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Controllable preparation method for single-walled carbon nanotube without sulfur impurities by growth promoter

A technology of single-walled carbon nanotubes and growth promoters, applied in the directions of carbon nanotubes, nanocarbons, chemical instruments and methods, etc., can solve the problems of reduced catalyst stability, difficult removal, high material requirements, etc., and is conducive to treatment. and recycling, beneficial to treatment and recycling, and the effect of broadening the scope of application

Active Publication Date: 2019-04-12
唯碳纳米科技(沈阳)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Adding a sulfur growth promoter will cause the prepared single-walled carbon nanotube sample to contain sulfur impurities, which will cause the poisoning and deactivation of the nanocatalyst loaded on the carbon nanotube (document three: Bartholomew, C.H.Applied CatalysisA:General ,2001,212(1-2),17-60), or reduce the stability of the catalyst, and release hydrogen sulfide gas under acidic conditions
Therefore, the presence of sulfur impurities limits the application of carbon nanotubes in the field of catalysis
In addition, traditional sulfur growth promoters are easy to form hydrogen sulfide gas with hydrogen in the reaction atmosphere. If hydrogen sulfide gas is discharged into the atmosphere, it will pollute the environment. If the tail gas is recycled, the cost of removing hydrogen sulfide is high and it is difficult to completely remove it.
On the other hand, the current growth temperature of high-quality single-walled carbon nanotubes by floating catalyst chemical vapor deposition is generally higher than 1100 ° C, which requires high material requirements for the reactor tube, making large-scale preparation more difficult

Method used

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  • Controllable preparation method for single-walled carbon nanotube without sulfur impurities by growth promoter
  • Controllable preparation method for single-walled carbon nanotube without sulfur impurities by growth promoter
  • Controllable preparation method for single-walled carbon nanotube without sulfur impurities by growth promoter

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Effect test

Embodiment 1

[0041] In this example, under the protection of 200 ml / min of argon gas, the temperature of the chemical vapor deposition furnace was first raised to 1100 ° C, and then 5000 ml / min of hydrogen and 5 ml / min of ethylene were introduced, containing the catalyst precursor two The toluene solution of ferrocene and growth promoter precursor selenophene is injected into the ultrasonic nozzle at a speed of 0.2 ml / hour, and the grown carbon nanotubes flow to the end of the tube with the airflow, and finally form carbon nanotubes on the porous filter membrane placed at the end. tube film.

[0042] Raman spectroscopy, scanning electron microscopy, transmission electron microscopy, and thermogravimetric analysis were performed on the single-walled carbon nanotube thin film sample (denoted as 1#) prepared above.

[0043] Such as figure 2 As shown in (a, b, c), the peaks of the Raman spectral breathing mode of SWNT films are concentrated, indicating that the diameter distribution of SWNTs...

Embodiment 2

[0045] In this example, under the protection of 200 ml / min of argon, the temperature of the chemical vapor deposition furnace was first raised to 900°C, and then 2000 ml / min of hydrogen and 15 ml / min of ethylene were introduced, containing the catalyst precursor two The toluene solution of ferrocene and growth promoter precursor selenophene is injected into the ultrasonic nozzle at a speed of 0.5 ml / hour, and the grown carbon nanotubes flow to the end of the tube with the airflow, and finally form carbon nanotubes on the porous filter membrane placed at the end. tube film.

[0046] The sharp peak shape of the breathing mode of the Raman spectrum of the single-walled carbon nanotube film indicates that the diameter distribution of the single-walled carbon nanotube is narrow, I G / I D is 170, indicating that the crystallinity of single-walled carbon nanotubes in the film is very high; scanning electron microscope observation shows that the surface of carbon nanotubes is very cl...

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Abstract

The invention relates to the field of controllable preparation of high-quality single-walled carbon nanotubes with low catalyst content and no sulfur impurities, in particular to a controllable preparation method for a single-walled carbon nanotube without sulfur impurities by a growth promoter. According to the method, selenophen is used as a precursor of the growth promoter, ferrocene is used asa catalyst precursor, and selenophen and ferrocene are dissolved in a toluene solvent; the formed solution is converted into aerosol by an ultrasonic nozzle, and then the aerosol is brought into a high-temperature zone by a carrier gas to catalyze ethylene decomposition and nucleation for growing a high-quality high-purity (IG / ID reaches 180 and the catalyst content is lower than 4.5 wt.%) single-walled carbon nanotube without sulfur impurities. The present invention uses selenium instead of sulfur as the growth promoter to achieve preparation of the high-quality single-walled carbon nanotubewith low catalyst residue and without sulfur impurities; and at the same time, hydrogen sulfide gas which is difficult to separate is avoided in tail gas of carbon nanotube growing, thus treatment and recycling of the tail gas are facilitated, and mass preparation of the high-quality single-walled carbon nanotube with a low catalyst content is achieved.

Description

technical field [0001] The invention relates to the field of controllable preparation of high-quality, high-purity single-wall carbon nanotubes without sulfur impurities, specifically a method for the controllable preparation of single-wall carbon nanotubes with low catalyst content by using a new type of growth promoter selenium. High-quality, high-purity, single-walled carbon nanotubes that do not contain sulfur impurities. At the same time, the tail gas does not contain hydrogen sulfide gas, which is conducive to tail gas treatment and recycling. Background technique [0002] Carbon nanotubes have chiral-dependent conductive properties, ballistic transport properties, excellent mechanical properties, excellent flexibility and low density, etc., so they are expected to be obtained in high-tech fields such as nanoelectronic devices, aviation, and aerospace. widely used. The preparation of carbon nanotubes is inseparable from catalysts, but the residual catalysts in carbon ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/159C01B32/162
CPCC01B32/159C01B32/162C01B2202/30
Inventor 刘畅李晓齐蒋松侯鹏翔成会明
Owner 唯碳纳米科技(沈阳)有限公司
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