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In the present paper, simple hydrothermal and solid-state methods are reported for the synthesis of metal chalcogenide (ZnSe), metal oxide (Co₃O₄) and their nano-heterostructure (ZnSe/Co₃O₄ 3:1, 1:1 and 1:3 ratios by weight), while their photocatalytic efficiencies are also investigated. The X-ray diffraction results corroborate the good crystallinity and purity of all synthesized products, i.e., ZnSe, Co₃O₄ and their nanocomposites. The scanning electron micro-images of ZnSe show a mixed morphology of nanoparticles (≈16 nm), including spherical and distorted cubes, while Co₃O₄ has a worm-like morphology (≈20 × 50 nm). The EDX results show that all the elements are present in accordance with their anticipated amounts in the products. The UV/visible absorption spectrum of ZnSe depicts a sharp absorption at around 480 nm, while Co₃O₄ demonstrates two prominent peaks, 510 nm and 684 nm. The prepared samples were employed for the photocatalytic degradation of Congo red dye and the nano-heterostructure (ZnSe/Co₃O₄ 3:1) shows an exceptional photocatalytic degradation efficiency of 96%. This enhanced photocatalytic activity was due to the synergic effect of ZnSe and Co₃O₄ that reduced the electron/hole recombination and caused suitable bandgap alignment.