Fine TiAl and NiAl powders have been synthesized by SHS with a reduction stage. Explored was the effect of green composition, stoichiometric ratio, and additives on the particle size, morphology, and phase composition of resultant powders. Addition of NaCl and excessive Mg was found to suppress crystallization. In the presence of heat-generating additives, such as Mg(ClO4)2 and CaO2, the synthesized powders had a particle size of below 3 μm. The morphology and phase composition of synthesized NiAl powders were investigated upon variation in the Al content of green mixture.