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A series of nanostructured fluorite-type Ce1-xYxO2-delta(0 LT = x LT = 0.35) solid solutions, prepared via high-energy milling of the CeO2/Y2O3 mixtures, are investigated by XRD, HR-TEM, EDS and Raman spectroscopy. For the first time, complementary information on both the long-range and short-range structural features of mechanosynthesized Ce1-xYxO2-delta, obtained by Rietveld analysis of XRD data and Raman spectroscopy, is provided. The lattice parameters of the as-prepared solid solutions decrease with increasing yttrium content. Rietveld refinements of the XRD data reveal increase in microstrains in the host ceria lattice as a consequence of yttrium incorporation. Raman spectra are directly affected by the presence of oxygen vacancies; their existence is evidenced by the presence of vibration modes at similar to 560 and similar to 600 cm(-1). The detailed spectroscopic investigations enable us to separate extrinsic and intrinsic origin of oxygen vacancies. It is demonstrated that mechanosynthesis can be successfully employed in the one-step preparation of nanocrystalline Ce1-xYxO2-delta solid solutions. (C) 2015 Elsevier Inc. All rights reserved.