High-temperature oxidation and crystallization mechanism of Fe73.5Si13.5B9Cu1Nb3 amorphous alloy

ZHANG Xiang; SONG Yingjie; LIU Haishun; XIONG Xiang; YANG Weiming; HAN Chenkang

doi:10.7498/aps.74.20250112

Abstract

Fe-based amorphous alloys are widely used in electronic devices such as high-frequency transformers and choke cores due to their low coercivity, low loss, and high saturation magnetic induction intensity. However, these alloys have a relatively low crystallization temperature and are prone to oxidation, which limits their applications in high-temperature environments. The addition of copper and niobium elements can suppress the growth of crystal nuclei and improve thermal stability. However, the influences on the alloy's high-temperature oxidation resistance and structural evolution are still unclear. In this work, static air oxidation is used to investigate the microstructure evolution of Fe_73.5Si_13.5B₉Cu₁Nb₃ amorphous alloy after high-temperature oxidation and its influence on magnetic properties. Besides, long-time oxidation, say, 3000 hours or longer at 500 ℃, is generally hard to perform in the laboratory. Thus, the Van’t Hoff’s rule is used to evaluate outcomes under the condition of the long-time and relatively low-temperature oxidation through using rapid high-temperature oxidation. Based on Van’t Hoff’s rule, the oxidation at 650 ℃ for 5 min will show similar or more severe oxidation effects on the microstructure of Fe_73.5Si_13.5B₉Cu₁Nb₃ alloy after oxidation at 500 ℃ for 2730 h. The microstructure evolution reveals that silicon and niobium in this alloy will quickly diffuse toward the sample surface during oxidation at 650 ℃, and these two elements will form a dense layer to impede oxygen diffusion. Meanwhile, an α-Fe(Si) phase, mainly composed of iron elements, will be generated in the alloy, with its grain size slowly increasing in the oxidation process. Thermodynamic analysis indicates that the segregation of silicon and niobium can preserve the thermodynamic stability of the alloy system during oxidation and suppress the formation of intermetallic compounds during crystallization. The magnetic hysteresis loop results show that the coercivity of Fe_73.5Si_13.5B₉Cu₁Nb₃ alloy after 5-min oxidation at 650 ℃ will stay at approximately 0.3 Oe, suggesting that the Fe_73.5Si_13.5B₉Cu₁Nb₃ alloy may be a candidate for operating at 500 ℃ for more than 2700 h. Subsequently, its coercivity gradually increases to 61 Oe as the oxidation time rises to 0.5 h, while its saturation magnetic induction intensity remains unchanged (~140 emu/g).

Keywords:

Authors and contacts

1.
School of Materials Science and Physics, China University of Mining and Technology, Xuzhou 221116, China
2.
State Key Laboratory of Powder Metallurgy, Central South University, Changsha 410083, China
3.
School of Mechanics and Civil Engineering, China University of Mining and Technology, Xuzhou 221116, China

Corresponding author: LIU Haishun, Liuhaishun@cumt.edu.cn

Funds: Project supported by the National Natural Science Foundation of China (Grant Nos. 52304388, 52371167) and the State Key Laboratory of Powder Metallurgy, Central South University, China (Grant No. Sklpm-KF-008).

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References

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图 1 淬态Fe_73.5Si_13.5B₉Cu₁Nb₃非晶薄带的TEM图像 (a) 明场像和 (b) 高角环形暗场像, 插图为选区电子衍射花样(SAED)

Figure 1. TEM images of as-quenched Fe_73.5Si_13.5B₉Cu₁Nb₃ amorphous ribbon: (a) Bright-field image and (b) high-angel annular dark-field image, the inset corresponds to the selected area electron diffraction pattern.

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图 2 淬态和经650 ℃氧化后Fe_73.5Si_13.5B₉Cu₁Nb₃合金的DSC曲线

Figure 2. DSC curves of as-quenched Fe_73.5Si_13.5B₉Cu₁Nb₃ amorphous ribbon and Fe_73.5Si_13.5B₉Cu₁Nb₃ alloys after oxidation at 650 ℃.

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图 3 淬态和经过650 ℃氧化的Fe_73.5Si_13.5B₉Cu₁Nb₃合金的XRD曲线

Figure 3. X-ray diffraction patterns of as-quenched Fe_73.5Si_13.5B₉Cu₁Nb₃ amorphous ribbon and FeSiBCuNb alloys after oxidation at 650 ℃ for different times.

DownLoad: Full-Size Img PowerPoint

图 4 经过650 ℃氧化3 min后Fe_73.5Si_13.5B₉Cu₁Nb₃非晶条带内部纳米晶的TEM表征　(a) 明场像; (b) 暗场像; (c) 选区电子衍射花样; (d) 晶粒尺寸分布图

Figure 4. The TEM characterization of newly formed nanograins in the amorphous ribbon after oxidation at 650℃ for 3 min: (a) Bright-field image; (b) dark-field image; (c) selected area electron diffraction pattern; (d) grain size distribution.

