The main automotive catalytic media, precious metal-doped ceria-zirconia oxides, fundamental system character is unknown. Understanding the catalytic system properties should allow for the production of an optimal model catalyst. This goal of this study is to gain understanding of ceria-zirconia-palladium systems and to determine a reproducible method for preparing catalysts with minimal surface-carbon. This study investigates ceria-zirconia-palladium catalyst preparation via aqueous chemistry methods and a sputter deposition technique for doping ceria-zirconia oxide mixtures. Prepared catalysts are characterized by X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). XPS allows the surface species, after catalyst doping and annealing, to be evaluated. Prepared catalyst EM analysis allows for surface morphology and particle characteristic evaluation. Prepared catalysts are exposed to UHV conditions, palladium sputtered-coated, and annealed at various temperatures. Temperature dependency is observed in both percentage of carbon, metal, and oxygen species present. This study led to a reproducible, low-carbon content, doping method for use in future pollutant reaction studies.