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In situ Raman spectroscopy was used at temperatures in the 50–480 °C range under oxidizing (20% O2/He) and reducing (5% H2/He) flowing gas atmospheres to compare the spectra obtained for a series of industrial rare earth doped CexZr1−xO2−δ oxygen storage capacity (OSC) mixed metal oxide materials of identical at % composition, which were prepared by the same chemical synthesis route, in which one synthesis parameter of the aqueous chemistry was slightly varied. The Raman fingerprint of the anionic sublattice is very sensitive to O atom relocations within the bulk of the material matrix and to the pertinent defect topology in each case. A protocol of sequential Raman measurements and analysis was proposed to discern subtle differences between the oxygen vacancy and defect topologies of the examined materials. It can be concluded that for two materials under comparison for their structures, identical Raman spectra are obtained only if the procedures followed for their preparation are identical; a slight variation of one single parameter (e.g., in the aqueous chemistry stage) results in discernible differences in the Raman spectra. The proposed procedure can serve as a tool for proving or disproving infringement of IPR (Intellectual Property Rights) protected preparation methods of ceria-based mixed metal oxide materials.

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