Abstract: A series of PtCu/C catalysts (with a CuPd loading of 20%) were prepared by ethylene glycol (EG) reduction method with different metal precursors, viz., CuSO₄/CuCl₂ and K₂PtCl₄/H₂PtCl₆. The morphology, structure and electrochemical performance of as-prepared PtCu/C catalysts were characterized by high-resolution transmission electron microscopy (TEM), X-ray diffraction (XRD), cyclic voltammetry (CV) and liner sweep voltammetry (LSV) techniques. The results indicate that the PtCu/C catalyst prepared with CuSO₄ and K₂PtCl₄ as precursors exhibit highest electrochemical performance, in which metal particles with a mean size of 2.3 nm are uniformly dispersed on the carbon support. Such a PtCu/C catalyst has an electro-chemical surface area (ECSA) of 73.0 m²/g_Pt and a mass activity (MA) of 126 mA/mg_Pt, both higher than the commercial Pt/C catalyst.