In this paper, submicron thin Pd–Cu alloy films are deposited using a dual sputtering technique, which allows a high composition control of the layer. The composition, surface morphology and phase structure of the sputtered layers are investigated by energy-dispersive spectrometry (EDS), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffractiometry (XRD). For example, the XRD data prove that the Pd–Cu layers are an alloy of Pd and Cu. Subsequently, the characterized Pd–Cu alloy layers are deposited on a silicon support structure to create a 750-nm thin Pd–Cu membrane for hydrogen separation. The reported membrane obtained a high flux of 1.6 mol H2/m2 s at a temperature of 725 K, while the selectivity is at least 500 for H2/He.