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Method for large-batch preparing overlength carbon nano pipe array and its apparatus

A technology of ultra-long carbon nanotubes and carbon nanotube arrays, which is applied in the fields of nanotechnology, nanotechnology, nanostructure manufacturing, etc., can solve the problems of limited collection substrates and inability to match reactors, and achieves easy operation, simple device, Requires a loose effect

Active Publication Date: 2006-01-25
TSINGHUA UNIV
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  • Abstract
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Problems solved by technology

In 2003, Windle et al. (Chem Phys Lett 2003: 372(5-6): 860-5) of the University of Cambridge reduced the thickness of silicon dioxide and obtained more carbon nanotubes per unit volume. Arrays, but the collection substrates they use are still limited to atomically flat sheet-like silica, so that this method still cannot match the existing various reactors, and is generally compatible with the real mass production of carbon nanotube arrays. still some distance
[0006] Recently, Ijima et al. (Science 2004; 306: 1362-4) proposed a method for preparing arrays of single-walled carbon nanotubes with a length of several millimeters, but the substrate used in this method and its treatment method are different from the aforementioned preparation of multi-walled carbon nanotubes. Arrays are similar, and there is still a considerable distance between large-scale engineering methods

Method used

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  • Method for large-batch preparing overlength carbon nano pipe array and its apparatus
  • Method for large-batch preparing overlength carbon nano pipe array and its apparatus
  • Method for large-batch preparing overlength carbon nano pipe array and its apparatus

Examples

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example 1

[0027] Fill the fixed-bed reactor with alumina spherical ceramic particles with a diameter of about 1 mm, and feed argon and hydrogen into the reactor from top to bottom (the airflow can also flow from top to bottom or from left to right), with a flow ratio of 5:1. Reaction temperature 850°C, 0.1 hour -1 Spray 5 mg / ml ferrocenebenzene solution into the reactor from the top of the reactor at a space velocity of 30 minutes, stop heating and cool to room temperature to take out the ceramic particles. The product on the particle surface is confirmed by scanning and transmission electron microscopy to be an array of multi-walled carbon nanotubes with a length of about 500 microns. figure 1 is the actual picture of the product, figure 2 , 3 The scanning and transmission electron microscope images respectively. Thermogravimetric analysis showed that the product did not contain any amorphous carbon, with a multi-walled tube content greater than 95%.

example 2

[0029] Zirconium dioxide spherical ceramic particles with an average particle size of about 50 microns are added to the reactor from the top of the moving bed, nitrogen and hydrogen are introduced from the bottom of the reactor, the flow rate is 20:1, the reaction temperature is 700 ° C, and the reaction time is 1 hour. -1 Add 100 mg / ml dicarbonylironcyclohexane solution from the bottom of the reactor at a space velocity of 100 mg / ml. After 30 minutes of reaction, open the valve, and the particles move into the separation section. This section strips the product array from the surface of the particles and collects them. The particles pass through the regeneration section at 600 ° C. After calcination, it is transported to the top of the reactor by the riser for recycling. The product is confirmed to be an array of multi-walled carbon nanotubes with a length of about 200 micrometers arranged by scanning and transmission electron microscopy.

example 3

[0031] Glass beads with an average particle size of about 100 microns are filled in a fluidized bed reactor, nitrogen and hydrogen protection gas are fed into the reactor from bottom to top at a flow ratio of 10:1, and the gas flow rate is adjusted to make the particles close to fluidization. Temperature 550°C, take 0.05 hours -1 Inject 20 mg / ml of ferrocene ethanol solution at a space velocity of 20 mg / ml, stop the supply of raw materials after 2 hours of reaction, increase the flow rate of the protective gas to completely fluidize the glass beads, and collect the product with a cyclone at the top of the reactor. After the product is completely released, switch The air valve is fed into the air to calcinate the remaining carbon deposits for 10 minutes and then return to the reaction conditions for the second cycle. The product is confirmed by scanning and transmission electron microscopy to be a neatly arranged array of multi-walled carbon nanotubes with a length of about 100...

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Abstract

A process and equipment for preparing ultra-long carbon nano-tube array in batch is disclosed. Said process includes such steps as providing monolithic reactor with artery structure, adding ZrO2, SiO2 or Al2O3 particles or their mixture, inserting structural member in fixed bed and chemical vapor deposition. Its advantages are high purity and output.

Description

Technical field: [0001] A method and device for mass-preparing ultra-long carbon nanotube arrays belong to the technical field of nanomaterial preparation. Background technique: [0002] Carbon nanotubes can be regarded as one-dimensional tubular nanostructures formed by curling graphite layers. They were discovered by Japanese electron microscope scientist Iijima in 1991. According to the number of curled graphite layers, carbon nanotubes are divided into multi-walled and single-walled carbon nanotubes. The excellent mechanical and electromagnetic properties of carbon nanotubes make them have immeasurable application prospects in many fields, especially in functional composite materials such as electrical conductivity, wave absorption, and reinforcement. Significant progress has been made at home and abroad. However, the premise of commercialization of these applications is the ability to prepare carbon nanotubes in large quantities and at low cost. [0003] At present, c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C23C16/26B82B3/00
Inventor 魏飞罗国华项荣
Owner TSINGHUA UNIV
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