Lee Chung-Hyo
J Nanosci Nanotechnol. 2017 Apr;17(4):2453-456. doi: 10.1166/jnn.2017.13363.
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.
我们已应用机械合金化(MA)工艺,使用元素Fe₂O₃–Al粉末混合物来生产软磁复合材料。通过X射线衍射、差示扫描量热仪和振动样品磁强计测量,研究了获得具有精细微观结构的软磁α-Fe/Al₂O₃复合材料的最佳球磨和烧结条件。结果发现,球磨5小时的α-Fe/Al₂O₃复合材料中α-Fe的平均晶粒尺寸估计在50nm范围内。球磨粉末的饱和磁化强度在机械合金化30分钟后显示出最大值88emu/g,并在机械合金化5小时后达到77emu/g。还观察到由于球磨导致α-Fe晶粒尺寸减小而引起的磁硬化现象。在火花等离子烧结(SPS)机中于1000°C和1100°C对球磨粉末进行致密化处理。场发射扫描电子显微镜(FE-SEM)观察表明,在1000°C烧结的α-Fe/Al₂O₃复合材料中α-Fe的平均晶粒尺寸在100nm范围内,这与通过所谓的霍尔图估计的值几乎相同。还可以看出,在1000°C烧结的SPS样品的矫顽力仍高达92奥斯特(Oe),这表明在SPS过程中磁性α-Fe相的晶粒生长趋于受到抑制。