Silver (Ag) nanoparticles with an average size of ca. 10 nm were uniformly deposited on the surface of alpha-Bi2Mo3O12 nanorods by using an ultrasound sonication method. Ultrasonic irradiation of preformed alpha-Bi2Mo3O12 spherical nanoparticles (ca. 200 nm) in pyridine resulted in alpha-Bi2Mo3O12 nanorods (ca. 100 nm diameter). Further, sonication of the mixture of alpha-Bi2Mo3O12 nanorods and Ag2O in pyridine yielded a nanocomposite of alpha-Bi2Mo3O12 nanorods with deposited Ag nanoparticles and pyridine. Calcination of the nanocomposite at 450 degrees C afforded pyridine-free alpha-Bi2Mo3O12 nanorods with deposited Ag nanoparticles. A plausible mechanism is proposed. The crystallized Ag nanoparticles are uniformly deposited on the surface, with bismuth (Bi) as the preferential binding site, as revealed by time-of-flight secondary ion mass spectrometry (TOF-SIMS). Structural, compositional and morphological characterization of the products is carried out by using transmission electron microscopy, energy-dispersive X-ray analysis, scanning electron microscopy, thermogravimetric analysis, X-ray diffraction, Xray photoelectron spectroscopy and TOF-SIMS. ((C) Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2007).