In this study, a solvothennal method was used to synthesize Titanium dioxide (TiO2) nanoparticles in the presence of oleic acid (OA) and oleylamine (OM) as morphology-directing agents. Functional nanocomposite fibers composed of poly(ethylene terephtalate) (PET) mixed with OA-OM capped TiO2 nanoparticles were developed by electrospinning process. The different variables that affect the stability of the process were optimized to produce uniform PET/TiO2 nanofibrous mats without heads. The morphology and thermal stability of PET/TiO2 nanotibers were investigated by Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and Thermo-gravimetric analysis (TGA).