In this study, we have synthesized highly photolumine scent TiO2/poly (phenylene vinylene) (PPV) hybrid nanoparticle-polymer fibers by electrospinning a PPV precursor added to a TiO2 sol-gel solution. The diameters of the hybrid fibers ranged from 100-300 nm and the average size of TiO2 nanoparticles within the fibers was 10-60 nm. FT-IR analysis indicated that a new band around 1632 cm(-1) assigned to the Ti-O-C vibration appeared, which resulted in the stronger luminance of the fluorescence of the TiO2/PPV hybrid fibers compared to free standing PPV nanofibers.