Fe基非晶/氮化物双层结构制备与表征
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摘要
以Fe-Si-B为代表的非晶合金薄带具有高磁导率、低矫顽力及低铁损等优异软磁性能,特别适用于作为变压器和传感器的关键材料。然而,其低的饱和磁矩限制了其作为软磁合金性能的进一步提高。铁氮化合物具有高的饱和磁矩,通过在非晶合金基体引入铁氮化合物,能够提高Fe-Si-B合金的饱和磁矩。采用高能离子注入的方式,在Fe-Si-B非晶薄带表面实现了非平衡渗氮,在保持非晶基体的情况下,制备出具有不同氮含量的铁基非晶/氮化物双层结构的非晶薄带,利用X射线衍射仪(XRD)、扫描电镜(SEM)、俄歇电子能谱仪(AES)和振动样品磁强计(VSM),研究了注入剂量对Fe基非晶带材结构和磁性能的影响。实验结果表明,通过调整离子注入剂量,可以制备出Fe基非晶/氮化物双层结构,并提高样品的饱和磁矩。随着注入剂量的增加,合金先是从完全非晶相转变为非晶/晶体复合相,最终转变为完全晶态;注入剂量为1×10~(16) ions·cm~(-2)的样品饱和磁矩最大,达1.70 T,比未注入样品提高18.1%。
Amorphous Fe-Si-B alloys were the representative material with several practical applications in transformers and inductors because of their excellent soft magnetic properties, such as high permeability, low coercivity and low core losses. However, a higher saturation magnetization M_s was required for soft magnet materials so as to obtain high performance. The introduction of iron-nitrides into the matrix could enhance the M_s, due to the high magnetic moment of iron-nitrides. The double-layer structure of iron-based amorphous/nitride was prepared by high energy ion implantation, with the amorphous matrix still remained. The effects of implantation dose on the structure and soft magnetic properties of Fe-based amorphous were studied by X-ray diffraction(XRD), scanning electron microscopy(SEM), Auger electron spectroscopy(AES) and vibration sample magnetometer(VSM). The results showed that Fe-based amorphous/nitride double-layer structures were prepared by adjusting the implantation dose of nitrogen ions. With the increase of implantation dose of N ions, the alloy changed from the complete amorphous phase to the amorphous/crystalline composite phase firstly and then it changed to complete crystalline phase. The amorphous ribbons with the dose of 1×10~(16) ions ·cm~(-2) exhibited the highest saturation magnetization M_s of 1.70 T, which was 18.1% higher than that of the original sample.
Amorphous Fe-Si-B alloys were the representative material with several practical applications in transformers and inductors because of their excellent soft magnetic properties, such as high permeability, low coercivity and low core losses. However, a higher saturation magnetization M_s was required for soft magnet materials so as to obtain high performance. The introduction of iron-nitrides into the matrix could enhance the M_s, due to the high magnetic moment of iron-nitrides. The double-layer structure of iron-based amorphous/nitride was prepared by high energy ion implantation, with the amorphous matrix still remained. The effects of implantation dose on the structure and soft magnetic properties of Fe-based amorphous were studied by X-ray diffraction(XRD), scanning electron microscopy(SEM), Auger electron spectroscopy(AES) and vibration sample magnetometer(VSM). The results showed that Fe-based amorphous/nitride double-layer structures were prepared by adjusting the implantation dose of nitrogen ions. With the increase of implantation dose of N ions, the alloy changed from the complete amorphous phase to the amorphous/crystalline composite phase firstly and then it changed to complete crystalline phase. The amorphous ribbons with the dose of 1×10~(16) ions ·cm~(-2) exhibited the highest saturation magnetization M_s of 1.70 T, which was 18.1% higher than that of the original sample.
引文
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[16] Dou Q Y, Li H W, Luo Y, Yu D B. Effect of Si to P concentration ratio on crystallization behavior, glass-forming ability and soft-magnetic properties of Fe77(P7-xSix)B13Nb2Cr1 alloys [J]. Rare Metals, 2016, 32(8): 712.
[17] Hasegawa R, O′Handley R C, Mendelsohn L I. Advances in Ferromagnetic Metallic Glasses [M]. American Institute of Physics, 1976. 298.
