Growth of out-of-plane standing MoTe2(1-x)Se2x/MoSe2 composite flake films by sol–gel nucleation of MoOy and isothermal closed space telluro-selenization

This study describes the sol–gel processing of MoOy on Si (1 0 0) to subsequently achieve out-of-plane MoTe2/MoSe2 flake composite films by an isothermal closed space vapor transformation. The oxide precursor films have been prepared from a Mo isopropoxide solution in isopropanol and acid catalysis induced by HCl. Thermal annealing at 200, 400 and 600 °C enhanced the condensation after xerogel formation. An x-ray absorption analysis demonstrates that films condensed at 200 °C are at an intermediate chemical state between MoO3 and MoO2. To achieve MoTe2/MoSe2 composite films, the precursor oxide films were reduced in H2 and exposed to the chalcogenides by isothermal closed space vapor transport at 600 °C. The multilayered nanocomposite films grow with an out-of-plane flake-like structure and an evident integration of Se in the MoTe2 phase according to a MoTe2(1-x)Se2x alloy, with an estimation of x of 0.25. The alloy and the orientation of the flakes are consistent with the bands present in the Raman spectrum. These films are attractive for applications requiring high surface area interfaces favoring gas or ion exchange reactions with transition metal dichalcogenides ; The current research was funded by grant CTQ2017-84309-C2-2-R from Ministerio de Ciencia e Innovación (Spain). The authors acknowledge the ESRF and the Ministerio de Ciencia, Innovación y Universidades (Spain), for provision of synchrotron radiation facilities and the Consejo Superior de Investigaciones Científicas (Spain) financial support for the operation of the beamline under Grant No. PIE 2010 6 OE 013