AuxAg1-x/AuyAg1-y multilayers and multisegment nanowires were deposited from a single solution containing KAu(CN)(2), KAg(CN)(2), and Na2CO3 (pH 13). Cyclic voltammograms for deposition from solutions containing Au(CN)(2)(-) and Ag(CN)(2)(-) show the characteristic deposition peaks for gold and silver. The composition of the deposited alloys is dependent on the deposition potential (or current) and solution chemistry. Multisegment nanowires were prepared by sequential deposition at -0.7 and -1.2 V from solutions containing Au(CN)(2)(-) and Ag(CN)(2)(-) solution in porous Al2O3 templates. The different segments deposited at -0.7 and -1.2 V are clearly distinguished by scanning electron microscopy and optical microscopy under blue light illumination. (C) 2003 The Electrochemical Society.