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NiAl is an important high temperature structural material, with a high melting point (1640°C), low density and excellent high temperature oxidation resistance. The room temperature ductility of NiAl may potentially be improved with the use of nanocrystalline grain size. However, a key question concerning the application of nanostructured NiAl is about its structural stability at high temperature. The current study is thus focused on the investigation of the structural stability of nanocrystalline NiAl using in-situ transmission electron microscopy (TEM) and differential thermal analysis (DTA).Nanocrystalline B2-NiAl was prepared by ball milling (24 hrs) from elemental Ni and Al powders. Subsequent consolidation into bulk form was performed using dynamic consolidation employing a 3-capsule plate-impact fixture at approximately 400 m/s [1-3]. Powder nanocrystalline NiAl was dispersed on a holey carbon film for TEM observation. TEM specimens of shock compacted bulk NiAl nanocrystals were prepared by cutting, polishing, dimpling and ion milling.