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纳米双相复合稀土永磁材料, 利用硬磁相高磁晶各向异性和软磁相高饱和磁化强度的优点, 通过铁磁交换耦合作用获得优异的磁性能. 但是如何解决软硬磁双相纳米微结构不匹配的问题, 控制软硬磁相同时达到理想的纳米尺度复合是关键. 本文研究了掺杂合金元素Ti对熔体快淬法制备的Nd2Fe14B/α-Fe快淬薄带晶化过程的影响. 结果表明, 掺杂合金元素Ti能影响Nd2Fe14B/α-Fe交换耦合磁体整个晶化动力学过程, 使α-Fe相的晶化激活能升高, 抑制其从非晶相中析出. 同时, 降低1∶7亚稳相的晶化激活能, 起到稳定亚稳相的作用. 而且随着晶化温度的进一步提高, α-Fe和Nd2Fe14B两相由1∶7亚稳相分解产生, 从而有效避免了α-Fe相的优先析出. 显微组织观察表明, 掺杂Ti的样品晶粒细小、分布均匀, 平均晶粒尺寸在20 nm左右, 没有特别大的α-Fe粒子出现. 当Ti的掺杂量原子百分数为1.0%时, 获得了最佳磁性能(BH)max = 12 MG·Oe (1 G = 10–4 T, 1 Oe = 79.57795 A/m).Nanocomposite magnet consisting of a fine mixture of magnetically hard and soft phase has received much attention for potential permanent magnet development. One of the important requirements for alloys to exhibit excellent magnetic properties is a nanocrystalline grain size. The soft and hard magnetic phases can simultaneously achieve ideal nanoscale composites. The effect of Ti additions in the amorphous crystallization process of the exchange-coupled nanocomposite Nd2Fe14B/α-Fe magnet prepared by melt spinning is investigated. The results show that Ti can change the crystallization kinetics of the NdFeB melt-spun ribbons. The Ti can increase the activation energy of α-Fe and contrarily reduce the activation energy of a metastable 1∶7 phase, so the growth speed of α-Fe decreases and the metastable 1∶7 phase can stably precipitate from the amorphous phase. When the annealing temperature increases, a metastable 1∶7 phase is decomposed into the α-Fe phase and the Nd2Fe14B phase. The microstructure observation shows that the grains of the alloys doped with Ti are fine and uniform, with an average grain size of about 20 nm, and no particularly large α-Fe particles appear. The optimal magnetic property is (BH)max = 12 MG·Oe (1 G = 10–4 T, 1 Oe = 79.57795 A/m) when Ti addition is 1.0%.
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Keywords:
- permanent magnet /
- crystallization process /
- doping /
- nanocomposite
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图 1 Nd8Fe86B6 (a), (b) 和 Nd8Fe85Ti1B6 (c), (d)合金快淬带的DSC分析曲线以及结晶过程中–ln(R/T 2)与1/T的关系曲线
Fig. 1. The DSC results and –ln(R/T 2) as a function of 1/T in the crystallization of Nd8Fe86B6 (a), (b) and Nd8Fe85Ti1B6 (c), (d) ribbons at different heating rates.
图 2 (a) Nd8Fe86B6和(b) Nd8Fe85Ti1B6快淬合金带的TMA曲线; (c) Nd8Fe86B6和(d) Nd8Fe85Ti1B6快淬合金带在不同温度3 min晶化处理后的XRD曲线
Fig. 2. TMA results of the ribbons of (a) Nd8Fe86B6, (b) Nd8Fe85Ti1B6; XRD patterns of (c) Nd8Fe86B6 (d) Nd8Fe85Ti1B6 ribbons annealed at different temperature for 3 min.
