Method for preparing nitrogen-atom doped carbon nanomaterial

A technology of carbon nanomaterials and nanomaterials, which is applied in the field of hybrid carbon materials and its preparation, can solve the problems of product specific surface area decrease, low nitrogen atom doping amount, and no improvement, etc., and achieve simple and easy process, high specific surface area Great, low-cost effect

Active Publication Date: 2017-05-24
SICHUAN UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

Although these methods have effectively increased the N doping amount of the product, the specific surface area of ​​the obtained product has been significantly reduced, which is not conducive to performance optimization.
That is to say, people are still mainly stuck in the idea of ​​changing the nitrogen source compound to increase the doping amount of nitrogen atoms, and have not improved the self-hybridization chemical reactivity of graphene or graphene derivatives (especially higher Starting from the basic idea of ​​temperature), seek a new way to solve the problem of low doping amount of nitrogen atoms

Method used

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  • Method for preparing nitrogen-atom doped carbon nanomaterial

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Effect test

Embodiment 1

[0028] Graphene is placed in a closed vacuum reactor, and the air in the reactor is replaced with argon for three times, then vacuumized, then filled with a mixture of fluorine and argon, and the initial partial pressure of fluorine in the reactor is controlled to be 30KPa, then raise the temperature to 80°C at a heating rate of 10°C / min and keep it warm for 300 minutes. After the reactor is naturally cooled to room temperature, the fluorinated graphene is taken out. Put the fluorinated graphene into the tube furnace and feed the mixed gas of ammonia / argon, the concentration of ammonia is 30%, the flow rate is 1Torr, and the temperature is raised to 700°C at a heating rate of 10°C / min, and kept warm 0.5 hours. After the tube furnace was cooled to room temperature, the obtained nitrogen-doped graphene was taken out.

[0029] The nitrogen content of this nitrogen-doped graphene is 5.4%, and the specific surface area is 443m 2 / g.

Embodiment 2

[0031] Place the multi-walled carbon nanotubes in a closed vacuum reactor, replace the air in the reactor with nitrogen three times, then evacuate it, then fill it with a mixture of fluorine and nitrogen, and control the initial partial pressure of fluorine in the reactor to 80KPa, then raise the temperature to 250°C at a heating rate of 20°C / min and keep it warm for 10 minutes. After the reactor is naturally cooled to room temperature, the fluorinated multi-walled carbon nanotubes are taken out. Put the fluorinated multi-walled carbon nanotubes into the tube furnace and pass through the ammonia / nitrogen mixed gas, wherein the concentration of ammonia is 2%, the flow rate is 20Torr, and the temperature is raised to 400°C at a heating rate of 20°C / min. And keep warm for 24 hours. After the tube furnace was cooled to room temperature, the obtained nitrogen-doped multi-walled carbon nanotubes were taken out.

[0032] The nitrogen content of the nitrogen-doped multi-walled carbon...

Embodiment 3

[0034] Graphene oxide is placed in a closed vacuum reactor, the air in the reactor is replaced with nitrogen for three times and then vacuumized, then filled with a mixture of fluorine and argon, and the initial partial pressure of fluorine in the reactor is controlled to 3KPa, then raise the temperature to 150°C at a heating rate of 1°C / min and keep it warm for 60 minutes. After the reactor is naturally cooled to room temperature, the fluorinated graphene oxide is taken out. Put the fluorinated graphene oxide into the tube furnace and feed the ammonia / argon mixed gas, wherein the concentration of ammonia is 15%, the flow rate is 10Torr, and at the same time, the temperature is raised to 550°C at a heating rate of 3°C / min, and Keep warm for 6 hours. After the tube furnace was cooled to room temperature, the nitrogen-doped graphene was obtained.

[0035] The nitrogen content of this nitrogen-doped graphene is 6.4%, and the specific surface area is 643m 2 / g.

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Abstract

The invention discloses a method for preparing a nitrogen-atom doped carbon nanomaterial. The method comprises the following steps: performing direct fluorination treatment on a carbon nanomaterial or derivatives thereof in an inert gas atmosphere by taking a fluorine gas mixture as a fluorination agent so as to obtain a fluorinated carbon nanomaterial; and performing high-temperature after-treatment on the obtained fluorinated carbon nanomaterial in an ammonia / argon mixed gas atmosphere, thereby obtaining the nitrogen doped carbon nanomaterial. With the adoption of a modification method of 'sequentially activating and doping' in the invention, an effective novel method for improving the nitrogen doping amount is explored in the field, and the obtained nitrogen doped carbon nanomaterial is high in nitrogen content, large in specific surface area, simple and feasible in process and low in cost and has excellent application prospects.

Description

technical field [0001] The invention belongs to the technical field of hybrid carbon materials and preparation thereof, and in particular relates to a preparation method of nitrogen atom-doped carbon nanomaterials. Background technique [0002] The global population is increasing, the economy is expanding rapidly, and the demand for energy is growing at an alarming rate. However, the limited supply of fossil fuel energy and the low energy utilization rate on a global scale make energy issues a global problem. Therefore, the development of new energy has become a very important research topic in the field of energy, and the development of advanced energy transfer and storage technology has become a research hotspot in the field of new energy. [0003] Compared with traditional materials, carbon nanomaterials have unique mechanical, catalytic, and photoelectric properties due to their size-dependent properties, and can be used in solar energy harvesting, hydrogen preparation a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/194C01B32/168C01B32/184B82Y30/00
CPCB82Y30/00C01P2006/12
Inventor 王旭刘向阳陈腾刘洋赖文川李玉龙
Owner SICHUAN UNIV
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