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Material processing is critical for obtaining high-performance solar cells, which influences the morphological, crystal, and electrical properties of the functional materials in a device. Sb 2 (S,Se) 3 can be considered as a quasi-binary compound since sulfur and selenium can be alloyed with a continuous ratio due to the identical crystal structure of Sb 2 S 3 and Sb 2 Se 3 and close ionic radius between sulfur and selenium. [1-3] This simple chemical composition allows for facile synthesis of Sb 2 (S,Se) 3 film with a well-defined crystal structure. In this regard, both

Continuously boosting the power conversion efficiency (PCE) and delving deeper into its functionalities are essential problems faced by the very new antimony selenosulfide (Sb2(S,Se)3) solar technology. Here, a convenient and effective solution post‐treatment (SPT) technique is used to fabricate high‐performance Sb2(S,Se)3 solar cells, where alkali metal fluorides are applied to improve the quality of Sb2(S,Se)3 films in terms of morphology, crystallinity, and conductivity. In particular, this approach is able to manipulate the S/Se gradient in the films and creates favorable energy alignment which facilitates the carrier transport. As a result, the fill factor and short‐circuit current density of Sb2(S,Se)3 solar cells (Glass/FTO/Zn(O,S)/CdS/Sb2(S,Se)3/Spiro‐OMeTAD/Au) based on the SPT strategy are significantly enhanced, achieving a champion efficiency of 10.7%. To date, this conversion efficiency value represents the highest efficiency of all Sb‐based solar cells. This study provides an effective post‐treatment strategy for improving the quality of Sb2(S,Se)3 film which sheds new light on the fabrication of high‐efficiency Sb2(S,Se)3 solar cells.