We present a systematic study of material processing and evaluation for TiO2 using microwave/far/mid-infrared light techniques. A mid-infrared free electron laser (MIR-FEL: 5-20 μm) facility (KU-FEL: Kyoto University Free Electron Laser) has been constructed in Institute of Advanced Energy Kyoto University, and first laser saturation at 13.2 μm was achieved in May 2008. Currently, we have started to develop a measurement system of phonon and electron interaction in metal oxides using MIR-FEL. In addition, we have also developed several new techniques to control the surface condition of TiO2 using microwave irradiation. © Springer 2010.