This paper investigates the structural, microstructural and magnetic properties of amorphous/nanocrystalline Fe32.5Co32.5Nb35 powders prepared by high-energy milling. The ball-milling of Fe, Co and Nb powders leads to alloying the element powders and the amorphous structure up to 96 h. The results showed that the coercive force increases as the milling time increases. Furthermore, the saturation magnetization decreases as a result of the electronic interactions between magnetic and nonmagnetic elements. After a suitable heat treatment the coercivity decreases and the magnetization increases noticeably. (C) 2012 Elsevier B.V. All rights reserved.