Abstract. 1 The effect of ultrasonic treatment (UST) on the physical-chemical properties of zinc-molybdenum system ZnO-MoO 3 (Zn: Mo = 15:85, 25:75, 50:50, 75:25) was studied. Using XRD, FT-IR and DTA methods it was shown that such treatment forms molybdenum suboxides (Magneli phases of Мо 4 О 11 and Мо 8 О 23 composition) and zinc molybdates (α-ZnMoO 4 , ZnMo 8 O 10 ). Specific character of reagents ratio on the formation of these compounds was determined. It was shown that UST changes porous structure of the compositions -non-porous mixture of oxides transforms into composites with micro-and mesopores, resulting in the increase of specific surface and significant reduction of particles size.