| Summary: | MoS<sub>2</sub> nanoflowers (NFs) obtained through a hydrothermal approach were used as the substrate for the deposition of tiny spherical bimetallic AuAg or monometallic Au nanoparticles (NPs), leading to novel photothermal-assisted catalysts with different hybrid nanostructures and showing improved catalytic performance under NIR laser irradiation. The catalytic reduction of pollutant 4-nitrophenol (4-NF) to the valuable product 4-aminophenol (4-AF) was evaluated. The hydrothermal synthesis of MoS<sub>2</sub> NFs provides a material with a broad absorption in the Vis-NIR region of the electromagnetic spectrum. The in situ grafting of alloyed AuAg and Au NPs of very small size (2.0–2.5 nm) was possible through the decomposition of organometallic complexes [Au<sub>2</sub>Ag<sub>2</sub>(C<sub>6</sub>F<sub>5</sub>)<sub>4</sub>(OEt<sub>2</sub>)<sub>2</sub>]<sub>n</sub> and [Au(C<sub>6</sub>F<sub>5</sub>)(tht)] (tht = tetrahydrothiophene) using triisopropilsilane as reducing agent, leading to nanohybrids <b>1</b>–<b>4</b>. The new nanohybrid materials display photothermal properties arising from NIR light absorption of the MoS<sub>2</sub> NFs component. The AuAg-MoS<sub>2</sub> nanohybrid <b>2</b> showed excellent photothermal-assisted catalytic activity for the reduction of 4-NF, which is better than that of the monometallic Au-MoS<sub>2</sub> nanohybrid <b>4</b>. The obtained nanohybrids were characterised by transmission electron microscopy (TEM), High Angle Annular Dark Field—Scanning Transmission Electron Microscopy—Energy Dispersive X-ray Spectroscopy (HAADF-STEM-EDS), X-ray photoelectron spectroscopy and UV-Vis-NIR spectroscopy.
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