A new nanocrystalline Fe71B23Nb6 alloy powder was prepared by mechanical alloying. The phase transformation and morphological and microstructural properties of the as-prepared alloy were investigated by scanning electron microscopy, laser granulometry, and X-ray diffraction with respect to the milling time (0- 200 h). During the milling process, it was observed that the dissolution of Nb and B atoms into the Fe matrix formed solid solutions of Fe (Nb), Fe (B), Fe23B6, Fe2B, and Fe (Nb, B). Moreover, the insertion of B atoms into the Nb network generated the Nb (B) phase. Furthermore, the minimum crystallite size was measured as approximately 1 nanometer. In addition, the dislocation density gradually increased with the extension of the milling time, and the crystallization of the partially amorphous phase occurred after 200 h of milling.
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