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Fluorinated graphene with large surface area and high thermal stability and preparation method thereof

A technology of fluorinated graphene and high thermal stability, which is applied in the direction of graphene, chemical instruments and methods, carbon fluoride, etc., can solve the problems of low thermal stability and low real specific surface area of ​​fluorinated graphene, and achieve specific surface area Improvement, easy thermal stability, and the effect of reducing energy consumption

Active Publication Date: 2017-05-17
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, due to the characteristics of the two-dimensional nanosheet structure, fluorinated graphene also has the problem of other two-dimensional nanomaterials such as graphene, that is, the stacking between sheets leads to the real specific surface area of ​​fluorinated graphene (2 / g) is much lower than the theoretical specific surface area (>2000m 2 / g)
In addition, the thermal stability of C-F bonds in fluorinated graphene is also significantly lower than that of C-F bonds in fluorinated graphite (about 600 °C)

Method used

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  • Fluorinated graphene with large surface area and high thermal stability and preparation method thereof
  • Fluorinated graphene with large surface area and high thermal stability and preparation method thereof

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Effect test

Embodiment 1

[0030] Mix graphene and potassium hydroxide uniformly at a ratio of 1:4, and then treat the mixture at 600°C for 5 hours under a nitrogen atmosphere to obtain activated graphene; place the activated graphene in a closed vacuum reactor, and replace the reactor with nitrogen Vacuum the air in the chamber three times, then fill it with a mixture of fluorine and nitrogen, and control the initial partial pressure of fluorine to 30KPa, then raise the temperature to 30°C at a heating rate of 3°C / min and keep it warm for 60 minutes, then cool naturally The fluorinated graphene is obtained at room temperature.

[0031] The fluorine content in the fluorinated graphene is 20%, and the specific surface area is 1800m 2 / g, the peak weight loss temperature is 560°C.

Embodiment 2

[0033] Mix graphene and potassium hydroxide uniformly at a ratio of 1:7, and then treat the mixture at 800°C for 1 hour under a nitrogen atmosphere to obtain activated graphene; place the activated graphene in a closed vacuum reactor and replace the reaction with argon Vacuum the air in the vessel three times, then fill it with a mixture of fluorine and argon, and control the initial partial pressure of fluorine to 40KPa, then raise the temperature to 150°C at a heating rate of 10°C / min and keep it warm for 150 minutes. Cool naturally to room temperature to obtain fluorinated graphene.

[0034] The fluorine content in the fluorinated graphene is 34%, and the specific surface area is 1600m 2 / g, the peak weight loss temperature is 565°C.

Embodiment 3

[0036]Mix graphene, magnesium citrate and potassium citrate uniformly at a ratio of 1:4:4, and then treat the mixture at 800°C for 0.5h under nitrogen and argon atmosphere to obtain activated graphene; place the activated graphene in a closed In the vacuum reactor, replace the air in the reactor with argon for three times, then evacuate it, then fill it with a mixture of fluorine and argon, and control the initial partial pressure of fluorine to 50KPa, and then increase the temperature at a rate of 10°C / min. Raise the temperature to 100°C and keep it warm for 300 minutes, then cool naturally to room temperature to obtain graphene fluoride.

[0037] The fluorine content in the fluorinated graphene is 43%, and the specific surface area is 1600m 2 / g, the peak weight loss temperature is 575°C.

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Abstract

The invention discloses fluorinated graphene with large surface area and high thermal stability. Firstly, graphene or graphene oxide is mixed with an activator, and high-temperature activation treatment is carried out in an inert gas atmosphere to obtain activated graphene, then a fluorine mixed gas is taken as a fluorinating reagent to carry out direct fluorination on the activated graphene so as to obtain the fluorinated graphene, wherein fluoride atoms and carbon atoms are covalently bonded, the fluorine content is 10 to 70%, the weight loss peak temperature is greater than 550 DEG C, and the specific surface area is more than 1000m<2> / g. The fluorinated graphene is prepared by using a new method of firstly carrying out activation and then fluorination, the fluoridation activity of the activated graphene and fluorine is obviously improved, the fluorinated graphene of which the fluorine content is 20 to 50% can be further formed at low temperature, and the new method is higher in process safety and capable of lowering the energy consumption and production cost, thereby being suitable for mass production, and further being capable of obtaining the fluorinated graphene with the large surface area and high thermal stability.

Description

technical field [0001] The invention belongs to the technical field of graphene derivatives and their preparation, in particular to a fluorinated graphene with a large specific surface area and high thermal stability and a preparation method thereof. Background technique [0002] Graphene is a new type of two-dimensional nanomaterial that has been found to be the thinnest, hardest, and has many advantages such as the strongest electrical and thermal conductivity. Therefore, graphene and its derivatives have not only become one of the revolutionary new materials in the field of materials. First, and the effective modification of graphene to prepare its multifunctional derivatives has also become the focus of research in the field of graphene. At present, graphene derivatives mainly include graphene oxide, graphane, semihydrogenated graphene, hydroxyl-modified hydrated graphene, chlorinated graphene, and fluorinated graphene. Among these graphene derivatives, in addition to t...

Claims

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Application Information

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IPC IPC(8): C01B32/10C01B32/184
CPCC01B2204/24C01B2204/32C01P2004/04
Inventor 王旭刘向阳陈腾刘洋赖文川李玉龙
Owner SICHUAN UNIV
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