Thio Sol–Gel Process for the Synthesis of Titanium Disulfide

A thio sol–gel process for the synthesis of titanium disulfide using titanium alkoxide as the metal source is demonstrated. The alkoxide reacts at room temperature with H₂S to form a precipitate which is a precursor to the sulfide. Through infrared spectroscopy and chemical analysis of the powder and gas chromatographic analysis of the liquid byproducts of the reaction, it is shown that a partially sulfidized alkoxide precursor forms through the displacement of alkoxy groups from the alkoxide by sulfur-bearing thiol groups. This thiolysis reaction is very similar to that which occurs in the case of sol–gel reactions to form oxides. The alkoxy–thiol species then undergo condensation–polymerization by the liberation of H₂S. When it is heat-treated in H₂S, this precursor transforms to TiS₂ at ∼700°C. Systematic heat treatments have been performed and the formation of TiS₂ has been observed using X-ray diffractometry. The change in the morphology has also been studied using scanning electron microscopy.