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Raman spectroscopy is a common method of studying carbon-based materials such as multi-walled carbon nanotubes (MWCNT). However, the analysis of this technique is non-trivial since recorded spectra may be a convolution of both molecular vibrations and phonon resonances. The energies of these physical processes may occur in the same energy regime, and hence several analytical approaches can be necessary for a full analysis. Due to the negligible quantities of non-graphitic carbon in MWCNT, the present fitting procedure focuses on understanding phonon resonances to elucidate how varying modifications of MWCNT ultimately influence their graphitic bulk structure. We have found this approach to provide greater insight into the structure of MWCNT when low quantities of amorphous carbon are present, when compared with methods which try to interpret both phonon scattering and molecular vibrations simultaneously. Different pre-treatments for the modification of the graphitic structure of MWCNT are compared, including aqueous acidic and gas phase methods, and statistically evaluated. Focusing on phonon resonances enables one to analyze the reaction process of nitrosulfuric acid pre-treatment at different temperatures. Thereby, it is possible to control the ratio between defects and graphitic structures in MWCNT samples and prepare samples with reproducible D/G ratios.

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The focus of the present work is to investigate the bonding characteristics of vanadium oxide species to different oxygen functional groups on multiwalled carbon nanotubes (MWCNT). Atomic layer deposition (ALD) was used to deposit atomically dispersed vanadium oxide species on MWCNT. To generate atomically dispersed vanadium, only one ALD cycle was applied for the deposition of vanadium. The MWCNT functional groups that are involved in the deposition process were identified by thermal analysis and grafting experiments. A variety of ALD process parameters were tested, and revealed that purging times between dosing of vanadium precursor and dosing of water as coreactant had a strong influence on the ratio of vanadium species that are physisorbed or chemisorbed to the MWCNT. The ALD process parameters were optimized to focus on the immobilization of the vanadium due to a chemical bond between vanadium species and MWCNT. Because of the direct correlation between catalytic stability and immobility of the vanadium species, the importance of knowledge about the influence of the ALD parameter onto the bond formation is essential. Raman spectroscopy and high resolution scanning transmission electron microscopy images were used to prove the single site structure of the vanadium oxide

A series of vanadia catalysts supported on mesoporous silica SBA-15 has been prepared with a loading in the range of 2-14 wt-% V and characterized under oxygen and propane oxidative dehydrogenation reaction conditions at elevated temperature up to 550 °C. In situ soft X-ray absorption spectra at the vanadium L-and oxygen K-edges and in situ synchrotron based X-ray photoemission spectra reveal a restructuring of vanadium species that results in an enhanced degree of dispersion of molecular vanadia species on the silica support. The impact of the X-ray beam on the XAS spectra of dispersed V x O y species has been studied and a brief perspective of X-ray based electron spectroscopy as a probe in catalyst characterization is given.