Rare earth Eu-doped lead zirconium titanate (PEZT) nanocrystalline powders with a composition near the morphotropic phase boundary (Zr/Ti = 52/48) were prepared by a modified sol-gel method. DTA/TG, IR and XRD were used to determine the thermal and phase changes in the formation of PEZT crystalline powders. The maximal doping content of Eu and the effect of Eu3+ cation substitution for Pb2+ cation on the microstructure of PZT were developed with XRD. The grain size of PEZT nanopowders is about 20 nm determined by TEM. (C) 2002 Elsevier Science B.V. All rights reserved.