Phothermal therapy (PTT) is one of the most promising techniques to treat cancer. Finding the ideal PTT agent nanomaterial has remained a challenge and has brought the interest of several researchers. In this work, we report the synthesis of molybdenum oxide (MoOx) nanoparticles (NPs), which exhibit absorption in the biological optical window ~840 nm, by using the laser ablation of solids in liquids (LASL) technique with nanosecond (ns) pulses. A Nd:YAG laser was used to synthesize the NPs in deionized (DI) water, free of surfactants or additives, which were optically characterized by absorption spectroscopy and TEM-EDX microscopy. Semi spherical NPs with a suitable average size and shape for potential use as PTT agents were obtained by laser ablation and ablation + fragmentation. The calculated band gap is 3.1 eV, which corresponds to MoO3. Micro-Raman spectroscopy studies determined that these NPs are composed of amorphous molybdenum oxide hydrates (MoO3 · xH2O).