Spectroscopic and structural studies of isochronally annealed cobalt oxide nanoparticles Original Research Article

X-ray absorption near edge structure (XANES) spectroscopy, X-ray photoelectron spectroscopy (XPS), and Synchrotron X-ray diffraction (SXRD) techniques are used to study as synthesized and isochronally annealed samples of cobalt oxide nanoparticles (NPs) grown using the wet chemical route. Quantitative phase composition determined using Linear Combination Fitting (LCF) on XANES data is found to be in reasonably good agreement with that obtained from Rietveld refinement on SXRD data. XPS data qualitatively indicate that Co3O4 concentration increases with increase in the annealing temperature, in confirmation with SXRD and XANES data. Larger shifts in the satellite peaks from the main peaks compared to these in bulk suggest larger crystal field splitting in nanoparticles as compared to the bulk.