Nanocrystalline lead zirconate titanate (PZT) powders, with a Zr:Ti ratio of 60:40, have been prepared from a solution of triethanolamine (TEA) and Ti4+, Zr4+, and Pb2+ ions. The metal ions were in solution through complex formation with TEA. The soluble metal-ion–TEA complex formed the precursor material when it was completely dehydrated. Heat treatment of the precursor at 450°C resulted in single-phase PZT powders. The precursor and the heat-treated powders have been characterized by using thermal analysis and X-ray diffractometry (XRD) studies. The average particle size, as measured from X-ray line broadening and transmission electron microscopy studies, was ∼20 nm. PZT powders modified with 3 mol% of lanthanum (PLZT) also were prepared through this route and were investigated via XRD studies. The dielectric constants of the PZT and PLZT powders were 12475 and 11262, and their corresponding Curie temperatures were 362° and 315°C, respectively.