Preparation of FeNiMo/SiO<sub>2</sub> composite core and regulation of soft magnetic properties

Xiong Zheng-Wei; Yang Jiang; Wang Yu; Yang Lu; Guan Xian; Cao Lin-Hong; Wang Jin; Gao Zhi-Peng

doi:10.7498/aps.71.20212317

Abstract

Nowadays, metal soft magnetic materials are mainly used in electronic components such as high-frequency inductors. Since all the elements in the soft magnetic alloys are transition metals, dense oxide layer is easily formed on their surfaces, which can affect the regulation of soft magnetic properties. In order to solve the problems, in this work, an innovative high-temperature pretreatment process in H₂/Ar mixture is adopted to pretreat FeNiMo raw powders. We confirm that the high temperature treatment in reducing atmosphere can effectively remove metal oxides from the FeNiMo material surface and increase the content of elemental states, thereby further significantly improving the effective permeability of FeNiMo raw powders. The pretreated FeNiMo powder is evenly coated with SiO₂ layers, forming the FeNiMo/SiO₂ soft magnetic composites. Compared with the untreated FeNiMo powder coated with SiO₂, the FeNiMo/SiO₂ pretreated with H₂/Ar mixture gas at high temperatures has high effective permeability and low loss. Our FeNiMo/SiO₂ cores prepared by the synergistic effect of high-temperature pretreatment process in H₂/Ar mixture and insulation coating process have more excellent soft magnetic properties than other iron-based soft magnetic composites. Therefore, the insulation coating after being pretreated at high temperature in reducing atmosphere can greatly improve the permeability and reduce the core loss of soft magnetic composites. This will provide a new strategy for enhancing the soft magnetic properties of the composite cores.

Keywords:

Authors and contacts

1.
Joint Laboratory for Extreme Conditions Matter Properties, School of Mathematics and Physics, Southwest University of Science and Technology, Mianyang 621010, China
2.
China Electronics Technology Group Corporation 9th Research Institute, Mianyang 621010, China
3.
Institute of Fluid Physics, China Academy of Engineering Physics, Mianyang 621900, China
4.
Sichuan Civil-military Integration Institute, Mianyang 621010, China

Corresponding author: Xiong Zheng-Wei, zw-xiong@swust.edu.cn ; Wang Yu, wangyu_dzkjdx@yahoo.com ;

Funds: Project supported by the National Natural Science Foundation of China (Grant Nos. 11904299, U1930124).

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References

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Cited By

图 1 SEM图　(a) F0; (b) F600; (c) FS0; (d) FS600

Figure 1. SEM images: (a) F0; (b) F600; (c) FS0; (d) FS600.

DownLoad: Full-Size Img PowerPoint

图 2 样品FS0的(a) SEM及对应的(b)—(f) EDS元素分布图　(a) SEM; (b) Fe; (c) Ni; (d) Mo; (e) O; (f) Si

Figure 2. (a) SEM image and (b)–(f) corresponding EDS element distribution of sample FS0: (a) SEM; (b) Fe; (c) Ni; (d) Mo; (e) O; (f) Si.

DownLoad: Full-Size Img PowerPoint

图 3 样品F0和F600的XPS图　(a)—(d)样品F0的XPS全谱, Fe 2p, Ni 2p和Mo 3d谱; (e)—(h)样品F600的XPS全谱, Fe 2p, Ni 2p和Mo 3d谱

Figure 3. XPS image of sample F0 and F600: (a)–(d) XPS survey spectrum, Fe 2p spectrum, Ni 2p spectrum and Mo 3d spectrum of sample F0; (e)–(h) XPS survey spectrum, Fe 2p spectrum, Ni 2p spectrum and Mo 3d spectrum of sample F600.

DownLoad: Full-Size Img PowerPoint

图 4 在B = 100 mT条件下, 测得的FeNiMo粉末在H₂/Ar混合气体中经过不同处理温度后压制成型的软磁粉芯的磁性能　(a) 有效磁导率; (b) 损耗

Figure 4. Magnetic properties measured at B = 100 mT of soft magnetic powder core that is prepared by the FeNiMo powder treated at different temperatures in H₂/Ar mixture: (a) Effective permeability; (b) core loss.

DownLoad: Full-Size Img PowerPoint

图 5 在B = 100 mT条件下, 测得的样品FS0和FS600在不同温度下退火后的磁性能　(a) 样品FS0的有效磁导率; (b) 样品FS0的损耗; (c) 样品FS600的有效磁导率; (d) 样品FS600的损耗. 图(c)中的插图为800 ℃烧结后复合粉芯截面的SEM图

Figure 5. Magnetic properties measured at B = 100 mT of samples FS0 and FS600 annealed at different temperatures: (a) Effective permeability of sample FS0; (b) core loss of sample FS0; (c) effective permeability of sample FS600; (d) core loss of sample FS600. The inset in panel (c) is the cross-section SEM image of the sample FS600 sintered at 800 ℃.

