高性能La-Co共替代M型永磁铁氧体的磁各向异性增强机理研究进展

刘若水; 王利晨; 俞翔; 孙洋; 何诗悦; 赵同云; 沈保根

doi:10.7498/aps.73.20240190

摘要

自20世纪末以来, La-Co共替代的M型铁氧体备受关注, 已成为高性能永磁铁氧体的基础材料. Co²⁺的未淬灭轨道矩被认为是增强铁氧体单轴各向异性的原因, 但其微观作用机理尚未完全解释清楚. 为了满足铁氧体材料日益增长的性能需求, 理解其磁各向异性增强机理至关重要, 并寻求从根源上的提升、低成本和高效的方法, 以制定开发高性能产品的指导原则. 本文综述了一系列研究工作, 旨在确定Co离子在晶格中的取代位置, 这是增强磁各向异性的关键. 这些研究为进一步提高永磁铁氧体的磁性能提供了重要的材料设计参考.

关键词:

Abstract

La-Co co-substituted M-type ferrite, which was first reported at the end of the 20th century, as the cornerstone of high-performance permanent magnet ferrites, has received increasing attention from researchers around the world. The unquenched orbital moments of Co²⁺ play a pivotal role in enhancing the uniaxial anisotropy of M-type ferrites. However, a comprehensive understanding of its microscopic mechanism remains elusive. In order to meet the increasing performance requirements of ferrite materials, it is imperative to clarify the mechanism behind the enhancement of magnetic anisotropy, and at the same time seek the guiding principles that are helpful to develop high-performance product quickly and economically. But its mechanism at a microscopic level has not been explained. This review comprehensively analyzes various studies aiming at pinpointing the crystal sites of Co substitution within the lattice. These investigations including neutron diffraction, nuclear magnetic resonance, and Mössbauer spectroscopy can reveal the fundamental origins behind the enhancement of magnetic anisotropy, thereby providing valuable insights for material design strategies aiming at further enhancing the magnetic properties of permanent magnet ferrites.The exploration of co-substitution sites has yielded noteworthy findings. Through careful examination and analysis, researchers have discovered the complex interplay between Co ions and the lattice structure, revealing the mechanisms of enhanced magnetic anisotropy. The current mainstream view is that Co ions tend to occupy more than one site, namely the 4f₁, 12k, and 2a sites, all of which are located within the spinel lattice. However, there have also been differing viewpoints, implying that further exploration is needed to uncover the primary controlling factors influencing Co occupancy. It is worth noting that the identification of specific Co substitution sites, especially the spin-down tetrahedron 4f₁, has achieved targeted modifications, ultimately fine-tuning the magnetic properties with remarkable precision.Furthermore, the reviewed research emphasizes the pivotal role of crystallographic engineering in tailoring the magnetic characteristics of ferrite materials. By strategically manipulating Co substitution, researchers have utilized the intrinsic properties of the lattice to amplify magnetic anisotropy, thereby unlocking new avenues for the advancement of permanent magnet ferrites.In conclusion, the collective findings outlined in this review herald a promising trajectory for the field of permanent magnet ferrites. With a detailed understanding of Co-substitution mechanisms, researchers are preparing to open up new avenues for developing next-generation ferrite materials with enhanced magnetic properties.

Keywords:

作者及机构信息

1.
中国科学院宁波材料技术与工程研究所, 宁波　315201

2.
中国科学院物理研究所, 北京凝聚态物理国家研究中心, 北京　100190

3.
中国科学院赣江创新研究院, 赣州　341119

4.
中国科学技术大学稀土学院, 合肥　230026

通信作者: 沈保根, shenbaogen@nimte.ac.cn

基金项目: 国家自然科学基金基础科学中心项目(批准号: 52088101)、浙江省“鲲鹏计划”和宁波市顶尖人才科技项目资助的课题.

Authors and contacts

1.
Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, China

2.
Beijing State Key Laboratory of Condensed Matter Physics, Institute of Physics, Chinese Academy of Sciences, Beijing 100190, China

3.
Ganjiang Innovation Research Institute, Chinese Academy of Sciences, Ganzhou 341119, China

4.
School of Rare Earths, University of Science and Technology of China, Hefei 230026, China

Corresponding author: Shen Bao-Gen, shenbaogen@nimte.ac.cn

Funds: Project supported by the Basic Science Center Program of the National Science Foundation of China (Grant No. 52088101), the Kunpeng Plan of Zhejiang Province, China, and the Ningbo Top Talent Program, Zhejiang, China.

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施引文献

图 1 从1950年代至2023年关于铁氧体作为永磁材料的科学论文发表量的历史演变(来源: Scopus-以关键词“Ferrite permanent magnet”搜索获得的结果)

Fig. 1. Historical evolution of the number of scientific papers published on ferrite as a permanent magnet material from the 1950 s to 2023 (Source: Scopus- search results by keyword “Ferrite permanent magnet”).

