Polyacrylonitrile (PAN) solution containing the iron oxide precursor iron (III)acetylacetonate (AAI) was electrospun and thermally treated to produce electricallyconducting, magnetic carbon nanofiber mats with hierarchical pore structures. Themorphology and material properties of the resulting multifunctional nanofibermats including the surface area and the electric and magnetic properties wereexamined using various characterization techniques. Scanning electron microscopyimages show that uniform fibers were produced with a fiber diameter of∼600 nm, and this uniform fiber morphology is maintained after graphitization with a fiber diameter of∼330 nm. X-ray diffraction (XRD) and Raman studies reveal that both graphite andFe3O4 crystals are formed after thermal treatment, and graphitization can be enhanced by thepresence of iron. A combination of XRD and transmission electron microscopy experimentsreveals the formation of pores with graphitic nanoparticles in the walls as well as theformation of magnetite nanoparticles distributed throughout the fibers. Physisorptionexperiments show that the multifunctional fiber mats exhibit a high surface area(200–400 m2 g−1) and their pore size is dependent on the amount of iron added and graphitizationconditions. Finally, we have demonstrated that the fibers are electrically conducting as wellas magnetically active.