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Method for directly growing semiconductor type single-walled carbon nanotube with floating catalyst and auxiliary oxygen

A technology of single-walled carbon nanotubes and floating catalysts, applied in the direction of nanotechnology, etc., can solve the problems of intrinsic structure damage of single-walled carbon nanotubes, small amount of semiconducting single-walled carbon nanotubes, and wide range of diameter distribution, and achieve Overcome the effects of wide diameter distribution, good industrial application prospects, and narrow diameter distribution

Active Publication Date: 2013-02-27
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

[0006] A technical problem solved by the present invention is to overcome problems such as cumbersome steps in the separation process of existing chemical and physical methods, serious damage to the intrinsic structure of single-walled carbon nanotubes, etc.; another technical problem solved by the present invention is to overcome the existing direct preparation of semiconductor Problems such as small amount of single-walled carbon nanotubes, wide range of diameter distribution, and small diameter

Method used

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  • Method for directly growing semiconductor type single-walled carbon nanotube with floating catalyst and auxiliary oxygen
  • Method for directly growing semiconductor type single-walled carbon nanotube with floating catalyst and auxiliary oxygen
  • Method for directly growing semiconductor type single-walled carbon nanotube with floating catalyst and auxiliary oxygen

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Experimental program
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Effect test

Embodiment 1

[0025] A piece of ferrocene containing 50wt% sulfur powder (the weight ratio of sulfur powder and ferrocene is 1:1) is placed in the low temperature zone of the chemical vapor deposition reduction furnace (CVD furnace, the diameter is 25mm, and the length of the constant temperature zone is 4cm) , in a hydrogen atmosphere of 500ml / min, the temperature was raised to 1100°C at a rate of 30°C / min, and 3ml / min of methane and 0.2ml / min of oxygen were introduced, and the ferrocene was simultaneously pushed to a furnace temperature of 80°C , the single-walled carbon nanotubes were grown for 30 minutes. After the chemical vapor deposition is finished, turn off methane and oxygen, and drop to room temperature under the protection of hydrogen.

[0026]10 mg of single-walled carbon nanotubes prepared in step (1) were uniformly placed in a heating furnace tube with a diameter of 25 mm and a constant temperature zone length of 4 cm, and oxidized at 370° C. for 10 h. After the sample was c...

Embodiment 2

[0029] (1) A piece of ferrocene containing sulfur powder (the weight ratio of sulfur powder and ferrocene is 1:10) is placed in the low temperature of chemical vapor deposition reduction furnace (CVD furnace, diameter is 25mm, constant temperature zone length is 4cm) Zone, under a hydrogen atmosphere of 600ml / min, the temperature was raised to 1100°C at a rate of 30°C / min, 3ml / min of methane and 0.1ml / min of oxygen were introduced, and the ferrocene was simultaneously pushed to a furnace temperature of 80 °C, the growth of single-walled carbon nanotubes is carried out, and the growth time is 30 minutes. After the chemical vapor deposition is finished, turn off methane and oxygen, and drop to room temperature under the protection of hydrogen.

[0030] (2) 10 mg of single-walled carbon nanotubes prepared in step (1) were evenly placed in a heating furnace tube with a diameter of 25 mm and a constant temperature zone length of 4 cm, and oxidized at 370° C. for 10 h. After the sa...

Embodiment 3

[0033] (1) A piece of ferrocene containing sulfur powder (the weight ratio of sulfur powder and ferrocene is 1:5) is placed in the low temperature of chemical vapor deposition reduction furnace (CVD furnace, diameter is 25mm, constant temperature zone length is 4cm) zone, under a hydrogen atmosphere of 800ml / min, the temperature was raised to 1100°C at a rate of 30°C / min, 3ml / min of methane and 0.3ml / min of oxygen were introduced, and the ferrocene was simultaneously pushed to a furnace temperature of 80 °C, the growth of single-walled carbon nanotubes is carried out, and the growth time is 30 minutes. After the chemical vapor deposition is finished, turn off methane and oxygen, and drop to room temperature under the protection of hydrogen.

[0034] (2) 5 mg of single-walled carbon nanotubes prepared in step (1) were evenly placed in a heating furnace tube with a diameter of 25 mm and a constant temperature zone length of 4 cm, and oxidized at 370° C. for 10 h. After the samp...

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Abstract

The invention relates to massive and controllable preparation field of semiconductor type single-walled carbon nanotubes, specifically to a method for directly growing the semiconductor type single-walled carbon nanotube with floating catalyst and auxiliary oxygen. The method comprises the following steps of: taking ferrocene as precursor of the catalyst, taking right amount of sulphur powder as growth promoter, and taking hydrogen as a carrier gas; simultaneously introducing a carbon source gas and small amount of oxygen to grow the single-walled carbon nanotube, and etching the small-diameter and metallic single-walled carbon nanotube in situ; and finally, obtaining a sample in which the semiconductor type single-walled carbon nanotube is dominant, wherein content of the semiconductor type single-walled carbon nanotube is 90 wt%, and diameter distribution of the semiconductor type single-walled carbon nanotube is 1.4-1.8 nm. With the method, massive and directly controlled growth of the semiconductor type single-walled carbon nanotube with narrower diameter distribution is realized; and the method solves the problems, such as that the separation process of the existing chemical and physical methods seriously damages the intrinsic structure of the single-walled carbon nanotube and the process is complex, and sample amount is less, diameter distribution is wider and the diameter is smaller in the direct preparation technology, and the like.

Description

technical field [0001] The invention relates to the field of direct, massive and controllable preparation of semiconducting single-walled carbon nanotubes, in particular to a method for directly growing semiconducting single-walled carbon nanotubes with an oxygen-assisted floating catalyst, in which single-walled carbon is grown by chemical vapor deposition on the floating catalyst An appropriate amount of oxygen is introduced in situ during the nanotube process to realize the macroscopic and controllable direct growth of semiconducting single-walled carbon nanotubes with narrow diameter distribution. Background technique [0002] The conductive properties of single-walled carbon nanotubes are closely related to their structure. Due to the different curling methods that make up their graphene sheets, they can be metallic or semiconducting, and carbon nanotubes have excellent transport properties. Therefore, carbon nanotubes are considered to be As an ideal material for const...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/02B82Y40/00
Inventor 侯鹏翔于冰刘畅成会明
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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