The features of the formation of compounds based on silver antimonate obtained in the AgNO3–Sb2O3–MoO3 system by the solid-phase reaction were investigated. For a synthesis temperature of 1023 K, a homogeneous concentration region
of the Ag2−xSb2−xMoxO6 solid solution with a structure of the defective pyrochlore type in the range of 0.0 ≤ x ≤ 2.0 was detected. The Rietveld method, within the constraints of the Fd-3m space group, was used to refinement
of X-ray diffraction data, specify the structural parameters of powders, and the correlation of structural disorder with their electrically conductive properties. Relative density and average particle size for ceramic samples sintered at 1223 K were determined using scanning electron microscopy.
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