Nanosheet of PdNiZn and nanosphere of PdNiZn/reduced-graphene oxide (RGO) with sub-3nm spheres have been successfully synthesized through a facile oil-water interfacial strategy. The morphology and composition of the films were determined by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive analysis of X-ray (EDAX) and elemental mapping. In the present study, we have developed a method to minimize the usage of precious Pd element. Due to the special structure and intermetallic synergies, the PdNiZn and PdNiZn/RGO nanoalloys exhibited enhanced catalytic activity and durability relative to Pd nanoparticles in Suzuki-Miyaura C-C cross-coupling reaction. Compared to classical cross-coupling reactions, this method has the advantages of a green solvent, short reaction times, low catalyst loading, high yields and reusability of the catalysts.