Nickel oxide-gadolinium doped ceria (NiO– Ce0.8Gd0.2O1.9) deserves special attention because of its high ionic conductivity. The nanocomposite fibers of this material are suitable as anode materials for low-temperature SOFCs. The composition and morphology of the nanofibers which prepared via electrospinning method were characterized by SEM, TEM and EDS. It was noticed that the fiber diameters gradually decreased from 190±77 nm to 75±27 nm by increasing the calcination temperature from 800 °C to 1000 °C. Further, the influence of the different parameters such as concentration of the polymeric pre-spinnable solution (CPS), concentration of the cationic solution (CCS), the applied voltage, tip-target distance, feed rate, diameter of the needle and the calcination temperature on the morphology of the fibers were investigated.