FeCoAIN薄膜的软磁性、动态磁性及热稳定性的研究
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摘要
随着电子信息技术的发展,磁感应元件越来越向微型化、集成化、高频化方向发展,而电磁干扰和电磁污染的逐步增加,也使我们对吸波材料提出了更高的要求。因此,具有高饱和磁化强度和良好高频动态特性的软磁性薄膜越来越受到重视,对高频软磁性薄膜的深入研究对于满足这些需求具有重要的意义。
FeCo合金因为具有最高的饱和磁化强度而备受关注,但是FeCo合金因具有较大的磁晶各向异性和磁滞伸缩系数而难以实现软磁性能。最近的研究表明Fe_(70)Co_(30)N、Fe_(60)Co_(40)N、Fe_(81)Co_(19)N薄膜具有良好的软磁性能,但其热稳定性能很差,当退火温度高于200℃时,其软磁性能基本消失。在FeCoN体系中掺入适当的元素有利于改善其热稳定性,因此本文工作用磁控溅射方法制备了一系列Fe:Co原子比为64.8:35.2的FeCoAlN薄膜,对它们结构,静态磁性,动态磁性以及热稳定性进行研究。研究结果表明FeCoAlN薄膜可以实现良好的软磁性和高频特性,并且(Fe_(64.8)Co_(35.2))AlN薄膜的热稳定性随着Al含量的提高而得到显著改善。主要结果如下:
(1)Al含量为3.7%的溅射态(Fg_(64.8)Co_(35.2))_(96.3)Al_(3.7)N薄膜,在N_2/(Ar+N_2)流量比(R)为9%时表现为良好的软磁性和面内单轴各向异性,磁导率谱表现出良好的高频特征,自然共振频率大于2GHz,磁导率实部在衰落前大于400。
(2)R为9%的(Fe_(64.8)Co_(35.2))AlN薄膜,当Al含量小于6.2%时,在溅射态表现出良好的软磁性和单轴各向异性,动态磁性表现为良好的一致共振模式,共振频率大于2GHz,随着Al含量进一步的增加,由于薄膜中应力的增加,矫顽力增大,单轴各向异性不明显,动态表现变差。
(3)薄膜的磁性热稳定性随着Al含量的提高明显改善,不同Al含量的薄膜在不同的最优退火温度T_(opt)以上热处理60 min后,由软磁性和单轴各向异性向硬磁和各向同性转变,动态磁性也相应变差,而最优退火温度T_(opt)随着Al含量的增加而提高。不含Al的(Fe_(64.8)Co_(35.2))N薄膜在150℃热处理时仍然保持较好的软磁性和动态特征,但在200℃热处理后,矫顽力急剧增加,难轴各向异性消失,磁导率很低,没有共振现象出现。含Al为13.5%的薄膜在400℃热处理后仍然保持良好的软磁性、单轴各向异性和一致共振的动态特性,自然共振频率1.89GHz,磁导率实部在衰落之前大于380。
(4)溅射态(Fe_(64.8)Co_(35.2))_(93.8)Al_(6.2)N薄膜的饱和磁化强度随着膜厚的变化几乎没有变化,这说明饱和磁化强度与膜厚和结构无关。而矫顽力随着膜厚的增加却逐渐减小,这可能是由于随着膜厚的增加,内应力逐渐减小,所以矫顽力也随之减小。
With the rapid development of electronic information technology,the magnetic induction devises are becoming more and more miniaturized and integrated and desired for high frequency applications.Meanwhile,we need more advanced microwave absorption materials to elimate the increasing interference and pollution of electromagnetic wave.Therefore,the soft magnetic films with high saturation magnetization and good dynamic characteristics in high frequency range have attracted more attentions.Systematical studies of the soft magnetic films for high frequency applications are of significance for the practical applications mentioned above.
FeCo alloys are important materials for their high saturation magnetization. But it is difficult for FeCo alloys to achieve low coercivity and in-plane uniaxial anisotropy due to its high magnetocrystalline anisotropy and magnetostriction. The recent studies have indicated that Fe_(70)Co_(30)N,Fe_(60)Co_(40)N,and Fe_(81)Co_(19)N films have good soft magnetic properties.But these films do not show soft magnetic properties after annealing at higher than 200℃.Addition of proper elements into the FeCoN films can improve thermal stability of the films.In our work of this thesis,a series of FeCoAlN films with Fe:Co ratio of 64.8:35.2 are prepared by the reactive radio frequency magnetron sputtering.The structure, static and dynamic magnetic properties,and thermal stabilities are studied.The results show that the FeCoAlN films can achieve good soft magnetic properties and dynamic characteristics in high frequency.The thermal stability of (Fe_(64.8)Co_(35.2))AlN films is evidently improved with increase of Al content.The main results are shown as follows:
(1) The as-deposited(Fe_(64.8)Co_(35.2))_(96.3)Al_(3.7)N films show good soft magnetic properties and in-plane uniaxial anisotropy when N_2/(Ar+N_2) flow rate ratio(R) is in 9%.These films show high resonance frequency above 2 GHz and the real part of permeability larger than 400 before rolloff.
