| Summary: | This work investigates the structure and chemical states of thin-film coatings obtained by pulsed laser codeposition of Mo and C in a reactive gas (H<sub>2</sub>S). The coatings were analysed for their prospective use as solid lubricating coatings for friction units operating in extreme conditions. Pulsed laser ablation of molybdenum and graphite targets was accompanied by the effective interaction of the deposited Mo and C layers with the reactive gas and the chemical states of Mo- and C-containing nanophases were interdependent. This had a negative effect on the tribological properties of Mo–S–C–H nanocomposite coatings obtained at H<sub>2</sub>S pressures of 9 and 18 Pa, which were optimal for obtaining MoS<sub>2</sub> and MoS<sub>3</sub> coatings, respectively. The best tribological properties were found for the Mo–S–C–H_5.5 coating formed at an H<sub>2</sub>S pressure of 5.5 Pa. At this pressure, the <i>x </i>= S/Mo ratio in the MoS<i><sub>x</sub></i>nanophase was slightly less than 2, and the a-C(S,H) nanophase contained ~8 at.% S and ~16 at.% H. The a-C(S,H) nanophase with this composition provided a low coefficient of friction (~0.03) at low ambient humidity and 22 °C. The nanophase composition in Mo–S–C–H_5.5 coating demonstrated fairly good antifriction properties and increased wear resistance even at −100 °C. For wet friction conditions, Mo–S–C–H nanocomposite coatings did not have significant advantages in reducing friction compared to the MoS<sub>2</sub> and MoS<sub>3</sub> coatings formed by reactive pulsed laser deposition.
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