An approach to synthesis lead zirconate titanate [Pb(Zr1 - xTix)O3; PZT] powders with a modified two-stage mixed oxide synthetic route has been developed. To ensure a single-phase perovskite formation, an intermediate phase of zirconium titanate (ZrTiO 4) was employed as starting precursor. The formation of perovskite phase in the calcined PZT powder has been investigated as a function of calcination temperature, soaking time and heating/cooling rates by differential thermal analysis (DTA) and X-ray diffraction (XRD) techniques. The morphology evolution was determined by scanning electron microscopy (SEM) technique. It has been found that the unreacted PbO and ZrTiO4 phases tend to form together with PZT, with the latter appearing in both tetragonal and rhombohedral phases, depending on calcination conditions. It is seen that optimisation of calcination conditions can lead to a 100% yield of PZT in a tetragonal phase. © 2003 Elsevier B.V. All rights reserved.