The crystallization behavior of an Fe73.5Cu1Nb3Si13.5B9 alloy was studied by differential scanning calorimetry. Two crystallization peak temperatures at infinitesimal heating rate were obtained to be 769 K (Tx1) and 910 K (Tx2), respectively. The associated activation energies by means of Kissinger’s peak shift method were obtained to be 340 and 428 kJ/mole, respectively. Initial permeability (μi) and Q values versus temperature was in situ investigated in the range from 300 to 873 K by a specially designed setup on toroid ribbon cores. Their variations with temperature reveal corresponding changes in magnetization and nanocrystallization, etc. Anomaly μi peaks at 428 K in the cooling curve instead of at room temperature. By isothermal annealing at 823 K, precipitous maxima in μi and Q appear at about 50 min. This in situ method may be too powerful to work out optimal annealing processes for a specific nanocrystalline alloy.

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