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Transition metal chalcogenide thin films of the type FexZrSe₂ have applications in electronic devices, but their use is limited by current synthetic techniques. Here, we demonstrate the synthesis and characterization of Fe-intercalated ZrSe₂ thin films on quartz substrates using the low-pressure chemical vapor deposition of the single-source precursor [Fe(η⁵-C₅H₄Se)₂Zr(η⁵-C₅H₅)₂]₂. Powder X-ray diffraction of the film scraping and subsequent Rietveld refinement of the data showed the successful synthesis of the Fe0.14ZrSe₂ phase, along with secondary phases of FeSe and ZrO₂. Upon intercalation, a small optical band gap enhancement (Eg(direct)opt = 1.72 eV) is detected in comparison with that of the host material.

Fe-doped TiSe2 thin-films were synthesized via low pressure chemical vapor deposition (LPCVD) of a single source precursor: [Fe(η5-C5H4Se)2Ti(η5-C5H5)2]2 (1). Samples were heated at 1000 °C for 1–18 h and cooled to room temperature following two different protocols, which promoted the formation of different phases. The resulting films were analyzed by grazing incidence X-ray diffraction (GIXRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM) and UV/vis spectroscopy. An investigation of the Fe doping limit from a parallel pyrolysis study of FexTiSe2 powders produced in situ during LPCVD depositions has shown an increase in the Fe–TiSe2–Fe layer width with Fe at% increase. Powders were analyzed using powder X-ray diffraction (PXRD) involving Rietveld refinement and XPS. UV/vis measurements of the semiconducting thin films show a shift in band gap with iron doping from 0.1 eV (TiSe2) to 1.46 eV (Fe0.46TiSe2).