In the present study, mechanical alloying process was employed for preparation of the nanocrystalline Ni50Al50 alloy through ball mill method. The structure properties of the alloy at various milling times of 0, 2, 4, 6 and 8hr were studied by X-ray diffraction and scanning electron microscopy (SEM) measurements. Several phases was formed successfully after 4hr of milling. At 6hr of milling, new intermetallic compound type (Ni3AI) was observed prospering, The particle size for various milling times decreased significantly, with increasing time of milling. The resulted morphology the milled powder shows a reduction of particle size which is in accordance with the XRD patterns. The results of EDX shows clearly atypical spectrums of both Ni and Al peaks.