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Preparation method of nitrogen-doped graphene

A nitrogen-doped graphene, nitrogen-doped technology, applied in the direction of graphene, nano-carbon, etc., can solve the problems that affect the performance and structural stability of graphene, the equipment and cost requirements are very high, and the structure of nitrogen components is difficult to combine , to achieve the effect of being suitable for mass production and application, low requirements for raw materials and equipment, and high content of nitrogen atoms

Active Publication Date: 2020-08-25
QUJING NORMAL UNIV
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Problems solved by technology

However, the disadvantage of these subsequent nitrogen doping methods is that the introduced nitrogen components are difficult to form a stable bonding structure inside the carbon layer, and at the same time, a large number of hole defects and unnecessary oxygen groups will be introduced into the graphene carbon layer, which seriously Affects the performance and structural stability of graphene; there are also carbon- and nitrogen-containing precursors as carbon and nitrogen sources, and nitrogen-doped graphene is directly synthesized by chemical vapor deposition or arc discharge
However, these methods involve complex processes such as the processing of the growth substrate, the separation and transfer of the graphene film, and these process conditions are harsh, and the requirements for equipment and cost are very high, making it difficult to scale production

Method used

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  • Preparation method of nitrogen-doped graphene

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Experimental program
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Effect test

Embodiment 1

[0038]Natural flake graphite (325 mesh) was placed in a crucible, and argon gas was introduced into the vacuum tube furnace at a flow rate of 0.15 L / min to remove the air in the furnace tube, and then ammonia gas was replaced at a flow rate of 0.1 L / min. The temperature was raised at a rate of 5°C / min to 900°C for 5 hours of heat preservation and heat treatment for nitriding and expansion. After the reaction furnace was naturally lowered to room temperature, the argon gas was changed for 0.5 hours to obtain nitrogen-doped graphite. Disperse nitrogen-doped graphite in N,N-dimethylformamide at a concentration of 0.5mg / mL, and disperse it ultrasonically for 6h at 100W power and 40kHz frequency; Centrifuge under g centrifugal force for 5min, absorb the supernatant with a straw, and obtain nitrogen-doped graphene.

[0039] Such as figure 1 As shown in the TEM photo, the nitrogen-doped graphene sheet prepared in Example 1 has a complete structure, and the size of the graphene sheet...

Embodiment 2

[0041] Natural flake graphite (325 mesh) was placed in a crucible, and argon gas was introduced into the vacuum tube furnace at a flow rate of 0.15 L / min to remove the air in the furnace tube, and then the gas flow was changed to ammonia gas at a flow rate of 0.6 L / min. The temperature was raised at a rate of 2°C / min to 500°C for 12 hours of heat preservation and heat treatment for nitriding and expansion. After the reaction furnace was naturally lowered to room temperature, the argon gas was changed for 0.5 hours to obtain nitrogen-doped graphite. Disperse nitrogen-doped graphite in ethanol at a concentration of 0.05mg / mL, and disperse it ultrasonically for 24h at 300W power and 60kHz frequency; then centrifuge the dispersion at 10000rpm, that is, about 10000×g centrifugal force for 5min, and use a pipette Aspirate the supernatant to obtain nitrogen-doped graphene.

[0042] Such as Figure 4 As shown, the energy spectrum analyzer test result shows that its nitrogen content i...

Embodiment 3

[0044] Natural flake graphite (325 mesh) was placed in a crucible, and argon gas was introduced into the vacuum tube furnace at a flow rate of 0.15 L / min to remove the air in the furnace tube, and then ammonia gas was replaced at a flow rate of 0.1 L / min. The temperature was raised at a rate of 5°C / min to 700°C for 5 hours of heat preservation and heat treatment for nitriding and expansion. After the reaction furnace was naturally lowered to room temperature, the argon gas was changed for 0.5 hours to obtain nitrogen-doped graphite. Disperse nitrogen-doped graphite in tetrahydrofuran at a concentration of 0.5 mg / mL, ultrasonically disperse it for 6 h at 100 W power and 40 kHz frequency; Aspirate the supernatant to obtain nitrogen-doped graphene.

[0045] Such as Figure 5 As shown, the energy spectrum analyzer test result shows that its nitrogen content is 12.99%.

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Abstract

The invention discloses a preparation method of nitrogen-doped graphene. The preparation method comprises the following steps of: carrying out heat treatment on graphite powder in a nitrogen-containing active atmosphere to carry out nitridation and expansion to obtain nitrogen-doped graphite; and dispersing the nitrogen-doped graphite in a solvent, carrying out ultrasonic dispersion and centrifugation, and collecting a supernatant to obtain the nitrogen-doped graphene material. By adopting the method disclosed by the invention, structural defects such as holes and chemical groups cannot be introduced into a graphene sheet layer can be avoided; the prepared nitrogen-doped graphene has the advantages of complete sheet layer, few defects, high nitrogen content, stable structure and the like.Compared with the prior art, the preparation method has the advantages of very simple, quick and efficient preparation process, low cost and easiness in realizing large-scale production and application.

Description

technical field [0001] The present invention relates to the technical field of graphene materials, and more specifically relates to a preparation method of nitrogen-doped graphene. Background technique [0002] Graphene is a new type of two-dimensional crystal material composed of six-membered rings of carbon atoms. Since it was discovered by scientists from the University of Manchester in 2004, due to its ultra-high specific surface area, excellent mechanical, electrical, optical, thermal and multifunctional properties and many other advantages, it has shown great importance in the fields of energy, electronics, and the environment. research value and application prospects. [0003] People try to improve and regulate the structure and properties of graphene through various chemical modification methods, especially the doping of chemical elements, which can greatly improve the structure and properties of graphene. Nitrogen atoms have an atomic size similar to that of carbo...

Claims

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Application Information

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IPC IPC(8): C01B32/19
CPCC01B32/19
Inventor 康艳茹赵祥曹琳李哲徐坤
Owner QUJING NORMAL UNIV
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