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Preparation method of nitrogen-doped graphene

A nitrogen-doped graphene and nitrogen source technology, applied in the field of nitrogen-doped graphene preparation, can solve the problems of complex operation, high equipment requirements, and high cost

Active Publication Date: 2013-01-23
OCEANS KING LIGHTING SCI&TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the existing method of preparing graphene by chemical vapor deposition requires the addition of a catalyst, which requires high equipment and complicated operation, resulting in high cost.

Method used

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  • Preparation method of nitrogen-doped graphene
  • Preparation method of nitrogen-doped graphene

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preparation example Construction

[0016] The embodiment of the present invention provides a method for preparing nitrogen-doped graphene with simple process, high yield, low production cost, and easy operation and control. The technological process of the preparation method of this nitrogen-doped graphene is as figure 1 Shown, adopt chemical vapor deposition method to prepare nitrogen-doped graphene, it comprises the following steps:

[0017] S1: Provide substrate, solid and / or liquid organic carbon source compound;

[0018] S2: preparing the organic carbon source compound into a solution or suspension;

[0019] S3: coating the solution or suspension containing the organic carbon source compound on the surface of the substrate;

[0020] S4: In an oxygen-free environment and under vacuum conditions, the substrate coated with the solution or suspension containing an organic carbon source compound is heated up to 500-1300 ° C, and then a gaseous nitrogen source compound is introduced to react to obtain the obta...

Embodiment 1

[0034]The preparation method of nitrogen-doped graphene, comprises the steps:

[0035] S11. Ultrasonic cleaning the nickel foil substrate with deionized water, ethanol, and acetone and then drying, preparing ferrocene into a solution with a mass percentage concentration of 20 wt%, and then spin-coating it on the surface of the substrate;

[0036] S12. Put the substrate coated with ferrocene into the reaction chamber, and seal the reaction chamber, and use mechanical pumps, Roots pumps and molecular pumps to pump the reaction chamber to 10 -3 Below Pa, and keep it for 10 minutes, turn off the molecular pump and start heating;

[0037] S13. When the substrate temperature reaches 500°C, keep the temperature constant, and then feed in nitrogen-containing substance ammonia gas with a flow rate of 10 sccm, and start to generate nitrogen-doped graphene; wherein, the amount of nitrogen gas fed in is related to the amount of ferrocene Relationship: The molar ratio of carbon to nitroge...

Embodiment 2

[0043] The preparation method of nitrogen-doped graphene, comprises the steps:

[0044] S21. Ultrasonic cleaning the copper foil substrate with deionized water, ethanol, and acetone and then drying it, and preparing a solution with a mass percent concentration of 5 wt% of nickelocene, and then spin-coating it on the surface of the substrate;

[0045] S22. put the substrate coated with nickelocene into the reaction chamber, and seal the reaction chamber, and use a mechanical pump, Roots pump and molecular pump to pump the reaction chamber to 10 step by step. -3 Below Pa, and keep it for 30 minutes, turn off the molecular pump and start heating;

[0046] S23. When the substrate temperature reaches 1300°C, keep the temperature constant, and then feed the nitrogen-containing substance methylamine with a flow rate of 200 sccm, and start to generate nitrogen-doped graphene; wherein, the amount of methylamine fed is the same as the amount of nickelocene Relationship: The molar ratio...

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Abstract

The invention provides a preparation method of nitrogen-doped graphene by a chemical vapor deposition method, which comprises the following steps of: providing a substrate with high temperature resistance, and a solid and / or liquid organic carbon source compound; preparing the organic carbon source compound into solution or suspension; coating the solution or suspension of the organic carbon source compound on the surface of the substrate; heating the substrate coated by solution or suspension containing the organic carbon source compound to 500-1300 DEG C under an oxygen-free and vacuum environment, then leading into gaseous nitrogen compound to react to obtain nitrogen-doped graphene. The preparation method of nitrogen-doped graphene provided by the invention prepares the solid and / or liquid organic carbon source compound into solution or suspension and coats directly on the surface of the substrate to make the organic carbon source compound react with the introduced nitrogen compound. The method provided by the invention has the advantages of having no need of adding a catalyst, simplifying the production process of nitrogen-doped graphene effectively and reducing the production cost. At the same time, the nitrogen-doped graphene prepared by the chemical vapor deposition method enables the doped graphene to be controlled easily in the amount, to be doped uniformly and to be high in electrochemical stability.

Description

technical field [0001] The invention belongs to the technical field of carbon materials, and in particular relates to a preparation method of nitrogen-doped graphene. Background technique [0002] Graphene is a two-dimensional carbon atom crystal discovered by Andre K. Geim of the University of Manchester in 2004. It is a single-layer or multi-layer extremely thin carbon material. Due to its unique structure and photoelectric properties, it has become a research hotspot in the fields of carbon materials, nanotechnology, condensed matter physics and functional materials, attracting many scientific and technological workers. Single-layer graphene has a large specific surface area, excellent electrical and thermal conductivity and low thermal expansion coefficient, and can be used in effect transistors, electrode materials, composite materials, liquid crystal display materials, sensors, etc. At present, the methods for preparing graphene mainly include graphite exfoliation, ch...

Claims

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Application Information

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IPC IPC(8): C01B31/02C01B32/186
Inventor 周明杰袁新生王要兵
Owner OCEANS KING LIGHTING SCI&TECH CO LTD
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