Lead lanthanum Zirconate Titanate (PLZT 7/65/35) powders were prepared by a sol-gel process, using lead acetate, lanthanum acetate, zirconium n-propoxide and titanium n-propoxide as precursors along with 2-methoxyethanol as the solvent. Nitric acid was used to catalyze the sol-gel reaction. FTIR spectroscopy characterized the starting precursors, monitored the sol to gel transformations involving solutions with different molar ratios of water to alkoxide precursors, and tracked the crystallization behavior of the gels upon heat treatment. Raman spectroscopy was employed at room temperature to follow vibrational spectral changes for the samples that were cooled after various stages of heat treatment and crystallization of the gels. The resulting spectral changes were analyzed in terms of the structural changes that occurred during the sol-gel process.