Synthesis and Spark Plasma Sintering of Soft Magnetic Composite in a Fe₂O₃–Al System by Mechanical Alloying.
We have applied mechanical alloying (MA) to produce soft magnetic composite material using a mixture of elemental Fe₂O₃–Al powders. An optimal milling and sintering conditions to obtain soft magnetic α-Fe/Al₂O₃ composite with fine microstructure were investigated by X-ray diffraction, differential scanning calorimeter and vibrating sample magnetometer measurements. It is found that the average grain sizes of α-Fe in α-Fe/Al₂O₃ composite ball-milled for 5 hours is estimated to be in the range of 50 nm. The saturation magnetization of ball-milled powders showed a maximum value of 88 emu/g after 30 min. of MA and reaches to 77 emu/g after 5 h of MA. The magnetic hardening due to the reduction of the α-Fe grain size with ball milling was also observed. Densification of the ball-milled powders was performed in the spark plasma sintering (SPS) machine at 1000 °C and 1100 °C. FE-SEM observation shows that the average grain size of α-Fe in α-Fe/Al₂O₃ composite sintered at 1000 °C is in the range of 100 nm, which is nearly same value estimated from the so-called Hall plot. It can be also seen that the coercivity of SPS sample sintered at 1000 °C is still high value of 92 Oe, suggesting that the grain growth of magnetic α-Fe phase during SPS process tends to be suppressed.