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In the present study, the mechanochemically prepared covellite, CuS and chalcocite, Cu₂S nanocrystals are compared in detail. Concretely, the SEM, EDS, N₂ adsorption, UV–Vis, PL, FTIR, ZP measurement, PCCS, XPS and DTA/TG were used. SEM, EDS and elemental mapping have shown that the agglomerates containing nanoparticles of the corresponding phases were formed as a result of milling. The nitrogen adsorption method has documented richer surface properties in the case of CuS sample. The specific surface area values were 2.7 m² g⁻¹ and 1.4 m² g⁻¹ for CuS and Cu₂S, respectively. UV–Vis and PL measurements have shown that these materials might be suitable for optoelectronic applications, as the optical bandgaps were 1.92 eV and 3 eV for CuS and Cu₂S, respectively. FTIR spectrum of CuS exhibited a peak at 621 cm⁻¹, which is characteristic for this material. ZP values were more …