高软磁低电导率Fe-Fe<sub>3</sub>N薄膜的N原子含量调控

陈震; 兰明迪; 李国建; 孙尚; 刘诗莹; 王强

doi:10.7498/aps.72.20221577

摘要

微电子器件具有广泛的应用前景, 为了使微电子器件具有优良的高频特性, 同时具有高饱和磁化强度、低矫顽力以及高电阻率软磁薄膜的研发成为其中的关键. 本文采用射频原子源辅助真空热蒸发方法制备了不同N原子含量的Fe-Fe₃N软磁薄膜. 高饱和磁化强度Fe₃N相含量和(102)取向度的增大, 使薄膜的饱和磁化强度增大, 相比于Fe薄膜, 饱和磁化强度提高了55.2%, 达到1705.6 emu/cm³ (1 emu/cm³ = 10³ A/m). 此外, Fe₃N(102)取向度的增大会产生较大的晶格错配, 阻碍Fe和Fe₃N晶粒的生长, 使薄膜晶粒尺寸降低, 矫顽力(50.3 Oe (1 Oe = 10³/(4π) A/m))比Fe薄膜降低了68.6%. 同时, 较大的晶格错配也会促进载流子散射, 提高了Fe-Fe₃N薄膜电阻率, 使得其电阻率(8.80 μΩ·m)比Fe薄膜增大了7倍. 因此, 本文为高饱和磁化强度、低矫顽力以及高电阻率软磁薄膜的研发提供了新方法.

关键词:

Abstract

Microelectronic devices have a wide range of application prospects. In order to make microelectronic devices that have excellent high-frequency characteristics, developing of soft magnetic films with high saturation magnetization, low coercivity and high resistivity becomes the key to the research. In this work, Fe-Fe₃N soft magnetic films with different numbers of N atoms are prepared by radio-frequency atomic source assisted vacuum thermal evaporation. Among them, the RF atom source provides N atoms with higher chemical activity than N molecules, which reduces the formation energy between Fe atoms and N atoms. The vacuum thermal evaporation is beneficial to accurately controlling the growth rate, impurity concentration and composition ratio of multiple compounds of the film at the atomic level. The combination of the two Fe aom and N atom is easier to form nitrides with Fe atoms. Thus in this way the Fe-N films with stable structure are obtained. In the prepared Fe-Fe₃N soft magnetic film, the introduction of N atoms makes the surface of the film more uniform, resulting in the increase of density. Compared with Fe, surface roughness is reduced by two times, and the crystallinity is obviously enhanced. Owing to the high saturation magnetization, the content of Fe₃N phase is increased by 29% and the (102) orientation of Fe₃N increases to 0.64. Therefore the directionality of the magnetic moment arrangement is improved. Comparing with Fe film, the saturation magnetization of the film is increased by 55.2%, reaching 1705.6 emu/cm³. In addition, with the increase of the (102) orientation of Fe₃N, a large number of lattice mismatches are produced, which impedes the growth of Fe and Fe₃N grains and reduces the grain size and anisotropy of the film. Thus the coercivity of the film decreases. The coercivity (50.3 Oe) is 68.6% lower than that of the Fe film. At the same time, the larger lattice mismatch results in the increase of heterointerface, which promotes the carrier scattering and increases the resistivity of Fe-Fe₃N thin film. The resistivity (8.80 μΩ·m) of Fe-Fe₃N thin film is 7 times higher than that of Fe thin film. Therefore, this research provides a new method for studying and developing soft magnetic films with high saturation magnetization, low coercivity and high resistivity.

Keywords:

作者及机构信息

1.
东北大学材料电磁过程研究教育部重点实验室, 沈阳　110819

2.
东北大学轧制技术及连轧自动化国家重点实验室, 沈阳　110819

3.
东北大学冶金学院, 沈阳　110819

4.
东北大学材料科学与工程学院, 沈阳　110819

5.
沈阳工业大学材料科学与工程学院, 沈阳　110870

通信作者: 李国建, gjli@epm.neu.edu.cn

基金项目: 国家重点研发计划 (批准号: 2021YFA1600204)资助的课题.

