Abstract

We propose a new method of quantifying the phases present in a binary mixture of nanopowder from deconvoluted valence band spectra using X-ray photoelectron spectroscopy (XPS). Polymorphs of iron oxide (γ-Fe2O3 and α-Fe2O3) and titania (anatase and rutile TiO2) nanopowders containing different weight percentages of the polymorphs were chosen for the present study. Pure iron oxide nanopowder (Fe3O4) was prepared by co-precipitation and was air annealed at 250 and 700 °C to obtain γ-Fe2O3 and α-Fe2O3 phases, respectively. In addition, anatase and rutile TiO2 were also used in the present study. A linear correlation between the percentage of the phase and the valance band peak area was observed in both the cases. The phase compositions of the nanopowder mixtures identified from the valence band spectra were compared with that of the X-ray Diffraction (XRD) data and the results were found to be in good agreement with each other. For nanoparticles of size >30 nm, no size dependent effect was observed in determining the phase composition but for particle size below 10 nm, size was found to have a detrimental role. These results showed that the phases of polymorphs can be quantified from XPS valence band analysis.

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