Preparation method and application of fluorinated graphene with high thermal stability, insulation and high thermal conductivity

A fluorinated graphene, high thermal stability technology, applied in the direction of graphene, chemical instruments and methods, carbon compounds, etc., can solve the problems of poor thermal stability, uneven distribution of fluorine, and poor thermal conductivity. It is easy to put into production in batches, the reaction is thorough, and the production efficiency is high.

Active Publication Date: 2022-05-06
SICHUAN UNIV
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  • Application Information

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Problems solved by technology

[0006] Based on this, the present invention provides a preparation method and application of fluorinated graphene with high thermal stability, insulation and high thermal conductivity, to solve the problem of direct fluorine in the prior art The fluorinated graphene product prepared by the chemical method presents a microstructure with uneven distribution of fluorine elements, but there are technical problems of poor thermal stability and weak intrinsic thermal conductivity.

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  • Preparation method and application of fluorinated graphene with high thermal stability, insulation and high thermal conductivity
  • Preparation method and application of fluorinated graphene with high thermal stability, insulation and high thermal conductivity
  • Preparation method and application of fluorinated graphene with high thermal stability, insulation and high thermal conductivity

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preparation example Construction

[0034] The preparation method of the fluorinated graphene with high thermal stability, insulation and high thermal conductivity provided by the invention comprises the following steps:

[0035] 1) Place the dried graphene in the fluorination kettle, vacuumize the inside of the fluorination kettle first, then pass nitrogen gas in and pump it out for multiple replacement treatments, and then raise the temperature of the fluorination kettle to 140-260°C; the replacement The treatment is to replace the air in the fluorination kettle by vacuumizing first, then introducing nitrogen and pumping out nitrogen. The multiple replacement processes here are to improve the replacement effect, and in specific implementation, the multiple times can be 2-5 times.

[0036] 2) The buffer kettle is subjected to the same replacement treatment in step 1) for many times, and then heated to the same temperature as the fluorination kettle in step 1); the replacement treatment method of this step is the ...

Embodiment 1

[0042] Put the graphene in the fluorination kettle, replace the air in the fluorination kettle and the buffer kettle with nitrogen three times, and then raise the temperature of the fluorination kettle and the buffer kettle to 140°C;

[0043] Pass the fluorination reaction mixed gas with the fluorine concentration of 20% mixed by fluorine gas and nitrogen gas into the buffer tank, and keep it for 10 minutes for thermal pre-dissociation;

[0044] Pass the fluorination reaction mixed gas after thermal pre-dissociation into the fluorination kettle until the pressure is 50Kpa, and perform the fluorination reaction for 1 hour. After the fluorination kettle is naturally cooled, take out the sample to obtain fluorinated graphene.

[0045] The sample of this embodiment is tested: the fluorine-carbon atomic ratio of the fluorinated graphene is 0.61 by XPS, and the thermal weight loss peak temperature of the TGA test is 576 ° C. The fluorinated graphene is applied to the cellulose compos...

Embodiment 2

[0047] Put the graphene in the fluorination kettle, replace the air in the fluorination kettle and the buffer kettle with nitrogen three times, then raise the temperature of both the fluorination kettle and the buffer kettle to 200°C;

[0048] Pass the fluorination reaction mixed gas with fluorine gas concentration of 10% mixed with fluorine gas and nitrogen gas into the buffer tank, and keep it for 10 minutes for thermal pre-dissociation;

[0049] Pass the fluorination reaction mixed gas after thermal pre-dissociation into the fluorination kettle until the pressure is 80Kpa, and perform the fluorination reaction for 1 hour. After the fluorination kettle is naturally cooled, take out the sample to obtain fluorinated graphene.

[0050] The sample of this embodiment is tested: the fluorine-to-carbon atomic ratio of the fluorinated graphene is 0.55 by XPS test, and the thermal weight loss peak temperature of the TGA test is 565 ° C. The fluorinated graphene is applied to the cellu...

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Abstract

The invention relates to a preparation method and application of fluorinated graphene with high thermal stability, insulation and high thermal conductivity, and the preparation method comprises the following steps: placing dried graphene in a fluorination kettle, vacuumizing the fluorination kettle, introducing nitrogen into the fluorination kettle, pumping out the nitrogen, carrying out replacement treatment for multiple times, and heating the fluorination kettle; carrying out replacement treatment on the buffer kettle for multiple times, and then heating to the temperature the same as that of the fluorination kettle; introducing the fluoridation reaction mixed gas into the heated buffer kettle, keeping for 10-30 minutes, and carrying out thermal pre-dissociation, so as to convert part of fluorine gas molecules in the fluoridation reaction mixed gas into fluorine atoms; and introducing the fluoridation reaction mixed gas subjected to thermal pre-dissociation into the heated fluoridation kettle, and carrying out fluoridation reaction on the fluoridation reaction mixed gas and graphene for 0.5-2 hours to obtain the fluorinated graphene with high thermal stability, insulation and high thermal conductivity. The fluorinated graphene prepared by the preparation method disclosed by the invention has more uniform fluorine element distribution, so that the fluorinated graphene has a relatively uniform lattice structure and further has excellent heat-conducting property.

Description

technical field [0001] The invention relates to the technical field of fluorinated graphene and its preparation, in particular to a preparation method and application of fluorinated graphene with high thermal stability, insulation and high thermal conductivity. Background technique [0002] With the rapid development of two-dimensional nanomaterials, graphene has become one of the most promising materials due to its excellent electrical and thermal conductivity and mechanical properties. However, in the application process, pristine graphene has problems such as zero energy gap, reactive inertness, and poor dispersion, so it is necessary to develop effective methods to chemically modify graphene. Among the many modification methods, the method of direct fluorination modification of graphene by using fluorine gas and its mixed gas has received the most extensive attention. Effective fluorination can reduce the interlayer forces of graphene and open the band gap of graphene, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/194C08K3/04
CPCC01B32/194C08K3/042C01B2204/24
Inventor 刘洋黄本元刘向阳王旭李玉龙刘昌莉
Owner SICHUAN UNIV
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