In this paper, the thermodynamic properties of nanocrystalline Ni3Al-based alloys prepared by mechanical attrition are reported. A broad exothermic transformation occurs on heating the nanocrystalline samples. The stored energy of cold work has been evaluated by measuring the enthalpy release during heating. The values obtained far exceed the energies achieved by conventional deformation processes. The specific heat increases by more than 5%, indicating changes in the vibrational and configurational part of the entropy. © 1993.