Method for preparing nitrogen-doped fluorinated graphene by using graphite fluoride

A technology of fluorinated graphene and fluorinated graphite, which is applied in the direction of graphene and nano-carbon, can solve the problems of weakening the performance of composite materials and low compatibility, and achieves easy operation and control, good compatibility and simple process route Effect

Pending Publication Date: 2019-01-18

SHANGHAI APPLIED TECHNOLOGIES COLLEGE

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Among them, fluorinated graphene is a new type of derivative of graphene, which not only maintains the high-strength properties of graphene, but also has high temperature resistance, corrosion resistance, friction resistance, stable chemical properties and excellent lubrication. However, d...

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Abstract

The invention relates to a method for preparing nitrogen-doped fluorinated graphene by using graphite fluoride, comprising the following steps: raw materials are weighed in proportion and are added into an agate pot, agate beads are added to help grinding, and uniform stirring is performed; the mixture is placed in a ball mill to be subjected to ball milling for 15 to 30 hours, wherein the ball milling frequency is 540 to 600 rpm; after ball milling is ended, the nitrogen-doped fluorinated graphene containing a small amount of impurities is ultrasonically dispersed in deionized water to obtaina water system mixed suspension; the water system mixed suspension obtained after ultrasonication is placed in a centrifuge tube for centrifugation, a fluorinated graphene stabilized suspension in which the upper layer is doped with nitrogen element is collected, and precipitate is discarded; and the water in the fluorinated graphene stabilized suspension in which nitrogen element is doped is removed by suction filtration, and vacuum drying is performed to obtain the nitrogen-doped fluorinated graphene. The preparation process of is relatively simple, and easy to operate and control, which can realize large-scale production; the prepared nitrogen-doped fluorinated graphene has good quality and improved hydrophilicity.

Application Domain

Graphene

Technology Topic

Ball millGraphene +9

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Examples

Experimental program(4)
Comparison scheme(1)

Example Embodiment

[0017] Example 1

[0018] (1) Weigh fluorinated graphite and ammonium carbonate at a mass ratio of 1:1, and add them to the agate pot (100ml in capacity), where the mass of fluorinated graphite is 4 grams; add agate beads to the agate pot;

[0019] (2) Fix the agate pot in the ball mill. During the 15-hour milling process, the milling frequency will be 540 rpm;

[0020] (3) Add deionized water to the mixture obtained in step 2 for repeated washing, and then perform suction filtration, vacuum drying and grinding to obtain fluorinated graphene solid powder.

[0021] Observed by scanning electron microscopy, it is found that the resulting product has a sheet-like structure, indicating that the fluorinated graphite has been successfully exfoliated into fluorinated graphene (as attached figure 1 ). Attached figure 2 It is the XPS spectrum of the obtained product. It can be seen from the figure that the original fluorinated graphite (FG) 294.6eV and 687eV have obvious carbon peaks and fluorine peaks, while nitrogen-doped fluorinated graphene (NG) has more than 400eV. A nitrogen peak appeared, indicating that nitrogen atoms have been successfully incorporated into fluorinated graphene.

Example Embodiment

[0022] Example 2

[0023] (1) Weigh and mix fluorinated graphite and ammonium carbonate separately, wherein the mass of fluorinated graphite is 4 grams, the mass of ammonium carbonate is 8 grams, and the mass ratio is 1:2; add agate beads to the agate pot;

[0024] (2) Fix the agate pot in the ball mill, and during the grinding process for 20 hours, the ball milling frequency is 540 revolutions/min;

[0025] (3) Add deionized water to the mixture obtained in step 2 for repeated washing, and then perform suction filtration, vacuum drying and grinding to obtain fluorinated graphene solid powder.

Example Embodiment

[0026] Example 3

[0027] (1) Mixing graphite fluoride with ammonium fluoride, wherein the mass of graphite fluoride is 4 grams, the mass of ammonium fluoride is 4 grams, and the mass ratio is 1:1; add agate beads to the agate pot;

[0028] (2) Fix the agate pot in the ball mill, and during the grinding process for 25 hours, the ball milling frequency is 600 rpm;

[0029] (3) Add deionized water to the mixture obtained in step 2 for repeated washing, and then perform suction filtration, vacuum drying and grinding to obtain fluorinated graphene solid powder.

[0030] The morphology of the obtained nitrogen-doped fluorinated graphene is better. image 3 The obvious lamella structure can be clearly seen. Attached Figure 4 It is the XPS spectrum of the obtained product. It can be seen from the figure that the original fluorinated graphite (FG) has obvious carbon peaks and fluorine peaks at 294.6eV and 687eV, while nitrogen-doped fluorinated graphene (NG) has more peaks at 400eV. A nitrogen peak appeared, indicating that nitrogen atoms have been successfully incorporated into fluorinated graphene.

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Method for preparing graphene solution based on supercritical carbon dioxide induction solution phase transformation technology

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Method for preparing nitrogen-doped fluorinated graphene by using graphite fluoride

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