Electroplating nickel-63, a radioactive isotope used in betavoltaic batteries and random number generators, requires precise control due to its limited availability and the generation of radioactive waste. To minimize waste and ensure effective plating, small plating baths are employed, optimizing the process within constrained conditions. X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS) were utilized to determine the optimal plating conditions and limiting conditions for nickel electroplating in a small plating bath. This study focuses on the use of low-concentration nickel solutions and small plating equipment, in contrast to the common industrial practice of using high concentrations of nickel. Here, it is important to optimize the plating parameters, especially the nickel concentration, current density, and bath temperature. An average thickness of 1.8 μm was found when plating with a nickel concentration of 0.06 M, a current density of 5 mA/cm2, and a solution temperature of 40 °C, while ideal conditions were found to achieve the theoretical maximum energy and 90% release rate when plating with nickel-63 instead of Ni.