Inconel-718 superalloy with a nominal composition of Ni-19.47Fe-18Cr-0.5Al-1Ti-5 Nb-3Mo-0.02Co-0.003B was synthesized by mechanical alloying of elemental powders. Mechanical alloying was carried out in a high energy Simoloyer attritor ball mill. A sufficient quantity of powder was removed at milling intervals of 0, 2, 4, 6, 8, 10, 12, 14, 16, 18, 20, and 22 h for characterization by XRD, SEM, and TEM. The dissolution time of different alloying elements have been discussed in view of their atomic scattering factors and Hume-Rothery principle with the help of XRD and TEM (SAED) analysis. Complete dissolution of Fe took place at 6 h of milling, Nb at 10 h, Cr at 18 h while Mo took 22 h. A complete single-phase solid solution of γ(FCC) matrix was obtained at 22 h of milling. Crystallite size was found to decrease while the lattice parameter increased with milling time. Lattice-strain and dislocation density increased initially and later decreased due to the dynamic recrystallization process taking place within the powder particles during milling. SEM analysis indicated flattening of powder particles during the initial (0 h–4 h) stages of milling followed by heavy cold-welding at the intermediate stages (6 h–12 h). In the final stages of milling (18 h–22 h), an equilibrium between cold welding and fracturing was reached.