This work presents results of studies of the real structure of nanocrystalline CeO₂-ZrO₂ (Ce:Zr=1:1) systems prepared via Pechini route and doped with La³⁺ or Gd³⁺ cations (x up to 30 at.%). X-ray diffraction, EXAFS, UV-Vis and Raman spectroscopy were applied for the bulk characterization, while the surface features were studied by XPS and SIMS. For both systems, the increase of Ln³⁺ content was accompanied by the decline of domain size and increase of the specific surface area and lattice parameter of fluorite-like phases. While for bigger La³⁺ the system becomes bi-phasic at xLa > 10 at.%, for smaller Gd³⁺ cation single-phase solid solution exists within all studied range. For both systems, depletion of the surface layer by smaller Zr⁴⁺ cations was revealed, while the surface content of a doping cation is either close to that in the bulk (La) or lower (Gd). Such a spatial distribution of components results in some ordering of cations within the particle. It is reflected in different modes of rearrangement of oxygen coordination polyhedra with the Gd or La content (by EXAFS), and redistribution of the intensity of reflections in XRD patterns not conforming to a simple model with statistical distribution of oxygen vacancies. Associated variation of average Ce(Zr)-O bond strength (SIMS) appears to affect the lattice oxygen mobility. This work is in part supported by INTAS 05-1000005-7663, RFBR-CNRS 05-03-34761 Projects and Integration Project 4.15 SB RAS.

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