| Summary: | Here we report a novel synthesis approach for the preparation of α-MoO<sub>3</sub>:Ln<sup>3+</sup> materials employing a two-step synthesis. Additionally, in this work the α-MoO<sub>3</sub>:Ln<sup>3+</sup> materials are reported as potential optical thermometers for the first time. In this synthesis approach, first MoS<sub>2</sub> 2D nanosheets were prepared, which were further heat treated to obtain α-MoO<sub>3</sub>. These materials were fully characterized by powder X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), X-ray fluorescence (XRF), thermogravimetry (TG) and differential thermal analysis (DTA), transmission electron microscopy (TEM), and luminescence spectroscopy. Temperature-dependent luminescence measurements were carried out to determine the optical thermometric properties of two different types of α-MoO<sub>3</sub>:Ln<sup>3+</sup> materials (Eu<sup>3+</sup>/Tb<sup>3+</sup> downshifting and Er<sup>3+</sup>/Yb<sup>3+</sup> upconversion luminescence systems). We demonstrate in this study that this class of material could be a potential candidate for temperature-sensing applications.
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