Plasma assisted calcination of composite submicron fibers (Ce(NO3)3/polyvinylpyrrolidone)as a novel method for inorganic submicron fibers preparation was studied. Special type of dielectric barrier discharge, so called Diffuse Coplanar Surface Barrier Discharge(DCSBD)was used for the plasma treatment of composite fibers at atmospheric pressure in ambient air for the purpose of oxidation and removing of organic base polymer by the active species produced in plasma. High decrease of C/Ce ratio and formation of porosity on fibers surface were observed after plasma calcination at exposure time in the order of minutes. Due to the low temperature approach and short treatment time, plasma assisted calcination is a suitable and perspective alternative to the conventional high-temperature calcination.