Abstract: Detailed investigations of Raman spectra and X-ray powder diffraction (XRPD) patterns of rutile-rich and anatase/brookite-poor flower-like nanocrystalline aggregates of Fe-doped TiO2 shed new light with regard to its microstructure and heterogeneity. The brookite phase has been detected from the Raman spectra, and the presence of different phases in pure and doped samples is discussed...