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图 5 经过650 ℃氧化3 min后Fe_73.5Si_13.5B₉Cu₁Nb₃条带内部的高角环形暗场像及其对应的Fe, Si, Nb和Cu元素的分布图

Figure 5. High-angel annular dark-field image combined elemental distribution maps of Fe, Si, Nb, and Cu among the Fe_73.5Si_13.5B₉Cu₁Nb₃ ribbon after oxidation at 650 ℃ for 3 min.

DownLoad: Full-Size Img PowerPoint

图 6 经过650 ℃氧化后Fe_73.5Si_13.5B₉Cu₁Nb₃非晶条带断面的二次电子显微图像　(a)—(c) 氧化1 min后未形成氧化层; (d)—(f) 氧化1 min后已形成氧化层; (g)—(i) 氧化3 min后的典型断面

Figure 6. SEM images of the fracture surface of Fe_73.5Si_13.5B₉Cu₁Nb₃ amorphous ribbons after oxidation at 650℃: (a)–(c) 1 min, showing no obvious oxide layer, (d)–(f) 1 min, exhibiting oxide layer, and (g)–(i) 3 min.

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图 7 经过650 ℃氧化后Fe_73.5Si_13.5B₉Cu₁Nb₃合金断面的特征区域显微结构和能谱分析结果　(a) 氧化1 min; (b) 氧化3 min

Figure 7. The SEM images and EDS maps from the typical fracture surface of Fe_73.5Si_13.5B₉Cu₁Nb₃ alloy after oxidation at 650 ℃ for (a) 1 min and (b) 3 min.

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图 8 经过650 ℃氧化后Fe_73.5Si_13.5B₉Cu₁Nb₃非晶条带粉末、铁硅粉末和铁硅铝粉末　(a)—(c) VSM曲线, 其中(b), (c)为VSM曲线局部放大图; (d)饱和磁感应强度和矫顽力对比

Figure 8. (a)–(c) VSM curves, (d) M and H_c of Fe_73.5Si_13.5B₉Cu₁Nb₃ amorphous powders after oxidation at 650 ℃ for different times, compared by FeWCr and FeSi₉Al₅ powders.

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表 1 650 ℃高温氧化不同时间后非晶条带析出纳米晶晶粒尺寸计算结果

Table 1. The calculated grain size of newly formed nanograins in Fe_73.5Si_13.5B₉Cu₁Nb₃ amorphous ribbons after oxidation at 650 ℃ for different times.

Sample No.	Oxidation time at 650 ℃/min	FWHM/(°)	2θ/(°)	D_hkl/nm
650-1	1	0.960	44.7696	9.35
650-3	3	0.647	45.1310	13.89
650-5	5	0.564	45.1976	15.94
650-30	30	0.464	45.1826	19.37
650-60	60	0.415	45.1820	21.66

