A nanostructured [email protected] catalyst is deposited on a supported carbon surface using the modified polyol reduction method for the oxygen reduction reaction (ORR) for the application in the proton exchange membrane fuel cell. The crystal structure and feature nanostructure of the [email protected] were established using the XRD and TEM, while their catalytic activity was studied using the cyclic voltammetry and electrochemical polarization techniques. The estimated average crystallite size of PdCr is increased with the calcination temperature from 9.66 to 37.54 nm as the calcination temperature increased to 973 K, while the annealing time slightly affects the crystallite size. The TEM examination reveals the uniform distribution of the PdCr nanoparticles upon the carbon surface. The calcination temperature and time play an important factor in controlling the structural and morphology parameters of [email protected] and the optimum activity and chemical stability were observed for samples calcined at 573 K for 3 h.