In this research, samples of an alloy with a bimodal structure were studied on the basis of a previously developed technology for obtaining hydrogen storage materials based on the Ti-Al-Nb system. The results of SPS of mechanically activated powder mixtures of the Ti-Al-Nb system at a temperature of 1300 °C make it possible to obtain an alloy with a predominantly bimodal structure. However, an insignificant presence of TiAl3, AlNb2 phases, and unreacted niobium is still observed in the structure. The mechanical properties of alloys of the Ti-Al-Nb system after sintering show abnormally low values of strength and ductility (less than 150 MPa). Two-stage heat treatment of alloys of the Ti-Al-Nb system leads to the decomposition of large precipitates of TiAl3 with the formation of O-phase nuclei, as well as to the complete dissolution of unreacted niobium and AlNb2 phases. Heat treatment of alloys of the Ti-Al-Nb system contributes to an increase in its strength by approximately 10 times (1310 MPa, MA-180), and ductility by 2 times (1322 MPa, MA-20). The surface fracture of samples obtained after testing is characterized by intergranular (intercrystalline) brittle fracture with “river” or “step” features.