The process of phase formation of new antimony pyrochlore (sp. gr. Fd-3m) Bi2.7Zn0.46Ni0.70Sb2O10 + ? during solid-phase synthesis from oxide precursors was studied. The process of solid-phase synthesis of antimony pyrochlore Bi2.7Zn0.46Ni0.70Sb2O10 + ? is a complex multi-stage process. It was shown that the interaction of oxide precursors occurs at a temperature of 600 ?С and higher, bismuth stibatate – Bi3SbO7 is formed as an impurity phase. Oxide precursors, including bismuth (III) and antimony (III, V) oxides, are fixed in the sample up to 750 ?С, at which the intermediate cubic phase Bi3M2/3Sb7/3O11 (sp. gr. Pn-3) is formed, stable up to 900 ?С. The pyrochlore phase in the sample appears at 650 ?С, a significant increase in the proportion of pyrochlore occurs at a temperature of 850 ?С and above. Phase-pure pyrochlore is formed at 950…1050 ?С. At a temperature of 1050 ?С, sintering of fine-grained ceramics occurs, a low-porosity microstructure is formed due to the fusion of small grains with the formation of coarse crystallites with a longitudinal size of 2…4 ?m. The unit cell parameter of pyrochlore in the range of 650…1050 ?С changes non-monotonically, at 800 ?С the minimum value of 10.464 ? is fixed, the unit cell constant of phase-pure pyrochlore Bi2.7Zn0.46Ni0.70Sb2O10 + ? is equal to 10.474 ?.