Abstract <p>Electroless nickel plating (ENP) is a crucial surface treatment process for metallic hardware on satellite launch vehicles, enhancing hardness, wear resistance, and corrosion resistance. Even minor variations in plating conditions can significantly alter the ENP’s mechanical properties in combating harsh environments that are experienced during the integration and flight conditions. This research work aims to optimize the process parameters of ENP in the gas cylinders of control systems for Launch vehicles made of M250 grade Maraging steel, using the least resources and time. As the initial step, the significantly influenced process parameters were identified, and their narrower ranges were determined using the one-variable-at-a-time (OVAT) approach. In this study, the energy dispersive X-ray fluorescence (EDXRF) method was experimented with to determine the coating thickness of specimens, among other destructive, nondestructive, and dimensional methods. The EDXRF method proved to be the most accurate and consistent, comparable to microscopy, and was employed as a reliable means of assessing coating thickness for all subsequent trials. A fractional factorial design (FFD) was employed to model the optimization process, followed by a rigorous assessment of coating thickness. The optimization model was validated by the accomplishment of the required thickness within the specified range with the required measurement accuracy. The capability and characteristics of the coating, as determined by the model, were reconfirmed through energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), and scanning electron microscopy (SEM) imaging and analysis. This comprehensive validation process instills confidence in the results, especially in the context of the inhospitable pre-launch and in-flight environments of the component.</p>