Spherical Pb(Zr,Ti)O3 powders were prepared from the aqueous acetate-base solution by ultrasonic spray pyrolysis. The raw materials were Pb(C2H302)'3H20, ZrO(C2H302)2 and a mixture of Ti(C3HTO)4 and C5H702. A single-phase PZT was formed at 900~ in air and at 700 ~ in 02 atmosphere. The PbTiO3 phase, as an intermediate product, was observed in the formation of PZT and no PbZrO3 phase was detected under our experimental conditions. The intensity of the PbTiO3 peak decreased with increasing reaction temperature in air, while the reverse effect of reaction temperat~ure was observed in 02. Spherical and irregular-shaped particles coexisted in the powder containing the minor PbTiO3 phase, while the particles of a single-phase PZT have spherical morphology with little evidence of irregular-shaped particle formation.