The microwave-assisted polyol reduction method was applied to the synthesis of core-shell gold/palladium bimetallic nanoparticles by the simultaneous reduction of the Au-III and Pd-II ions. The thickness of the palladium shell was calculated to be similar to3 nm, and the gold core diameter is 9 nm. The structure and composition of the bimetallic particles were characterized by high-resolution transmission electron microscopy equipped with a nanoarea energy-dispersive X-ray spectroscopy attachment, transmission electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy.