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Thin films are the backbone of the electronics industry, and their widespread application in heat sensors, solar cells, and thin-film transistors has attracted the attention of researchers. The current study involves the deposition of a hetero-structured (ZnO/Zn/ZnO) thin film on a well-cleaned glass substrate using the DC magnetron sputtering technique. The samples were then annealed at 100, 200, 300, 400, and 500 °C. The structural, morphological, and electrical characteristics of the annealed samples as well as one as-deposited sample were then examined using atomic force microscopy (AFM), scanning electron microscopy (SEM), X-ray diffraction (XRD), and a Hall effect measuring apparatus. XRD analysis showed a hexagonal ZnO crystal structure for the samples annealed at 300 and 400 °C, whereas the samples annealed at 100 and 200 °C showed metallic zinc and hexagonal ZnO, and the crystallinity decreased for the sample annealed at 500 °C with pure hexagonal crystal symmetry. According to the AFM study, as the annealing temperature increases, the average roughness (R_a) decreases. Temperature has an inverse relationship with particle size. The optimal annealing temperature was determined to be 400 °C. Over this temperature range, the average roughness and particle size increased. Similarly, when R_a decreased, the conductivity increased and the resistance decreased. A fundamental difficulty is that the heating of the heterostructure to 400 °C melts the Zn-based intermediate layer, which alters the Zn phase and disrupts the sample homogeneity.