Controllable preparation method of high-oxidation-resistance high-purity single/double-wall carbon nanotube

A technology of double-walled carbon nanotubes and single-walled carbon nanotubes, applied to the controllable preparation method of single/double-walled carbon nanotubes, which can solve the problem of difficult large-scale production, high oxidation resistance, and purity of single or double-walled carbon nanotubes Low-level problems, to achieve controllable preparation, selectivity, and easy purification

Active Publication Date: 2012-01-18
唯碳纳米科技(沈阳)有限公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a floating catalyst chemical vapor deposition method for directly preparing a large amount of single / double-walled carbon nanotubes with high purity, controllable layer number and high oxidation resistance; for the first time, high purity and high oxidation resistance have been realized The chemical vapor deposition method of single or double-walled carbon nanotubes overcomes the problems of low purity and difficulty in large-scale production of single or double-walled carbon nanotubes with high oxidation resistance prepared by the existing arc method

Method used

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  • Controllable preparation method of high-oxidation-resistance high-purity single/double-wall carbon nanotube
  • Controllable preparation method of high-oxidation-resistance high-purity single/double-wall carbon nanotube
  • Controllable preparation method of high-oxidation-resistance high-purity single/double-wall carbon nanotube

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Experimental program
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Effect test

Embodiment 1

[0023] (1) A piece of ferrocene containing 0.5wt% sulfur powder is placed in the low-temperature zone of the chemical vapor deposition furnace (CVD furnace, the diameter is 50mm, and the length of the constant temperature zone is 8cm), and the temperature is raised at 30° C. / min under a hydrogen atmosphere. Raise the rate to 1100°C, increase the hydrogen flow rate to 12,000ml / min, inject 20ml / min of methane, and push the ferrocene containing sulfur powder to the furnace temperature of 215°C at the same time to grow carbon nanotubes. The growth time was 30 minutes. After the chemical vapor deposition is finished, turn off the methane, and drop to room temperature under the protection of low hydrogen flow rate (the hydrogen flow rate is 100ml / min).

[0024] (2) 30 mg of carbon nanotubes prepared in step (1) were evenly placed in a heating furnace tube with a diameter of 50 mm and a constant temperature zone length of 8 cm, and oxidized at 370° C. for 10 h. After the sample was ...

Embodiment 2

[0027] (1) A piece of ferrocene containing 1wt% sulfur powder is placed in the low-temperature zone of the chemical vapor deposition furnace (CVD furnace, the diameter is 50mm, and the length of the constant temperature zone is 8cm), at a heating rate of 30°C / min under a hydrogen atmosphere Raise to 1100°C, increase the hydrogen flow rate to 10,000ml / min, feed 30ml / min of methane, and push the ferrocene containing sulfur powder to the furnace temperature of 180°C at the same time to grow carbon nanotubes. The time is 30 minutes. After the chemical vapor deposition is finished, turn off the methane, and drop to room temperature under the protection of low hydrogen flow rate (the hydrogen flow rate is 100ml / min).

[0028] (2) 30 mg of carbon nanotubes prepared in step (1) were evenly placed in a heating furnace tube with a diameter of 50 mm and a constant temperature zone length of 8 cm, and oxidized at 370° C. for 10 h. After the sample was cooled to room temperature, it was t...

Embodiment 3

[0031] (1) A piece of ferrocene containing 1wt% sulfur powder is placed in the low-temperature zone of the chemical vapor deposition furnace (CVD furnace, the diameter is 50mm, and the length of the constant temperature zone is 8cm), at a heating rate of 30°C / min under a hydrogen atmosphere Raise to 1100°C, increase the flow rate of hydrogen to 5000ml / min, feed 30ml / min of methane, and push the ferrocene containing sulfur powder to a furnace temperature of 180°C at the same time to grow carbon nanotubes. The time is 30 minutes. After the chemical vapor deposition is finished, turn off the methane, and drop to room temperature under the protection of low hydrogen flow rate (the hydrogen flow rate is 100ml / min).

[0032] (2) 30 mg of carbon nanotubes prepared in step (1) were evenly placed in a heating furnace tube with a diameter of 50 mm and a constant temperature zone length of 8 cm, and oxidized at 370° C. for 10 h. After the sample was cooled to room temperature, it was ta...

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Abstract

The invention relates to the field of the controllable preparation of high-oxidation-resistance single / double-wall carbon nanotubes, in particular to a controllable preparation method of high-oxidation-resistance high-purity single / double-wall carbon nanotubes. The controllable preparation method comprises the following steps of: introducing carbon-source gas by utilizing a floating-catalyst chemical vapor-deposition method and using ferrocene as a catalyst precursor and sulfur powder as a growth promoter at a higher temperature, growing the high-oxidation-resistance carbon nanotubes under a high hydrogen-gas carrier-gas flow quantity, and simultaneously realizing the controlled growth of the single-wall or double-wall carbon nanotubes by regulating and controlling the quantity of the added growth promoter for sulfur to obtain the high-purity high-oxidation-resistance single / double-wall carbon nanotubes, wherein the single-wall or double-wall carbon nanotubes account for more than 90 percent of the total content of carbon tubes, and the highest oxidation-resisting temperatures of the single-wall and double-wall carbon nanotubes are respectively 770 DEG C and 785 DEG C. The single / double-wall carbon nanotubes with high crystallization degrees, fewer structural defects and high purity are obtained by the method, have the characteristics of excellent electrical conductivity, highelasticity, high strength and the like and are expected to be applied to transparent conductive films and the related devices of the transparent conductive films.

Description

technical field [0001] The invention relates to the field of controllable preparation of single / double-wall carbon nanotubes with high oxidation resistance, in particular to a controllable preparation method of high oxidation resistance, high purity, single / double-wall carbon nanotubes, using floating catalyst chemical gas phase The deposition method grows carbon nanotubes with high oxidation resistance under a high hydrogen carrier gas flow rate, and at the same time, the controlled growth of single-walled or double-walled carbon nanotubes is realized by adjusting the amount of sulfur growth promoter added. Background technique [0002] Using carbon nanotubes to assemble transparent conductive films (Transparent Conductive Films, TCFs) is one of the main application directions of carbon nanotubes; flexibility is the biggest advantage of carbon nanotube transparent conductive films compared with traditional oxide transparent conductive films. The main preparation methods of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02B82Y40/00
Inventor 侯鹏翔于冰刘畅成会明
Owner 唯碳纳米科技(沈阳)有限公司
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