Cerium oxide decorated on nickel hydroxide anchored on reduced graphene oxide (Ce-Ni(OH)2/rGO) composite with hexagonal structures were synthesized by facile hydrothermal method. Fourier transform infrared spectroscopy (FT-IR), highresolution transmission electron microscopy with selected area diffraction (HRTEM-SAED), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Brunauer– Emmett–Teller (BET) surface area analysis and electrochemical technology were used to characterize the composite. Due to its unique two-dimensional structures and synergistic effect among Ce2O3, Ni(OH)2 and rGO components indicated twodimensional hexagonal nano Ce-Ni(OH)2/rGO composite is promising electrode material for improved electrochemical H2O2 sensing application. From 50 to 800 μM, the H2O2 concentration was linearly proportional to the oxidation current, with a lower detection of limit of 10.5 μM (S/N = 3). The sensor has a higher sensitivity of 0.625 μA μM−1 cm− 2. In addition, the sensor demonstrated high selectivity, repeatability and stability. These findings proved the viability of the synthetic method and the potential of the composites as a H2O2 sensing option.