A detailed analysis of TUBALL single‐walled carbon nanotubes (SWCNTs) after two‐step purification involving acid purification treatment with concentrated HCl, HNO3, H2SO4 and solution of HNO3:H2SO4 followed by magnetic processing is presented. The purity degree from iron higher than 99% is achieved, and the yield obtained by the above process is about 75 wt.%. Such high purity of the resultant sample is achieved by removing of the external iron nanoparticles by acid treatment and following extraction of nanotubes containing encapsulated nanoparticles under applied magnetic field. A comprehensive characterization of SWCNTs by Raman, optical absorption, and X‐ray photoelectron spectroscopies reveals purification‐induced changes in the integrity, composition, and electronic properties of SWCNT.
Filling of single-walled carbon nanotubes (SWCNTs) and extraction of the encapsulated species from their cavities are perspective treatments for tuning the functional properties of SWCNT-based materials. Here, we have investigated sulfur-modified SWCNTs synthesized by the ampoule method. The morphology and chemical states of carbon and sulfur were analyzed by transmission electron microscopy, Raman scattering, thermogravimetric analysis, X-ray photoelectron and near-edge X-ray absorption fine structure spectroscopies. Successful encapsulation of sulfur inside SWCNTs cavities was demonstrated. The peculiarities of interactions of SWCNTs with encapsulated and external sulfur species were analyzed in details. In particular, the donor–acceptor interaction between encapsulated sulfur and host SWCNT is experimentally demonstrated. The sulfur-filled SWCNTs were continuously irradiated in situ with polychromatic photon beam of high intensity. Comparison of X-ray spectra of the samples before and after the treatment revealed sulfur transport from the interior to the surface of SWCNTs bundles, in particular extraction of sulfur from the SWCNT cavity. These results show that the moderate heating of filled nanotubes could be used to de-encapsulate the guest species tuning the local composition, and hence, the functional properties of SWCNT-based materials.
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