Amorphous organic-inorganic hybrid thin films (Ti-thiolate) deposited on thermal SiO 2 substrate by atomic layer deposition/molecular layer deposition are converted into textured titanium disulfide (TiS 2) ultrathin films, of thickness down to 5.5 nm, upon annealing under Ar/H 2 (5%) atmosphere at mild temperature ( 300 °C). Two annealing strategies were investigated by in situ synchrotron x-ray fluorescence, allowing us to master the mineralization of the amorphous Ti-thiolate into titanium disulfide. Stoichiometry and crystallinity of the thin films were characterized by x-ray photoelectron spectroscopies, Raman scattering, and x-ray absorption at the S K-edge. Lamellar structure parallel to the substrate surface was observed by transmission electron microscopy.

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