Preparation method of nitrogen doped graphene and application of nitrogen doped graphene

A nitrogen-doped graphene and graphene technology, applied in the field of graphene, can solve the problems of nitrogen-doped graphene preparation limitations, high heating temperature, harsh preparation conditions, etc., to promote doping, increase pressure, and low production cost Effect

Active Publication Date: 2014-03-12
NINGBO GRAPHENE INNOVATION CENT CO LTD
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Problems solved by technology

[0005] Due to the preparation method of nitrogen-doped graphene in the prior art, higher heating temperature is req

Method used

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  • Preparation method of nitrogen doped graphene and application of nitrogen doped graphene
  • Preparation method of nitrogen doped graphene and application of nitrogen doped graphene
  • Preparation method of nitrogen doped graphene and application of nitrogen doped graphene

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preparation example Construction

[0026] The embodiment of the present invention discloses a method for preparing nitrogen-doped graphene, and the specific steps are:

[0027] The carbon material and the compound containing active nitrogen element are placed in a closed container, heated to 100~300°C, and nitrogen-doped graphene is obtained after the reaction, the compound containing active nitrogen element is gas and / or solid, and the carbon The material is graphene or graphene oxide.

[0028] According to the present invention, in the above-mentioned process of preparing nitrogen-doped graphene, the graphene oxide is specifically prepared as follows:

[0029] Graphene oxide colloid with a concentration of 1mg / ml~15mg / ml is ultrasonicated for 0.5~2h, and freeze-dried to obtain graphene oxide. In order to ensure that the graphene oxide is broken more evenly and finely, the concentration of the graphene oxide is preferably 5-10 mg / ml, and the time of the ultrasound is preferably 1-1.5 h. The above-mentioned p...

Embodiment 1

[0039] Take 100ml of graphene oxide colloid with a concentration of 1mg / ml, mix it with 1g of ammonium bicarbonate evenly, freeze-dry, place the obtained powder in a sealed container and heat to 100°C, and keep it warm for 5h. After the reaction is finished, the reactor is opened after being cooled to room temperature, and the black product nitrogen-doped graphene is obtained.

[0040] Such as figure 1 as shown, figure 1 For the transmission electron microscope figure of the nitrogen-doped graphene prepared in embodiment 1, by figure 1 It can be seen that the nitrogen-doped graphene sheet structure obtained by the present invention is complete. Such as figure 2 as shown, figure 2 is the TEM selected area electron diffraction pattern of nitrogen-doped graphene, by figure 2 It can be seen that the nitrogen-doped graphene lattice structure obtained by the present invention is complete. Such as image 3 as shown, image 3 Be X-ray photoelectron spectrum curve, curve a a...

Embodiment 2

[0042] Take 100ml of graphene oxide colloid with a concentration of 5mg / ml, mix it with 100mg of ammonium carbonate evenly, freeze-dry, place the obtained powder in a sealed container and heat to 200°C, and keep it warm for 10h. After the reaction is finished, the reactor is opened after being cooled to room temperature, and the black product nitrogen-doped graphene is obtained.

[0043] as attached image 3 as shown, image 3 For the X-ray photoelectron spectrum curve of the nitrogen-doped graphene prepared in Example 2, curve c in the figure is the X-ray photoelectron spectrum curve of the nitrogen-doped graphene prepared in the present embodiment, as can be seen from curve c, after reacting for 10h , an obvious nitrogen doping peak appeared in graphene.

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Abstract

The invention provides a preparation method of nitrogen doped graphene and an application of the nitrogen doped graphene in super capacitors. The preparation method of the nitrogen doped graphene specifically comprises the following steps: putting a carbon material and a compound containing active nitrogen elements in an enclosed container, and heating to a temperature of 100 to 300 DEG C so as to obtain the nitrogen doped graphene. In the preparation process of the nitrogen doped graphene, under a heating condition, nitrogen elements in the compound containing active nitrogen elements are mixed into the carbon material so as to obtain the nitrogen doped graphene. The nitrogen doped graphene preparation method mentioned above avoids adopting a high reaction temperature, and has the advantages of mild preparation conditions and low production cost. The prepared nitrogen doped graphene is used as an electrode material of a super capacitor, and the specific capacity of the super capacitor can reach 190 F/g, when the electric current density is 5 A/g. The capacity retention ratio is 96.3% after 10000 times of circulation.

Description

technical field [0001] The invention relates to the technical field of graphene, in particular to a preparation method and application of nitrogen-doped graphene. Background technique [0002] Graphene is composed of carbon six-membered rings and has a two-dimensional periodic honeycomb lattice structure. This unique two-dimensional structure makes it have various excellent properties such as extremely high strength, good electrical conductivity, and excellent light transmission. Therefore, graphene has important application value in fields such as field emission transistors, supercapacitors, and lithium-ion batteries. [0003] Doping is a common method to adjust the electronic properties of semiconductor materials. Studies have shown that the energy band structure of graphene is adjusted after doping, which greatly expands the application range of graphene and improves its performance accordingly. For example, using doped graphene as the electrode material of a supercapaci...

Claims

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Application Information

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IPC IPC(8): C01B31/04H01G11/38C01B32/184
CPCY02E60/13
Inventor 刘兆平曹海亮周旭峰唐长林
Owner NINGBO GRAPHENE INNOVATION CENT CO LTD
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