Amorphous Mg50Ni50 alloy was produced by mechanical alloying (MA) of the elemental powders Mg and Ni using a SPEX 8000D mill. The alloyed powders were microstructurally characterized by X-ray diffraction (XRD). The thermal transformation of amorphous Mg50Ni50 into stable intermetallics (Mg50Ni50 → remaining amorphous + Mg2Ni → Mg2Ni + MgNi2) was analyzed using the Kissinger and isoconversional methods based on the non-isothermal differential scanning calorimetry (DSC) experiments. The apparent activation energies (Ea) and the transformation diagrams, temperature-time-transformation (T-T-T) and temperature-heating rate-transformation (T-HR-T), were obtained for both processes. A good agreement was observed between the calculated transformation curves and the experimental data, which verifies the reliability of the method utilized.