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New [Y2-xMx][Sn2-xMx]O7-3x/2 (0 ?x? 0.30 for M = Mg and 0 ?x? 0.36 for M = Zn) solid solutions with the pyrochlore structure were synthesized via high-temperature solid-state reaction method. Powder X-ray diffraction (PXRD) patterns and Fourier transform infrared (FT-IR) spectra showed that these materials are new non-stoichiometric solid solutions with the pyrochlore type structure. The structural parameters for the solids obtained were successfully determined by Rietveld refinement based on the analysis of the PXRD diagrams. Lattice parameter (a) of these solid solutions decreases when x increases in both series. All samples obtained have the pyrochlore structure Fd-3m, no. 227 (origin at center -3m) with M2+ (M = Mg2+ or Zn2+) cations in Y3+ and Sn4+ sites, thus creating vacancies in the anionic sublattice.

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