The electrochemical activity of the Cu2O/AlZn-LDH, deposited on the FTO electrode, was investigated in NaOH (0.1 M) media. The thin film Cu2O/AlZn-LDH was characterized by techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDX). Based on the obtained results from XRD, Cu2O/AlZn-LDH was prepared in the nanometer size with good crystalline quality. The SEM images were shown the synthesis of a thin film Cu2O/AlZn-LDH nanocomposite on the FTO electrode. The water oxidation results show that Cu2O-Zn/Al-LDH modified FTO electrode is an improved electrocatalyst and has high activity at water oxidation in alkaline media with the onset potential about 0.6 V vs. SCE and overpotential of 380 mV at10 mA/cm. The improved water oxidation activity at Cu2O/AlZn-LDH can be attributed to the good conductivity of the nanocomposite.