In this work, iron oxide nanoparticle loaded carbon fibers were prepared by electrohydrodynamic co-casting a polymer and particle mixture followed by carbonization. The precursor used to generate carbon fibers was a linear molecular chain polymer: polyacrylonitrile (PAN). A solution containing iron (II, III) oxide (Fe3O4) particles and the PAN polymer dissolved in dimethylformamide (DMF) was electrohydrodynamically co-cast into fibers. The fibers were stabilized in air and carbonized in hydrogen at elevated temperatures. The microstructure and composition of the fibers were analyzed using scanning electron microscopy (SEM). A quantitative metallographic analysis method was used to determine the fiber size. It was found that the iron (II, III) oxide particles distributed uniformly within the carbonized fibers. Photosensitivity of the particle containing fibers was characterized through measuring the open circuit potential of the fiber samples under the visible light illumination. Potential applications of the fibers for photovoltaics and photonic sensing were discussed.