超低损耗FeSiAl磁粉芯的制备与性能

蹇汉杰; 鲍康馨; 孙旗; 王力; 盛汝昌; 赵利明; 冒爱琴; 郑翠红

超低损耗FeSiAl磁粉芯的制备与性能

1.
安徽工业大学, 材料科学与工程学院, 马鞍山 243002
2.
马鞍山新康达磁业有限公司, 马鞍山 243002

基金项目: 安徽省科技厅重点研发项目(202104a05020031)

详细信息

通讯作者:
郑翠红，硕士，教授，硕士生导师，主要研究方向为无机非金属材料　E-mail: zhch@ahut.edu.cn

中图分类号: TM271; TB332
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- 文章访问数: 54
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- 被引次数: 0
出版历程
- 收稿日期: 2024-06-25
- 修回日期: 2024-07-30
- 录用日期: 2024-07-31
- 网络出版日期: 2024-08-19

Preparation and performance of ultra-low core loss FeSiAl soft magnetic composites

1.
School of Materials Science and Engineering, Anhui University of Technology, Ma’anshan, Anhui 243002
2.
Ma’anshan New Conda Magnetic Industrial Co., Ltd, Ma’anshan, Anhui 243002

Funds: Key R&D Project of Anhui Provincial Department of Science and Technology (202104a05020031)

摘要

摘要: 目前家电、汽车和手机等产品的电子元器件日益呈现小型化、智能化的发展趋势，因此，降低磁粉芯(SMCs)在高频、大功率下应用时的功率损耗是适应其发展的必要措施。将气雾化Fe-9.6 wt%Si-5.4 wt%Al（FeSiAl）磁粉进行磷化绝缘处理，经预热处理、成型和退火热处理，得到了超低损耗FeSiAl复合磁粉芯(SMCs)。分析结果表明，磷化后的FeSiAl磁粉经热处理后，颗粒表面包覆的磷酸盐转变为硅酸盐，且磁粉中晶粒长大，磁粉的矫顽力降低；制得的磁粉芯功率损耗也明显降低，这主要归因于磁滞损耗的显著降低；当磷酸使用量为0.5 wt%时，50 kHz下功率损耗由79.44 mW·cm⁻³降低至58.56 mW·cm⁻³。
- FeSiAl /
- 磁粉芯 /
- 磷化处理 /
- 预热处理 /
- 功率损耗
Abstract: Currently, electronic components applied in household electric appliances, cars and mobile phones are increasingly presenting a trend of miniaturization and intelligence. Thus, it is urgent to reduce the core loss of soft magnetic composites (SMCs) apply at high frequency and high power. In this work, gas atomized Fe-9.6wt%Si-5.4wt%Al (FeSiAl) magnetic powder was firstly subjected to a phosphating process for electrical insulation, then the phosphated FeSiAl magnetic powder was heated, formed, and annealed, resulting in FeSiAl SMCs. Analytical results show that the particle surface of the phosphated FeSiAl magnetic powder was transformed from phosphate to silicate after heat treatment, accompanied by an increase in its crystalline size and a decrease in its coercivity. Core loss of the obtained SMCs also decreases apparently, due to the significant decrease in their hysteresis loss. Moreover, when the amount of the phosphoric acid used reaches 0.5 wt%, the core loss decreases from 79.44 mW·cm⁻³ to 58.56 mW·cm⁻³ at 50 kHz.
- FeSiAl /
- Soft magnetic composites /
- Phosphatiztion /
- Heating treatment /
- Core loss

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图 1 实验流程示意图

Figure 1. Diagram of experimental proces

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图 2 (a)磷化后及 (b)预热处理磁粉颗粒SEM图像；(c)磷化后颗粒EDS元素分布图；磁粉XRD分析图谱

Figure 2. SEM images of (a)phosphated and (b)heated powders, (c)EDS results of phosphated powders

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图 3 磷酸含量对磁粉芯(SMCs) (a)密度、(b)有效磁导率的影响

Figure 3. Effects of the proportion of H₃PO₄ on the SMCs (a)ρ, (b)μ_e

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图 4 磁粉芯的功率损耗随频率变化图

Figure 4. P_cv of SMCs varies with frequency

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图 5 样品的涡流损耗和磁滞损耗随频率变化关系图

Figure 5. P_e and P_h of SMCs varies with frequency

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图 6 FeSiAl磁粉的XRD 图谱

Figure 6. XRD pattern of FeSiAl magnetic powder

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图 7 磁粉芯样品磁滞回线

Figure 7. Hysteresis loops of SMCs

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图 8 FeSiAl粉的XPS分析图谱

Figure 8. XPS spectra of FeSiAl powder

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图 10 磷化后及预热处理FeSiAl粉 (a)XRD图谱(b)FTIR光谱

