High yiel vapor phase deposition method for large scale sing walled carbon nanotube preparation

a carbon nanotube and vapor phase deposition technology, applied in the field of high yiel vapor phase deposition method for large-scale sing-walled carbon nanotube preparation, can solve the problem of not being able to increase the production volume of nanotube materials from laboratory to industrial scale, and unable to produce a sufficient amount of materials, etc. problems, to achieve the effect of high yield

Inactive Publication Date: 2003-01-16
DUKE UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

0015] Accordingly, the present invention provides vapor phase method that employs a metal catalyst supported on an aerogel, for instance on Al.sub.2O.sub.3 aerogel and/or on Al.sub.2O.sub.3/SiO.sub.2 aerogel. The catalyst/support employed in the present invention was made by solvent-gel synthesis with subsequent removal of the liquid solvent by drying selected from the group consisting of supercritical drying, freeze drying and combinations thereof, with supercritical drying being preferred. The inventive method involves vapor phase depositin...

Problems solved by technology

Although carbon nanotube materials possess many unique and technically important properties, lack of a way to produce a sufficient amount of materials has limited not only the study of the fundamental properties but also the development of more practical applications.
However, both techniques suffer from the problem that it is hard to increase the production volume of the nanotube materials from laboratory scale to industrial scale.
Hence, although the report for ethylene and t...

Method used

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  • High yiel vapor phase deposition method for large scale sing walled carbon nanotube preparation
  • High yiel vapor phase deposition method for large scale sing walled carbon nanotube preparation

Examples

Experimental program
Comparison scheme
Effect test

example ii

[0061] The procedure of Example I was substantially repeated, except this time with a methane flow for about 60 minutes (instead of about 30 minutes) and a temperature of about 900.degree. C. (instead of various temperatures of about 800.degree. C. about 850.degree. C., about 900.degree. C., and about 950.degree. C.) and a flow rate of about 1158 sccm (instead of about 1000 sccm), during SWCNT growth. The yield measured by TGA was about 200%.

example iii

Comparison

[0062] Also, a catalyst / support made from the same Al.sub.2O.sub.3 wet gel, but dried differently to make xerogel, was compared. The aerogel supported catalyst showed a yield of about 200% of high purity SWCNT under a methane flow at about 900.degree. C. for about 60 minutes, as reported by Example I. On the other hand, the xerogel supported catalyst showed a weight gain of <5% under the same conditions.

example iv

[0063] The procedure was repeated as per the Fe / Mo catalyst supported on Al.sub.2O.sub.3 aerogel, but this time with the Fe / Mo catalyst instead supported on SiO.sub.2 aerogel prepared by a similar method.

[0064] The weight gain of the catalyst on SiO.sub.2 aerogel under the same conditions, about 900.degree. C. under a methane flow for about 60 minutes, was almost 10%. Thus, it appears that although a SiO2 aerogel support works (i.e., about 10%), it is preferred with the inventive method to employ an Al.sub.2O.sub.3 aerogel support or an Al.sub.2O.sub.3 / SiO.sub.2 aerogel support to obtain improvements that are far superior (i.e., weight gain of about 100% or greater).

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Abstract

An improved vapor phase deposition method for preparation of single walled carbon nanotubes on an aerogel supported metal catalyst. The total yield of SWCNTs often is at least about 100%, based the weight of the catalyst, for a reaction time of at least about 30 minutes.

Description

[0002] The present invention relates, in general, to a vapor phase deposition method for the preparation of single walled carbon nanotubes, where the method employs a metal catalyst on a support. More particularly, the present invention relates to an improved method where the support comprises an aerogel, such as an Al.sub.2O.sub.3 aerogel or an Al.sub.2O.sub.3 / SiO.sub.2 aerogel, as compared to prior art methods that employed supports that are powders. The improved method results in far higher yields of single walled carbon nanotubes than the prior art methods.1 Abbreviations ASB aluminum tri-sec-butoxide AFM atomic force microscope (acac).sub.2 bis(acetylacetonato) cm centimeter C centrigrade CVD chemical vapor deposition EtOH ethanol g gram kg kilogram kV kilovolt m meter ml milliliter MW molecular weight MWCNT multi-walled carbon nanotube nm nanometer psi pounds per square inch SEM scanning electron microscope SWCNT single walled carbon nanotube sccm standard cubic centimeter per...

Claims

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Application Information

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IPC IPC(8): D01F9/127
CPCB82Y30/00D01F9/127
Inventor LIU, JIE
Owner DUKE UNIV
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