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Preparation method of single-walled carbon nano-tube with adjustable diameter

A technology of carbon nanotubes and carbon sources, applied in nanostructure manufacturing, nanotechnology, nanotechnology, etc., can solve the problems of large changes in purity, unfavorable continuous reaction space, large-scale production, poor diameter and chirality adjustability, etc. , to achieve the effect of improving the purity

Inactive Publication Date: 2009-11-25
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

Among them, the hydrogen arc method is a non-equilibrium reaction process, so the controllability of the product structure is poor, and the purity varies greatly. Due to the limited reaction space, it is not conducive to continuous and large-scale production, and a large number of graphite flakes generated in the process are difficult to obtain during post-processing. It is not easy to remove, which affects the determination and application of the intrinsic properties of single-walled carbon nanotubes; the chemical vapor deposition method can continuously prepare a large number of single-walled carbon nanotubes, but the diameter distribution of the currently prepared single-walled carbon nanotubes is still large, and Its diameter and chirality are poorly tunable, which affects the application of single-walled carbon nanotubes in high-performance nanoelectronic devices

Method used

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  • Preparation method of single-walled carbon nano-tube with adjustable diameter
  • Preparation method of single-walled carbon nano-tube with adjustable diameter
  • Preparation method of single-walled carbon nano-tube with adjustable diameter

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Effect test

Embodiment 1

[0022] The carrier gas (buffer gas) hydrogen flow rate is 2.6cm / s, the carbon source methane flow rate is 0.005cm / s, the catalyst is ferrocene, and the sulfur-containing growth promoter is thiophene (C 4 h 4 S), the molar ratio of sulfur to iron is 1:35, the volatilization temperature of the catalyst is 120° C., the temperature of the reaction zone is 1100° C., the heating rate is 20° C. / min, and the temperature is kept for 5 minutes.

[0023] Observation under the transmission electron microscope ( figure 1 ) shows that the product is very pure and has less impurity content; observation of high-magnification projection photos shows that the product is a single-walled carbon nanotube ( figure 2 ); in this embodiment, the diameters of the single-walled carbon nanotubes are in the range of 1.8±0.2nm, and the purity of the single-walled carbon nanotubes is 40-80wt%.

Embodiment 2

[0025] The carrier gas is a mixed gas of hydrogen and argon (the molar ratio is 2:1). Thiophene (C 4 h 4 S), the molar ratio of sulfur to iron is 1:35, the volatilization temperature of the catalyst is 80° C., the temperature of the reaction zone is 1100° C., the heating rate is 30° C. / min, and the heat preservation is 50 minutes.

[0026] Observation under an electron microscope showed that the product was single-walled carbon nanotubes; in this embodiment, the diameters of the single-walled carbon nanotubes were within the range of 1.6±0.2 nm, and the purity of the single-walled carbon nanotubes was 40-80 wt%.

Embodiment 3

[0028] The carrier gas hydrogen flow rate is 3.2cm / s, the carbon source ethylene flow rate is 0.005cm / s, the catalyst is nickelocene, and the sulfur-containing growth promoter is carbon disulfide (CS 2 ), the molar ratio of sulfur to iron was 1:15, the volatilization temperature of the catalyst was 60°C, the temperature of the reaction zone was 1100°C, the heating rate was 40°C / min, and the heat preservation was 125min.

[0029] Observation under an electron microscope showed that the product was single-walled carbon nanotubes; in this embodiment, the diameters of the single-walled carbon nanotubes were within the range of 2.0±0.2 nm, and the purity of the single-walled carbon nanotubes was 40-80 wt%.

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Abstract

The invention relates to a preparation technique of carbon nano-tubes, in particular to a preparation method of a single-walled carbon nano-tube with adjustable diameter, which is suitable to prepare the single-walled carbon nano-tube with adjustable diameter. The single-walled carbon nano-tube with adjustable diameter can be produced by adopting organic compound catalyst containing iron, cobalt or nickel with ultra high hydrogen flow and ultra low carbon source flow, and sulfur-containing growth promoter after the organic compound catalyst and the sulfur-containing growth promoter are uniformly mixed in a gas state and are input into a reaction region, wherein the mol ratio of hydrogen and carbon source is more than 300, and the mol ratio of sulfur and iron, cobalt or nickel is 1 / 100-1 / 5. The invention inhibits the scission reaction of hydrocarbon with ultra high flow by adopting large-flow hydrogen as buffer gas, and large-flow hydrogen etches the generated agraphitic carbon and minor diameter single-walled carbon nano-tube, thereby improving the purity of the produced single-walled carbon nano-tube and narrowing the diameter.

Description

Technical field: [0001] The invention relates to a preparation technology of carbon nanotubes, specifically a method for preparing single-wall carbon nanotubes with adjustable diameter, which is suitable for preparing single-wall carbon nanotubes with adjustable diameters. Background technique: [0002] Carbon nanotubes are seamless tubular structures with one or more layers of graphene curled according to a certain helical angle, and the diameter is on the order of nanometers. Carbon nanotubes have a unique one-dimensional nanostructure and many excellent properties. Its discovery has opened up a new research field for nanomaterials, nano-optoelectronics, nanochemistry, microelectronics and other disciplines. The properties of SWNTs depend on their diameter and chirality. [0003] After years of hard work by scientists from various countries, although some achievements have been made in the preparation of single-walled carbon nanotubes, such as the large-scale preparation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02B82B3/00
Inventor 成会明刘庆丰任文才李峰丛洪涛
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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