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Method for continuously synthesizing single-wall carbon nano tube by high temperature chemical vapor deposition method

A technology of single-wall carbon nanotubes and vapor deposition method, which is applied in the direction of nanotechnology, nanotechnology, nanostructure manufacturing, etc., can solve the problems of inability to prepare and synthesize single-wall carbon nanotubes, and achieve the goal of improving structural defects and saving carrier gas The effect of using and simplifying process conditions

Inactive Publication Date: 2010-11-24
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The necessary condition for the growth of single-walled carbon nanotubes is to ensure that the carbon source is decomposed under the catalysis of common catalysts Fe, Co, and Ni. When the reaction temperature exceeds 1200 ° C, the commonly used liquid carbon source ethanol / acetone / n-hexane Word decomposition has occurred to produce an amorphous carbon structure that cannot be used to prepare synthetic single-walled carbon nanotubes

Method used

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  • Method for continuously synthesizing single-wall carbon nano tube by high temperature chemical vapor deposition method
  • Method for continuously synthesizing single-wall carbon nano tube by high temperature chemical vapor deposition method
  • Method for continuously synthesizing single-wall carbon nano tube by high temperature chemical vapor deposition method

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Effect test

Embodiment 1

[0030] The synthesis is carried out in a horizontal corundum tube reactor. Under the protection of nitrogen gas, the temperature is raised to 1500°C at a heating rate of 10°C / min, and then ethanol / methanol dissolved in ferrocene is fed by an electronic peristaltic pump. Mix solution (volume ratio 9:1), concentration is 0.1g / 100ml, thiophene concentration is 0.1ml / 100ml, feed rate is 0.5ml / min, the flow rate of regulating argon is 20l / h, and reaction time continues 3 hours. The product is collected at the outlet, and the surface of the product is sprayed with ethanol solution to obtain a fibrous single-walled carbon nanotube product, such as figure 1 shown. The obtained product is a single-wall carbon nanotube bundle, and the size of a single single-wall carbon nanotube is about 1 nm. Single-walled carbon nanotubes are relatively pure, with a small amount of metal iron particles adsorbed on the surface. The field emission scanning electron microscope picture is as follows: f...

Embodiment 2

[0033] The synthesis is carried out in a horizontal corundum tube reactor. Under the protection of argon, the temperature is raised to 1500 °C at a heating rate of 10 °C / min, and then the ethanol / Methanol mixed solution (volume ratio 9: 1), concentration is 0.1g / 100ml, thiophene concentration is 0.5%, feed rate is 0.5ml / min, the flow rate of regulating argon is 20l / h, and reaction time continues 3 hours. The product is collected at the outlet, and the obtained product is a single-wall carbon nanotube bundle, and the size 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.

[0034] The single-walled carbon nanotubes synthesized by the above method were laid flat on a corundum boat, and the corundum boat was placed in a corundum tube reaction tube for heat treatment. The furnace temperature was raised to 400°C at a rate of 10°C / min and kept for 1 hour. Af...

Embodiment 3

[0036] The synthesis is carried out in a horizontal corundum tube reactor. Under the protection of nitrogen gas, the temperature is raised to 1500°C at a heating rate of 10°C / min, and then ethanol / methanol dissolved in ferrocene is fed by an electronic peristaltic pump. Mix solution (volume ratio 7: 3), concentration is 0.1g / 100ml, thiophene concentration is 1%, feed rate is 0.5ml / min, the flow rate of regulating argon is 20l / h, and reaction time continues 3 hours. The product is collected at the outlet, and the product is attached to a glass substrate to obtain a film-like product such as image 3 shown. The obtained product is a single-wall carbon nanotube, and the size of a single single-wall carbon nanotube is about 4 nm. Single-walled carbon nanotubes are relatively pure, and there are more metal iron particles adsorbed on the surface. Scanning electron microscope pictures of the original single-walled carbon nanotube samples obtained are as follows: Figure 4 shown. ...

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Abstract

The invention relates to a method for continuously synthesizing a single-wall carbon nano tube by a high temperature chemical vapor deposition method, belonging to the technical field of chemosynthesis. The method comprises the following specific steps: introducing inert gas in an alundum tube reactor and heating to 1300-1500 DEG C; introducing a mixing solution containing a catalyst, a carbon source and an additive, thiophene and inert gas in the alundum tube reactor; collecting a product at the opening of the alundum tube reactor; paving the product in an alundum boat, placing the alundum boat in the alundum tube reactor for heat treatment, heating to 400-500 DEG C at a speed of 10 DEG C / min and keeping the temperature for 1h; sealing the two ends of the alundum tube, introducing inert gas, heating to 800-900 DEG C at a speed of 10 DEG C / min and keeping the temperature for 1h; introducing argon, cooling to room temperature, and enabling the product to react with diluted hydrochloric acid; and filtering, washing and drying. The raw materials are simple and easily obtained and have no obvious inflammable danger; the product is easy to collect and has high yield; the device is simple and can realize continuous operation; and the invention has low cost and no environmental pollution and can be applied to large-scale production.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for continuously synthesizing single-walled carbon nanotubes by high-temperature chemical vapor deposition. Background technique [0002] Single-walled carbon nanotubes (SWCNTs) have attracted widespread interest due to their unique structures, extremely high mechanical properties, tunable electrical properties, and good stability. The discovery of SWCNT has opened up a new field full of vitality for the research of nanoelectronics, nanochemistry and nanomaterials. SWCNT was first discovered by the graphite arc method. After the unremitting efforts of scientists, preparation methods such as laser evaporation and chemical vapor deposition (CVD) have been developed. Carbon nanotubes prepared by graphite arc method and laser evaporation method have higher purity and crystallization degree, but lower yield. The chemical vapor deposition method is divided into ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02B82B3/00
Inventor 马杰
Owner TONGJI UNIV
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