Fe 68 Zr 20 B 12 amorphous alloy prepared by mechanical alloying technique of 60 h of duration was annealed at different temperatures (420-720• C) during 1 h. Microstructure and magnetic property of as-milled and annealed alloy were investigated by X-ray diffraction, transmission electron microscopy, the Mössbauer spectroscopy and vibrating sample magnetometer techniques. Fe 68 Zr 20 B 12 powders milled during 60 h exhibit amorphous character. After annealing at 420• C, α-Fe phase precipitates from amorphous matrix. Transmission electron microscopy analysis shows the nucleation and growth of α-Fe grains. The Mössbauer results of the annealed alloy at 670• C show that the Fe 3 B phase precipitates already and there is still remaining amorphous phase. Coercivity increases with increasing annealing temperature, which is closely related to the microstructures after annealing.
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