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Oxidation‐State Analysis of Ceria by X‐ray Photoelectron Spectroscopy
Author(s) -
Allahgholi Aschkan,
Flege J. Ingo,
Thieß Sebastian,
Drube Wolfgang,
Falta Jens
Publication year - 2015
Publication title -
chemphyschem
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.016
H-Index - 140
eISSN - 1439-7641
pISSN - 1439-4235
DOI - 10.1002/cphc.201402729
Subject(s) - cerium , x ray photoelectron spectroscopy , oxidation state , cerium oxide , analytical chemistry (journal) , oxide , phase (matter) , superposition principle , x ray , spectroscopy , spectral line , chemistry , synchrotron radiation , materials science , metal , inorganic chemistry , physics , nuclear magnetic resonance , optics , organic chemistry , chromatography , quantum mechanics , astronomy
Three different methods to determine the oxide‐phase concentration in mixed cerium oxide by hard X‐ray photoelectron spectroscopy are applied and quantitatively compared. Synchrotron‐based characterization of the O 1s region was used as a benchmark to introduce a method based on the weighted superposition of the Ce 3d spectra of the pure Ce 3+ and Ce 4+ phases, which was shown to lead to reliable and highly accurate determination of the mean oxidation state in mixed cerium oxides. The results obtained reveal a linear relation between the third distinct final state ( u ′′′) satellite peak intensity of the Ce 4+ phase and the Ce 4+ concentration by proper inclusion of Ce 3+ ‐related plasmon satellite peaks, which contradicts previous claims of nonlinear behavior. In contrast, quantitative conventional peak‐fitting procedures were shown to be well suited for the Ce 2p region due to its relatively simple structure. Additional satellite features observed in the Ce 3d spectrum of CeO 2 were proposed to originate from plasmon contributions.