FTIR spectroscopy, SAXS and electrical conductivity studies of the hydrolysis and condensation of zirconium and titanium alkoxides

Abstract

A continuous flowing-rapid mixing technique was combined with FTIR, SAXS and electrical conductivity to study the early stages of polymer formation and growth during the acid-catalyzed hydrolysis and condensation of titanium and zirconium alkoxides. Reaction times as short as 80 milliseconds were investigated. FTIR spectroscopy was used to monitor the water and M−OR concentrations during the reaction. Hydrolysis of ∼25–50% of the alkoxy groups was facile. The FTIR and SAXS data showed that condensation was also very rapid. The activity and mobility of the ions in the solution were monitored by electrical conductivity measurements. The decrease in the normalized solution conductivity during the reaction correlated with the loss of [M−OR]. Furthermore, the radius of gyration of the growing polymers increased rapidly in regimes where the conductivity and [M−OR] decreased fastest. This finding suggests that the mobility of some of the charge carrying species decreases because of the growth in size of the polymers.