Combustion of powder mixtures under adiabatic conditions -Self-propagating High-temperature Synthesis (SHS)-is an efficient and attractive technique to synthesize a host of materials for high technology applications, namely, ceramics, intermetallics, composites and functionally graded materials. Conditions necessary for and general features of this technique are briefly reviewed. Experimental investigations on synthesis of nickel monoaluminide from stoichiometric mixtures of component powders by this technique using plane-wave propagation mode is carried out. Effects of reaction parameters namely, bulk density of compacts, amount of inert dilutions and atmospheres on velocity of combustion wave propagation and combustion peak temperature are investigated. From the dependence of propagation velocity on combustion temperature an activation energy of 170.99 kJ/mole is obtained for SH-synthesis of NiAl. The synthesized products showed equiaxed large grained microstructures.