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Herein, the properties of the organic heterostructures with triple‐layer ZnO/Ag/ZnO as a replacement for ITO and mixed layer containing arylenevinylene oligomer (based on triphenylamine or carbazole) donor and nonfullerene (perylene diimide) acceptor mixed in the ratio 1:2 and the effect of a buffer layer of PEDOT‐PSS intercalated between triple layer and mixed organic layer are discussed. The UV−vis transmission and photoluminescence (PL) properties are investigated in correlation with the surface topography and reveal a good match between the absorption and emission domain, which can favor the generation of the charge carriers. The heterostructure with the mixed layer based on triphenylamine oligomer shows the widest absorption domain, and the PL spectra of the heterostructures realized with either triphenylamine or carbazole oligomer show peaks corresponding to the radiative decay of the donor and acceptor. The I−V characteristics in the dark indicate a slightly nonlinear behavior and the current is affected by the charge carriers recombination on the defects present in the thick mixed layer deposited by matrix‐assisted pulsed laser evaporation. The effect of the PEDOT‐PSS buffer layer on the electrical properties of the organic heterostructure with ZnO/Ag/ZnO electrode is also investigated. [ABSTRACT FROM AUTHOR]