A comprehensive analysis was conducted to examine the crystal phase composition, surface and cross-section morphology, elemental composition, thickness, and corrosion resistance of coatings. X-ray diffraction (XRD) was employed to investigate the texture and crystal phase of the materials while scanning electron microscopy (SEM) and energy-dispersive spectroscopy (EDS) were utilized to assess the surface and cross-section structure. Additionally, electrochemical techniques were employed to evaluate the corrosion performance. Compared to DC electroplating, the corrosion potential of pulsed galvanized ferroalloy alloy coating increased from −1031 mV to −1008 mV, and the corrosion current density decreased from 3.122 × 10⁻⁵ A∙cm⁻² to 0.321 × 10⁻⁵ A∙cm⁻². Moreover, the corrosion rate value of the coating obtained by the pulse rectifier (0.386 × 10⁻⁵ g m⁻² h⁻¹) was lower than that obtained by the DC power supply (3.75 × 10⁻⁵ g m⁻² h⁻¹). Additionally, pulsed electrodeposition reduced the iron content of the coating by 0.7%, thereby enhancing its corrosion resistance and flatness. The impedance parameters of the zinc–iron alloy coating acquired through the 30% duty cycle monopulser process exhibit superior performance compared to DC electroplating. Evidently, the monopulse coating’s structure enhances crystal packing density, augments coating thickness, improves adhesion to the substrate interface, and optimizes grain distribution uniformity. These factors are crucial determinants of the corrosion behavior exhibited by Ze–Fe coating.

In this study, pre-treated low-carbon steel substrates were electroplated with Zinc–Nickel (ZN) alloy composite coatings enhanced by the incorporation of nano-silicon dioxide (SiO₂) particles in an alkaline solution. ZN deposits with varying concentrations of nano-SiO₂—specifically, 1, 2, 3, 5, and 10 wt%—were achieved by adjusting the ratio between the nano-SiO₂ and ZN alloy electroplating solutions. The influence of the nano-SiO₂ content on both the quality of the coating and its corrosion behavior was investigated in detail. Scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), and an atomic force microscope (AFM) were utilized to assess the surface, cross-section structure, elemental composition, and thickness of the coatings. Notably, the addition of nano-SiO₂ improved the microstructure of the coating, leading to a reduction in grain size as well as enhancements in uniformity and density while revealing that co-deposition reached an optimal concentration at 3 wt% nano-SiO₂. The corrosion behavior of coated specimens was evaluated through electrochemical impedance spectroscopy (EIS) and polarization techniques within a 3.5 wt% NaCl solution serving as a corrosive medium. Specifically, for typical prepared coatings, the corrosion current density decreased from 1.410 × 10⁻⁴ A·cm⁻² to 5.762 × 10⁻⁶ A·cm⁻², which is a remarkable reduction by one to two orders of magnitude relative to the SiO₂-free coatings mentioned previously. These findings provide a straightforward approach for selecting 3 wt% nano-SiO₂ as an effective additive in ZN composite coatings.