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Copper, antimony and sulfur in elemental form were applied for one-pot solid-state mechanochemical synthesis of skinnerite (Cu₃SbS₃) in a laboratory mill and an industrial mill. This synthesis was completed after 30 min of milling in the laboratory mill and 120 min in the industrial mill, as corroborated by X-ray diffraction. XRD analysis confirmed the presence of pure monoclinic skinnerite prepared in the laboratory mill and around 76% monoclinic skinnerite, with the secondary phases famatinite (Cu₃SbS₄; 15%), and tetrahedrite (Cu_11.4Sb₄S₁₃; 8%), synthesized in the industrial mill. The nanocrystals were agglomerated into micrometer-sized grains in both cases. Both samples were nanocrystalline, as was confirmed with HRTEM. The optical band gap of the Cu₃SbS₃ prepared in the laboratory mill was determined to be 1.7 eV with UV–Vis spectroscopy. Photocurrent responses verified with I–V measurements under dark and light illumination and Cu₃SbS₃ nanocrystals showed ~45% enhancement of the photoresponsive current at a forward voltage of 0.6 V. The optical and optoelectrical properties of the skinnerite (Cu₃SbS₃) prepared via laboratory milling are interesting for photovoltaic applications.