• The β-Ni(OH) 2 is synthesized by co-precipitate followed by hydrothermal treatment. • The β-Ni(OH) 2 is modified with Mg 2+ and Mn 2+ to create a superior cathode material. • Mg 2+ and Mn 2+ dopants improved the specific capacity and stability of Ni-electrode. • Mg 2+ and Mn 2+ dopants suppressed the O 2 evolution side reaction. Ni(OH) 2 is one of the most interesting electrode substances for high-performance nickel–iron batteries owing to its low cost, high specific capacitance, and environmental compatibility. However, the Ni(OH) 2 cathode electrode exhibits poor performance due to (i) competitive reactions such as the oxidation of the active material and oxygen evolution. (ii) the reduced charge acceptance of the Ni(OH) 2 positive electrode is related to a relatively long distance between the Ni(OH) 2 particles and the nearest portion of the substrate. In this study, β-Ni(OH) 2 is used as a starting material. Then, the Ni 2+ in the compound β-Ni(OH) 2 material is partially substituted with Mg 2+ and Mn 2+ , separately, and the performance of the as-prepared materials was optimized and examined. XRD, FTIR, TG-DTA, SEM/EDS, and ICP-OES confirmed the formation of the expected compositions. The Ni 0.95 Mg 0.05 (OH) 2 and Ni 0.9 Mn 0.1 (OH) 2 based-samples were optimal compositions with promising electrochemical activities. The partial substitution of Mg 2+ allowed separation of anodic/cathodic peaks and oxygen evolution. For example, the anodic and cathodic peaks are easier to identify because their potential shifted to more negative potentials. When using three-electrode configurations, the un-doped Ni(OH) 2 electrode discharge capacity showed a reduction of 76% after the 100th cycle. In contrast, the Ni 0.95 Mg 0.05 (OH) 2 and Ni 0.9 Mn 0.1 (OH) 2 electrode demonstrated a reduction of only 15% and 12% in discharge capacities after 100th cycles, respectively. When using a two-electrode configuration, the obtained discharge capacities were 40 mAh/g for the un-doped Ni(OH) 2 electrode, 120 mAh/g for the Ni 0.95 Mg 0.05 (OH) 2 electrode, and 159 mAh/g for the Ni 0.9 Mn 0.1 (OH) 2 electrode with an electrode cycle life of 43.49%, 88.24%, 88.54%, respectively.