Characterization of Titanium and Zirconium Valerate Sol-Gel Films

Abstract

FTIR and XPS have been used to characterize titanium and zirconium valerate thin films prepared using sol-gel techniques. Films were prepared by hydrolysis of titanium(IV) isopropoxide or zirconium(IV) n-propoxide in excess valeric acid at room temperature. Film solution chemistry, from precursors to cast films, was followed with FTIR. The structure and chemical composition of films spin cast from fresh and day-old solutions were determined. Results of these studies suggest that all films consist of a metal-oxygen polymer backbone coordinated with bidentate valerate ligands. No evidence for the presence of alkoxide ligands has been found. A small amount of water is present in all cast films. While solution aging experiments indicate that the zirconium film structure does not change with solution reaction time, carboxylate ligand concentrations are higher in titanium films made from aged solutions. Titanium films made from aged solutions contain slightly less than 1.5 valerate ligands/titanium atom. Zirconium films are more highly carboxylated with almost two valerate groups per metal center. 57 refs., 6 figs., 1 tab.