Hexagonal CdSe and hexagonal CdS nanoparticles have been prepared using Cd(Ac) 2 and less hazardous elemental Se or S as precursors, respectively, with the aid of ultrasound irradiation under an atmosphere of H 2/Ar (5/95, V/V). The products consist of 7–10 nm nanocrystallites which aggregated in the form of polydispersive nanoclusters with sizes in the range 30–40 nm in the case of CdSe, and near monodispersive nanoclusters with a mean size of about 40 nm in the case of CdS. X-ray diffraction, high-resolution TEM and SAED patterns (selected area electron diffraction patterns) show that the as-prepared particles are well crystallized. X-ray photoelectron spectroscopy (XPS) measurements further confirm the formation of CdSe and CdS. Diffuse reflection spectra indicate that both the CdSe and the CdS nanocryslallites are direct band-gap semiconductors with band-gap values of about 1.83 and 2.62 eV, respectively. Control experiments demonstrate that the hydrogen is the reducing agent, and the extreme high temperature induced by the collapse of the bubble accelerates the reduction of elemental Se or S by hydrogen. An ultrasound assisted in situ reduction/combination mechanism is proposed.