Lead zirconate titanate (PZT) ceramic powder has been synthesized from metal nitrate solutions using the EDTA-gel method with different nitric acid/EDTA ratios. It was found that the thermal decomposition of the precursor was strongly affected by the nitric acid/EDTA ratio, the amount of sample, the atmosphere, and the heating rate. Crystallization of the perovskite PZT phase initiated at external temperatures as low as 250°C, as a result of the exothermic decomposition reaction of the nitrate-EDTA complexes. Possible reaction schemes are suggested and discussed to describe the thermal decomposition of PZT-EDTA precursors under different experimental conditions.