Authors and contacts

1.
Key Laboratory of Electromagnetic Processing of Materials (Ministry of Education), Northeastern University, Shenyang 110819, China

2.
State Key Laboratory of Rolling Technology and Continuous Rolling Automation, Northeastern University, Shenyang 110819, China

3.
School of Metallurgy, Northeastern University, Shenyang 110819, China

4.
School of Materials Science and Engineering, Northeastern University, Shenyang 110819, China

5.
School of Materials Science and Engineering, Shenyang University of Technology, Shenyang 110870, China

Corresponding author: Li Guo-Jian, gjli@epm.neu.edu.cn

Funds: Project supported by the National Key R&D Program of China (Grant No. 2021YFA1600204).

文章全文

参考文献

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施引文献

图 1 不同N₂流量的N发射光谱(a)以及N原子峰的面积比和峰强度图(b)

Fig. 1. N emission spectra (a) and the area ratio and peak intensity of N atom peaks at different N₂ fluxes (b)

下载: 全尺寸图片幻灯片

图 2 不同N₂流量下的Fe-Fe₃N薄膜XRD图谱

Fig. 2. XRD patterns of Fe-Fe₃N thin films under different N₂ flow rates.

下载: 全尺寸图片幻灯片

图 3 不同N₂流量下Fe-Fe₃N薄膜的N 1s (a)和Fe 2p_3/2 (b) XPS精细谱、Fe—N键与Fe—Fe键含量比(c)

Fig. 3. N 1s (a) and Fe 2p_3/2 (b) XPS fine spectra, Fe—N bond and Fe—Fe bond content ratio (c) of Fe-Fe₃N films under different N₂ flow rates.

下载: 全尺寸图片幻灯片

图 4 0 sccm薄膜和15 sccm薄膜中Fe-N体系相图^[45]和Fe和N原子的百分含量

Fig. 4. Phase diagram of Fe-N system in 0 sccm film and 15 sccm film^[45] and percentage of Fe and N atoms.

下载: 全尺寸图片幻灯片

图 5 不同N₂流量下Fe-Fe₃N薄膜的SEM表面形貌图和AFM三维形貌图　(a) 0 sccm; (b) 10 sccm; (c) 13 sccm; (d) 15 sccm

Fig. 5. SEM and AFM 3 D morphologies of Fe-Fe₃N films under different N₂ flow rates: (a) 0 sccm; (b) 10 sccm; (c) 13 sccm; (d) 15 sccm

下载: 全尺寸图片幻灯片

图 6 室温时不同N₂流量下Fe-Fe₃N薄膜面内易轴方向的M-H曲线和0 sccm薄膜、15 sccm薄膜不同方向的M-H曲线

Fig. 6. M-H curves of the in-plane easy axis direction of Fe-Fe₃N films under different N₂ flow rates at room temperature and M-H curves of 0 sccm films and 15 sccm films in different directions.

下载: 全尺寸图片幻灯片

图 7 Fe-Fe₃N薄膜晶体取向示意图

Fig. 7. Schematic diagram of crystal orientation of Fe-Fe₃N films.

下载: 全尺寸图片幻灯片

图 8 不同N₂流量下Fe-Fe₃N薄膜室温的迁移率和载流子浓度

Fig. 8. Mobility and carrier concentration of Fe-Fe₃N films at room temperature under different N₂ flow rates.

下载: 全尺寸图片幻灯片

图 9 不同N₂流量下Fe-Fe₃N薄膜室温的饱和磁化强度、矫顽力以及电阻率

Fig. 9. Room temperature saturation magnetization, coercivity and resistivity of Fe-Fe₃N films under different N₂ flow rates.

