In this work, we report the synthesis and characterization of unsupported Pt-CeO 2 (1:1 wt. % Pt:CeO 2 ratio) and Pt-Pd (1:1 wt. % Pt:Pd ratio) electrocatalysts as candidate cathodes for alkaline direct methanol fuel cells (A-DMFCs). The catalytic activity of the cathodes for the oxygen reduction reaction (ORR) in the absence and presence of methanol, in KOH as electrolyte, was evaluated at room temperature. The materials were prepared by chemical reduction with NaBH 4 , and pyrolysis at 300 and 600 °C under a H 2 /N 2 atmosphere. The XRD results indicated the formation of polycrystalline materials with particle sizes ranging from 9 to 19 nm. Analysis by HRTEM showed the formation of nanostructures with lattice fringes corresponding to Pt, Pd (i.e., the Pt-Pd cathode), or CeO 2 (i.e., the Pt-CeO 2 material). The electrochemical characterization in 0.1 mol L −1 KOH showed that the Pt-Pd is highly active for the ORR in alkaline medium, delivering higher onset potential and mass activity than Pt-alone. Meanwhile, the Pt-CeO 2 material showed slightly lower ORR mass activity than Pt. However, in the presence of methanol, the Pt-CeO 2 nanocatalyst demonstrated significantly higher selectivity and tolerance capability to the alcohol than Pt and Pt-Pd.