Figure 10. (a) XRD pattern (b) FTIR spectrum of FeSiAl powder after phosphating and heating

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图 9 磷化后磁粉XPS分析图谱

Figure 9. XPS spectra of phosphated FeSiAl powder

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图 11 磷化预热处理后磁粉的 XPS分析图谱

Figure 11. XPS spectra of heated FeSiAl powder after phosphating

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图 12 磷化及预热处理过程磁粉表面反应示意图

Figure 12. Diagram about reactions of phosphating and heating process on the surface of FeSiAl powder

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表 1 磁粉芯的电阻率、功率损耗、涡流损耗和磁滞损耗

Table 1. Comparison of electrical resistivity, core loss, eddy current loss and hysteresis loss of SMCs

Sample	Core loss/(mW·cm⁻³)	Eddy current coefficient	Eddy current loss/(mW·cm⁻³)	Hysteresis coefficient	Hysteresis loss/(mW·cm⁻³)	Electrical resistivity/(Ω·cm)
0.5 wt%HP/FeSiAl	79.44	1.74×10⁻⁶	43.53	7.01×10⁻³	35.03	25.23×10⁶
0.5 wt%HPT/FeSiAl	58.56	1.63×10⁻⁶	40.73	3.23×10⁻³	16.17	2.48×10⁶
Notes: B_m—Maximum magnetic induction intensity=100 mT; f—Frequency=50 kHz

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表 2 本文与此前报道磁粉芯性能对比

Table 2. Comparison of previously reported SMCs properties and this work

Sample	Core loss/(mW·cm⁻³)		Permeability	Refs
Sample	f=50 kHz	f=100 kHz	Permeability	Refs
0.5 wt%HPT/FeSiAl	58.56	190.1	52.1 (f=100 kHz)	This work
SiO₂@FeSiAl	77.6	216.53	57(f=1 MHz)	[18]
MoS₂/FeSiAl	181	454	90.6(f=1 MHz)	[19]
2.25 wt%WS₂/FeSiAl	171	431	62~64(f=50 kHz)	[20]
Commercially SMCs	<120		60(f=100 kHz)	NCD Co., Ltd.
Notes:B_m—Maximum magnetic induction intensity=100 mT; f—Frequency; SiO₂@FeSiAl—SiO₂ coated spherical-FeSiAl SMC;MoS₂/FeSiAl and 2.25 wt%—WS₂/FeSiAl MoS₂ and 2.25 wt%WS₂ coated FeSiAl SMCs respectively;Commercially SMCs—Atomized FeSiAl SMCs produced by Ma’anshan New Conda Magnetic Industrial Co., Ltd.

