Bromination of double-walled carbon nanotubes

Double-walled carbon nanotubes (DWCNTs) synthesized by catalytic chemical vapor deposition (CCVD) have been functionalized by bromine vapor at room temperature. At least two different bromine species were detected in the product using X-ray photoelectron spectroscopy (XPS) and thermal gravimetric analysis. The primary form is negatively charged Br2 molecules exhibiting an intense resonance at ∼238 cm−1 in the Raman spectrum. The electron transfer from the nanotubes to the adsorbed molecules is detected from C 1s XPS and near-edge X-ray absorption fine structure spectra. The optical absorption spectra reveal that although the metallic nanotubes are more reactive to Br2, the outer semiconducting nanotubes also readily interact with Br2 adsorbates. The secondary bromine form is attributed to covalent C-Br bonding, and its possible sources are discussed in the light of quantum-chemical calculations. Analysis of the XPS, Raman, and optical absorption spectra of the Br-DWCNTs annealed at 100-170 ° C indicates preservation of a part of bromine molecules in samples that affects the electronic and vibration properties of nanotubes

Thermal Decomposition of Co-Doped Calcium Tartrate and Use of the Products for Catalytic Chemical Vapor Deposition Synthesis of Carbon Nanotubes.

Thermal decomposition of Co-doped calcium tartrate in an inert atmosphere or air was studied using thermogravimetric analysis and X-ray absorption fine structure (XAFS) spectroscopy. It was shown that the powder substance containing 4 at.% of cobalt completely decomposes within 650-730 °C, depending on the environment, and the formation of Co clusters does not proceed before 470 °C. The products of decomposition were characterized by transmission electron microscopy, XAFS, and X-ray photoelectron spectroscopy. Surfaceoxidized Co metal nanoparticles as large as ∼5.6 ( 1.2 nm were found to form in an inert atmosphere, while the annealing in air led to a wide distribution of diameters of the nanoparticles, with the largest nanoparticles (30-50 nm) mainly present as a Co3O4 phase. It was found that the former nanoparticles catalyze the growth of CNTs from alcohol while a reducing atmosphere is required for activation of the latter nanoparticles. We propose the scheme of formation of CaO-supported catalyst from Co-doped tartrate, depending on the thermal decomposition conditions