Atmospheric pressure plasma assisted calcination by the preparation of TiO2 submicron fibers as a low-temperature alternative to the conventional thermal annealing was studied. A special type of dielectric barrier discharge was used for plasma treatment of hybrid titanium butoxide/polyvinylpyrrolidone (Ti(Bu)/PVP) fibers prepared by forcespinning to decompose and oxidize the base polymer and precursor. The obtained fibers were characterized by changes in chemical bonds on the surface using Fourier Transform Infrared Spectroscopy (FTIR), chemical composition by using Energy-Dispersive X-Ray Spectroscopy (EDX), X-ray Photoelectron Spectroscopy (XPS). The morphology of fibers was investigated by Scanning Electron Microscopy (SEM). A significant decrease of organic components was reached by short plasma exposure times less than 1 h. The obtained fibers exhibit a high surface porosity without degradation of the fibrous structure. The results obtained indicate that atmospheric pressure plasma assisted calcination can be a viable low-temperature, energy-and time-saving alternative or pre-treatment method for the conventional high-temperature thermal calcination. (C) 2017 Elsevier B.V. All rights reserved.