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Process for directly synthesizing ultra-long single-wall continuous nano carbon tube

A technology of single-walled carbon nanotubes and process methods, applied in the direction of single-walled carbon nanotubes, carbon nanotubes, and oriented carbon nanotubes, can solve the problems of benzene toxicity, environmental pollution, and high carbon content in benzene, and achieve directional Good performance, simple operation, continuous growth effect

Inactive Publication Date: 2002-08-28
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the high carbon content of benzene, it is only suitable for the preparation of multi-walled carbon nanotubes and carbon nanofibers
And benzene is toxic and pollutes the environment

Method used

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  • Process for directly synthesizing ultra-long single-wall continuous nano carbon tube
  • Process for directly synthesizing ultra-long single-wall continuous nano carbon tube
  • Process for directly synthesizing ultra-long single-wall continuous nano carbon tube

Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach

[0012] The equipment main body of the vertical floating catalytic cracking method is a vertical ceramic reaction tube 1 (outer diameter 68mm, inner diameter 58mm, length 1600mm), and this tube is vertically placed in the electric resistance furnace 2 (rated temperature is 1200 ℃, rated power 6KW). The upper part of the reaction vessel is an evaporator 3, including an air inlet 4 and a reaction solution (a mixed solution of n-hexane, ferrocene, and thiophene) inlet 5. The reaction solution 6 is introduced into the evaporator 3 through the liquid micro-flow pump 7 (the evaporation temperature is 150-200° C.) and introduced into the reaction vessel 1 together with the carrier gas (hydrogen) in the form of steam. A product collection bottle 8 , a filter 9 and an exhaust gas outlet 10 are installed below the reaction vessel 1 . The specific operation steps are as follows:

[0013] (1) First pass argon gas at 100ml / min and start to raise the furnace temperature. When it reaches abo...

Embodiment 1

[0021] (1) First flow argon gas at 100ml / min and start to heat up. When it reaches about 1000°C, start to flow hydrogen gas and stop argon gas.

[0022] (2) The temperature is raised to the predetermined reaction temperature (1100° C.), and the reaction solution is introduced to start the preparation of the product. In the reaction solution, n-hexane (C 6 h 14 ) as carbon source, ferrocene (Fe(C 5 h 5 ) 2 , 0.010g / ml) as catalyst, thiophene (G 4 h 4 S, 0.6wt.%) as an additive.

[0023] (3) The reaction solution introduction flow rate is 0.5ml / min, and the hydrogen flow rate is 200ml / min.

[0024] (4) Stop heating after keeping warm for about 60 minutes. Cool with argon (100ml / min) and stop the hydrogen, and collect the product after the temperature drops to room temperature.

[0025] (5) Scanning electron microscopy and transmission electron microscopy were used to detect the microscopic morphology of the product. The product is a 20 cm long filament, which is compos...

Embodiment 2

[0028] (1) First flow argon gas at 100ml / min and start to heat up. When it reaches about 1000°C, start to flow hydrogen gas and stop argon gas.

[0029] (2) The temperature is raised to the predetermined reaction temperature (1150° C.), and the reaction solution is introduced to start the preparation of the product. The reaction solution adopts n-hexane (C 6 h 14 ) as carbon source, ferrocene (Fe(C 5 h 5 ) 2 , 0.020g / ml) as catalyst, thiophene (C 4 h 4 S, 0.4wt.%) as an additive.

[0030] (3) The reaction solution introduction flow rate is 0.5ml / min, and the hydrogen flow rate is 250ml / min.

[0031] (4) Stop heating after keeping warm for about 60 minutes. Cool with argon (100ml / min) and stop the hydrogen, and collect the product after the temperature drops to room temperature.

[0032] (5) Scanning electron microscopy and transmission electron microscopy were used to detect the microscopic morphology of the product. The product is a 20cm long filament, which is comp...

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Abstract

A technological process for preparing ultra-long single-wall continuous nanometre carbon tubes by the vertical floating catalytic cracking method includes such steps as preparing reaction solution from n-hexane as carbon source, ferrocene as catalyst and thiophene as additive, introducing it in the form of vapour along with hydrogen gas into a reactor for catalytic cracking. Under specific technological parameters, ultra-long cord-shape single-wall nm carbon tube bundle can be obtained, the tubes have good orientation, their purity up to 85%, they are continuous and straight with length up to20 cm (length to diameter ratio greater than 108). The said method only needs one vertical electric furnace and no need of pre-reduction. Its advantages include good orientation performance, high purity, long length, simple operation and low cost.

Description

technical field [0001] The invention relates to a preparation process of carbon nanomaterials, in particular to a synthesis process method of single-walled carbon nanotubes. Background technique [0002] The discovery of single-walled carbon nanotubes has greatly promoted the development of nanotechnology research and its applications. In 1996, Smalley's research group reported a method for synthesizing high-purity single-walled carbon nanotubes by laser evaporation in the journal Science (Science, 1996, 273(5274): 483-487). In 1997, Journet et al. reported in the journal Nature (Nature, 1997, 388: 756-758) the process of preparing single-walled carbon nanotubes in batches by the DC arc method. In addition, the preparation of single-walled carbon nanotubes by catalytic cracking technology has also become one of the focuses of this research field, because this method is the most likely method to realize the large-scale industrialization of carbon nanotubes. In the literatur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C23C16/26C30B25/00
CPCB82Y30/00B82Y40/00C01B2202/02C01B2202/08C01B2202/34C01B2202/36C23C16/26C30B25/00Y10S977/742Y10S977/75C30B29/02C30B29/605C01B32/162C01B32/164Y10T428/2918
Inventor 朱宏伟徐才录吴德海魏秉庆P·M·阿加亚
Owner TSINGHUA UNIV
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