Preparation method of graphene

A graphene and fluorinated graphite technology, applied in the field of carbon materials, can solve the problems of inability to restore the two-dimensional crystal structure of graphene, affect the electrical conductivity of graphene, destroy the crystal structure of graphene, etc., achieve excellent electrical properties, restore two-dimensional crystal structure, etc. Crystal structure, the effect of ensuring high yield

Inactive Publication Date: 2016-08-24
LANZHOU UNIVERSITY OF TECHNOLOGY
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Problems solved by technology

[0004] Usually, the oxidation process severely damages the crystal structure of graphene, while the reduction process does not fully restore graphene to its two-dimensional crystal str

Method used

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preparation example Construction

[0029] The invention provides a kind of preparation method of graphene, concrete steps are as follows:

[0030] Under heating conditions, the graphite fluoride and hydrazine hydrate are subjected to a reduction reaction in a liquid phase reaction system to obtain graphene.

[0031] In the present invention, the source of the fluorinated graphite is not particularly limited, and fluorinated graphite well known to those skilled in the art can be used, for example, a commercially available product of fluorinated graphite. In the present invention, the molar ratio of fluorine atoms to carbon atoms in the fluorinated graphite is preferably 1:(0-1.25), and the content of carbon atoms in the fluorinated graphite is not zero, more preferably 1:(0.25 ~1.25), most preferably 1:(0.5~1.25).

[0032] In the present invention, the graphite fluoride and hydrazine hydrate undergo a reduction reaction in a liquid phase system to obtain graphene. In the present invention, the liquid phase sys...

Embodiment 1

[0047] Add 0.5 g of graphite fluoride to 500 mL of hydrazine hydrate solution with a concentration of 50 wt%, and after ultrasonic treatment for 30 min, transfer the mixed solution to a 500 mL round bottom flask, control the reaction temperature at 80°C, and stir magnetically for 6 hours.

[0048] Purification of Graphene

[0049] After the reaction was over, it was naturally cooled to room temperature. The reaction product was transferred to a beaker and filtered. The product is washed out with deionized water, and then centrifuged and washed five times with deionized water, 95% ethanol and acetone at a centrifugal speed of 6000r / min-10000r / min to obtain the graphene product.

[0050] drying of graphene

[0051] The graphene product obtained is vacuum-dried in a vacuum oven for 12h. The vacuum degree of the vacuum drying oven is 0.7MPa, and the temperature is 70°C.

[0052] The present invention carries out morphology and structural characterization of the obtained graphe...

Embodiment 2

[0068] Add 0.1 g of graphite fluoride to 100 mL of hydrazine hydrate solution with a concentration of 35 wt %, and after ultrasonic treatment for 30 min, transfer the mixture to a 500 mL three-neck flask, control the reaction temperature at 80°C, and mechanically stir for 2 hours.

[0069] The purification process is as in Example 1.

[0070] drying of graphene

[0071] The obtained graphene product was freeze-dried in a liquid nitrogen freeze dryer for 24 hours. The temperature of the freeze dryer is minus 48°C.

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Abstract

The invention provides a preparation method of graphene. The method comprises the specific steps that graphite fluoride and hydrazine hydrate are subjected to a reduction reaction in a liquid phase reaction system to obtain graphene. According to the scheme, the graphite fluoride is used as a raw material, and peeling and reduction of the graphite fluoride can be completed only through one-step reaction. The involved reaction is a liquid phase chemical reaction. The uniformity and high yield of the product are ensured, the two-dimensional crystal structure of graphene can be recovered to the maximum limit, and therefore the excellent electrical performance of the graphene is reserved. Experiment results show that the conductivity of the obtained graphene is 2670 S/m and is much higher than that of graphene obtained through a chemical oxidation reduction method in the prior art.

Description

technical field [0001] The invention relates to the technical field of carbon materials, in particular to a method for preparing graphene. Background technique [0002] Graphene is a completely sp 2 The two-dimensional crystal material composed of hybrid carbon atoms and only one atom thick has high specific surface area, high strength, and excellent electrical conductivity, thermal conductivity, and mechanical properties. It is expected to be used in micro-nano electronic devices, optoelectronic devices, and field emission materials. , sensors, solar cells, composite materials and other fields have been widely used. [0003] The preparation methods of graphene mainly include mechanical exfoliation method, epitaxial growth method, chemical vapor deposition method and chemical redox method. Among them, the chemical redox method is a common method to realize the macro-preparation of graphene, including two processes of chemical oxidation and reduction. The chemical oxidatio...

Claims

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Application Information

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IPC IPC(8): C01B31/04
CPCC01P2002/82C01P2004/04
Inventor 陈丽李娜
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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