图 3 (a) Nd8Fe86B6合金快淬带650 ℃晶化10 min后局部TEM图谱; Nd8Fe85Ti1B6合金快淬带在不同温度下晶化3 min后的TEM图谱 (b) 快淬; (c) 600 ℃; (d) 650 ℃; (e) 700 ℃. 插图为对应的高分辨电子衍射谱
Fig. 3. TEM micrographs of (a) Nd8Fe86B6 ribbons annealed at 650 ℃ for 10 min, and Nd8Fe85Ti1B6 ribbons annealed at different temperature for 3 min: (b) as-spun; (c) 600 ℃; (d) 650 ℃; (e) 700 ℃. The insets are the corresponding electron diffraction patterns.
图 4 Nd8Fe85Ti1B6快淬合金带650 ℃晶化60 min后的形貌像(a)和晶格像(b)
Fig. 4. TEM micrographs (a) and electron diffraction patterns (b) of Nd8Fe85Ti1B6 ribbons annealed at 650 ℃ for 60 min.
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[1] Zeng H, Li J, Liu J P, Wang Z L, Sun S 2002 Nature 420 395
Google Scholar
[2] Liu Z, He J, Ramanujan R V 2021 Mater. Des. 209 110004
Google Scholar
[3] Quesada A, Granados-Miralles C, López-Ortega A, Erokhin S, Lottini E, Pedrosa J, Bollero A, Aragón A M, Rubio-Marcos F, Stingaciu M, Bertoni G, Fernández C de J, Sangregorio C, Fernández J F, Berkov D, Christensen M 2016 Adv. Electron. Mater. 2 1500365
Google Scholar
[4] 庞利佳, 孙光飞, 陈菊芳, 强文江, 张锦标, 黎文安 2006 物理学报 55 3049
Google Scholar
Pang L J, Sun G F, Chen J F, Qiang W J, Zhang J B, Li W A 2006 Acta Phys. Sin. 55 3049
Google Scholar
[5] Hernando A, Gonzalez J M 2000 Hyperfine Interact. 130 221
Google Scholar
[6] 夏静, 张溪超, 赵国平 2013 物理学报 62 227502
Google Scholar
Xia J, Zhang X C, Zhao G P 2013 Acta Phys. Sin. 62 227502
Google Scholar
[7] Yang C J, Park E B 1997 J. Magn. Magn. Mater. 168 278
Google Scholar
[8] Mohseni F, Pullar R C, Vieira J M, Amaral J S 2020 J. Phys. D:Appl. Phys. 53 494003
Google Scholar
[9] Kuma J, Kitajima N, Kanai Y, Fukunaga H 1998 J. Appl. Phys. 83 6623
[10] Attyabi S N, Radmanesh S M A, Seyyed Ebrahimi S A, Dehghan H 2022 J. Supercond. Novel Magn. 35 1229
Google Scholar
[11] Skomski R, Coey J M D 1993 Phys. Rev. B 48 15812
Google Scholar
[12] Bauer J, Seager M, Zerm A, Kronmüller H 1996 J. Appl. Phys. 80 1667
Google Scholar
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Google Scholar
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Google Scholar
[15] Yang S, Song X P, Li S, Liu X, Tian Z, Gu B, Du Y 2003 J. Magn. Magn. Mater. 263 134
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Google Scholar
[17] Kim C, Ding S L, O Y J, Zha L, Yun C, Yang W Y, Han J Z, Liu S Q, Du H L, Wang C S, Yang J B 2021 J. Phys. D:Appl. Phys. 54 245003
Google Scholar
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Google Scholar
He X M, Zhong W, Du Y W 2018 Acta Phys. Sin. 67 227501
Google Scholar
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Google Scholar
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Google Scholar
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Google Scholar
[22] Zhang S Y, Xu H, Ni J S, Wang H L, Hou X L, Dong Y D 2007 Physica B 393 153
Google Scholar
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Google Scholar
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Google Scholar
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Google Scholar
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Google Scholar
[27] Yang S, Song X, Du Y 2003 Microelectron. Eng. 66 121
Google Scholar
[28] Kelly P E, O’Grady K, Chantrell R W 1989 IEEE Trans. Magn. 25 3881
Google Scholar
[29] Wohlfarth E P 1958 J. Appl. Phys. 29 595
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