Amorphous Fe 73.5 Cu 1 Nb 3 Si 13.5 B 9 , Fe 5 Co 70 Si 15 B 10 and Pd 81 Cu 7 Si 12 alloys, produced by superfast quenching from the melt followed by fast heating to 723–923 K and soaking for 10 s in vacuum were investigated. The crystallization of an amorphous Fe 73 Ni 0.5 Cu 1 Nb 3 Si 13.5 B 9 alloy was determined by methods of transmission electron microscopy (in situ). The Fe 73.5 Cu 1 Nb 3 Si 13.5 B 9 alloy annealed at 923 K for 10 s produces a grain size of 6 nm, with phases α-FeSi13 at.%, (FeNb) 2 B, and (FeNb)B. An Fe 5 Co 70 Si 15 B 10 alloy annealed at 923 K for 10 s produces a grain size of 25 nm, with phases - α-Fe, α-Co, β-Co, Fe 3 Si, Co 2 Si, and (FeCo) 2 B. A Pd 81 Cu 7 Si 12 alloy annealed at 823 K for 10 s produces a grain size of 25 nm, with phases - Pd, Pd-Cu(γ), Pd 5 Si, i-Pd x Si.