Fe84Zr7B9 amorphous alloy prepared by a single-roller rapid quenching method was annealed under different heat treatment conditions (different annealing temperatures, heating rates, and vacuum pressure in the cooling process). The different heat treatment conditions result in different crystallization process. The different vacuum pressures used during cooling resulted indifferent distributions of Fe, Zr, and B in the crystallization phase, thus affording completely different crystalline phases. After low-temperature heat treatment, the saturation magnetization of the alloys treated with continuous vacuum is higher than that of the alloys treated without continuous vacuum, and the coercivity values of the alloys treated with and without continuous vacuum were similar. After high-temperature heat treatment, the saturation magnetization and the coercivity values of the alloys treated without continuous vacuum are higher than those of the alloy treated with continuous vacuum.