Thio sol–gel synthesis of titanium disulfide from titanium thiolates
2000; Royal Society of Chemistry; Volume: 10; Issue: 12 Linguagem: Inglês
10.1039/b006181f
ISSN1364-5501
AutoresClaire J. Carmalt, Christopher W. Dinnage, Ivan P. Parkin,
Tópico(s)Inorganic Chemistry and Materials
ResumoTitanium 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(SBut)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 Ti1.25S2.
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