Silicides, known for their exceptional oxidation resistance at high temperatures, are promising materials for advanced applications. Among them, MoSi₂ and Ti₅Si₃ stand out. In this study, a Ti29Mo18Si53 composition was selected to produce a MoSi2-40 wt%Ti5Si3 composite via mechanically activated self-propagating high-temperature synthesis (MASHS). Elemental powders were milled, synthesized in a tubular furnace, and sintered using spark plasma sintering (SPS). The resulting (Ti0.8, Mo0.2)Si2-MoSi2-Ti5Si3 composite maintained stability through sintering, achieving 99 % of its theoretical density, a hardness of 10.9 ± 0.4 GPa, and a fracture toughness of 5.11 MPa m0.5. To evaluate processing effects a second sample, prepared under similar condition but with concurrent synthesis and sintering in the SPS, achieved 97 % density, 7.1 ± 0.5 GPa hardness, and 4.97 MPa m0.5 fracture toughness. Additionally, pure Ti₅Si₃ and MoSi₂ were synthesized separately via MASHS, mixed to form a MoSi₂-40 wt% Ti₅Si₃ composite, and then consolidated by SPS. This composite reached 96 % density, 11 ± 0.6 GPa hardness, and 3.8 MPa m0.5 fracture toughness. Moreover, the (Ti₀.₈Mo₀.₂)Si₂-MoSi₂-Ti₅Si₃ composite demonstrated superior oxidation resistance compared to Ti₅Si₃ and similar to monolithic MoSi₂ up to 1000 °C.
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