Ceramic hollow spheres of MoS2 and MoO3 were obtained by sonochemical synthesis of MoS2 and MoO3 templated on silica nanoparticles (diameters 50-500 nm) followed by acid etching to remove the silica core. The resulting hollow materials have been characterized by elemental analysis, XPS, SEM, TEM, optical absorption, and hydrodesulfurization (HDS) studies. The TEM studies on the hollow ceramic materials indicate the formation of dispersed free spheres with a hollow core. The hollow materials obtained from thermally treated MoS2/SiO2 (450-700 degrees C) show the formation of layered MoS2 (lattice fringes approximately 6.2 A) with a wall thickness of 6-8 layers. The MoS2 hollow spheres are extremely active catalysts for the HDS of thiophene. Hollow spheres of MoO3 are prepared in a similar fashion. Surprisingly, upon heating, hollow crystals of MoO3 with sharp-edged truncated cubes containing inner voids are formed from the initial spheres.