Thermal evolution in air and argon of nanocrystalline MoS2 synthesized under hydrothermal conditions

Nanocrystalline molybdenum sulfide was synthesized between 150°C and 225°C under hydrothermal conditions starting from ammonium heptamolybdate and thiourea. Samples were characterized with X-ray powder diffraction, electron microscopy, nitrogen adsorption, thermoanalysis and infrared spectroscopy. The hydroxyls involved in the synthesis and adsorbed on crystals surface hindered crystallization and samples still recrystallized after the final dehydroxylation step above 300°C, just when hydroxyls were isolated from each other. This also promoted sulfur bond breaking that gave rise to partial transformation of the MoS2 into MoO2 when the annealing atmosphere was argon, and to the total transformation of the sulfide into MoO3 when it was air. The initial MoS2 crystals were bend; many of them were isolated, and others associated in bundles that formed worm-like grains interacting with each other to produce spherical grains aggregated in clusters. This morphology gave rise to samples with a low specific surface area.