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Method of continuously synthesizing large diameter single wall carbon nano-tube

A single-walled carbon nanotube, large-diameter technology, applied in nanotechnology, nanotechnology, nanostructure manufacturing, etc., can solve the problems of inability to achieve large-scale continuous production, short preparation duration, strict process requirements, etc., and achieve easy handling. , the effect of reducing the phenomenon of bunching, and the simple and easy-to-obtain raw materials

Inactive Publication Date: 2007-04-18
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method is easy to achieve continuous mass production, but it has strict requirements on the process
[0003] Found through literature search to prior art, Ecole Centrale Paris, LaboratoireMSS / MAT Quang-Hong Yang[Large-Diameter Single-Walled Carbon NanotubesSynthesized by Chemical Vapor Deposition (chemical vapor deposition method synthesizes large-diameter single-walled carbon nanotubes), Adv .Mater. (Advanced Materials) 2003, 15(10), 792. The method of chemical vapor deposition was used to prepare and synthesize large-diameter SWCNTs, but the catalytic decomposition method they adopted, the duration of large-diameter SWCNTs preparation was very short and could only last A few minutes, the output is very low, and the product can only be collected on the inner wall of the quartz glass tube, which cannot achieve the purpose of large-scale continuous production

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The synthesis is carried out in a horizontal quartz reactor. Under the protection of nitrogen gas, the temperature is raised to 1000°C, and the heating rate is 20°C / min, and then the ethanol dissolved in ferrocene and thiophene is fed into Solution, the concentration is 0.5g / 300ml, the concentration of thiophene is 0, the feed rate is 0.8ml / min, the flow rate of regulating argon is 120l / h, and the reaction time lasts for 3 hours. A filmy product was collected at the outlet. The obtained product is a single-wall carbon nanotube bundle, and the diameter of a single single-wall carbon nanotube is about 2 nm. Single-walled carbon nanotubes are relatively pure, with a small amount of metal iron particles adsorbed on the surface.

Embodiment 2

[0016] The synthesis is carried out in a horizontal quartz reactor. Under the protection of argon, the temperature is raised to 1100°C, and the heating rate is 20°C / min. For methanol solution, the concentration of ferrocene is 4g / 300ml, the concentration of thiophene is 3ml / 300ml, the feed rate is 0.5ml / min, the flow rate of argon gas is adjusted to be 180l / h, and the reaction time lasts for 3 hours. A filmy product was collected at the outlet. The original product was treated in nitric acid at 120°C for one hour, washed and dried to obtain a purified product. The average diameter of the obtained SWCNTs is about 5.79nm, the diameter of the largest single SWCNTs is 10.5nm, the phenomenon of bunching is reduced, and more SWCNTs appear in the form of single roots. Statistical data analysis showed that the proportion of 4-9.5nm large-diameter SWCNTs reached 78%.

Embodiment 3

[0018] Under the protection of argon, the temperature was raised to 1100°C at a rate of 20°C / min, and then an ethanol solution dissolved with ferrocene and thiophene was introduced with an electronic peristaltic pump. The concentration of ferrocene was 6g / 300ml, and the concentration of thiophene was The concentration is 3ml / 300ml, the feeding rate is 0.1ml / min, the argon flow rate is adjusted to 160l / h, and the reaction lasts for 2 hours. Film-like products are collected at the outlet, and the obtained products contain iron nanoparticles, single single-wall carbon nanotubes, single-wall carbon nanotube bundles and a small amount of multi-wall carbon nanotubes. The average diameter of SWCNTs is around 5nm.

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Abstract

The present invention relates to a method for continuously synthesizing large-diameter single-wall carbon nano tube, belonging to the field of nano material preparation technology. Said method is characterized by that it includes the following steps: using transition metal organics ferrocene as catalyst, using thiophene as accelerating agent, using methyl alcohol or ethyl alcohol as carbon source and solent, using inert gas as protection gas and carrier gas, introducing the carbon source and catalyst into high-temperature zone, in the high-temperature zone making the metal iron atoms decomposed out from metal organics ferrocene be agglomerated and formed into nano iron particles, under the catalytic action of high-temperature and transition metal iron particles making the carbon decomposed out from methyl alcohol or ethyl alcohol be formed into large-diameter single-wall carbon nano tube, at the same time continuously supplying alcohol and metal organics ferrocene, collecting formed single-wall carbon nano tubes in collector so as to implement continuous synthesis of large-diameter single-wall carbon nano tube.

Description

technical field [0001] The invention relates to a method in the technical field of nanomaterial preparation, in particular to a method for continuously synthesizing large-diameter single-walled carbon nanotubes, that is, using alcohol as a carbon source and thiophene as a growth control agent for floating catalytic continuous synthesis of large-diameter single-walled carbon nanotubes. A method for walled carbon nanotubes (SWCNTs). Background technique [0002] Depending on the curling angle, SWCNTs have zigzag), armchair and other helical structures. Different helical structures and diameters make SWCNTs have different properties. The discovery of SWCNTs has opened up a new field of vitality for the research of nanoelectronics, nanochemistry, and nanomaterials. In 1997, the discovery and application of SWCNTs was rated as one of the top ten scientific discoveries of the year by the world authoritative magazine Science. The application of SWCNTs is restricted by many factor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02B82B3/00
Inventor 王健农马杰苏连锋
Owner SHANGHAI JIAO TONG UNIV
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