Preparation and electromagnetic properties of high silicon steel soft magnetic composite cores by FCVD-SPS
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摘要: 采用流化气相原位沉积结合放电等离子烧结工艺成功制备了高硅钢软磁复合铁芯Fe-6.5% Si/SiO2（质量分数），并系统研究了复合铁芯微观结构与电磁性能的关系。结果表明，高硅钢软磁复合铁芯中的Fe-6.5% Si颗粒被SiO2绝缘层均匀并且致密的包围，Fe-6.5% Si/SiO2复合铁芯表现出高磁感、高电阻率、良好的频率稳定性、低矫顽力、以及低铁损等优异的电磁特性，饱和磁感应强度为175 emu·g-1，矫顽力为15 Oe，相对磁导率为350（80 kHz），电阻率为8.6×10-5?·m，0.2 T、5 kHz外场下铁损仅为11.8 W·kg-1。Abstract: The high silicon steel soft magnetic composite cores (Fe-6.5%Si/SiO2 by mass) were successfully prepared by fluidized in-situ chemical vapor deposition combined with the following spark plasma sintering process. The dependence of microstructures on the electrical and magnetic properties of Fe-6.5%Si/SiO2 composite cores was investigated. The results indicate that, most of the conductive Fe-6.5%Si particles are firstly coated with SiO2 in chemical vapor deposition, and then the highly compact and insulated Fe-6.5%Si/SiO2 composite cores are quickly obtained in the next spark plasma sintering. The as-prepared Fe-6.5%Si/SiO2 composite cores display the excellent electromagnetic properties as the saturation magnetization of 175 emu·g-1, the coercivity of 15 Oe, the relative permeability of 350 at 80 kHz, the electrical resistivity of 8.6×10-5?·m, and the core loss of 11.8 W·kg-1 at the magnetic field of 0.2 T and 5 kHz.
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图 1 流化气相原位沉积工艺制备Fe–6.5%Si/SiO2粉末流程
Figure 1. Preparation technology illustration of Fe–6.5%Si/SiO2 powders by FCVD
图 2 原料及流化气相原位沉积后Fe–6.5%Si合金粉末扫描电子显微形貌：（a），（b）流化气相原位沉积前原料粉末；（c）（d）流化气相原位沉积后合金粉末
Figure 2. SEM images of Fe–6.5%Si alloy powders before and after FCVD: (a), (b) Fe–6.5%Si alloy raw powders before FCVD; (c), (d) Fe–6.5%Si alloy powders after FCVD
图 3 Fe–6.5%Si合金粉末在流化气相原位沉积前后的X射线衍射图谱
Figure 3. XRD patterns of Fe–6.5%Si alloy powders before and after FCVD
图 4 无SiO2包覆Fe–6.5%Si软磁铁芯和Fe–6.5%Si/SiO2软磁铁芯的截面扫描电子显微形貌和X射线衍射图谱：（a）无SiO2包覆Fe–6.5%Si软磁铁芯截面显微形貌；（b）Fe–6.5%Si/SiO2软磁铁芯截面显微形貌；（c）X射线衍射图谱
Figure 4. Cross-section SEM images and XRD profiles of Fe–6.5%Si cores and Fe–6.5%Si/SiO2 composite cores: (a) cross-section SEM images of Fe–6.5%Si cores; (b) cross-section SEM images of Fe–6.5%Si/SiO2 composite cores; (c) XRD patterns
图 5 退火后无SiO2包覆Fe–6.5%Si软磁铁芯和Fe–6.5%Si/ SiO2软磁复合铁芯磁滞回线
Figure 5. Hysteresis loops of Fe–6.5%Si cores and Fe–6.5%Si/ SiO2 composite cores after annealing
图 6 退火后无SiO2包覆Fe–6.5%Si软磁铁芯和Fe–6.5%Si/ SiO2软磁复合铁芯的相对磁导率随测试频率变化趋势
Figure 6. Relative permeability with frequency of Fe–6.5%Si cores and Fe–6.5%Si/SiO2 composite cores after annealing
表 1 流化气相原位沉积前后Fe–6.5%Si合金粉末表面成分
Table 1. Surface chemical compositions of Fe–6.5%Si alloy powders before and after FCVD
% 元素 流化气相原位沉积前原料粉末表面成分/% 流化气相原位沉积后粉末表面成分/% 质量分数 原子数分数 质量分数 原子数分数 Fe 92.77 86.58 82.68 63.72 Si 7.23 13.42 8.89 13.63 O 0 0 8.43 22.65 总计 100 100 100 100 
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表 2 无SiO2包覆Fe–6.5%Si软磁铁芯、Fe–6.5%Si/SiO2软磁复合铁芯和JFE生产的传统Fe–6.5%Si软磁铁芯电磁性能比较
Table 2. Electric and magnetic characteristics of Fe–6.5%Si cores, Fe–6.5%Si/SiO2 composite cores, and Fe–6.5%Si alloy cores by JFE
分类 厚度/ mm 电阻率/ (Ω·m) 铁损，Wi/j* / (W·kg; -1) W1/50 W1/400 W1/1 k W0.5/2 k W0.2/5 k 无SiO2包覆Fe–6.5%Si软磁铁芯 10 9.7 × 10;-7 21.7 108.2 358.4 248.2 191.3 Fe–6.5%Si/SiO2软磁复合铁芯（本实验） 10 8.6 × 10;-5 1.6 11.2 36.8 22.4 11.8 传统Fe–6.5%Si软磁铁芯（JFE） — — 1.2 14.5 51.6 29.1 17.9 *Wi/j是指在外场强度i（单位：T）、外场频率j（单位：Hz）条件下测试材料的铁损值。
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