In this research, we reported facile synthesis of efficient \(Ni_3Fe\) electrocatalyst nanostructures deposited on conducting carbon fibers surface by a simple chemical bath deposition method at moderate temperature. The composition, phase and electrocatalytic property of as-prepared binder-free electrocatalyst was characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and electrochemical measurements. The as-synthesized \(Ni_3Fe@t-CF\) presented excellent performance and durability as water oxidation electrocatalyst in alkaline electrolyte owing to non-segregated deposition of \(Ni_3Fe\) nanostructures on conducting surface of carbon, high electrochemical surface area, and the fast absorption and desorption of water molecules during oxygen evolution reaction due to the \(3D\) architecture of conducting interlaced carbon fibers template.