Abstract: PtCu/C membrane catalysts were prepared by ion beam sputtering (IBS) with moving bimetallic Pt and Cu targets; they were post-processed by vacuum annealing in combination with acid etching. High resolution transmission electron microscopy (HRTEM & STEM) and atomic force microscope (AFM) were employed to characterize the surface morphology of post-processed samples; the alloying degree of Pt and Cu was determined by the X-ray diffraction (XRD). Through cyclic voltammetry (CV) and linear sweep voltammetry (LSV), the electrochemical hydrogen evolution properties of the PtCu/C membrane catalysts were investigated. The results indicated that the PtCu/C membrane catalyst annealed at 400 ℃ and etched by HNO₃ exhibits honeycomb nano-porous structure; the loading of Pt is reduced by about 8.77%, whereas the catalytic activity is enhanced by about 20.62%, in comparison compared with the original PtCu/C membrane catalyst.