AbstractThe present study reports a novel and fast nitrogen plasma treatment approach to boost hydrogen evolution on antimony(III) sulphide (Sb2S3) thin films via light‐driven water splitting. The Sb2S3 films were synthesised by electrodepositing antimony followed by sulphurisation, and then using different treatment times under nitrogen plasma. The plasma treatment time did not result in significant changes in the microstructural and optical properties, compared to the non‐plasma films. However, the wettability drastically changed from superhydrophobic for the non‐plasma film to hydrophilic once treated. Photoelectrochemical analysis showed a substantial photocurrent density increase (24‐fold) for the film treated for 10 s in comparison with the non‐plasma film. Further characterisation by X‐ray photoelectron spectroscopy and scanning electron microscopy revealed chemical and morphological modifications for the films treated, which explain the enhancement of photoelectroactivity and wettability.