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[1]	ZHONG X, LIU Y, LI J, et al. Structure and magnetic properties of FeSiAl-based soft magnetic composite with AlN and Al₂O₃ insulating layer prepared by selective nitridation and oxidation[J]. Journal of Magnetism and Magnetic Materials, 2012, 324(17): 2631-2636. doi: 10.1016/j.jmmm.2012.03.026
[2]	SHOKROLLAHI H, JANGHORBAN K. Soft magnetic composite materials (SMCs)[J]. Journal of Materials Processing Technology, 2007, 189(1-3): 1-12. doi: 10.1016/j.jmatprotec.2007.02.034
[3]	NIE W, YU T, WANG Z, et al. High-performance core-shell-type FeSiCr@MnZn soft magnetic composites for high-frequency applications[J]. Journal of Alloys and Compounds, 2021, 864: 158215-158221. doi: 10.1016/j.jallcom.2020.158215
[4]	许欣蓓, 鲁书潮, 鲍康馨, 等. 气雾化铁硅铝磁粉粒度级配对磁粉芯性能的影响[J]. 磁性材料及器件, 2024: 1-10. XU Xinpei, LU Shuchao, BAO Kangxin, et al. Effect of grading of gas atomized Fe-Si-Al powders on properties of the soft magnetic cores[J]. Journal of Magnetic Materials and Devices, 2024: 1-10. (in Chinese)
[5]	刘国忠, 杨啸峰, 张公平, 等. 金属磁粉芯绝缘包覆研究进展[J]. 磁性材料及器件, 2021, 52(6): 93-100. LIU Guozhong, YANG Xiaofeng, ZHANG Gongping, et al. Research progress in preparation of insulating coatings on metal soft magnetic cores[J]. Journal of Magnetic Materials and Devices, 2021, 52(6): 93-100(in Chinese).
[6]	郭海山, 陈建川, 钟小溪, 等. FeSiAl磁粉芯制备工艺研究进展[J]. 热加工工艺, 2021, 50(24): 17-20. GUO Haishan, CHEN Jianchuan, ZHONG Xiaoxi, et al. Research progress of preparation technology of FeSiAl magnetic particle core[J]. Hot Working Technology, 2021, 50(24): 17-20(in Chinese).
[7]	Taghvaei A H, Shokrollahi H, Janghorban K, et al. Eddy current and total power loss separation in the iron–phosphate–polyepoxy soft magnetic composites[J]. Materials & Design, 2009, 30(10): 3989-3995.
[8]	贺泓鑫, 侯海彬, 李奇, 等. 磁粉芯的研究现状及发展趋势[J]. 磁性材料及器件, 2023, 54(6): 95-104. HE Hongxin, HOU Haibin, LI Qi, et al. Research status and development trend of magnetic powder cores[J]. Journal of Magnetic Materials and Devices, 2023, 54(6): 95-104(in Chinese).
[9]	王尧, 朱乾科, 陈哲, 等. 成型压强对FeSiB磁粉芯磁性能的影响[J]. 功能材料, 2020, 51(8): 8165-8169. doi: 10.3969/j.issn.1001-9731.2020.08.026 WANG Yao, ZHU Qianke, CHEN Zhe, et al. The influence of forming pressure on the magnetic properties of FeSiB magnetic powder cores[J]. Journal of Functional Materials, 2020, 51(8): 8165-8169(in Chinese). doi: 10.3969/j.issn.1001-9731.2020.08.026
[10]	HSING H, CHEN C H, CHEN C C. Magnetic properties of FeSiCr alloy powder coils made by gel casting process[J]. Journal of Materials Science: Materials in Electronics, 2021, 32(11): 14584-14591. doi: 10.1007/s10854-021-06017-y
[11]	LI S, ZHANG M, ZHAN Z, et al. Study on novel Fe-based core-shell structured soft magnetic composites with remarkable magnetic enhancement by in-situ coating nano-ZnFe₂O₄ layer[J]. Journal of Magnetism and Magnetic Materials, 2020, 500: 166321-166327. doi: 10.1016/j.jmmm.2019.166321
[12]	LUO Z, FAN X, HU W, et al. Properties of Fe₂SiO₄/SiO₂ coated Fe-Si soft magnetic composites prepared by sintering Fe-6.5wt%Si/Fe₃O₄ composite particles[J]. Journal of Magnetism and Magnetic Materials, 2020, 499: 166278-166284. doi: 10.1016/j.jmmm.2019.166278
[13]	LI W, XIAO S, LI W, et al. Hybrid amorphous soft magnetic composites with ultrafine FeSiBCr and submicron FeBP particles for MHz frequency power applications[J]. Journal of Magnetism and Magnetic Materials, 2022, 555: 169365. doi: 10.1016/j.jmmm.2022.169365
[14]	HUANG H, ZHANG R, SUN H, et al. High density Fe-based soft magnetic composites with nice magnetic properties prepared by warm compaction[J]. Journal of Alloys and Compounds, 2023, 947: 169460-169469. doi: 10.1016/j.jallcom.2023.169460
[15]	SUN K, FENG S, JIANG Q, et al. Intergranular insulating reduced iron powder-carbonyl iron powder/SiO₂-Al₂O₃ soft magnetic composites with high saturation magnetic flux density and low core loss[J]. Journal of Magnetism and Magnetic Materials, 2020, 493: 165705-165711. doi: 10.1016/j.jmmm.2019.165705
[16]	WANG J, LIU X, ZHENG Z, et al. Reduction of core loss for FeSi soft magnetic composites prepared using atomic layer deposition-based coating and high-temperature annealing[J]. Journal of Alloys and Compounds, 2022, 909: 164655-164665. doi: 10.1016/j.jallcom.2022.164655
