Polycrystalline tubulenes and highly disordered sheets Of MoS2 were obtained by precipitating ammonium thiomolybdate solutions [(NH4)(2)MoS4] with two different tetraalkylammonium surfactants used as templates, hexadecyltrimethylammonium bromide [CH3(CH2)(15)N(CH3)(3)Br] and tetrabutylammonium hydroxide [(CH3(CH2)(3))(4)NOH]. Dried and thermally treated samples were characterized by X-ray diffraction, thermal analysis, scanning and transmission electron microscopy. The surfactant-templated hybrid phase (R4N-MoS4) showed the (00l) diffraction peak series characteristic of a lamellar mesostructure. The hybrid phase was decomposed at temperatures above 600 degrees C yielding a MoS2 phase, which show unusual well-aligned bundles of tubulenes and sponge-like morphology. (c) 2005 Elsevier B.V. All rights reserved.