In attempt to ultimately control the characteristics of the PZT films, wehave decided to investigate some of the basic chemistry associated withthese solutions. Frequently, these solutions have been generated from GroupIV metal alkoxides in acetic acid (HOAc). Therefore, studies of the simple reactivity between M(OCHMe2)4 (M = Ti, Zr) and HOAc have beenundertaken. These reactions were monitored by 1H, 13C, 17O NMR, FT-IR, TGA/DTA, and single crystal X‐ray studies.Films were produced from spin‐coat deposition of crystalline material (fromthe titanium reaction) in toluene and aged solutions as well.