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Nanoparticles of Au–Pd with core–shell structure were synthesized through the coreduction of HAuCl4and Na2PdCl4in aqueous media by using cetyltrimethylammonium chloride as a reducing agent. The morphology and structure of the core–shell NPs were confirmed by transmission electron microscopy, X-ray diffraction, and UV–vis spectroscopy. We further demonstrate that the core–shell structure is formed as a synergistic result of low interfacial energy and small lattice mismatch between Au and Pd, different redox potentials of PdCl42–/Pd and AuCl4–/Au, and low reduction rates of HAuCl4and Na2PdCl4. The catalyst of Au–Pd core–shell nanoparticles supported on Ni2P–graphite nanoplatelets (Au@Pd/Ni2P-GNPs) exhibits a noticeably higher activity than Pd and Pt catalysts in electrochemical ethanol oxidation. Moreover, we show that the activity and stability of Au–Pd core–shell for ethanol oxidation can be significantly enhanced using Ni2P nanoparticles as a cocatalyst. The prepared Au@Pd/Ni2P-GNPs catalyst exhibits a current density of 1.348 A mg–1metal, which is 2.1 times as high as that of Au@Pd/GNPs without Ni2P nanoparticles deposited.