The brittleness of FINEMENT amorphous nanocrystalline alloys caused by annealing is an urgent problem to be solved because it limits the scope of their engineering application. We are herein to investigate the rejuvenation behavior of the as-annealed samples that not only are in a relaxed state but also the nanocrystals are precipitated in the amorphous matrix. The results show that the thermal temperature for cryogenic thermal cycling (CTC) treatment should not be larger than 483 °C in order to recover the enthalpy of relaxation. Further, the more suitable temperature for CTC treatment differs with the time that the as-annealed ribbon is employed. Meanwhile, the improvement of mechanical properties of the rejuvenated samples was examined with the help of hardness, flat plate bending, and nanoindentation experiments, and the results correspond well to the maximum of the relaxation enthalpy recovery. In addition, molecular dynamics simulations were used to visualize the changes in the local structure and found that the increased local five-fold symmetric clusters have increased the amorphousness of the amorphous nanocrystalline ribbon through CTC treatment.
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