NANOPERM-type alloy Fe76Mo8Cu1B15 is investigated in amorphous and in partially crystallized state. Samples were prepared by 1 h isothermal annealing in vacuum at temperatures ranging from 330 °C up to 700 °C. Bulk and surface microstructural characteristics were studied using transmission and conversion electron Mössbauer effect techniques, respectively. Surface features were checked by the help of atomic force microscopy. Presence of nanocrystalline bcc-Fe phase was detected during the first crystallization stage. The crystallization process starts at 450 °C and it is more pronounced in surface regions than in the bulk. With progressing crystallization, hyperfine parameters especially of the amorphous residual phase are altered. Distinctions in surface morphology are revealed between wheel and air side of the ribbon-shaped samples.