Synthesis of α-Mo–Mo5SiB2–Mo3Si nanocomposite powders by two-step mechanical alloying and subsequent heat treatment

A two-step mechanical alloying process followed by heat treatment was developed as a novel approach for fabrication of Mo–12.5 mol%Si–25 mol%B nanocomposite powders. In this regard, a Si–43.62 wt.% B powder mixture was milled for 20 h. Then, Mo was added to the mechanically alloyed Si–B powders in order to achieve Mo–12.5 mol%Si–25 mol%B powder. This powder mixture was further milled for 2,5,10 and 20 h. All of the milled powders were annealed at 1100 °C for 1 h. After first step of milling, a nanocomposite structure composed of boron particles embedded in Si matrix was formed. On the other hand, an α-Mo/MoSi2 nanocomposite was produced after second step while no ternary phases between Mo, Si and B were formed. At this stage, the subsequent annealing led to formation of α-Mo and Mo5SiB2 as major phases. The phase evolutions during heat treatment of powders can be affected by milling conditions. It should be mentioned that the desirable intermetallic phases were not formed during heat treatment of unmilled powders. On the other hand, α-Mo–Mo5SiB2–Mo3Si nanocomposites were formed after annealing of powders milled for 22 h. With increasing milling time (at the second step), the formation of Mo3Si during subsequent heat treatment was disturbed. Here, an α-Mo–Mo5SiB2–MoSi2 nanocomposite was formed after annealing of 30 and 40 h milled powders.

► α-Mo–MoSi2 nanocomposite was produced after double step mechanical alloying.
► Heat treatment of unmilled powders led to the formation of small Mo2B phase.
► Heat treatment of double step MAed powders led to the formation of Mo5SiB2 phase.
► α-Mo–Mo5SiB2–Mo3Si nanocomposite was formed after heat treatment of 22 h MAed powder.
► α-Mo–Mo5SiB2–MoSi2 nanocomposite was formed after heat treatment of 30 h MAed powder.