The Ag-Ni films have attracted the attention of material scientists and researchers due to its applications as magnetic materials, catalyst, optical materials, etc. In the bulk, the formation of a single-phase solid solution of the Ag-Ni alloy film is difficult due to the large differences in the atomic size and the positive enthalpy of mixing. However, the immiscibility in the Ag and Ni constituents is diminished in the nanosized level. The electrodeposition method has established itself as a most suitable method for synthesis of single-phase Ag-Ni alloy films due to its time efficiency, cost-effectiveness, and ability to mass production of single-phase solid solutions. In this method, the miscibility of alloying elements (i.e., Ag and Ni) and the quality of the Ag-Ni film can also be easily controlled by tuning the electrodeposition process parameters such as the magnitude of the applied current density, temperature of the electrolyte, additives in electrolytes, etc. This chapter presents a detailed overview of the process parameters affecting the miscibility, morphology, and the quality of the single solid solution of Ag-Ni film. Furthermore, the nucleation and growth mechanism of Ag-Ni film and the effect of the curvature of the deposited film's particles in the miscibility of the Ag and Ni elements have also been discussed in detailed.