| Summary: | In the present study, MoO<sub>3</sub>:MoS<sub>2</sub> hybrid thin layers have been synthesized through partial oxidation of MoS<sub>2</sub>. We have demonstrated that the reaction requires darkness conditions to decrease the oxidation rate, thus obtaining the hybrid, MoO<sub>3</sub>:MoS<sub>2</sub>. A simple liquid-phase exfoliation (LPE) is carried out to achieve homogenous MoS<sub>2</sub> nanoflakes and high reproducibility of the results after MoS<sub>2</sub> oxidation. XPS analyses reveal the presence of MoO<sub>3</sub>, MoS<sub>2</sub>, and MoOxSy in the hybrid layer. These results are also confirmed by X-ray diffraction and high-resolution TEM. Optical absorbance reveals that the absorption peaks of the MoO<sub>3</sub>:MoS<sub>2</sub> hybrid are slightly redshifted with the appearance of absorption peaks in the near-infrared region due to the defects created after the oxidation reaction. The composition and atomic percentages of each component in the hybrid layer as a function of reaction time have also been reported to give perspective guides for improving electronic and optoelectronic devices based on 2D-MoS<sub>2</sub>.
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