DownLoad: Full-Size Img PowerPoint

图 6 样品F600, FS0和FS600的有效磁导率和损耗对比图

Figure 6. Comparison diagram of effective permeability and core loss of samples F600, FS0 and FS600.

DownLoad: Full-Size Img PowerPoint

图 7 样品FS600在不同磁感应强度下的损耗

Figure 7. Core loss of sample FS600 under different magnetic fields.

DownLoad: Full-Size Img PowerPoint

图 8 不同SMCs高频稳定性的对比

Figure 8. Comparison of high frequency stability of different SMCs.

DownLoad: Full-Size Img PowerPoint

表 1 不同SMCs软磁性能的对比

Table 1. Comparison of the magnetic properties of different SMCs.

SMCs	50 kHz		100 kHz		B / mT	Ref.
SMCs	μ_eff	P_s / (kW·m^–3)	μ_eff	P_s / (kW·m^–3)	B / mT	Ref.
FeNiMo/ SiO₂	46.8	18.97	46.7	55.52	20	This work
		217.3		773.7	50
		1026		3905	100
FeNiMo/ Al₂O₃	87.6	321.78	—	—	100	[11]
FeNiMo/ resin	—	—	30	~6180	100	[12]
Fe/Al₂O₃	88.1	310.65	—	—	20	[8]
Fe/NiZn	43.5	94.83	43.14	199.3	20	[13]
FeSiCr/ SiO₂	36	311	—	—	50	[14]
Fe/Al₂O₃	—	—	～35	400—500	20	[15]

DownLoad: CSV

表 A1 根据测试结果拟合所得的数值

Table A1. Values fitted according to the test results.

Fixed condition	Constant
Fixed condition	C_m	α	β
B = 20 mT	0.02702	1.56019	2.44999
B = 50 mT	0.01310	1.96241	2.26657
B = 100 mT	0.02483	1.91492	2.18883
f = 20 kHz	0.03042	1.34380	2.36837
f = 50 kHz	0.10170	1.63830	2.36837
f = 100 kHz	0.03017	1.30323	2.83566

