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Abstract : Nanomaterials have excellent chemical and physical properties and have wide applications in the modern time. One of the important methods for preparing nanocomposites (Al2O3/ZnO) is the electrochemical deposition method, which is characterized by speed, ease and inexpensive. The nanocomposite characterizes by Advanced techniques such as x-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), ultraviolet-visible (UV-Vis), energy dispersive x-ray (EDX), and atomic force microscopy (AFM). The analysis showed that the shape of nanocomposite was Nano rod, the band gap value was 3.23(e.v) and average crystal size was (8.4 nm).