Fine, spherical Zr0.8Sn0.2TiO4 powders were prepared by spray pyrolysis, using an ultrasonic transducer, from an aqueous solution of metal chlorides. The synthesized powders had a spherical morphology and many shell fragments. The observed shell fragments were attributed to the impermeable surface crust formed during thermal decomposition of the droplets. The raw materials for the preparation of Zr0.8Sn0.2TiO, were analysed prior to any treatments because the properties of the surface crust could be related to those of the raw materials. ZrOCl2 . 8H(2)O was supposed to affect the shell fragments as well. Spherical Zr0.8Sn0.2TiO4 powders without shell fragments could be prepared using ZrO(CH3COO)(2) in place of ZrOCl2 . 8H(2)O.