Chemically homogeneous SrBi2Ta2O9 (SBT) sol was synthesized using ethoxy tantalum, strontium acetate, and bismuth subnitrate as starting materials, methoxyethylene as a solvent and acetic acid (HOAc) as a catalyst. Single-phased perovskite phase SBT ferroelectric ultrafine powder was obtained after the dried gel was treated at 350degreesC for 30 min and calcined at 800degreesC for 1 h. FT-IR, XRD, TEM and TG-DTA were employed to investigate the transformation processes of sol to gel and gel to ultrafine SBT powder. Acetic acid not only acts as an acid catalyst, but also changes the alkoxide precursor as a ligand at a molecular level. Bidentate acetates replace OR groups and are directly bounded to the tantalum, leading to the formation of Ta (OR)(x)(OAc)(5-x). The perovskite SBT phase formed via intermediate phase Bi3TaO7 and a Bi-deficient pyrocholore phase. (C) 2002 Elsevier Science Ltd. All rights reserved.