Bicompartmental (BC) Ag/Cu nanoparticles were synthesized using a two-step polyol reduction process. Initially, Ag nanoparticles with an average diameter of 21 +/- 3 nm were prepared from AgNO3 using a microwave (MW)-polyol method. Then, Cu(OAc)(2)center dot H2O was added dropwise under MW or oil-bath heating. The formation of BC Ag/Cu nanoparticles with an average size of 29 +/- 6 nm in high yield (98%) was confirmed using energy-dispersive X-ray spectroscopic (EDS) measurements.