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Preparation method of ultra-long few-walled carbon nanotube array

A carbon nanotube array and ultra-long technology, which is applied in the direction of carbon nanotubes, nanocarbons, chemical instruments and methods, etc., can solve the problems such as difficult to realize the preparation of long array carbon nanotubes, low growth rate, cumbersome purification process, etc. It is beneficial to macro preparation and large-scale application, and solves the effect of low yield

Active Publication Date: 2020-05-19
JIANGXI COPPER TECHNOLOGY RESEARCH INSTITUTE CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the above work, the length of the prepared carbon nanotubes is usually about 10 μm, and it is difficult to achieve the preparation of long array carbon nanotubes above 100 μm. At the same time, most of the grown multi-walled tubes
In the patent CN 101665248A, although it can prepare single and double-walled carbon nanotubes, its growth rate is very low, and the catalyst content in the product is very high, which requires a cumbersome purification process

Method used

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  • Preparation method of ultra-long few-walled carbon nanotube array
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  • Preparation method of ultra-long few-walled carbon nanotube array

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preparation example Construction

[0019] The invention discloses a preparation method of an ultra-long few-walled carbon nanotube array. The method uses a sheet material as a carrier, regulates the size and distribution density of catalyst active particles through a stoichiometric ratio, and uses cheap carbon-containing gas or liquid as a carbon source. , the catalyst is loaded through the container, and sulfur is introduced to fully increase the contact surface between the catalyst and the carbon source gas and expand the space for carbon tube growth, and prepare a few-walled ultra-long carbon nanotube array with a growth rate of The ratio of the mass of the nanotube to the mass of the catalyst used is more than 10 times.

[0020] Described method specifically comprises the following steps:

[0021] S1) Prepare the sheet catalyst, disperse the prepared catalyst on the container, and set aside;

[0022] S2) Put the container treated in S1) in the reactor, vacuumize it, feed inert gas, heat, feed mixed gas, co...

Embodiment 1

[0038] Example 1: Preparation of ultra-long carbon nanotube arrays from Fe / Mg / Al sheet material liquefied petroleum gas carbon source.

[0039] The active metal iron is loaded onto the layered double hydroxy metal hydroxide sheet material, and the stoichiometric ratio is adjusted so that iron accounts for 10wt% of the sheet material, and the Fe / Mg / Al sheet catalyst is prepared by coprecipitation method, which will be prepared The catalyst in the ethanol solvent was ultrasonically dispersed for 20 minutes, and the dispersion was even. The mass ratio of the catalyst to ethanol was 1:200. The dispersed solution was sprayed on the stainless steel mesh with a watering can, and the distribution density of the catalyst on the stainless steel mesh was 1mg / cm 3 , place the stainless steel mesh sprayed with the catalyst neatly in the tube furnace as figure 1 As shown, the arrangement of multi-layer stainless steel mesh increases the utilization rate of the tube furnace while making the ...

Embodiment 2

[0040] Example 2: Fe / Mg / Al sheet material liquefied natural gas plus sulfur carbon source to prepare ultra-long carbon nanotube arrays.

[0041] The active metal iron is loaded onto the layered double hydroxy metal hydroxide sheet material, and the stoichiometric ratio is adjusted so that iron accounts for 10wt% of the sheet material, and the Fe / Mg / Al sheet catalyst is prepared by coprecipitation method, which will be prepared The catalyst in the ethanol solvent was ultrasonically dispersed for 20 minutes, and the dispersion was even. The mass ratio of the catalyst to ethanol was 1:200. The dispersed solution was sprayed on the stainless steel mesh with a watering can, and the distribution density of the catalyst on the stainless steel mesh was 1mg / cm 3 , place the stainless steel mesh sprayed with the catalyst neatly in the tube furnace. After evacuation, 1000 sccm argon gas was introduced to scrub the gas, and the temperature was raised to 900 °C under the protection of argo...

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Abstract

The invention belongs to the technical field of carbon material preparation. The invention relates to a preparation method of a carbon nanotube array, in particular to a preparation method of a super-long few-walled carbon nanotube array. According to the method, a lamellar material is used as a carrier, wherein the size and the distribution density of active particles of the catalyst are regulated and controlled through a stoichiometric ratio; cheap carbon-containing gas or liquid is used as a carbon source; a catalyst is loaded by a container, and sulfur element is introduced, so that the contact surface between the catalyst and the carbon source gas is fully enlarged, the growth space of the carbon tubes is enlarged, and the few-wall super-long carbon nanotube array is prepared; the growth rate is more than 10 times of the ratio of the mass of the grown carbon nanotubes to the mass of the used catalyst, the length can reach more than 200 microns, and the Raman IG / ID value is not less than 3.0. The preparation method is simple and efficient, low in raw material cost, high in product purity and excellent in graphitization degree, industrial production can be achieved by carrying large equipment such as an industrial rotary furnace, a fluidized bed and a moving bed, and the preparation method has great significance in promoting industrial production and application of high-quality carbon nanotubes.

Description

Technical field: [0001] The invention belongs to the field of carbon material preparation technology and application technology, and in particular relates to a preparation method of an ultra-long few-wall carbon nanotube array. Background technique: [0002] Carbon nanotubes are a typical one-dimensional nanomaterial among many nanomaterials, and have received extensive attention and in-depth research since their discovery. Structurally, carbon nanotubes can be regarded as a seamless tube structure formed by curling one-dimensional graphite layers. According to the number of curled graphite layers, carbon nanotubes can be divided into single-walled carbon nanotubes and multi-walled carbon nanotubes. Among them, those with a graphite layer of about 2 to 7 layers are also called few-walled carbon nanotubes. Single-walled or few-walled carbon nanotubes have better physical and chemical properties than multi-walled tubes due to their high specific surface area and low defect de...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/162
CPCC01B32/162C01B2202/36C01B2202/34
Inventor 徐乐乐陈名海阮超
Owner JIANGXI COPPER TECHNOLOGY RESEARCH INSTITUTE CO LTD
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