Abstract
Amorphous, polymeric molybdenum sulfide has attracted significant attention as a non-platinum group electrocatalyst for the hydrogen evolution reaction (HER). To elucidate the influence of oxygen incorporation on molybdenum sulfide catalysts, MoOxSy electrocatalysts were synthesized via a potentiostatic electrodeposition method. The presence of oxygen and the associated molybdenum oxidation state were modified by postsynthesis treatments of air exposure, annealing in an inert atmosphere, and annealing in a sulfur flux. The as deposited sample exhibited the best performance, requiring only 171 mV to reach a cathodic current density of 10 mA/cm2. While the modified films exhibited worse HER performance compared to the as deposited sample, by utilizing extensive X-ray photoelectron spectroscopy studies, we highlighted the importance of the Mo5+ oxidation state while identifying a previously unreported state within MoOxSy catalysts between Mo4+ and Mo5+.
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