下载: 全尺寸图片幻灯片

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[2]	Huang M Q, Wu C, Jiang Y Z, Yan M 2015 J. Alloy. Compd. 644 124 Google Scholar
[3]	Shokrollahi H, Janghorban K J 2012 Mater. Process. Tech. 189 1 Google Scholar
[4]	Patelli N, Cugini F, Wang D, Sanna S, Solzi M, Hahn H, Pasquini L 2021 J. Alloy. Compd. 890 161863 Google Scholar
[5]	Kim D, Kim J, Lee J, Kang M K, Kim S, Park S H, Kim J, Choa Y H, Lim J H 2019 J. Electrochem. Soc. 166 131 Google Scholar
[6]	Swain M, Kong H, Lee J, Park S, Jeen H 2018 Mater. Res. Express 5 116104 Google Scholar
[7]	Zhang Y, Turghun M, Huang C J, Wang T, Wang F F, Shi W Z 2018 Acta Metall. Sin. Engl. 31 623 Google Scholar
[8]	Brajpuriya R, Rajan S, Jani S, Vyas A 2018 Surf. Interface Anal. 51 371 Google Scholar
[9]	Liu S Y, Ma Y H, Chang L, Li G J, Wang J H, Wang Q 2018 Thin Solid Films 651 1 Google Scholar
[10]	Li G J, Li M M, Wang J H, Du J J, Wang K, Wang Q 2017 J. Magn. Magn. Mater. 423 353 Google Scholar
[11]	Meng B Y, Yang B, Zhang X X, Zhou B H, Li X P, Yu R H 2020 Mater. Chem. Phys. 242 122478 Google Scholar
[12]	Adi W A, Yunasfi 2020 Mat. Sci. Eng. B 262 114760 Google Scholar
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[36]	Ahmad Z, Cross G B, Vernon M, Gebregiorgis D, Deocampo D, Kozhanov A 2019 Appl. Phys. Lett. 115 223101 Google Scholar
[37]	Kikuchi T, Somintac A S, Ariyada O, Wada M, Ohachi T 2006 J. Cryst. Growth 292 221 Google Scholar
[38]	Kuwano K, Nezu A, Matsuura H, Akatsuka H 2016 Jpn. J. Appl. Phys. 55 086101 Google Scholar
[39]	Agarwal S, Hoex B, Van De Sanden M C M, Maroudas D, Aydil E S 2003 Appl. Phys. Lett. 83 4918 Google Scholar
[40]	Du J J, Li G J, Wang Q, Ma Y H, Cao Y Z, He J C 2015 Vacuum 121 88 Google Scholar
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[43]	Cheng Y H, Zheng R K, Liu H, Tian Y, Li Z Q 2009 Phys. Rev. B 80 174412 Google Scholar
[44]	Lv Z Q, Fu W T, Sun S H, Wang Z H, Fan W, Qv M G 2010 Solid State Sci. 12 404 Google Scholar
[45]	Wriedt H, Gokcen G, Nafziger R H 1987 Mater. Sci. 8 355 Google Scholar
[46]	Fan X A, Wu Z Y, Li G Q, Wang J, Xiang Z D, Gan Z H 2016 Mater. Design 89 1251 Google Scholar
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[48]	Khan W, Wang Q, Jin X, Feng T F 2017 Materials 10 217 Google Scholar
[49]	杜娇娇, 李国建, 王强, 马永会, 王慧敏, 李萌萌 2015 金属学报 51 799 Google Scholar Du J J, Li G J, Wang Q, Ma Y H, Wang H M, Li M M 2015 Acta Metall. Sin. 51 799 Google Scholar
[50]	Aravindh S A, Jaya S M, Valsakumar M C, Sundar C S 2012 Superlattice. Microst. 51 92 Google Scholar
[51]	Yartseva N S, Yartsev S V, Parlebas J C 2008 Surf. Sci. 602 3388 Google Scholar
[52]	Sun Y, Gao R W, Han B P, Liu M, Han G B, Feng W C 2007 Prog. Nat. Sci-Mater. 17 131 Google Scholar
[53]	Ding J, Li Y, Chen L F, Deng C R, Shi Y, Chow Y S, Gang T B 2001 J. Alloys Compd. 314 262 Google Scholar
[54]	Herzer G 1990 IEEE. Trans. Mag. 26 1397 Google Scholar
[55]	Kronmvler H, Fischer R, Seeger M, Zern A 1996 J. Phys. D Appl. Phys. 29 2274 Google Scholar
[56]	Zhao N, Wang W, Lei X, Ye Z T, Chen X D, Ding H, Yang H 2017 J. Mater. Sci. 28 15701 Google Scholar
[57]	Gupta R, Tayal A, Amir S M, Gupta M, Gupta A, Horisberger M, Stahn J 2011 J. Appl. Phys. 111 103520 Google Scholar
[58]	Naganuma H, Nakatani R, Endo Y, Kawamura Y, Yamamoto M 2016 Sci. Technol. Adv. Mat. 5 101 Google Scholar
[59]	Mayadas A F, Shatzkes M 1970 Phys. Rev. B 1 1382 Google Scholar
[60]	Zhang Z Z, Wu S X, Niu Y, Jiang J, Wang C 2019 J. Mater. Sci. 30 5177 Google Scholar

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高软磁低电导率Fe-Fe₃N薄膜的N原子含量调控