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For the first time, a novel BiPO₄/Bi₂S₃ heterostructures with different morphologies have been fabricated through a facile and rapid one pot precipitation route followed by anion-exchange strategy for the photoreduction of toxic Cr(VI) to harmless Cr (III). The hybrid structures systematically investigated using XRD, FE-SEM, EDS, TEM, HRTEM, XPS, FT-IR, UV–vis DRS, and PL. Changing the solvent type has a significant role for controllable morphologies of BiPO₄/Bi₂S₃ hybrid as well as the catalytic activity. The BiPO₄/Bi₂S₃ hybrid synthesized in diethylene glycol (DEG) performed the highest reduction efficiency of Cr(VI) within 20 min, compared with pure hexagonal phase of BiPO₄ under visible light. The rate constant for BiPO₄/Bi₂S₃ synthesized in DEG found to be 20.3 times larger than that for pure BiPO₄. In addition, the presence of tartaric acid as hole scavenger could enhance the Cr(VI) reduction efficiency …