is raw material, and graphite powder average particle size is 20 μ m in the present embodiment; Adopt Hummer method to oxidize 5h; Be heated to expansion temperature 1050 ℃ rapidly with 35 ℃ / s heating rate, in argon (flow velocity 200 milliliters / Min) rapid expansion in an atmosphere with a residence time of 20s; reduction at 450°C in a reducing atmosphere of hydrogen (100ml / min) + argon (100ml / min) for 2h; ultrasonic dispersion in NMP at 40°C for 2h, The ultrasonic dispersion power is 400W; the graphite and thick graphite flakes that have not been completely peeled off are removed by high-speed centrifugation at 15,000 rpm.

[0030] Observation under an electron microscope showed that the obtained graphene had a smooth surface and a thickness of about 1 nm-2.4 nm, of which 1 layer accounted for 77%, 2 layers accounted for 22%, and 3 layers accounted for 1%. In the present embodim...

Embodiment 3

[0032]The difference from Example 1 is:

[0033] The natural flake graphite powder of size<30 μm is raw material, and graphite powder average particle size is 20 μm in the present embodiment; Adopt Hummer method to oxidize 5h; Be heated rapidly to expansion temperature 1050 ℃ with 35 ℃ / s heating rate, in argon (flow velocity 200 milliliters Rapid expansion under an atmosphere of 450°C, hydrogen (100ml / min) + argon (100ml / min) for 2h; ultrasonic dispersion in NMP for 2h at 40°C , the ultrasonic dispersion power is 500W; 15,000 rpm high-speed centrifugation is used to remove graphite and thick graphite flakes that have not been completely peeled off.

[0034] Observation under an electron microscope shows that the obtained graphene has a flat surface and a thickness of about 1nm-3nm, of which 1 layer accounts for 34%, 2 layers account for 45%, and 3 layers account for 21%. In the present embodiment, the conductivity of single-layer graphene is 1.1×10 3 S / cm.

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Abstract

The invention relates to technology for preparing graphene, in particular to a method for massively preparing high-quality graphene with a controllable layer number, which is suitable for massively preparing the high-quality graphene with the controllable layer number. In the method, graphite with different sizes and crystallinities is used as the raw material. The method comprises the following steps of: oxidizing the graphite by an Hummer method; swelling and splitting the oxidized graphite by a rapid heating method to obtain stripped graphite; reducing the stripped graphite at a high temperature; uniformly dispersing the reduced graphite in solution of a surfactant by an ultrasonic method; and removing the graphite which is not totally stripped and thick graphite sheets with large sizes by a high-speed centrifugation method so as to obtain the high-quality graphene with the controllable layer number. In the method, the layer number of the graphene is controlled according to different oxidization and splitting degrees of the graphite with different sizes and crystallinities, mixed gas of hydrogen and argon is used for reducing and stripping the graphite to further remove oxygenic functional groups in the graphene and improve the electrical conductivity of the graphene so as to prepare the high-quality graphene with the controllable layer number.

Description

Technical field: [0001] The invention relates to a graphene preparation technology, in particular to a mass preparation method of high-quality graphene with a controllable layer number, which is suitable for mass production of high-quality graphene with a controllable layer number. Background technique: [0002] Graphene refers to a single layer of carbon atoms tightly packed into a two-dimensional honeycomb lattice structure, which is the basic unit for constructing other dimensional carbon materials (zero-dimensional fullerene, one-dimensional carbon nanotubes, three-dimensional graphite) . Due to its unique structure and excellent electrical, thermal, and mechanical properties, graphene is expected to be widely used in high-functional nanoelectronic devices, composite materials, catalytic materials, battery materials, field emission materials, gas sensors, and gas storage. Therefore, in just three to four years since the stable existence of graphene was obtained in 2004,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 成会明任文才吴忠帅高力波刘碧录
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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