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图 2 TDK公司铁氧体磁体的磁特性变化^[23]

Fig. 2. Changes in magnetic properties of ferrite magnets in TDK corporation^[23].

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图 3 2021—2025年三大领域永磁铁氧体需求预测(数据来源: 中国电子材料协会磁性材料分会华经产业研究院^[25])

Fig. 3. Forecast of ferrite magnets demand in three major fields, 2021—2025 (Data source: Huajng Industrial Research Institute of Magnetic Materials Branch, China Electronic Materials Association^[25]).

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图 4 BaFe₁₂O₁₉单位晶胞的晶体结构和各Fe晶位示意图

Fig. 4. Crystal structure of the unit cell of BaFe₁₂O₁₉ and the schematic diagrams of each Fe crystal site.

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图 5 (a) Sr_1–xLa_xCo_xFe_12–xO₁₉在1200 ℃烧结温度下的磁性能^[9]; (b)各向同性Sr铁氧体经La-Co添加后的磁性能变化(空心符号表示La-Co添加样品, 实心符号表示Cr₂O₃添加样品)^[62]; (c)在–100—+140 ℃温度范围内, x = 0.0—0.2的La-Co替代Sr铁氧体的B_r[α(B_r)]和H_cJ[β(H_cJ)]的温度系数^[62]

Fig. 5. (a) Magnetic properties of Sr_1–xLa_xCo_xFe_12–xO₁₉ at a sintering temperature of 1200 ℃^[9]; (b) variation of magnetic properties of isotropic Sr ferrite with La-Co addition (hollow symbols denote the La-Co added samples and solid symbols denote the Cr₂O₃ added samples)^[62]; (c) in the temperature range of –100 ℃ to +140 ℃, the temperature coefficients of B_r[α(B_r)] and H_cJ[β(H_cJ)] for La-Co substituted Sr ferrites with x = 0.0–0.2^[62].

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图 6 离子RE替代SrM铁氧体的(a)饱和磁化强度和(b)磁各向异性^[89]

Fig. 6. (a) Saturation magnetization and (b) magnetic anisotropy of RE-substituted SrM^[89].

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图 7 在四面体和八面体配位环境中晶体场分裂和Co²⁺ (3d⁷)的占据^[49]

Fig. 7. Crystal field splitting and Co²⁺ (3d⁷) occupation in tetrahedral and octahedral coordination environments^[49].

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图 8 对于Sr_1–xLa_xFe_12–yCo_yO₁₉, WDX测定的Co浓度y与La浓度x的比值(虚线分别代表x = y和y/x = 0.75)^[140], x > y样品中的La³⁺电荷补偿由Co²⁺和Fe²⁺完成

Fig. 8. Ratio of Co concentration y to La concentration x determined by WDX for Sr_1–xLa_xFe_12–yCo_yO₁₉ (dashed lines represent x = y and y/x = 0.75, respectively) ^[140]. Charge compensation for La³⁺ in the sample x > y is accomplished by Co²⁺ and Fe²⁺.

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图 9 Na₂O助熔剂法制备的(a) La-SrM和(b) La-Co SrM单晶的难、易轴磁化曲线^[140]; (c) (Na/Ca-)La-Co替代SrM系列样品在5 K下的磁各向异性场H_A随Co替代浓度的变化^{[140,142–145]}(图中直线帮助判断H_A增长趋势)

Fig. 9. Hard- and easy-axis magnetization curves of (a) La-SrM and (b) La-Co SrM single crystals prepared by the Na₂O flux method^[140]; (c) variation of the magnetic anisotropy field H_A with the concentration of Co substitution for a series of samples of (Na/Ca-)La-Co substituted SrM at 5 K ^{[140,142–145]} (the straight line helps to determine the trend of the H_A growth).

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图 10 (a) SrFe_12–xCo_xO₁₉在5 K下的磁各向异性场H_A随Co浓度x的变化, 与文献[140]中La-Co SrM单晶(蓝色方块)的数据进行对比, 高亮区域表明, 在该Co浓度范围内, Co-SrM的H_A高于La-Co SrM, 插图是Co-SrM和La-Co SrM晶格参数c/a比值; (b)所有样品H_A的温度依赖性^[151]

Fig. 10. (a) Variation of the magnetic anisotropy field H_A of SrFe_12–xCo_xO₁₉ as a function of Co concentration x at 5 K, compared with data for La-Co SrM single crystals (blue squares) from the literature^[140]. The highlighted regions indicate that the H_A of Co-SrM is higher than that of La-Co SrM in this Co concentration range. And the inset is the ratio of the lattice parameters c/a for Co-SrM and La-Co SrM. (b) Temperature dependence of H_A for all samples^[151].

