Abstract The sequence of structural transformations of amorphous alloys Fe53.3Ni26.5B20.2 and Co28.2Fe38.9Cr15.4Si0.3B17.2 during heat treatment in a wide temperature range was studied by transmission electron microscopy and differential scanning calorimetry. The response of mechanical properties (plasticity, hardness, crack resistance) during transition from an amorphous to a crystalline state was investigated. The nature of discovered embrittlement phenomenon and plasticizing effect in amorphous alloys during annealing was discussed.