Electrospinning allows to prepare uniform one-dimensional inorganic–organic composite nanofibers from solutions containing the polymer to spin. In this work, doped Ti-oxide nanofibers with high surface area (100m2/g) properties have been synthesized via a novel electrospinning procedure. The metals used for titanium oxide doping were nickel, niobium, and tantalum, and the polymer used to spun the solutions of mixed oxide precursors was polyvinyl acetate. Structure and morphology of the materials after calcination at 800°C were investigated by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Energy Dispersion of X-rays (EDX), N2-adsorption/desorption and Thermogravimetry–Differential Scanning Calorimetry (TG–DSC).