Zinc stannate (ZnSnO 3 ) and zinc stannate-coated nm-CaCO 3 (ZS-CaCO 3 ) were synthesised from precursors which for the latter were formed by a homogeneous precipitation method with ultrasonic and azeotropic technology. The calcined products of ZnSnO 3 and ZS–-CaCO 3 were characterised by XRD and TG/DTA. The results indicated the optimal temperature for calcining was at 500°C. The surface of nm-CaCO 3 was characterised by XPS and TEM, and the results showed that ZnSnO 3 had effectively coated the surface of nm-CaCO 3 . The grain size of ZS-CaCO 3 was about 50–70 nm.