In order to prepare high quality Mo(Si,Al)2 feedstock characterized with C40 phase, higher Al doping amount andexcellent flowability, Mo(Si1-x,Alx)2 with different Al contents (x=0, 0.1, 0.2, 0.3, 0.4, 0.5) were synthesized by self-propagatinghigh-temperature synthesis first and Mo(Si0.6,Al0.4)2 was confirmed as the suitable material through X-ray diffraction analysis. Aseries of tests with different parameters of induction plasma spheroidization were applied to improving the flowability of feedstock.Mo(Si,Al)2 feedstock with excellent flowability (26.2 s/50 g) was prepared through adding hydrogen into sheath gas and decreasingthe powder feeding rate. The composition segregation occurred in the spheroidized powder after Al consumption and oxidation. Theinhomogeneous structure of the same particle was caused by the asymmetric heating and cooling when particle passed through theplasma jet.