Cadmium is an industrially applied plating metal used in aerospace applications, but electrodeposition of cadmium is toxic, and current production method will soon be banned. Therefore, electrodeposition of alternative alloys in environmentally friendly solutions is an attractive research area. An additive‐free, nonaqueous, deep eutectic solvent (DES) containing Ni and Zn halide salts is developed in a greener environmental method. Gamma‐phase nanocrystalline Ni2Zn11 is coated onto hot‐rolled mild steel via pulse reverse current (PRC) in the developed nonaqueous solvent. The employed DES’ relatively low viscosity and sufficient conductivity enable the simultaneous reduction of Ni2+ and Zn2+ cations on microelectrode. Electrochemical quartz crystal microbalance (eQCM) analysis proves the absence of the commonly reported problem of electrode blocking during electrodeposition, revealing an efficiency of 86.07%. Appropriate PRC parameters are applied for scaled macroelectrode deposition. The plating profile exhibits 20 μm‐thick alloy deposition without cracks around 3 h. Scanning electron microscopy–electron‐dispersive spectroscopy and X‐ray diffraction analyses reveal that 15.5 wt% Ni is in the nanograin phase, and all crystal planes belong to the γ‐Ni2Zn11 phase, which is needed as an alternative to cadmium plating. Hardness and corrosion tests performed on the γ‐Ni2Zn11 coating reveal better hardness and corrosion resistance with supporting morphological evidence.