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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 nanotechnology, nanotechnology, nanostructure manufacturing, etc., can solve the problems of inability to prepare and synthesize single-wall carbon nanotubes, achieve structural defects, shorten growth time, The effect of saving the use of carrier gas

Inactive Publication Date: 2012-07-25
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, the temperature is raised to 1500℃, and the heating rate is 10℃ / min, and then the ethanol / methanol dissolved with ferrocene is introduced by the electronic peristaltic pump The mixed solution (volume ratio 9:1), the concentration is 0.1g / 100ml, the thiophene concentration is 0.1ml / 100ml, the feed rate is 0.5ml / min, the flow rate of argon is adjusted to 20l / h, and the reaction time lasts for 3 hours. Collect the product at the outlet, spray the ethanol solution on the surface of the product to obtain the fibrous single-walled carbon nanotube product, such as figure 1 Shown. The resulting product is a single-walled carbon nanotube bundle, and the size of the single-walled 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 pict...

Embodiment 2

[0033] The synthesis is carried out in a horizontal corundum tube reactor. Under the protection of argon gas, the temperature is increased to 1500°C, and the heating rate is 10°C / min, and then the ethanol / ferrocene dissolved in ferrocene is introduced by an electronic peristaltic pump. Methanol mixed solution (volume ratio 9:1), the concentration is 0.1g / 100ml, the thiophene concentration is 0.5%, the feed rate is 0.5ml / min, the flow rate of argon is adjusted to 20l / h, and the reaction time lasts for 3 hours. The product is collected at the outlet, and the resultant product is a single-walled carbon nanotube bundle, and the size of a single single-walled 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 prepared and synthesized by the above method were laid flat in a corundum boat, and the corundum boat was put into the corundum tube re...

Embodiment 3

[0036] The synthesis is carried out in a horizontal corundum tube reactor. Under the protection of nitrogen, the temperature is raised to 1500℃, and the heating rate is 10℃ / min, and then the ethanol / methanol dissolved with ferrocene is introduced by the electronic peristaltic pump The mixed solution (volume ratio 7:3), the concentration is 0.1g / 100ml, the thiophene concentration is 1%, the feed rate is 0.5ml / min, the flow rate of argon is adjusted to 20l / h, and the reaction time lasts for 3 hours. Collect the product at the outlet and attach the product to the glass substrate to obtain a film-like product such as image 3 Shown. The obtained product is a single-walled carbon nanotube, and the size of a single-walled carbon nanotube is about 4 nm. Single-walled carbon nanotubes are relatively pure and have more metal iron particles adsorbed on the surface. The obtained scanning electron microscope picture of the original sample of single-walled carbon nanotubes is as follows F...

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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 hydrochloricacid; 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 specifically relates to a method for continuously synthesizing single-walled carbon nanotubes by a high-temperature chemical vapor deposition method. Background technique [0002] Single-walled carbon nanotubes (SWCNT) have a unique structure, extremely high mechanical properties, adjustable electrical properties and good stability, which have aroused widespread interest. The discovery of SWCNT has opened up a new field full of vitality for the research of nanoelectronics, nanochemistry, and nanomaterials. SWCNT was originally 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. The purity and crystallization degree of carbon nanotubes prepared by graphite arc method and laser evaporation method are higher, and the yield is lower. The chemical vapor deposition me...

Claims

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Application Information

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