In the present study, mechanical alloying process was employed for preparation of the nanocrystalline (Fe85Ni15)(97)Al-3 alloy through ball mill method. The structure, mechanical properties, and magnetic behavior of the alloy at various milling times of 0, 4, 16, 32 and 64 h were studied by X-ray analysis, vibrating sample magnetometer (VSM) and scanning electron microscopy (SEM) measurements. The bcc Fe(Ni) phase was successfully formed within 32 h ball-milling. It was found that an increment in the milling time leads to higher lattice parameter while it decreases the grain size from 172 to 16 nm. Also, the VSM test results indicated that by increasing the milling time to 32 h, the saturation magnetization (M-s) and coercivity (H-c) increased. (c) 2020 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.