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Third generation γ-titanium aluminides with nominal compositions Ti–45Al–5Nb–0.2B–0.2C and Ti–45Al–10Nb–0.2B–0.2C were investigated to identify the phase transformation and their morphological stability with temperature. Electron microscopy and differential scanning calorimetry were employed for the characterization of phases and for recording the corresponding transformations, respectively. It has been inferred that the order–disorder transformation temperatures α2 → α increased with increasing Niobium (Nb), while the α-transus temperature decreases. The stability of the microstructure for both alloys with temperature were also investigated. Mass change measured for the heating rates 20 °C s−1 and 30 °C s−1 reveals that the alloy Ti–45Al–10Nb–0.2–0.2C shows stability up to 1100 °C, and the alloy Ti–45Al–5Nb–0.2B–0.2C is stable up to 900 °C. The orientation relationship between the phases indicates that with the change in shape of the α phase from lamellar to equiaxed, it deviates from the Blackburn orientation relationship.