In this study, Vulcan XC-72 R supported PdNix, and PdNiZr bimetallic catalysts were synthesized by using sodium borohydride (NaBH4) and formic acid as reduction agents. The structural properties and morphological qualities of these nanocatalysts were evaluated by XRD, SEM, and TEM analysis. The XPS analysis spectra for Pd/C, PdNi/C, and PdNiZr/C catalysts showed that Pd, Ni, Zr, and C elements successfully entered the structure. The weights in percent metals of the Pd/C, PdNi/C, and PdNiZr/C catalysts were determined by EDX analysis. In addition, these catalysts' electrochemical properties, activity, and stability, such as their electrochemically active surface area (ESA), were examined using cyclic voltammetry (CV) chronoamperometry, chronopotentiometry, and electrochemical impedance spectroscopy. Polarization curves were created for Pd/C, PdNi/C, and PdNiZr/C catalysts utilized as cathode electrocatalysts in a single cell at temperatures of 40 °C, 50 °C, 60 °C, and 70 °C. The PdNiZr/C and PdNi/C catalysts were determined to have higher performance than the Pd/C catalyst. Power densities of Pd/C, PdNi/C, and PdNiZr/C catalysts were measured to be 27.54 mWcm−2, 114 mWcm−2, and 188 mWcm−2, at 70 °C, respectively.