Thio sol-gel process for the synthesis of titanium disulfide

Journal Article · Sun May 01 00:00:00 EDT 1994 · Journal of the American Ceramic Society; (United States)

DOI:https://doi.org/10.1111/j.1151-2916.1994.tb05422.x· OSTI ID:7108014

Sriram, M A; Kumta, P N ^[1]

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1. Carnegie Mellon Univ., Pittsburgh, PA (United States). Dept. of Materials Science and Engineering

Sulfides of transition metals (titanium, molybdenum, vanadium, tungsten, etc.) represent an important class of materials well-known for their catalytic and electrochemical properties. The catalytic properties make them potentially useful in hydrodesulfurization reactions, and their electrochemical response makes them suitable as active cathodes in rechargeable batteries. 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 H[sub 2]S 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 H[sub 2]S. When it is heat-treated in H[sub 2]S, this precursor transforms to TiS[sub 2] at [approximately]700 C. Systematic heat treatments have been performed and the formation of TiS[sub 2] has been observed using X-ray diffractometry. The change in the morphology has also been studied using scanning electron microscopy.

• OSTI ID: 7108014
• Journal Information: Journal of the American Ceramic Society; (United States), Vol. 77:5; ISSN 0002-7820
• Country of Publication: United States
• Language: English

Related Subjects

36 MATERIALS SCIENCE
25 ENERGY STORAGE
ELECTRIC BATTERIES
CATHODES
TITANIUM SULFIDES
CHEMICAL PREPARATION
CATALYSTS
HYDROGEN SULFIDES
X-RAY DIFFRACTION
CHALCOGENIDES
COHERENT SCATTERING
DIFFRACTION
ELECTROCHEMICAL CELLS
ELECTRODES
HYDROGEN COMPOUNDS
SCATTERING
SULFIDES
SULFUR COMPOUNDS
SYNTHESIS
TITANIUM COMPOUNDS
TRANSITION ELEMENT COMPOUNDS
360601* - Other Materials- Preparation & Manufacture
250903 - Energy Storage- Batteries- Materials
Components
& Auxiliaries