Aluminum-based metallic glasses are the new promising family of materials. However, the effect of heat treatment on the structure and properties of Al–Y–Ni–Co amorphous alloys has not been widely studied so far. In this paper, Al85Y8Ni5Co2 amorphous alloy strips were obtained by hardening on a rotary copper wheel. The effect of vacuum annealing at temperatures ranging from 100 to 500 °C for 30 minutes on the structure and hardness of these strips was investigated. Transmission electron microscopy, X-ray diffraction analysis, and differential scanning calorimetry were used to study changes in the structure of strips after heat treatment. Vickers microhardness was measured to investigate the effect of annealing on the mechanical properties of strips. The results obtained allowed for the conclusions made about changes in hardness depending on the Al85Y8Ni5Co2 alloy strip structure. It was found that as the temperature rises, strip microhardness increases reaching a maximum value of 575±7 HV after annealing at 350 °C, then it decreases with a further increase in the annealing temperature. It was shown that the Al85Y8Ni5Co2 alloy strips remain completely amorphous and no crystalline phases are detected in their structures after annealing at temperatures up to 250 °C for 30 minutes. A sharp increase in hardness after annealing at 350 °C is associated with 10–30 nm nanocrystals of an aluminum solid solution formed in the amorphous matrix and surrounded by a residual amorphous matrix, while further hardness decrease is associated with the increasing sizes of these crystals and Al3Y and Al19Ni5Y3 intermetallics formed in the structure.
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