Ma. Sriram et Pn. Kumta, THIO SOL-GEL PROCESS FOR THE SYNTHESIS OF TITANIUM DISULFIDE, Journal of the American Ceramic Society, 77(5), 1994, pp. 1381-1384
A thio sol-gel process for the synthesis of titanium disulfide using t
itanium alkoxide as the metal source is demonstrated. The alkoxide rea
cts at room temperature with H2S to form a precipitate which is a prec
ursor to the sulfide. Through infrared spectroscopy and chemical analy
sis of the powder and gas chromatographic analysis of the liquid bypro
ducts of the reaction, it is shown that a partially sulfidized alkoxid
e precursor forms through the displacement of alkoxy groups from the a
lkoxide by sulfur-bearing thiol groups. This thiolysis reaction is ver
y similar to that which occurs in the case of sol-gel reactions to for
m oxides. The alkoxy-thiol species then undergo condensation-polymeriz
ation by the liberation of H2S. When it is heat-treated in H2S, this p
recursor transforms to TiS2 at approximately 700-degrees-C. Systematic
heat treatments have been performed and the formation of TiS2 has bee
n observed using X-ray diffractometry. The change in the morphology ha
s also been studied using scanning electron microscopy.