[17]	HE Y, LI G, YANG S, et al. Improvements of magnetic performances for carbonyl iron soft magnetic composites (CI-SMCs) induced by Mn-based phosphating coating[J]. Journal of Alloys and Compounds, 2023, 958: 170498-170506. doi: 10.1016/j.jallcom.2023.170498
[18]	LI W, LI Wc, WU J, et al. Particles size-dependent magnetic properties of a FeSiAl soft magnetic composite with hybrid insulating coating for MHz applications[J]. Materials Science and Engineering: B, 2023, 291: 116387-116395. doi: 10.1016/j.mseb.2023.116387
[19]	ZHU S, DUAN F, NI J, et al. Soft magnetic composites FeSiAl/MoS₂ with high magnetic permeability and low magnetic loss[J]. Journal of Alloys and Compounds, 2022, 926:
[20]	ZHU S, DUAN F, FENG S, et al. Efficient inorganic-coated FeSiAl/WS₂ soft magnetic composites with low magnetic loss[J]. Journal of Alloys and Compounds, 2023, 936: 168190-168197. doi: 10.1016/j.jallcom.2022.168190
[21]	GUO R, YU G, ZHU M, et al. Regulation of magnetic and electrical performances in core-shell-structured FeSiCr@BaTiO₃ soft magnetic composites[J]. Journal of Alloys and Compounds, 2022, 895: 162724-162730. doi: 10.1016/j.jallcom.2021.162724
[22]	WANG J, LI G, HE Y, et al. Improvement in core losses for FeSiAl soft magnetic composites induced by powder annealing treatment[J]. Journal of Materials Research and Technology, 2023, 24: 2500-2513. doi: 10.1016/j.jmrt.2023.03.168
[23]	唐进军, 何配群. 磷化液中金属离子的分析[J]. 电镀与环保, 2009, 29(1): 49-50. doi: 10.3969/j.issn.1000-4742.2009.01.016 TANG Jingjun, HE Peiqun. Analysis of metal ions in phosphating solution[J]. Electroplating & Pollution Control, 2009, 29(1): 49-50(in Chinese). doi: 10.3969/j.issn.1000-4742.2009.01.016
[24]	CHEN Z, LIU X, KAN X, et al. Phosphate coatings evolution study and effects of ultrasonic on soft magnetic properties of FeSiAl by aqueous phosphoric acid solution passivation[J]. Journal of Alloys and Compounds, 2019, 783: 434-440. doi: 10.1016/j.jallcom.2018.12.328
[25]	HUANG M, WU C, JIANG Y, et al. Evolution of phosphate coatings during high-temperature annealing and its influence on the Fe and FeSiAl soft magnetic composites[J]. Journal of Alloys and Compounds, 2015, 644: 124-130. doi: 10.1016/j.jallcom.2015.04.201
[26]	HU B, WANG X, SHU H, et al. Improved electrochemical properties of BiF₃/C cathode via adding amorphous AlPO₄ for lithium-ion batteries[J]. Electrochimica Acta, 2013, 102: 8-18. doi: 10.1016/j.electacta.2013.03.168
[27]	LUO Z, FAN X, HU W, et al. Effect of sintering temperature on microstructure and magnetic properties for Fe-Si soft magnetic composites prepared by water oxidation combined with spark plasma sintering[J]. Journal of Magnetism and Magnetic Materials, 2019, 491: 165615-165622. doi: 10.1016/j.jmmm.2019.165615
[28]	ZHOU Q, LI C, LI X, et al. Reaction behavior of ferric oxide in system Fe₂O₃–SiO₂–Al₂O₃ during reductive sintering process[J]. Transactions of Nonferrous Metals Society of China, 2016, 26(3): 842-848. doi: 10.1016/S1003-6326(16)64175-4
[29]	LUO Z, FAN X, HU W, et al. Enhanced magnetic properties and reduced core loss of intergranular insulating Fe-Si soft magnetic composites with three-shell SiO₂-Fe₂SiO₄-SiO₂ insulating layer[J]. Journal of Solid State Chemistry, 2019, 270: 311-316. doi: 10.1016/j.jssc.2018.11.034
[30]	LIU X, MA Y, HE Q, et al. Some IR features of SiO₄ and OH in coesite, and its amorphization and dehydration at ambient pressure[J]. Journal of Asian Earth Sciences, 2017, 148: 315-323. doi: 10.1016/j.jseaes.2017.03.016
[31]	MOUNIR F, KARIMA H, KHALED B, et al. Modeling Li-ion conductivity in LiLa(PO₃)₄ powder[J]. Physica B: Condensed Matter, 2012, 407(13): 2593-2600. doi: 10.1016/j.physb.2012.03.077
[32]	SAITO T, TAKEMOTO S. Core Loss in Fe-Si Powder Cores[J]. Journal of the Magnetics Society of Japan, 2013, 37(3-2): 155-160.
[33]	WANG J, QIU Z, XU J, et al. Evolution of coating layers during high-temperature annealing and their effects on magnetic behavior of Fe(Si) soft magnetic composites[J]. Advanced Powder Technology, 2022, 33(12): 103876-103889. doi: 10.1016/j.apt.2022.103876