High-dispersed core–shell Ni/Pt/C nano-electrocatalysts were prepared by “modified polyol process” method. Effect of the experimental parameters, such as the pretreatment of XC-72 supports, the method of adding the XC-72 supports, the concentration of the precursors, on the characteristic and the dispersion of the Ni/Pt nanoparticles on carbon were studied in details. The prepared core–shell Ni/Pt/C catalysts were characterized with X-ray diffraction (XRD), transmission electron microscopy (TEM), and electrochemical methods. The results exhibit that the choice of method of adding the XC-72 support into the solution before formation of the Ni core and appropriately lower concentration of the precursor can obtain high dispersed Ni/Pt/C catalysts, which showed remarkably enhanced activity for oxygen reduction reaction (ORR).

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