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Ni-loaded nanocrystalline ceria-zirconia solid solutions prepared via modified Pechini route as stable to coking catalysts of CH 4 dry reforming DOI 10.1515/chem-2016-0039 received November 5, 2016 accepted November 27, 2016. Abstract: Mixed nanocrystalline Ce-Zr-O oxides (Ce/Zr = 1 or 7/3) were prepared by modified Pechini route using ethylene glycol solutions of metal salts. Detailed characterization of their real structure and surface properties by X-ray diffraction on synchrotron radiation with the full-profile Rietveld analysis, high resolution electron microscopy with elemental analysis, Raman spectroscopy, UV-Vis and X-ray photoelectron spectroscopy revealed a high homogeneity of cations distribution in nanodomains resulting in stabilization of disordered cubic phase. This provides a high dispersion of NiO loaded on these mixed oxides by wet impregnation, a high reactivity and mobility of oxygen in these catalysts and strong interaction of Ni with support in the reduced state. This helps to achieve a high activity and coking stability of developed catalysts in CH 4 dry reforming in feeds with CH 4 concentration up to 15% and CH 4 /CO 2 ratio =1.