A novel heterostructure of CdS nanoparticles/WO3 nanowhiskers was synthesized using a simple two-step process; thermal evaporation and chemical bath deposition. First, WO3 nanowhiskers (NWs) were grown on a tungsten substrate by thermal evaporation of WO3 powder in a tube furnace at 1050 degrees C. Sequentially, CdS nanoparticles (NPs) were deposited on WO3 nanowhiskers by chemical bath deposition. CdS nanoparticles modified WO3 nanowhiskers showed enhanced visible light absorption compared to bare WO3 nanowhiskers. The photocatalytic activity was studied by the photodegradation of methylene blue. CdS NP/WO3 NW heterostructures showed remarkably enhanced photodecomposition efficiencies compared to bare WO3 nanowhiskers. (C) 2009 American Vacuum Society. [DOI:10.1116/1.3212913]