PbTiO3 powders have been prepared by mild annealing (2 h at 600 degrees C) of PbCO3:TiO2 mixtures previously subjected to mechanical activation, while a thermal treatment of about 12 h at T > 850 degrees C is needed to obtain PbTiO3 from a physical mixture. Although the temperature and enthalpy of the DSC peak corresponding to PbCO3 decomposition are not affected by mechanical energy, in the case of the mechanically activated mixtures an exothermic event due to the reaction PbO + TiO2 -> PbTiO3 shows up. Furthermore, SEM micrographs and the XRD line broadening allow to conclude that PbTiO3 Powders obtained from activated mixtures are of nanometer size. PbTi3O7 has been prepared starting from mechanically activated PbCO3:3TiO(2) mixtures by 1 h annealing at 850 degrees C while 100 h at 800 degrees C were required to yield this compound from unmilled mixtures. (c) 2006 Springer Science + Business Media, Inc.