DownLoad: CSV

map

[1]	Xie D Z, Lin K H, Lin S T 2014 J. Magn. Magn. Mater. 353 34 Google Scholar
[2]	Ustinovshikov Y, Shabanova I 2013 J. Alloys Compd. 578 292 Google Scholar
[3]	Füzer J, Kollár P, Olekšáková D, Roth S 2009 J. Alloys Compd. 483 557 Google Scholar
[4]	丁燕红, 李明吉, 杨保和, 马叙 2011 60 097502 Google Scholar Ding Y H, Li M J, Yang B H, Ma X 2011 Acta Phys. Sin. 60 097502 Google Scholar
[5]	Streckova M, Bures R, Faberova M, Medvecky L, Fuzer J, Kollar P 2015 Chin. J. Chem. Eng. 23 736 Google Scholar
[6]	Yi Y, Peng Y D, Xia C, Wu L Y, Ke X, Nie J W 2019 J. Magn. Magn. Mater. 476 100 Google Scholar
[7]	Sunday K J, Darling K A, Hanejko F G, Anasori B, Liu Y C, Taheri M L 2015 J. Alloys Compd. 653 61 Google Scholar
[8]	Peng Y D, Nie J W, Zhang W J, Ma J, Bao C X, Cao Y 2016 J. Magn. Magn. Mater. 399 88 Google Scholar
[9]	Zhong X X, Chen J C, Wang L, Li B J, Li L Z 2018 J. Alloys Compd. 735 1603 Google Scholar
[10]	Fan X A, Wang J, Wu Z Y, Li G Q 2015 Mater. Sci. Eng., B 201 79 Google Scholar
[11]	Yao Z X, Peng Y D, Xia C, Yi X W, Mao S H, Zhang M T 2020 J. Alloys Compd. 827 154345 Google Scholar
[12]	Neamtu B V, Geoffroy O, Chicinaş I, Isnard O 2012 Mater. Sci. Eng., B 177 661 Google Scholar
[13]	Peng Y D, Yi Y, Li L Y, Ai H Y, Wang X X, Chen L L 2017 J. Magn. Magn. Mater. 428 148 Google Scholar
[14]	张凯, 王征, 张义, 魏荣飞, 兰中文, 余忠, 傅膑 2018 磁性材料及器件 49 52 Google Scholar Zhang K, Wang Z, Zhang Y, Wei R F, Lan Z W, Yu Z 2018 J. Magn. Mater. Devices 49 52 Google Scholar
[15]	Lei J, Zheng J W, Zheng H D, Qiao L, Ying Y, Cai W, Li W C, Yu J, Lin M, Che S L 2019 J. Magn. Magn. Mater. 472 7 Google Scholar
[16]	Zhang Z Q, Cong L C, Yu Z C, Qu L N, Qian M M, Huang W M 2020 Mater. Adv. 1 54 Google Scholar
[17]	Tu X, Gallon H J, Whitehead J C 2013 Catal. Today 211 120 Google Scholar
[18]	冯波, 武鹏, 李永龙 2021 天然气化工 46 66 Feng B, Wu P, Li Y L 2021 Nat. Gas Chem. Ind. 46 66
[19]	Cong L C, Yu Z C, Liu F B, Huang W M 2019 Catal. Sci. Technol. 9 1208 Google Scholar
[20]	张亚菊, 谢忠帅, 郑海务, 袁国亮 2020 69 127709 Google Scholar Zhang Y J, Xie Z S, Zheng H W, Yuan G L 2020 Acta Phys. Sin. 69 127709 Google Scholar
[21]	Ray S K, Dhakal D, Lee S W 2018 Chem. Eng. J. 347 836 Google Scholar
[22]	Xiang M L, Li D B, Zou J, Li W H, Sun Y H, She X C 2010 J. Nat. Gas Chem. 19 151 Google Scholar
[23]	Wu K Z, Zhao J J, Zhang X Y, Zhou H W, Wu M X 2019 J. Taiwan Inst. Chem. Eng. 102 212 Google Scholar
[24]	Liu Y L, Zhang H, Ouyang P, Li Z C 2013 Electrochim. Acta 102 429 Google Scholar
[25]	Chen X Y, Zhang Z J, Li X X, Shi C W, Li X L 2006 Chem. Phys. Lett. 418 105 Google Scholar
[26]	严密, 彭晓领 2006 磁学基础与磁性材料(杭州: 浙江大学出版社) 第120页 Yan M, Peng X L 2006 Fundamentals of Magnetism and Magnetic Materials (Hangzhou: Zhejiang University Press) p120 (in Chinese)
[27]	Takahashi S, Harada S, Tamaki S 1989 J. Phys. Soc. Jpn. 58 2075 Google Scholar
[28]	Zhang L M, Huang X H, Song X L 2008 Fundamentals of Materials Science (2nd Ed.) (Wuhan: Wuhan University of Technology Press) p454 (in Chinese) [张联盟, 黄学辉, 宋晓岚 2008 材料科学基础(第二版) (武汉: 武汉理工大学出版社) 第454页]
[29]	Wang Z, Liu X S, Kan X C, Zhu R W, Yang W, Wu Q Y, Zhou S Q 2019 Curr. Appl. Phys. 19 924 Google Scholar
[30]	Steinmetz C P 1984 Proc. IEEE 72 197 Google Scholar
[31]	Reinert J, Brockmeyer A, De Doncker R W A A 2001 IEEE Trans. Ind. Appl. 37 1055 Google Scholar
[32]	Zheng J W, Zheng H D, Lei J, Ying Y, Qiao L, Cai W, Li W C, Yu J, Tang Y P, Che S L 2020 J. Magn. Magn. Mater. 499 166255 Google Scholar
[33]	Luo F, Fan X A, Luo Z G, Hu W T, Wang J, Wu Z Y, Li G Q, Li Y W, Liu X 2020 J. Magn. Magn. Mater. 498 166084 Google Scholar
[34]	Li L Y, Chen Q L, Gao Z, Ge Y C, Yi J H 2019 J. Alloys Compd. 805 609 Google Scholar
[35]	任劲松, 李勃, 王进, 庞新峰, 郭海 2018 电子元件与材料 37 51 Google Scholar Ren J S, Li B, Wang J, Pang X F, Guo H 2018 Electron. Compon. Mater. 37 51 Google Scholar
[36]	Guo R D, Wang S M, Yu Z, Sun K, Jiang X N, Wu G H, Wu C J, Lan Z W 2020 J. Alloys Compd. 830 154736 Google Scholar

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Preparation of FeNiMo/SiO₂ composite core and regulation of soft magnetic properties

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Corresponding author: Xiong Zheng-Wei, zw-xiong@swust.edu.cn ; Wang Yu, wangyu_dzkjdx@yahoo.com ;

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Preparation of FeNiMo/SiO2 composite core and regulation of soft magnetic properties

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Corresponding author: Xiong Zheng-Wei, zw-xiong@swust.edu.cn ; Wang Yu, wangyu_dzkjdx@yahoo.com ;

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Preparation of FeNiMo/SiO₂ composite core and regulation of soft magnetic properties