Molybdenum oxide (MoOx) is a well-studied transition-metal semiconductor material, and has a wider band gap than MoS2 which makes it become a promising versatile probe in a variety of fields, such as gas sensor, catalysis, energy storage ect. However, few MoOx nanomaterials possessing photoluminescence have been reported until now, not to mention the application as photoluminescent probes. Herein, a one-pot method is developed for facile synthesis of highly photoluminescent MoOx quantum dots (MoOx QDs) in which commercial molybdenum disulfide powder and hydrogen peroxide (H2O2) are involved as the precursor and oxidant, respectively. Compared with current synthesis methods, the proposed one has the advantages of rapid, one-pot, easily prepared, environment friendly as well as strong photoluminescence. The obtained MoOx QDs is further utilized as an efficient photoluminescent probe, and a new off-on sensor has been constructed for phosphate (Pi) determination in complicated lake water samples, attributed to the fact that the binding affinity of Eu(3+) ions to the oxygen atoms from Pi is much higher than that from the surface of MoOx QDs. Under the optimal conditions, a good linear relationship was found between the enhanced photoluminescence intensity and Pi concentration in the range of 0.1-160.0 μM with the detection limit of 56 nM (3σ/k). The first application of the photoluminescent MoOx nanomaterials for ion photochemical sensing will open the gate of employing MoOx nanomaterials as versatile probes in a variety of fields, such as chemi-/bio-sensor, cell imaging, biomedical and so on.

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