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The present research describes a modified sol–gel technique used to obtain nano-crystalline lead zirconate titanate (PZT) powders by using triethanolamine (TEA) as a polymerizing agent. The metal ions chemically interacted with TEA in the precursor sol and gel under refluxing conditions. Drying and aging treatments led to development of a precursor–polymeric gel network. A single-phase perovskite structure was formed at 470°C. The PZT gel and powders were characterized by using X-ray diffraction, simultaneous thermal analysis, and Fourier transform infrared spectroscopic techniques. The nano-crystalline morphology was examined by using a transmission electron microscope (TEM). The average particle size determined from TEM was less than 15 nm.