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图 11 (a) (La, Co)_0.4共替代M型锶铁氧体单晶的零场⁵⁹Co NMR谱; (b)高频区放大的单晶⁵⁹Co NMR谐振S2和S3^[115]

Fig. 11. (a) Zero-field ⁵⁹Co NMR spectrum of (La, Co)_0.4 substituted M-type ferrite single crystal; (b) amplified ⁵⁹Co NMR resonances S2 and S3 in the high-frequency region^[115].

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图 12 La-Co SrM中Co的电荷和自旋态以及替代晶位的总结^[115], 说明了S1的两种情况, Co²⁺的主要替代晶位发生在(a)八面体4f₂晶位, (b)四面体4f₁晶位

Fig. 12. Charge and spin states of Co in La-Co SrM and summary of alternative crystal sites^[115]. Two cases of S1 are illustrated: The main alternative sites for Co²⁺ occur in (a) the octahedral 4f₂, (b) the tetrahedral 4f₁.

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图 13 Co浓度(y)对S1信号恢复场(H_r)的依赖性. 作为参考, 5 K时各向异性场H_A的Co浓度依赖性如红点所示. 插图为S2和S3的H_r^[116]

Fig. 13. Dependence of Co concentration (y) on the recovery field (H_r) of S1signal. As a reference, the Co concentration dependence of the anisotropic field H_A at 5 K is shown in red dots. The insets show the H_r of S2 and S3^[116] .

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图 14 当前La-Co SrM中Co占位的主流观点

Fig. 14. Current view of Co occupnacy in La-Co SrM.

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表 1 国内外永磁铁氧体产品的最高性能

Table 1. Top performance of domestic and international ferrite magnets.

公司	国家	牌号	B_r/mT	H_cb/(kA·m^–1)	H_cJ/(kA·m^–1)	(BH )_max/(kJ·m^–3)
TDK^[23]	日本	FB13B	475	340	380	44.0
TDK^[23]		FB14H	470	355	430	43.1
日立金属^[31]		NMF-15	480	342	382	44.0
横店东磁^[27]	中国	DM4748	460	328	368	41.5
北矿磁材^[28]		BMS-9.3	420	318	398	33.5
江益磁材^[29]		JPM-12B	450	310	350	38.2
龙磁科技^[30]		SM13N	450	278	298	38.1

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表 2 磁铅石型铁氧体AFe₁₂O₁₉中A和Fe晶位的相对磁矩方向

Table 2. Relative magnetic moment orientations of A and Fe sites in AFe₁₂O₁₉.

元素	Wyckoff晶位	氧配位数	晶位形状	磁矩方向
A	2d	12	—	—
Fe	2a	6	八面体	↑
	2b	5	双锥体	↑
	4f₁	4	四面体	↓
	4f₂	6	八面体	↓
	12k	6	八面体	↑

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表 3 各国研究者用不同测量方法关于La-Co SrM中Co占据晶位的研究结论(●: 肯定或很可能; ▲: 可能, 但值得怀疑)

Table 3. Conclusions of researchers from various countries on the occupation of crystalline sites by Co in La-Co SrM using different measurements (●: certain or very likely; ▲: possible, but doubtful).

样品	作者和年份	国家	检测方法	Co²⁺占位
样品	作者和年份	国家	检测方法	2a	2b	4f₁	4f₂	12k
多晶	Pieper等, 2002^[100]	澳大利亚	⁵⁷Fe-NMR			●	●
	Pieper等, 2002^[101]	澳大利亚	⁵⁷Fe, ¹³⁹La和 ⁵⁹Co-NMR			▲	●
	Moral等, 2002^[102]	法国	⁵⁷Fe-Mössbauer, Raman	●			●
	Le Breton等, 2002^[103]	法国	⁵⁷Fe-Mössbauer	●	▲		●
	Wiesinger等, 2002^[104]	澳大利亚	⁵⁷Fe-Mössbauer, ⁵⁷Fe和⁵⁹Co-NMR	●		▲	●
	Lechevallier等, 2003^[97]	法国	⁵⁷Fe-Mössbauer	●			●
	Lechevallier等, 2004^[105]	法国	⁵⁷Fe-Mössbauer	●			●
	Choi等, 2006^[106]	韩国	⁵⁷Fe-Mössbauer		●		●	●
	Kobayashi等, 2011^[107]	日本	Neutron Diffraction, EXAFS, XMCD	●		●		●
	Kouřil, 2013^[109]	捷克	⁵⁷Fe-NMR	●	▲	●	▲	▲
	Wu等, 2015^[110]	中国	Raman, XPS	●		●		●
	Ohtsuka等, 2016^[111]	日本	TEM-EDXS	●		●		●
	Mahadevan等, 2020^[112]	印度	⁵⁷Fe-Mössbauer, Raman	●	●		●
单晶	Nagasawa等, 2016^[113]	日本	⁵⁷Fe-Mössbauer			▲	▲
	Oura等, 2018^[114]		⁵⁷Fe-Mössbauer, XES	●		●
	Sakai等, 2018^[115]		⁵⁷Fe和⁵⁹Co-NMR	●		●		●
	Nakamura等, 2019^[116]		⁵⁹Co-NMR	●		●		●
	Nagasawa等, 2020^[117]		外场作用下的⁵⁷Fe-Mössbauer			●

