The alloy composition Mo–37Si–40Ti (at.%) was synthesized by arc melting in order to obtain nearly single-phase (Mo,Ti) 5 Si 3 . At 750–1300°C, the intermetallic compound was found to be superior to both single-phase Mo 5 Si 3 and single-phase Ti 5 Si 3 with regard to oxidation resistance. Upon oxidation, formation of a protective SiO 2 –TiO 2 duplex scale was observed, which dramatically reduces outward diffusion of Ti. The results indicate that Ti alloying is a promising concept to further improve oxidation resistance of Mo-based alloys such as Mo–Si–B.