Abstract

Titanium disulfide, TiS₂, has been successfully prepared via a thio ‘sol–gel’ process using titanium(IV) thiolate precursors as the metal source. Four precursors have been investigated, namely [Ti(SBu^t)₄], [Et₂NH₂][Ti₂(SCH₂Ph)₉], [Et₂NH₂][Ti(SC₆F₅)₄(NEt₂)] and [Et₂NH₂]₃[Ti(SC₆F₅)₅][SC₆F₅]₂. The titanium(IV) thiolate reacts at room temperature with H₂S to form a precipitate which upon annealing at 800 °C under H₂S results in the formation of crystalline TiS₂. The TiS₂ produced was analysed by powder X-ray diffraction, scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDXA) and Raman spectroscopy. Annealing the precipitate obtained from the thio ‘sol–gel’ process at 600 °C under H₂S results in the formation of a mixture of crystalline TiS₂ and Ti_1.25S₂.