Gold nanocrystals were prepared by a microwave (MW)polyol method using di-, tetra, and poly(ethylene glycol)s. When these polyols were heated to 240 degrees C at a heating rate of 160 degrees C/min and held at 240 degrees C for 5 min, icosahedral particles with average diameters of 55-85 nm were prepared from HAuCl4/PVP in di-, tetra- and poly(ethylene glycol)s at high yield (>91%). Plate-like and decahedral particles were obtained at high yields front HAuCl4/PVP/NaCl.