Nitrogen-doped carbon nanotube and preparation method thereof

A carbon nanotube and nitrogen-doped carbon technology, which is applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of low nitrogen content in nitrogen-doped carbon nanotubes, and achieves simple equipment and process and easy operation. , the effect of easy large-scale industrial production

Active Publication Date: 2014-09-10
OCEANS KING LIGHTING SCI&TECH CO LTD +2
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Problems solved by technology

[0004] At present, the easy-to-achieve large-scale industrial preparation method of nitrogen-doped carbon nanotubes is the high-temperature thermal doping method, but the biggest problem of this method is that the nitrogen content of the prepared nitrogen-doped carbon nanotubes is low

Method used

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preparation example Construction

[0024] The preparation process of the nitrogen-doped carbon nanotubes of the present invention is roughly as follows: carbon nanotubes→modified carbon nanotubes→nitrogen-doped carbon nanotubes.

[0025] Specifically, the preparation process of nitrogen-doped carbon nanotubes of the present invention is divided into the following steps:

[0026] (1) Modified carbon nanotubes: place carbon nanotubes with a purity of 99% under a plasma with an output power of 100-300W, and react for 1-2 hours to obtain modified carbon nanotubes;

[0027] Wherein, the plasma is hydrogen plasma, argon plasma or helium plasma.

[0028] (2) Preparation of nitrogen-doped carbon nanotubes: Add the modified carbon nanotubes to a reactor in which urea is dissolved in anhydrous ethanol solution (the mass ratio of modified carbon nanotubes to nitrogen doping agent is 1:1 ~1:5), fully stirred for 2 hours, dried at 80°C for 6h, placed in an inert gas atmosphere with a flow rate of 400ml / min, and then raised...

Embodiment 1

[0034] (1) Modified carbon nanotubes: place carbon nanotubes with a purity of 99% under helium plasma, adjust the power to 100W, and process for 2 hours to obtain modified carbon nanotubes;

[0035] (2) Preparation of nitrogen-doped carbon nanotubes: Add the modified carbon nanotubes into a test tube of anhydrous ethanol solution dissolved in ammonia (the mass ratio of carbon nanotubes to urea is 1:2), stir for 2 hours, and place Dry at 80°C for 6 hours, then place it in an argon gas with a flow rate of 400ml / min to form an argon atmosphere, raise the temperature to 800°C at a rate of 20°C / min, and keep it for 1 hour, at a flow rate of 400ml / min The argon atmosphere was lowered to room temperature, and the resulting solid product was added into a 10% HCl solution, stirred for 4 hours, filtered and washed with deionized water, and the solid product was dried in a vacuum oven at 60°C for 12 hours. , to obtain nitrogen-doped carbon nanotubes.

Embodiment 2

[0037] (1) Modified carbon nanotubes: place carbon nanotubes with a purity of 99% under argon plasma, adjust the power to 150W, and process for 1 hour to obtain modified carbon nanotubes;

[0038] (2) Preparation of nitrogen-doped carbon nanotubes: Add the modified carbon nanotubes into an anhydrous ethanol solution dissolved in urea (the mass ratio of carbon nanotubes to urea is 1:3), stir for 2 hours, and place at 80 Dry at ℃ for 6 hours, then place it in nitrogen gas with a flow rate of 400ml / min to form a nitrogen atmosphere, raise the temperature to 850°C at a heating rate of 10°C / min, and keep it for 0.5 hours, then drop it in a nitrogen atmosphere with a flow rate of 400ml / min to room temperature, the resulting solid product was added to a 10% HCl solution, stirred for 4 hours, filtered and washed with deionized water, and the solid product was dried in a vacuum oven at 60°C for 12 hours to obtain nitrogen-doped carbon nanotubes.

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Abstract

The invention relates to a nitrogen-doped carbon nanotube and a preparation method thereof. The method comprises the following steps: placing a carbon nanotube in a reactor with plasma for 1 to 2 h so as to obtain a modified carbon nanotube; mixing the modified carbon nanotube with a nitrogen doping agent, successively carrying out full stirring and drying, then introducing inert gas into the reactor so as to allow an inert atmosphere to be formed in the reactor, then carrying out heating to 800 to 900 DEG C, maintaining the temperature for 0.5 to 1 h and carrying out cooling to room temperature after a reaction; and cleaning and drying the obtained solid product so as to obtain the nitrogen-doped carbon nanotube. According to the invention, the carbon nanotube treated by plasma has a great number of defects and has high nitrogen content during nitrogen doping; and the preparation method has the advantages of low cost and easy realization of large-scale industrial production.

Description

technical field [0001] The invention relates to the field of chemical material synthesis, in particular to a nitrogen-doped carbon nanotube and a preparation method thereof. Background technique [0002] In the 1990s, the use of carbon materials as energy storage materials promoted the vigorous development of supercapacitors and lithium-ion batteries. As a one-dimensional carbon material, carbon nanotubes have very high electrical conductivity, and carbon nanotubes are very easy to derivatize, so their derivatives have also attracted extensive attention from researchers. [0003] Carbon nanotube derivatives mainly include nitrogen-doped carbon nanotubes and boron-doped carbon nanotubes. Among them, the nitrogen atom in the nitrogen-doped carbon nanotube has one more electron than the outer layer of the carbon atom, and it is N-type doped, which has better energy storage performance than the carbon nanotube without doping, and the nitrogen-doped The higher the nitrogen cont...

Claims

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Application Information

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IPC IPC(8): C01B31/02B82Y30/00C01B32/168
Inventor 周明杰钟辉王要兵袁新生
Owner OCEANS KING LIGHTING SCI&TECH CO LTD
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