In the present work, nickel-iron layered double hydroxide was prepared by the hydrothermal method. The synthesized electrocatalyst was studied using X-ray diffraction pattern, infrared spectroscopy, nitrogen absorb-desorption, and scanning electron microscopy. The results confirmed the synthesis of a high surface area electrocatalyst. In the next step, the electrocatalytic activity of the synthesized sample was investigated by dropping the sample on the glassy carbon electrode at neutral media. The voltammetric results show a decrease in the onset potential and overpotential of hydrothermal nickel-iron layered double hydroxide in compared to the nickel-iron layered double hydroxide which was synthesized by the co-precipitation method. High surface area, low onset potential, high stability, and repeatability are the prominent features of this electrocatalyst.