Abstract A wet procedure to prepare stoichiometric and homogeneous PZT powder (Pb(Zr 0.52Ti 0.48)O 3) is described. Starting reagents are tetra- n-butyl zirconate, titanate, and lead acetate. The synthesis is based upon the coprecipitation of metal hydroxides Pb(OH) 2, ZrO(OH) 2, TiO(OH) 2 and lead oxalate PbC 2O 4 in the pH range 9–10. Monophasic and sub-micrometer-sized PZT powder was obtained by calcination of the mixture of hydroxides and oxalate at 700°C. The study shows that highly tetragonal PZT phase appeared after heating at 500°C only. No intermediate phase such as PbTiO 3 was detected. The presence of two different lead precursors in the precipitate—Pb(OH) 2 and PbC 2O 4—involved this low-temperature PZT formation without intermediate mixed oxide. Dense and compositionally homogenous PZT ceramics were obtained by sintering the calcined powder at 1200°C. These samples exhibited good dielectric and piezoelectric properties.