[2] Suzuki K, Kataoka N, Inoue A, A Makino, T Masumoto. High saturation magnetization and soft magnetic properties of bcc Fe-Zr-B alloys with ultrafine grain structure [J]. Materials Transactions, JIM, 1990, 31(8): 743.
[3] Suzuki K, Makino A, Inoue A, Makino A, Masumoto K. Soft magnetic properties of nanocrystalline bcc Fe-Zr-B and Fe-M-B-Cu (M= transition metal) alloys with high saturation magnetization [J]. Journal of Applied Physics, 1991, 70(10): 6232.
[4] Willard M A, Laughlin D E, McHenry M E, Thoma D, Sickafus K, Cross J, Harris V. Structure and magnetic properties of (Fe0.5Co0.5)88Zr7B4Cu1 nanocrystalline alloys [J]. Journal of Applied Physics, 1998, 84(12): 6773.
[5] Willard M A, Huang M Q, Laughlin D E, McHenry M E. Magnetic properties of HITPERM (Fe, Co)88Zr7B4Cu1 magnets [J]. Journal of Applied Physics, 1999, 85(8): 4421.
[6] Hasegawa R. Applications of amorphous magnetic alloys in electronic devices [J]. Journal of Non-Crystalline Solids, 2001, 287(1-3): 405.
[7] Luborsky F, Becker J, Walter J, Liebermann H. Formation and magnetic properties of Fe-B-Si amorphous alloys [J]. IEEE Transactions on Magnetics, 1979, 15(4): 1146.
[8] Ogawa Y, Naoe M, Yoshizawa Y, Hasegawa R. Magnetic properties of high Bs Fe-based amorphous material [J]. Journal of Magnetism and Magnetic Materials, 2006, 304(2): e675.
[9] Wang S S, Hu Q, Zhao X M, Sheng Y W, Zhao W D, Liu Y J. Performance characterization of Gas-atomized Fe-6.5%Si-x%Ni powders [J]. Chinese Journal of Rare Metals, 2017, 41(11): 1231.(王山山, 胡强, 赵新明, 盛艳伟, 赵文东, 刘英杰. 气雾化法制备Fe-6.5%Si-x%Ni合金粉末及其性能的研究 [J]. 稀有金属, 2017, 41(11): 1231.)
[10] Atmani H, Grognet S, Teillet J. Crystallization-nitriding process of FeSiB and FeSiBCuNb ribbons: influence of additive (Cu, Nb) pair and nitrogen on structure, magnetic and magnetostrictive parameters [J]. Journal of Non-Crystalline Solids, 2001, 290(2): 194.
[11] Grognet S, Atmani H, Zuberek R, Teillet J. Structural and magnetic study of nitrogenated FeCu-(Nb, Zr)-SiB ribbons [J]. Journal of Magnetism and Magnetic Materials, 2000, 215: 391.
[12] Grognet S, Le Breton J M, Atmani H, Teillet J. Microstructural study of nanocrystalline Fe-(Cu-Nb)-Si-B ribbons obtained by a nitriding thermochemical treatment [J]. Journal of Magnetism and Magnetic Materials, 2000, 210(1): 167.
[13] Liu W S, Tang J C, Du Y W. Nanocrystalline soft magnetic ribbon with α″-Fe16N2 nanocrystallites embedded in amorphous matrix [J]. Journal of Magnetism and Magnetic Materials, 2008, 320(21): 2752.
[14] Tang J, Zhang M, Wu A, Liu W, He Y. Electrical resistivity and magnetostriction of nanocrystalline Fe-N-B ribbon [J]. Journal of Magnetism and Magnetic Materials, 2009, 321(18): 2772.
[15] Tang J C, Hong J M, Wu A H, Liu W S, He Y H, Du Y W. Saturation magnetostriction of α″-Fe16N2 phase [J]. Journal of Alloys and Compounds, 2009, 479(1-2): 32.
[16] Dou Q Y, Li H W, Luo Y, Yu D B. Effect of Si to P concentration ratio on crystallization behavior, glass-forming ability and soft-magnetic properties of Fe77(P7-xSix)B13Nb2Cr1 alloys [J]. Rare Metals, 2016, 32(8): 712.
[17] Hasegawa R, O′Handley R C, Mendelsohn L I. Advances in Ferromagnetic Metallic Glasses [M]. American Institute of Physics, 1976. 298.