This research describes the synthesis of organomodfied sillica nanoparticles (NP)s /polyvinyl alcohol (PVA) nanocomposites (NC)s through consecutive three-steps. In the first step the surface modifier, namely 1-(benzo[d]thiazol-2-yl)-3-(3-(triethoxysilyl)propyl)urea, was prepared from the reaction of benzo[d]thiazol-2-amine and 3-isocyanatopropyl triethoxysilane. With success in the first step, the surface modifications of silica NPs were achieved by sol-gel procedure and at the final step, the preparation of PVA/silicaNCs were targeted. The optical properties and morphology of the NPs and NCs were characterized. This investigation clearly showed that the new coupling agent could effectively prevent the agreggation of NPs.