ZSM-5 crystals, of which granule size is about 120 µm along c axis, are employed as a good host material for TiO 2 loading. Optical microscopy photographs, X-ray powder diffraction spectra and surface area calculated from nitrogen adsorption data at −196 °C have been carried out and show that the titanium dioxide clusters are infiltrating into the pores of ZSM-5. TiO 2 /ZSM-5 host-guest material, regardless of whether being prepared by microwave and water bath heating, shows similar features except for the TiO 2 contents. The materials have a photoluminescence emission peak at 2.85 eV, which is ascribed to the band edge emission. A red shift was observed on the photoluminescence emission spectra when NH 3 adsorbed into the pores of TiO 2 /ZSM-5 material.