(2) The as-deposited(Fe_(64.8)Co_(35.2))AlN films with R of 9%show good soft magnetic properties and the uniaxial anisotropy when Al content is lower than 6.2%.The dynamic characteristics exhibit the uniform resonance mode.The resonance frequencies are higher than 2 GHz.With the further increase of Al content,the coercivity become larger and the uniaxial anisotropy become lower. The dynamic characteristics are deteriorated.The reason may be the increase of stresses in the films with the increase of Al content.
(3) Thermal stability of the films is evidently improved with increase of Al content.The magnetic properties of the films with different Al content transform from soft magnetic and uniaxial anisotropic properties to hard magnetic and isotropic properties when they are annealed at the temperature higher than an optimal temperature(T_(opt)).T_(opt) clearly increases with the increase of Al content in the films.The Fe_(64.8)Co_(35.2)N film without Al become hard magnetic and isotropic properties after annealed at 200℃.No resonance show in the permeability spectrum.The(Fe_(64.8)Co_(35.2))_(86.5)Al_(13.5)N film annealed at 400℃for 60 min still remain the good soft magnetic properties,uniaxial anisotropy and uniform resonance mode of permeability spectrum.The resonance frequency is about 1.89 GHz and the real part of permeability is higher than 380 before rolloff.
(4) Saturation magnetization of the as-deposited(Fe_(64.8)Co_(35.2))_(93.8)Al_(6.2)N films does not change with the variation of film thickness.This may be due to the saturation magnetization has nothing to do with the film thickness and structure. The coercivity increase as the film thickness is gradually reduced,which may be due to the increase with the thickness,internal stress gradually decreased,the coercivity also decreases.
FeCo合金因为具有最高的饱和磁化强度而备受关注,但是FeCo合金因具有较大的磁晶各向异性和磁滞伸缩系数而难以实现软磁性能。最近的研究表明Fe_(70)Co_(30)N、Fe_(60)Co_(40)N、Fe_(81)Co_(19)N薄膜具有良好的软磁性能,但其热稳定性能很差,当退火温度高于200℃时,其软磁性能基本消失。在FeCoN体系中掺入适当的元素有利于改善其热稳定性,因此本文工作用磁控溅射方法制备了一系列Fe:Co原子比为64.8:35.2的FeCoAlN薄膜,对它们结构,静态磁性,动态磁性以及热稳定性进行研究。研究结果表明FeCoAlN薄膜可以实现良好的软磁性和高频特性,并且(Fe_(64.8)Co_(35.2))AlN薄膜的热稳定性随着Al含量的提高而得到显著改善。主要结果如下:
(1)Al含量为3.7%的溅射态(Fg_(64.8)Co_(35.2))_(96.3)Al_(3.7)N薄膜,在N_2/(Ar+N_2)流量比(R)为9%时表现为良好的软磁性和面内单轴各向异性,磁导率谱表现出良好的高频特征,自然共振频率大于2GHz,磁导率实部在衰落前大于400。
(2)R为9%的(Fe_(64.8)Co_(35.2))AlN薄膜,当Al含量小于6.2%时,在溅射态表现出良好的软磁性和单轴各向异性,动态磁性表现为良好的一致共振模式,共振频率大于2GHz,随着Al含量进一步的增加,由于薄膜中应力的增加,矫顽力增大,单轴各向异性不明显,动态表现变差。
(3)薄膜的磁性热稳定性随着Al含量的提高明显改善,不同Al含量的薄膜在不同的最优退火温度T_(opt)以上热处理60 min后,由软磁性和单轴各向异性向硬磁和各向同性转变,动态磁性也相应变差,而最优退火温度T_(opt)随着Al含量的增加而提高。不含Al的(Fe_(64.8)Co_(35.2))N薄膜在150℃热处理时仍然保持较好的软磁性和动态特征,但在200℃热处理后,矫顽力急剧增加,难轴各向异性消失,磁导率很低,没有共振现象出现。含Al为13.5%的薄膜在400℃热处理后仍然保持良好的软磁性、单轴各向异性和一致共振的动态特性,自然共振频率1.89GHz,磁导率实部在衰落之前大于380。
(4)溅射态(Fe_(64.8)Co_(35.2))_(93.8)Al_(6.2)N薄膜的饱和磁化强度随着膜厚的变化几乎没有变化,这说明饱和磁化强度与膜厚和结构无关。而矫顽力随着膜厚的增加却逐渐减小,这可能是由于随着膜厚的增加,内应力逐渐减小,所以矫顽力也随之减小。
With the rapid development of electronic information technology,the magnetic induction devises are becoming more and more miniaturized and integrated and desired for high frequency applications.Meanwhile,we need more advanced microwave absorption materials to elimate the increasing interference and pollution of electromagnetic wave.Therefore,the soft magnetic films with high saturation magnetization and good dynamic characteristics in high frequency range have attracted more attentions.Systematical studies of the soft magnetic films for high frequency applications are of significance for the practical applications mentioned above.
