Six representative isotope-labeled samples of titanium dioxide were synthesized: Ti(16)O(2), Ti(17)O(2) and Ti(18)O(2), each in anatase and rutile forms. Their Raman scattering was analyzed at temperatures down to 5 K. Spectral assignment was supported by numerical simulation using DFT calculations. The combination of experimental and theoretical Raman frequencies with the corresponding isotopic shifts allowed us to address various still-open questions about the second-order Raman scattering in rutile, and the analysis of overlapping features in the anatase spectrum.
Double wall carbon nanotubes were prepared by vacuum annealing of single wall carbon nanotubes filled with C60. Strong evidence is provided for a highly defect free and unperturbed environment in the interior of the tubes. This is concluded from unusual narrow Raman lines for the radial breathing mode of the inner tubes. Lorentzian linewidths scale down to 0.35 cm(-1) which is almost 10 times smaller than linewidths reported so far for this mode. A splitting is observed for the majority of the Raman lines. It is considered to originate from tube-tube interaction between one inner tube and several different outer tubes. The highest RBM frequency detected is 484 cm(-1) corresponding to a tube diameter of only 0.50 nm. Labeling of the Raman lines with the folding vector is provided for all inner tubes. This labeling is supported by density functional calculations.
The synthesis of a unique isotope engineered system, double-wall carbon nanotubes with natural carbon outer and highly 13C enriched inner walls, is reported from isotope enriched fullerenes encapsulated in single-wall carbon nanotubes (SWCNTs). The material allows the observation of the D line of the highly defect-free inner tubes that can be related to a curvature induced enhancement of the electron-phonon coupling. Ab initio calculations explain the inhomogeneous broadening of inner tube Raman modes due to the distribution of different isotopes. Nuclear magnetic resonance shows a significant contrast of the isotope enriched inner SWCNTs compared to other carbon phases and provides a macroscopic measure of the inner tube mass content. The high curvature of the small diameter inner tubes manifests in an increased distribution of the chemical shift tensor components.
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