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Method for preparing single-wall carbon nanotube fiber by using mixed gaseous carbon source

A technology of single-walled carbon nanotubes and gaseous carbon sources, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of quality, purity, and output at the same time, and achieve good industrial Application prospects, high strength, large output effect

Active Publication Date: 2015-07-08
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to provide a method for directly macro-preparing high-quality, high-purity single-wall carbon nanotube fibers by a floating catalyst CVD method with a mixed gaseous carbon source, which realizes the convenience, Efficient and controllable preparation, which solves the scientific and technical problem that the quality, purity and yield of single-walled carbon nanotubes prepared by the floating catalyst CVD method cannot be balanced at the same time

Method used

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  • Method for preparing single-wall carbon nanotube fiber by using mixed gaseous carbon source
  • Method for preparing single-wall carbon nanotube fiber by using mixed gaseous carbon source
  • Method for preparing single-wall carbon nanotube fiber by using mixed gaseous carbon source

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Effect test

Embodiment 1

[0039] The flaky mixture containing ferrocene and sulfur powder (the weight ratio of ferrocene and sulfur powder is 100:1, after mixing evenly, press it into a tablet under 10MPa pressure) is placed in the low temperature zone in the tube, at 100sccm (ml / min ) under an argon protective atmosphere, the furnace temperature was raised to 1100°C at a rate of 20°C / min. After the temperature stabilized, the flow rate of argon was adjusted to 200 sccm, and 5 sccm methane, 0.2 sccm ethylene, and 200 sccm hydrogen were introduced simultaneously. When the gas flow is stable, the catalyst precursor is heated to 90°C to sublimate it. At this time, it can be seen that continuous cylindrical carbon nanotube macroscopic bodies ( figure 1 , CNT sock) flows out of the high temperature zone with the carrier gas, and is pre-set mechanical traction and collection at the tail end to form single-walled carbon nanotube fibers.

[0040] The above samples (referred to as 1#) were characterized by sc...

Embodiment 2

[0042] The flaky mixture containing ferrocene and sulfur powder (the weight ratio of ferrocene and sulfur powder is 100:1, after mixing evenly, press it into a tablet under 10MPa pressure) is placed in the low temperature zone in the tube, at 100sccm (ml / min ) under an argon protective atmosphere, the furnace temperature was raised to 1000°C at a rate of 20°C / min. After the temperature stabilized, the flow rate of argon was adjusted to 100 sccm, and 1 sccm methane, 0.2 sccm acetylene, and 100 sccm hydrogen were introduced simultaneously. When the gas flow is stable, the catalyst precursor is heated to 60°C to sublimate it. At this time, it can be seen that the continuous cylindrical carbon nanotube macroscopic body formed in the reactor flows out of the high temperature zone with the carrier gas, and is mechanically drawn and collected at the tail end to form single-walled carbon nanotube fibers.

[0043] The above samples (marked as 2#) were characterized by scanning electro...

Embodiment 3

[0045] The flaky mixture containing ferrocene and sulfur powder (the weight ratio of ferrocene and sulfur powder is 100:1, after mixing evenly, press it into a tablet under 10MPa pressure) is placed in the low temperature zone in the tube, at 100sccm (ml / min ) under an argon protective atmosphere, the furnace temperature was raised to 1000°C at a rate of 20°C / min. After the temperature was stabilized, the flow rate of argon was adjusted to 400 sccm, and 10 sccm methane, 2 sccm propylene, and 400 sccm hydrogen were fed simultaneously. When the gas flow is stable, the catalyst precursor is heated to 150°C to sublimate it. At this time, it can be seen that the continuous cylindrical carbon nanotube macroscopic body formed in the reactor flows out of the high temperature zone with the carrier gas, and is mechanically drawn and collected at the tail end to form single-walled carbon nanotube fibers.

[0046] The above samples were characterized by scanning electron microscope, tran...

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Abstract

The invention relates to the field of direct, massive, and controllable preparation of a high-quality single-wall carbon nanotube, and particularly provides a method for massively preparing a high-quality high-purity single-wall carbon nanotube fiber via a CVD method by using a floating catalyst of a mixed gaseous carbon source. A volatile organometallic compound, such as ferrocene, is taken as a precursor of the catalyst; sulfur powder and a sulfur-contained organic compound are taken as growth promoters; methane and a second low-carbon hydrocarbon are taken as carbon sources; a mixed gas of argon / hydrogen is taken as a carrier gas; and the growth of the single-wall carbon nanotube fiber is achieved at a temperature of 1000-1200 DEG C. The impurity content of the obtained single-wall carbon nanotube fiber is less than 15%; the concentrated oxidation temperature of the single-wall carbon nanotube is over 800 DEG C; and the G / D ratio of the single-wall carbon nanotube is more than 100. During the growth process of the single-wall carbon nanotube via the CVD method by using the floating catalyst, methane and a second low-carbon hydrocarbon are taken as carbon sources; and the massive, continuous, and controllable growth of the high-quality high-purity single-wall carbon nanotube fiber is realized in the presence of a low-flow protective gas mixed by argon and hydrogen.

Description

technical field [0001] The invention relates to the field of direct, large-scale and controllable preparation of high-quality single-wall carbon nanotubes, in particular to a method for macro-preparing high-quality, high-purity single-wall carbon nanotube fibers by a mixed gaseous carbon source floating catalyst CVD method. In the process of growing single-walled carbon nanotubes by floating catalyst CVD, using methane and low-carbon hydrocarbon gases as carbon sources, under the protective atmosphere of argon and hydrogen at a lower flow rate, high-quality, high-purity single-walled carbon nanotube fibers were achieved macro preparation. Background technique [0002] The excellent mechanical and electrical properties, high thermal conductivity, good thermal and chemical stability, high specific surface area and low density of single-walled carbon nanotubes make them have many potential applications. Both theoretical prediction and experimental research results show that th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02B82Y30/00B82Y40/00
Inventor 侯鹏翔李国显刘畅成会明
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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