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Antimony selenide thin films were prepared through potentiostatic co‐electrodeposition by applying −0.6 V from a bath composed of 2.5 mM K(SbO)C4H4O6 ⋅ 0.5 H2O and 2.0 mM SeO2 in a supporting electrolyte of 0.5 M Na2SO4/H2SO4 at pH 2. The films were subjected to different thermal treatment (TT) conditions under a Se(vapor)/N2 atmosphere. Cyclic voltammetry was used to evaluate the electrochemical process of each element separately as well as the binary system on Pt and FTO working electrodes. The morphology, composition, band gap, crystallography, and photoactivity toward hydrogen gas production of the films were evaluated as a function of TT conditions, in order to obtain insight into their effects on film properties. Under all conditions, the films showed homogeneous and rough surfaces and a stoichiometric Sb2Se3 composition. The non‐thermal‐treated film was non‐crystalline, whereas after TT, all films showed a pure orthorhombic Sb2Se3 phase. It was observed that the crystallographic texturization of films in the (120) plane, caused by some TT conditions, is detrimental to the photoactivity. At the optimized TT conditions (300 °C for 3 h), the film presented good crystallographic and optoelectronic properties and photoactivity, with a photocurrent value of 168.15 μA cm−2 (at the standard hydrogen gas evolution potential) and a band gap of around 1.1 eV.

Cobalt-modified Sb₂Se₃ showed improved photoelectrochemical properties towards the HER and initial photocorrosion stability, which were associated with grain-boundary inversion.

Sb 2 Se 3 is presented as a promising light absorber material of low-cost and good photoelectrocatalytic activity. Among the different synthetic methods for this semiconductor, electrodeposition has gained attention. In this context, a study of the electrodeposition parameters is an important aspect for obtaining films with optimized photocatalytic characteristics. Thus, in this work, we studied the effect of precursor concentration, the total charge of deposition, the type of supporting electrolyte, bath temperature, and the deposition potential on obtaining antimony selenide thin films electrochemically and on the morphological, structural, and optoelectronic properties of these films. One of the most interesting observations was the huge impact of these parameters on the morphology. The Serich films showed a tendency to have a rod-like morphology and relatively better stability to photocorrosion. The thickness of the film is another parameter that hugely affected the photocatalytic properties. From the evaluation of the photocurrent values presented by the films, the optimized electrodeposition parameters were found.