Ultra-long carbon nanotube preparation device and preparation method

A technology for ultra-long carbon nanotubes and preparation devices, which is applied in the fields of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., which can solve the problem of smooth passage of unfavorable airflow, inability to obtain mass production capacity, and reduction of substrate utilization. and other problems to achieve the effect of improving safety, high crystallinity and increasing production

Active Publication Date: 2016-07-06
江苏联科纳米科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the extremely limited substrate of fixed beds precludes mass production capabilities
Tsinghua University used millimeter-scale ceramic balls as the growth substrate to grow carbon nanotubes (Chinese invention patent, ZL2005100120667.8), which effectively expanded the specific surface area of ​​the substrate. However, this method is difficult in a fixed bed system due to the gas flow containing carbon sources Diffusion to the lower layer of the container containing ceramic microspheres, so that basically only a layer of ceramic balls on the surface can become an effective substrate for the growth of carbon nanotubes, which greatly reduces the utilization of the substrate, so it is often forced to insert some complex porous components into the fixed bed Reactors or moving bed and fluidized bed reactors with higher cost and more complicated operation
Inserting porous components in a fixed bed reactor is not conducive to the smooth passage of gas flow, and carbon nanotubes and deposited carbon may grow attached to the porous components and block them, causing the reaction gas path to be blocked and causing danger
More importantly, this reaction system requires the introduction of more than 10% hydrogen, which further increases the risk factor

Method used

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  • Ultra-long carbon nanotube preparation device and preparation method

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Embodiment 1

[0037] like figure 1 Shown, be the used structure of main implementation method of the present invention, comprise the steps:

[0038] Put the quartz glass microspheres into the quartz boat and push them into the reaction zone of the quartz tube, use benzene as the carbon source, dissolve 1% ferrocene as the catalyst, the growth temperature is 720°C, the carrier gas is nitrogen, and the carrier gas flow rate is 20ml / min, the growth time is 0.5 hours. The injection rate of the mixture of benzene and ferrocene is 0.1ml / h. After the growth is over, stop injecting the mixed solution, start injecting water, and inject 1 volume of 0.5 ml, stop the water supply after the temperature drops to 400 degrees, open the outlet flange to scrape off the carbon nanotubes on the tube wall at one time and collect them in the tube. in the collection container placed under the tail.

Embodiment 2

[0040]Put the quartz glass microspheres into the quartz boat and push them into the reaction zone of the quartz tube, use acetone as the carbon source, and dissolve 4% ferric chloride as the catalyst, the growth temperature is 600°C, the carrier gas is argon, and the carrier gas flow rate is 800ml / min, the growth time is 2 hours. When the injection rate of the mixture of acetone and ferric chloride is 10ml / h. Stop injecting the toluene ferrocene solution after the growth is over, start water injection, the injection volume is 100ml, stop the water flow when the temperature drops to 400 degrees, open the inlet flange to take out the carbon nanotubes, the microscopic appearance of the carbon nanotubes is as follows image 3 shown.

Embodiment 3

[0042] Put the quartz glass microspheres into the quartz boat and push them into the reaction zone of the quartz tube, using n-hexane as the carbon source, dissolving 2% ferric nitrate as the catalyst, the growth temperature is 1000°C, and the carrier gas is a mixture of argon and nitrogen. The carrier gas flow rate was 1600ml / min, and the growth time was 8 hours. The injection rate of n-hexane and ferric nitrate mixture is 25ml / h. Stop injecting the mixed solution after the growth is over, start injecting water, the injection volume is 300ml, stop the water flow when the temperature drops to 400 degrees, and take out the carbon nanotubes after the temperature drops to room temperature.

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Abstract

The invention provides an ultra-long carbon nanotube preparation device and an ultra-long carbon nanotube preparation method. According to the invention, large-scale preparation of ultra-long high-conductivity carbon nanotube powder is realized based on a floating catalysis chemical vapor deposition technology and with the designs of an improved fixed bed and a special substrate. According to the invention, a liquid carbon source safe under a pure inert atmosphere is selected, and quartz glass microspheres with good chemical stability are adopted as a substrate. With intermittent water etching and an improved sampling device, the carbon nanotubes can be rapidly moved out of the reaction system and can collected. With the preparation method provided by the invention, operation process is simple, and cost is greatly saved.

Description

technical field [0001] The invention relates to the technical field of carbon nanomaterial preparation, in particular to a device for large-scale preparation of ultra-long and highly conductive carbon nanotubes by floating catalytic chemical vapor deposition technology and a preparation method thereof. technical background [0002] In recent years, with the increasing technology of mass-manufacturing carbon nanotubes, the large-scale application of carbon nanotubes has gradually developed, especially for nano-reinforced phases of composite materials. However, currently commercially available carbon nanotubes usually exist in the form of flocculation, and generally have the characteristics of short length, thin tube diameter, and many defects, resulting in low electrical conductivity. It is difficult to obtain effective dispersion and conduction when used in the preparation of composite materials. The threshold is low, and there is no significant advantage over conductive car...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02B82Y30/00
Inventor 陈名海陈宏源李清文徐坤元
Owner 江苏联科纳米科技有限公司
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