Lead zirconate (PbZrO3) powder has been synthesized by a solid-state reaction via a rapid vibro-milling technique. The effects of calcination temperature, dwell time and heating/cooling rates on phase formation, morphology, particle size and chemical composition of the powders have been investigated by TG-DTA, XRD, SEM and EDX techniques. The results indicated that at calcination temperature lower than 800 degrees C minor phases of unreacted PbO and ZrO2 were found to form together with the perovskite PbZrO3 phase. However, single-phase PbZrO3 powders were successfully obtained at calcination conditions of 800 degrees C for 3 h or 850 degrees C for 1 h, with heating/ cooling rates of 20 degrees C/min. Higher temperatures and longer dwell times clearly favored the particle growth and formation of large and hard agglomerates.