Electrospun Poly (vinylidene fluoride) (PVdF) fine fiber of 100-300 nm in diameter in ribbon shape was synthesized through the electrospinning process via sol-gel. In order to synthesize infusible nanofibers all processing of dehydrofluorination and carbonization was investigated. Iron nanoparticles was doped with PVDF nanofibers in order to be effective in surface area, and porosity to increase the hydrogen storage. The composition, morphology, structure and surface area of PVDF/Iron Oxide nanofibers were investigated by thermo gravimetric analysis (TGA) to determinate the temperature of possible decomposition and crystallinity, scanning electron microscopy (SEM), transmission electron microscopy (TEM), Micromeritics (ASAP2020) used to study the textural properties of the sample, like surface area, total pore volume, and micro pore volume. The result shows that the PVDF without dehydrofluorination treatment for infusibility become melt at around 160 °C. By adding the iron oxide nanoparticles as a catalyst it can improve the characteristic of the carbon fiber for hydrogen storage. In best of our knowledge, PVDF doping with iron oxide investigated for first time.