DownLoad: CSV

[1]	Lang R Q, Chen H Y, Zhang J R, Li H P, Guo D F, Kou J Y, Zhao J, Fang Y K, Wang X Q, Qi X W, Wang Y D, Ren Y, Wang H Z 2024 Adv. Sci. 11 2402162 Google Scholar
[2]	Panda A K, Mohanta O, Mitra A, Jiles D C, Lo C C H, Melikhov Y 2007 J. Magn. Magn. Mater. 316 e886 Google Scholar
[3]	董哲, 陈国钧, 彭伟锋, 高温应用软磁材料 2005 金属功能材料 12 35 Google Scholar Dong Z, Chen G J, Peng W F 2005 Met. Funct. Mater. 12 35 Google Scholar
[4]	熊政伟, 杨江, 王雨, 杨陆, 管弦, 曹林洪, 王进, 高志鹏 2022 物理学报 71 157502 Google Scholar Xiong Z W, Yang J, Wang Y, Yang L, Guan X, Cao L H, Wang J, Gao Z P 2022 Acta Phys. Sin. 71 157502 Google Scholar
[5]	Silveyra J M, Ferrara E, Huber D L, Monson T C 2018 Science 362 80 Google Scholar
[6]	Zhang R, Zhou C, Chen K Y, Cao K Y, Zhang Y, Tian F H, Murtaza A, Yang S, Song X P 2021 Scr. Mater. 203 114043 Google Scholar
[7]	Santhosh Kumar R, Rashmi, Sundara Rajan J 2022 IEEE International Conference on Nanoelectronics, Nanophotonics, Nanomaterials, Nanobioscience & Nanotechnology (5NANO) Kottayam, India, April 28–29, 2022 p1
[8]	Knipling K E, Daniil M, Willard M A 2009 Appl. Phys. Lett. 95 2 Google Scholar
[9]	Luo Z G, Fan X A, Zhang Y L, Yang Z J, Wang J, Wu Z Y, Liu X, Li G Q, Li Y W 2021 J. Alloy. Compd. 862 158595 Google Scholar
[10]	Du T, Varaprasad B S D C S, Guo Z, Gellman A J, Zhu J G, Laughlin D E 2021 J. Magn. Magn. Mater. 539 168347 Google Scholar
[11]	Wu L C, Li Y H, He A N, Zhu Z W, Zhang H F, Zhang W 2023 Intermetallics 163 108040 Google Scholar
[12]	Yu R H, Basu S, Ren L, Zhang Y, Parvizi-Majidi A, Unruh K M, Xiao J Q 2000 IEEE Tran. Magn. 36 3388 Google Scholar
[13]	Corodeanu S, Hlenschi C, Chiriac H, Óvári T A, Lupu N 2023 IEEE International Magnetic Conference Sendai, Japan, May 15–19, 2023
[14]	Zhou J, Li X S, Hou X B, Ke H B, Fan X D, Luan J H, Peng H L, Zeng Q S, Lou H B, Wang J G, Liu C T, Shen B L, Sun B A, Wang W H, Bai H Y 2023 Adv. Mater. 35 2304490 Google Scholar
[15]	Ma Y, Wang Q, Zhou X Y, Hao J M, Gault B, Zhang Q Y, Dong C, Nieh T G 2021 Adv. Mater. 33 2006723 Google Scholar
[16]	Shi R M, Wang Z, Han Y M 2019 AIP Adv. 9 055222 Google Scholar
[17]	Fu P X, Shi J L, Shi R C, Zhang Y Y, Qi J T, Yang Y Z 2023 Mater. Today Commun. 36 106685 Google Scholar
[18]	Wu Y, Dai Z K, Liu R R, Zhou H T 2024 J. Alloy. Compd. 981 173713 Google Scholar
[19]	Zhang Y K, Zhu J, Li S, Wang J, Ren Z M 2022 J. Mater. Sci. Technol. 102 66 Google Scholar
[20]	Kowalczyk M, Ferenc J, Liang X B, Kulik T 2006 J. Magn. Magn. Mater. 304 e651 Google Scholar
[21]	Han L L, Maccari F, Soldatov I, Peter N J, Souza Filho I R, Schafer R, Gutfleisch O, Li Z M, Raabe D 2023 Nat. Commun. 14 8176 Google Scholar
[22]	Wang Y F, Xu J, Liu Y J, Liu Z W 2022 Mater. Charact. 187 111830 Google Scholar
[23]	Silveyra J M, Illeková E 2014 J. Alloy. Compd. 610 180 Google Scholar
[24]	Shivaee H A, Golikand A N, Hosseini H R M, Asgari M 2010 J. Mater. Sci. 45 546 Google Scholar
[25]	García J A, Pierna A R, Elbaile L, Crespo R D, Vara G, Marzo F F, Tejedor M 2006 J. Non-Cryst. Solids 352 5118 Google Scholar
[26]	Zhu Z H, Yin L, Hu Q, Song H 2014 Rare Metal Mat. Eng. 43 1037 Google Scholar
[27]	Blázquez J S, Conde C F, Conde A, Roth S, Güth A 2006 J. Magn. Magn. Mater. 304 627 Google Scholar
[28]	May J E, Oliveira M F, Kuri S E 2003 Mater. Sci. Eng. A 361 179 Google Scholar
[29]	Stuart F A F C 1912 Huygens Institute-Royal Netherlands Academy of Arts and Sciences (KNAW) Amsterdam, Netherlands, March 30, 1912 p1159
[30]	余秀冬, 刘海顺, 薛琳, 张响, 杨卫明 2024 物理学报 73 98801 Google Scholar Yu X D, Liu H S, Xue L, Zhang X, Yang W M 2024 Acta Phys. Sin. 73 98801 Google Scholar
[31]	Liu H S, Du Y W, Miao X X, Han K, Shen X P, Bu W K 2008 Rare Metals 27 545 Google Scholar
[32]	Luo T, Liu H L, Huang C M, Yue G, Hou F T, Yang Y Z 2023 J Mater. Sci. Mater. Electron. 34 2167 Google Scholar
[33]	Jonghee H, Seoyeon K, Sungwoo S, Jan S, Haein C Y 2020 Metals 10 1297 Google Scholar
[34]	郭琦, 邓志旺, 朱乾科, 陈峰华, 胡勇, 张克维 2020 铸造技术 41 1005 Guo Q, Deng Z W, Zhu Q K, Chen F H, Hu Y, Zhang K W 2020 Foundry Technology 41 1005
[35]	张哲峰, 屈瑞涛, 刘增乾 2016 金属学报 52 1171 Google Scholar Zhang Z F, Qu R T, Liu Z Q 2016 Acta Metall. Sin. 52 1171 Google Scholar
[36]	Lu L, Du P C, Jiang T X, Zhou T C, Wen Q B, Wang Y L, Zeng Y, Xiong X 2025 J. Eur. Ceram. Soc. 45 116885 Google Scholar
[37]	Sun Y, Li J W, Xie L, He A N, Dong Y Q, Liu Y X, Wang C J, Zhang K W 2021 J. Non-Cryst. Solids 566 120839 Google Scholar

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High-temperature oxidation and crystallization mechanism of Fe_73.5Si_13.5B₉Cu₁Nb₃ amorphous alloy

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Corresponding author: LIU Haishun, Liuhaishun@cumt.edu.cn

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