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表 4 (Na/Ca-)La-Co替代SrM系列样品在5 K下的磁各向异性场H_A

Table 4. Magnetic anisotropy field H_A at 5 K for (Na/Ca-)La-Co substituted SrM series samples.

样品	制备方法	替代浓度		5 K时的磁各向异性场 H_A/kOe
样品	制备方法	x	y	5 K时的磁各向异性场 H_A/kOe
Sr_1–xLa_xFe_12–yCo_yO₁₉^[140]	Na₂O助熔剂法生长的单晶	0	0	17.50
		0.055	0.032	17.22
		0.139	0.077	19.46
		0.242	0.108	18.62
		0.289	0.152	21.57
		0.367	0.212	24.36
		0.511	0.161	22.17
		0.472	0.266	25.57
Sr_1–xLa_xFe_12–yCo_yO₁₉^[142]	高氧压移动溶剂浮区法生长的单晶	0.2	0.2	21.77
Sr_1–xLa_xFe_12–yCo_yO₁₉^[142]	高氧压移动溶剂浮区法生长的单晶	0.4	0.4	27.96
Sr_1–xLa_xFe_12–yCo_yO₁₉^[143]	高氧压固相反应法合成的多晶	0.21	0.21	21.18
		0.30	0.30	21.76
		0.39	0.39	24.41
		0.41	0.41	27.06
		0.72	0.72	34.12
		0.93	0.93	42.35
		1.00	1.00	56.76
Ca_13–n–xLa_xFe_n–yCo_yO₁₉ (n = 11.87—11.93, 根据不同Co替代量而改变)^[144]	CaO助熔剂法生长的单晶	0.52	0.07	15.26
		0.52	0.10	17.35
		0.56	0.17	23.15
		0.48	0.16	25.65
		0.59	0.27	28.31
		0.37	0.17	26.89
		0.56	0.36	31.54
Na_axLa_xFe_n–yCo_yO₁₉ (a = 0.25—0.41, n = 11.84—11.97, 根据不同Co 替代量而改变)^[145]	Na₂O助熔剂法生长的单晶	0.82	0.12	25.72
		0.79	0.21	25.61
		0.83	0.31	29.61

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表 5 通过中子衍射和Rietveld分析得到7个候选模型, 显示了Co的占据晶位^[107]

Table 5. Seven candidate models obtained by neutron diffraction and Ritveld analysis showing Co occupied sites^[107].

模型	2a	2b	4f₁	4f₂	12k
1	—	—	1.00	—	—
2	—	—	—	—	1.00
3	0.35	—	0.65	—	—
4	0.31	—	—	—	0.69
5	—	—	0.88	0.12	—
6	—	—	0.47	—	0.53
7	0.22	—	0.38	—	0.40

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表 6 Co²⁺和Co³⁺的高、低自旋值, 其中给出了八面体、四面体和双锥体对称的低自旋值, 而其中具有$ {{\mathrm{e}}}_{{\mathrm{g}}}^{4}{{\mathrm{t}}}_{2{\mathrm{g}}}^{3} $构型的四面体Co²⁺只有S = 3/2的单自旋态

Table 6. High and low spin values of Co²⁺ and Co³⁺. The low spin values of octahedral, tetrahedral and bipyramidal symmetries are given, where the tetrahedron Co²⁺ with $ {{\mathrm{e}}}_{{\mathrm{g}}}^{4}{{\mathrm{t}}}_{2{\mathrm{g}}}^{3} $ configuration has only S = 3/2 single spin states.

类别	高自旋	低自旋
类别	高自旋	八面体	四面体	双锥体
Co²⁺(d⁷)	3/2	1/2	—	1/2
Co³⁺(d⁶)	2	0	1	1

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表 7 Sr_1–xLa_xFe_12–yCo_yO₁₉ (x = 0.289, y = 0.152)的⁵⁹Co共振^[155]

Table 7. ⁵⁹Co resonances of Sr_1–xLa_xFe_12–yCo_yO₁₉ (x = 0.289, y = 0.152)^[155].

记号	中心频率/MHz	局域场大小/T	相对丰度
S1	86	8.6	0.73
S2	307	30.6	0.16
S3	386	38.5	0.11
S4	529	52.7	＜0.002

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