The optically transparent poly(methyl methacrylate-co-maleic anhydride) P(MMA-co-MA)/SiO2-TiO2, hybrid materials were prepared using 3-aminopropyl triethoxysilane as a coupling agent for organic and inorganic components. Real-time FTIR was used to monitor the curing process of hybrid sol, indicating that imide group formation decreased with increasing titania content. scanning electron microscopy, atomic force microscopy, and differential scanning calorimetry results confirmed their homogeneous inorganic/organic network structures. TGA analysis showed that incorporated titania greatly prohibits the thermodegradation of hybrid films, especially at the content of 5.3 wt %, showing an increase of about 32.6 degrees C at 5% loss temperature in air. The UV degradation behavior of P(MMA-co-MA) studied by quasi-real-time FTIR showed that TiO2, incorporated in the hybrid network provides a photocatalytic effect rather than a UV-shielding effect. (c) 2005 Wiley Periodicals, Inc.