NiAl intermetallic compound was synthesized by mechanical alloying of elemental mixtures of Ni and Al powders in a Spex mill. The compound formation took place according to a mechanically induced self-propagating reaction (MSR), and the influence of milling variables on its ignition time was determined using a factorial design. Results indicated ignition time as a function of initial particle size of Ni, process control agent, and ball-to-powder ratio. Also, an interaction between ball-to-powder ratio, process control agent, and a set of balls was found to control the average particle size of as-milled powders. (c) 2011 Elsevier B.V. All rights reserved.