High-energy ball milling and powder metallurgy methods were used to produce a partially alloyed nickel and molybdenum of γ-Ni₃Mo composition (Ni-25at.%Mo). Milled powders were cold-compacted, sintered/solutionized at 1300°C for 100h sintering followed by quenching. Three transformation studies were performed. First, the intermetallic γ-Ni₃Mo was formed from the supersaturated solution at temperatures ranging between 600°C and 900°C for up to 100h. The 100% stable γ-Ni₃Mo phase was formed at 600°C after 100h, while aging at temperatures ranging between 650°C and 850°C for 25h was not sufficient to complete the transformation. The δ-NiMo phase was observed only at 900°C as cellular and basket strands precipitates. Second, the reversed peritectoid transformation from γ-Ni₃Mo to α-Ni and δ-NiMo was performed. Supersaturated solid solution samples were first aged at 600C for 100h followed by quenching to form the equilibrium γ-Ni₃Mo phase. After that, the samples were heat treated between 910°C and 1050°C for up to 10h followed by quenching. Regardless of heat-treatment temperature, samples heat-treated for shorter times exhibited small precipitates of δ-NiMo along and within grain boundaries of α-Ni phase, and it coarsened with time. Third, the transformation from the supersaturated solution α-Ni to the peritectoid two-phase region was performed. The samples were aged between 910°C and 1050°C for up to 10h followed by quenching. Precipitates of δ-NiMo were observed in the α-Ni matrix as small particles and then coarsened with aging time. In all three cases, hardness values increased and peaked in a way similar to that of traditional aging, except that the peak occurred much rapidly in the second and third cases. In the first case, hardness increased by about 113.6% due to the development of the new phases, while the hardness increased by 90.5% and 77.2% in the second and third cases, respectively. / Master of Science