Lead zirconate titanate (PbZr 1−x Ti x O 3 ) was synthesized by the “oxidant peroxo method (OPM)” with “x” between 0.25 and 0.50. Titanium metal was dissolved into a hydrogen peroxide/ammonia aqueous solution, followed by the addition of lead and zirconium nitrate solution. The amorphous precipitated precursor obtained was crystallized by heat treatment between 400 and 1000°C. Images of transmission microscopy showed spherical particles with average diameter between 20 and 60nm, and the presence of necks between particles treated at 700°C. All of the unpressed powders were characterized by X-ray diffractometry and FT-Raman spectroscopy. Powder samples with “x” up to 0.35 showed rhombohedral structure when treated at temperatures higher than 500°C, and tetragonal structure when “x” was higher than 0.40. Analysis of XRD and Raman spectroscopy of the precursor powders showed amorphous-like structures, however powders treated at 400°C showed a structure identified as an intermediate pyrochlore phase, independently of the Zr and Ti mole ratio.