Synthesis and structural characterization of molybdenum sulfide tubulenes

Polycrystalline tubulenes and highly disordered sheets of MoS2 were obtained by precipitating ammonium thiomolybdate solutions [(NH4)2MoS4] with two different tetraalkylammonium surfactants used as templates, hexadecyltrimethylammonium bromide [CH3(CH2)15N(CH3)3Br] and tetrabutylammonium hydroxide [(CH3(CH2)3)4NOH]. 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 (0 0 l) diffraction peak series characteristic of a lamellar mesostructure. The hybrid phase was decomposed at temperatures above 600 °C yielding a MoS2 phase, which show unusual well-aligned bundles of tubulenes and sponge-like morphology.