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A nanostructured Pd-Cr catalyst was deposited on a supported carbon surface using the modified borohydride reduction method for the oxygen reduction reaction (ORR) to be utilized as an efficient catalyst in the proton-exchange membrane fuel cell. The crystal structure and feature nanostructure of the Pd-Cr@carbon were established through the use of X-ray powder diffraction (XRD) and transmission electron microscopy (TEM). Meanwhile, its catalytic activity was studied using the cyclic voltammetry and electrochemical polarization techniques. Based on the XRD analysis, it was observed that the Pd phase with the fcc crystal structure was dominant, while the Pd-Cr phase with tetragonal crystal structure was detected only for the as-prepared sample and samples calcined at 573 K. The estimated average crystallite size of the Pd phase increased from 9.66 to 37.54 nm as the calcination temperature increased to 973 K, and the calcination time had a slight effect on the crystallite size. On the other side, the average crystallite size for the formed Pd-Cr phase slightly increased from 43.74 nm for the as-prepared sample to 44.90 nm for the sample calcined at 573 K for 3 h. The TEM examination revealed the uniform distribution of the Pd and Pd-Cr nanoparticles upon the carbon surface. The calcination temperature and time played an important role in controlling the structural and morphology parameters of Pd-Cr@carbon. The adsorption/desorption potentials were found to be dependent on the calcination temperature and time and hence the particle and crystallite sizes. The optimum ORR activity and chemical stability were observed for samples calcined at 773 K for 3 h.
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