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The complete identity of a second-phase precipitate detected by transmission electron microscopy in combustion-synthesized NiAl was established. The crystal structure, including the point group, the space group and the lattice parameters, was determined by convergent and selected-area electron diffraction techniques. Energy dispersive X-ray spectroscopy was used for the determination of the chemical composition. Analysis established the phase to be the solid solution of NiO in Al2O3 and presented evidence of the hitherto unreported room-temperature solubility.