XPS Study of the reduction of cerium dioxide

Abstract X‐ray photoelectron spectroscopy of cerium oxides is discussed. The well‐resolved 3d 3/2 (5d 6s) 0 4f 0 2p 6 peak at 916.70 eV cannot be used for calculating the amount of reduction because the correlation between its intensity and the concentration of Ce(IV) and CE(III) species is not liner. We have therefore develped a complete anlaysis of the whole spectrum. The deconvolution procedure is explained in detail and the method is applied to two examples: a CeO 2 /Al 2 O 3 sample and a Pd/CeO 2 catalyst reduced under hydrogen.