As-quenched and nanocrystalline HITPERM-type (Fe 1−x Co x ) 86 Hf 7 B 6 Cu 1 alloys were investigated by conventional Mössbauer spectroscopy. The spectrum of as-quenched alloy presents a typical broadened and overlapped sextet, which confirms that the as-quenched alloy in fully amorphous state. After nanocrystallization, each spectrum of the alloys studied consists of three components: crystalline phase, interface and residual amorphous matrix except x=0.8 alloy. Co addition increases the hyperfine field and the maximum value exhibits in the x=0.2 alloy. The Fe concentration in bcc-FeCo crystals and the fraction of crystalline phase influenced by Co addition are opposite. The forming of boride phases after prolonged annealing decline the soft magnetic properties of the alloy studied.