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Graphene preparation method

A graphene and graphene dispersion technology, applied in graphene, nano-carbon and other directions, can solve the problems of mismatched Hansen solubility parameters, high boiling point of organic solvents, inability to achieve peeling, etc., and achieve convenient production and low oxygen content. , the effect of high yield

Inactive Publication Date: 2014-05-07
SOUTH CHINA AGRI UNIV
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  • Claims
  • Application Information

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Problems solved by technology

However, the existing liquid-phase exfoliation methods have the disadvantages of high boiling point of organic solvents, toxicity and difficulty in removal, or mismatch with the Hansen solubility parameter of graphene and cannot achieve exfoliation.

Method used

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Effect test

Embodiment 1

[0040] Add 1g of graphite powder to 120mL of water, the size of the graphite powder is 100 microns, place in a closed reaction kettle, stir at 600rpm, and heat to 240°C, keep for 5 hours for hydrothermal exfoliation. After cooling, the solution was centrifuged at a speed of 1000 rpm for 60 min, and the upper layer liquid after centrifugation was taken with a pipette to obtain a graphene dispersion uniformly dispersed in a mixed solvent. The graphene dispersion was subjected to high-speed centrifugation at 8000 rpm for 15 minutes to obtain the lower solid which was graphene. The weighed graphene yield is about 4.1%.

[0041] The graphite powder before the preparation of the present embodiment is detected, and the scanning electron microscope picture is as follows: figure 1 shown;

[0042] Various detections are carried out to the graphene prepared by the present embodiment, and the scanning electron microscope picture is as follows figure 2 The transmission electron microsc...

Embodiment 2

[0044] Add 1g of graphite powder to 120mL of water, the size of the graphite powder is 10 microns, place in a closed reaction kettle, stir at 500rpm, and heat to 300°C, keep for 3 hours for hydrothermal exfoliation. After cooling, the solution was centrifuged at a speed of 10,000 rpm for 30 min, and the upper layer liquid after centrifugation was taken with a pipette to obtain a graphene dispersion uniformly dispersed in a mixed solvent. The graphene dispersion was subjected to high-speed centrifugation at 10000 rpm for 5 minutes to obtain the lower solid which was graphene. The yield of graphene is about 3.2% by weight.

Embodiment 3

[0046] Add 1g of graphite powder to 120mL of water, the size of graphite powder is 500 microns, place in a closed reaction kettle, stir at 1500rpm, and heat to 180°C, keep for 6 hours for hydrothermal exfoliation. After cooling, the solution was centrifuged at a speed of 500 rpm for 90 min, and the upper layer liquid after centrifugation was taken with a pipette to obtain a graphene dispersion uniformly dispersed in a mixed solvent. The graphene dispersion was centrifuged at 8000 rpm for 90 minutes at a high speed to obtain the lower solid which was graphene. The yield of graphene is about 2.4% by weight.

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Abstract

The invention belongs to the technical field of carbon material preparation, and discloses a graphene preparation method based on a liquid phase stripping method and a hydrothermal method. The graphene preparation method comprises the following steps: adding powdered graphite and water into a reaction kettle; sealing, then stirring, heating to a reaction temperature, keeping constant temperature, continuously stirring and reacting; after ending reaction, cooling, taking out a mixed solution in the reaction kettle so as to carry out centrifugal separation, wherein solids at a lower layer are unreacted powered graphite, and supernatant liquid is graphene dispersion liquid; and carrying out centrifugal separation on the graphene dispersion liquid so as to obtain solids, namely graphene. According to the graphene preparation method, water is used as a solvent so as to overcome the shortcomings that an organic solvent is high in boiling point and difficult to remove and has toxicity, or as Hansen solubility parameters of the organic solvent cannot meet the solubility parameters of graphene, the concentration of the dispersion liquid is relatively low. The yield of the prepared graphene is high; the prepared graphene has very few defects and is very low in oxygen content; and the intrinsic electrical property of the graphene is maintained.

Description

technical field [0001] The invention belongs to the technical field of carbon material preparation, and in particular relates to a method for preparing graphene. Background technique [0002] Graphene has excellent physical, chemical and mechanical properties, and the preparation of high-quality graphene is crucial to the application of graphene. At present, there are many methods for preparing graphene, mainly including mechanical exfoliation method, chemical vapor deposition method, redox method, and silicon carbide epitaxial growth method. The quality of graphene prepared by mechanical exfoliation is the best, but it is very accidental, and it is difficult to control the number of layers; the quality of graphene prepared by chemical vapor deposition is high, but the electronic properties of graphene are greatly affected by the substrate , and the performance is not as good as that of graphene produced by mechanical exfoliation; redox method can obtain a large amount of s...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B32/19
Inventor 刘应亮刘向荣郑明涛肖勇雷炳富董汉武张浩然
Owner SOUTH CHINA AGRI UNIV
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