High purity single walled carbon nanotubes (SWCNTs) were prepared from arc discharge produced cloth-like soot by a new purification strategy, in which liquid oxidation and steam oxidation were combined with a freeze-drying process to remove the metallic and carbonaceous impurities. The process gives a product of >98 purity, which is acquired from a gram-scale dirty raw soot with an overall yield of ~75 of the SWCNTs. The purity of the samples was characterized by thermogravimetric analysis, scanning and transmission electron microscopy, Raman and Vis-NIR spectroscopy, and magnetometry. A highly pure SWCNT sample with relative purity of 170.4 and I_q/I_D value of 78.92 is achieved. Experiments showed that HNO3/HCl refluxing combined with freeze-drying is the key process that renders the crude SWCNTs hydrophilic with a large surface area, and thus remarkably increases the efficiency of the steam treatment to remove most of the carbonaceous impurities.
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Beijing National Laboratory for Molecular Sciences, Department of Chemical Biology, College ofChemistry and Molecular Engineering Peking University, Beijing 100871, China;