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Highly uniform dispersed bimetallic Pt3Zn alloy nanocrystals (NCs) with unique geometries are obtained via a facile one‐pot synthesis process by regulating different reductants. To investigate the morphology and composition of the prepared catalysts, the transmission electron microscopy, X‐ray diffraction and X‐ray photoelectron spectroscopy are utilized. Electrochemical measurements reveal that the Pt3Zn NCs significantly exhibited larger electrochemically active surface areas and excellent catalytic activity towards electro‐oxidation of methanol and ethanol in comparison to the commercial Pt/C. The optimized Pt3Zn (AA) NCs exhibit excellent mass activities in both methanol oxidation reaction (1251.4 mA mgPt−1) and ethanol oxidation reaction (975.7 mA mgPt−1) in acidic media, which are respectively 4.28 times and 3.02 times higher than those of commercial Pt/C. Moreover, the Pt3Zn NCs show a higher stability and better resistance to the COads poisoning. The activity enhancements are attributed to electronic effects and a bifunctional mechanism. [ABSTRACT FROM AUTHOR]