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A NiAl/TiB2 nanocomposite is synthesized by mechanical alloying elemental powders. Upon milling for a certain time, an abrupt exothermic reaction occurs and a large amount of NiAl and TiB2 compounds form simultaneously. It is suggested that two separate chemical reactions,i.e. Ni+Al →NiAl and Ti+2B→TiB2, are involved during the exothermic reaction. Additionof Ti and B to Ni-Al system impedes the structural evolution of Ni and Al powders and delays the abrupt reaction. The final products are equilibrium phases without any metastable phases formed. This type of reaction is suggested to be suitable for alloy systems with two large heatrelease reactions.