The study of Cu clusters is a critical research topic in the field of Fe-based nanocrystalline alloys. Herein, nanocrystalline Fe40.5Co40.5Zr7Mo2B9Cu1 alloys were prepared by annealing an as-quenched alloy. The first onset crystallization temperature (Tx1), first crystallization peak temperature (Tp1), second onset crystallization temperature (Tx2), and second crystallization peak temperature (Tp2) determined by differential scanning calorimetry were selected as annealing temperatures. The alloy subjected to annealing was investigated in terms of microstructural evolution and magnetic properties, such as Cu-specific differences between the as-quenched sample and those annealed at Tp1 and Tp2. The as-quenched alloy was amorphous and featured a uniform elemental distribution and composition comparable with the nominal one. In the alloy annealed at Tp1, the Co content of nanocrystals was similar to that of the residual amorphous matrix, whereas the Cu distribution was heterogeneous and characterized by clusters with sizes less than 7 nm. The alloy annealed at Tp2 exhibited fewer but larger Cu clusters and higher Co contents in Fe-deficient areas. Furthermore, lower Co contents were observed in Fe(Co) grains, and Cu nanocrystals were not detected by transmission electron microscopy. With increasing temperature, coercivity decreased and then increased, whereas specific saturation magnetization increased and then decreased.
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