In this study, titanium dioxide (TiO(2)) nanofibers with diameters ranging from 200-500 nm are successfully prepared via an electrospinning technique using a solution that contains polyvinyl pyrrolidone (PVP) and tetrabutyl titanate (TBT). Three key processing parameters are evaluated on the morphology of the fibers formed. Firstly, the PVP : TBT molar ratio is strongly correlated with the morphology of the fibers formed, and two extremes in the fiber morphology are observed as a result of varying the PVP : TBT molar ratio. Secondly, the electric field strength has been found to most strongly affect the fiber diameter, which increases as the electric field strength increases. Thirdly, the electrospun TiO(2)/PVP composite nanofibers are calcined at different temperatures. The process of removing organic components, the phase formation and the phase transition of the inorganic TiO(2) are investigated using thermo-gravimetry-differential scanning calorimetry, infra-red and X-ray diffraction analyses.