FeCo alloys are important materials for their high saturation magnetization. But it is difficult for FeCo alloys to achieve low coercivity and in-plane uniaxial anisotropy due to its high magnetocrystalline anisotropy and magnetostriction. The recent studies have indicated that Fe_(70)Co_(30)N,Fe_(60)Co_(40)N,and Fe_(81)Co_(19)N films have good soft magnetic properties.But these films do not show soft magnetic properties after annealing at higher than 200℃.Addition of proper elements into the FeCoN films can improve thermal stability of the films.In our work of this thesis,a series of FeCoAlN films with Fe:Co ratio of 64.8:35.2 are prepared by the reactive radio frequency magnetron sputtering.The structure, static and dynamic magnetic properties,and thermal stabilities are studied.The results show that the FeCoAlN films can achieve good soft magnetic properties and dynamic characteristics in high frequency.The thermal stability of (Fe_(64.8)Co_(35.2))AlN films is evidently improved with increase of Al content.The main results are shown as follows:
(1) The as-deposited(Fe_(64.8)Co_(35.2))_(96.3)Al_(3.7)N films show good soft magnetic properties and in-plane uniaxial anisotropy when N_2/(Ar+N_2) flow rate ratio(R) is in 9%.These films show high resonance frequency above 2 GHz and the real part of permeability larger than 400 before rolloff.
(2) The as-deposited(Fe_(64.8)Co_(35.2))AlN films with R of 9%show good soft magnetic properties and the uniaxial anisotropy when Al content is lower than 6.2%.The dynamic characteristics exhibit the uniform resonance mode.The resonance frequencies are higher than 2 GHz.With the further increase of Al content,the coercivity become larger and the uniaxial anisotropy become lower. The dynamic characteristics are deteriorated.The reason may be the increase of stresses in the films with the increase of Al content.
(3) Thermal stability of the films is evidently improved with increase of Al content.The magnetic properties of the films with different Al content transform from soft magnetic and uniaxial anisotropic properties to hard magnetic and isotropic properties when they are annealed at the temperature higher than an optimal temperature(T_(opt)).T_(opt) clearly increases with the increase of Al content in the films.The Fe_(64.8)Co_(35.2)N film without Al become hard magnetic and isotropic properties after annealed at 200℃.No resonance show in the permeability spectrum.The(Fe_(64.8)Co_(35.2))_(86.5)Al_(13.5)N film annealed at 400℃for 60 min still remain the good soft magnetic properties,uniaxial anisotropy and uniform resonance mode of permeability spectrum.The resonance frequency is about 1.89 GHz and the real part of permeability is higher than 380 before rolloff.
(4) Saturation magnetization of the as-deposited(Fe_(64.8)Co_(35.2))_(93.8)Al_(6.2)N films does not change with the variation of film thickness.This may be due to the saturation magnetization has nothing to do with the film thickness and structure. The coercivity increase as the film thickness is gradually reduced,which may be due to the increase with the thickness,internal stress gradually decreased,the coercivity also decreases.
引文
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(3) M.MansuriPur,Physical Principles of Magneto-optical Recordings[M],Cambridge University Press,1993.
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(7) 宛德福,马兴隆,磁学物理学[M],北京:电子工业出版社,1999.
(8) 付煜,超高密度磁记录磁头材料Fe-Co薄膜的研究[D],兰州大学,2006.
(9) E.C.Stoner,and E.P.Wohlfarth,A Mechanism of Magnetic Hysteresis in Heterogeneous Alloys[J],Phil.Tran.Roy.Soc.,1948,A-240:599-642.
(10) G.Herzer,Grain structure and magnetism of nanocrystalline ferromagnets [J],IEEE Trans.Magn.1989,25(5):3327-3329.
(11) G.Herzer,Grain size dependence of coercivity and permeability in nanocrystalline ferromagnets[J],IEEE Trans.Magn.1990,26(5),1397-1402.
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