Palladium nanoparticles supported by alumina nanofibers have been successfully synthesized by electrospinning using palladium chloride incorporated into a solution of polyvinyl pyrrolidone and aluminum acetate. Palladium agglomerate sizes and the surface morphology of the electrospun nanofibers were determined by transmission electron microscopy. Palladium nanoparticles appeared to be well dispersed within the electrospun nanofiber structure. X-ray diffraction, x-ray photoelectron spectroscopy, and Raman scattering spectroscopy techniques were used to identify the crystalline form and distinguish between oxidized and metallic palladium particles after heating and hydrogenation.