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Fe75Co5Zr10B10 amorphous alloy prepared by melt-spinning was annealed at various temperatures. The thermal property and microstructures were investigated by dierential thermal analysis, X-ray diraction, and transmission electron microscopy. The crystallization process of Fe75Co5Zr10B10 amorphous alloy is complex. The α-Fe phase precipitates from the amorphous matrix in the initial stage of crystallization. The α-Mn type (χ) phase precipitates at 570• C, but transforms to α-Fe phase and the Laves C14(λ) phase at higher temperature. In the nal stage of crystallization, Fe3Zr, Fe2Zr, and unknown phases are observed and the λ-phase disappears. The α-Fe phase preferentially nucleates after annealing at 530• C for 10 min and the χ-phase preferentially nucleates after annealing at 600• C for 10 min. The nucleation barrier of χ-phase is larger than that of α-Fe phase. The local structure of χ-phase is more similar to amorphous phase.