To obtain the electrocatalyst with an improved electrocatalytic performance towards formic acid electrooxidation (FAEO),a simple impregnation method is used to prepare Pt3Ni nanoparticles loaded on carbon black,assisted with electrochemically dealloying process.The X-ray powder diffraction (XRD) results as well as transmission electron microscopy (TEM) analysis of as-synthesized electrocatalyst demonstrates that the reduction temperature has a great influence on the FAEO activity of the dealloyed Pt3Ni nanoparticles.X-ray photoelectron spectroscopy (XPS) analyses confirm the variation in the electronic structure of platinum by incorporation of nickel atoms which reduces chemisorption of toxic carbon monoxide and promotes the dehydrogenation pathway of FAEO.The size of the dealloyed Pt3Ni nanoparticles remains within the range of about 2.7 nm.All electrochemical results illustrate that the performance of the asobtained electrocatalyst towards the FAEO is significantly enhanced.Moreover,the carbon black content,incorporation of Ni atoms,and reduction temperature conditions have been proven to be the key factors for modification of the crystal structure and morphology which leads to enhanced catalytic performance.