Magnetocaloric properties of additively manufacturing La(Fe, Si)<sub>1</sub><sub>3</sub>-based gradient alloys with wide temperature range

XIE Longlong; QIN Yazhou; SUN Jiayi; QIAO Kaiming; LIU Jian; ZHANG Hu

doi:10.7498/aps.74.20251317

Abstract

Magnetic refrigeration technology, featuring environmental friendliness, energy efficiency and high performance, is recognized as a next-generation refrigeration technology with the potential to replace gas compression refrigeration technology. However, current magnetic refrigeration materials typically exhibit an excessively narrow phase transition temperature range (≤10 K), thus necessitating the stacking of materials with multiple compositions to meet the practical refrigeration temperature span. In this study, the typical La(Fe, Si)₁₃-based magnetic refrigeration material is selected, and an innovative gradient laser powder bed fusion technology is adopted to obtain 3D-print La_0.70Ce_0.30Fe_11.65–xMn_xSi_1.35 alloys with horizontal compositional gradients (where the Mn content varies continuously from 0 to 0.64). Systematic characterization of their microstructures, magnetic properties, and magnetocaloric effects indicates that this technology enables a controllable gradient distribution of compositions along the powder bed plane and high-throughput preparation, thereby achieving a continuous variation of the Curie temperature of the gradient alloy over a wide temperature range from 134 K to 174 K. With the increase of Mn content, the phase transition of the alloy gradually changes from a weak first-order phase transition to a second-order phase transition, and the peak shape of the magnetic entropy change curve shifts from “sharp and high” to “broad and flat”. The full width at half maximum of the temperature range is extended to 83.3 K, allowing the gradient alloy to maintain high refrigeration capacity (RC ~130 J/kg, 3 T) at all time. This study breaks through the bottlenecks of traditional material preparation and performance via gradient additive manufacturing, providing a novel technical pathway for achieving high-throughput preparation and performance optimization of magnetic refrigeration materials.

Keywords:

Authors and contacts

1.
School of Materials Science and Engineering, University of Science and Technology Beijing, Beijing 100083, China
2.
Asia New Materials (Beijing) Co., Ltd., Beijing 100176, China
3.
School of Materials Science and Engineering, Shanghai University, Shanghai 200444, China
4.
CAS Key Laboratory of Magnetic Materials and Devices, Ningbo Institute of Material Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, China

Corresponding author: LIU Jian, liujian@shu.edu.cn ; ZHANG Hu, zhanghu@ustb.edu.cn

Funds: Project supported by the National Key Research and Development Program of China (Grant No. 2021YFB3501204), the National Natural Science Foundation of China (Grant Nos. 52171169, 52101210), the Open Fund of the State Key Laboratory for Advanced Metals and Materials, China (Grant No. 2023-ZD01), the Concept Verification Support Program of University of Science and Technology Beijing, China (Grant No. GNYZ-2024-6), and the Open Project of Sino-Foreign Humanities Exchange Research on Science, Technology and Civilization of University of Science and Technology Beijing, China (Grant Nos. 2024KFZD001, 2024KFYB004).

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References

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Cited By

图 1 La(Fe, Si)₁₃原始粉末的形状和尺寸分布　(a), (b) Mn0和Mn0.64粉末的SEM图像; (c), (d) Mn0和Mn0.64粉末的粒径分布结果

Figure 1. Morphology and size distribution of as-prepared La(Fe, Si)₁₃ powders: (a), (b) SEM images of Mn0 and Mn0.64 powders; (c), (d) particle size distribution results of Mn0 and Mn0.64 powders.

DownLoad: Full-Size Img PowerPoint

图 2 打印态CGAs的制备　(a) 制备流程图; (b) 不同形状梯度样品的宏观图像; (c) 沿梯度方向切片所得的62个样品, 编号为S1—S62

Figure 2. Preparation of as-printed CGAs: (a) Preparation flow chart; (b) macrographs of gradient samples with different shapes; (c) 62 samples obtained by slicing along the gradient direction, numbered as S1—S62.

DownLoad: Full-Size Img PowerPoint

图 3 退火态CGAs的结构和成分演变　(a) XRD图谱; (b) 通过Rietveld精修得到的对应晶格参数; (c) EDS点扫描得到的1:13相Fe和Mn含量

Figure 3. Microstructural and compositional evolution of as-annealed CGAs: (a) XRD patterns; (b) corresponding lattice parameters via Rietveld refinement; (c) Fe and Mn contents of the 1:13 phase by EDS point scanning.

DownLoad: Full-Size Img PowerPoint

图 4 退火态CGAs的磁相变　(a) 10 mT外磁场下的M-T曲线; (b) dM/dT曲线; (c) 居里温度

Figure 4. Magnetic phase transition temperatire of as-annealed CGAs: (a) M-T curves under magnetic field of 10 mT; (b) dM/dT curves; (c) Curie temperature results.

DownLoad: Full-Size Img PowerPoint

图 5 退火态CGAs在0—3 T磁场下测得的磁化等温线

Figure 5. Magnetization isotherms of as-annealed CGAs measured under a magnetic field of 0–3 T.

DownLoad: Full-Size Img PowerPoint

图 6 3 T磁场下退火态CGAs的磁熵变随温度的变化曲线

Figure 6. Temperature dependence of |ΔS_M| for CGAs under a magnetic field change of 3 T.

DownLoad: Full-Size Img PowerPoint

[1]	Xie L L, Liang C G, Qin Y Z, Zhou H, Yu Z Y, Chen H D, Naeem M Z, Qiao K M, Wen Y J, Zhang B C, Wang G F, Li X, Liu J, Franco V, Chu K, Yi M, Zhang H 2024 Adv. Func. Mater. 35 2414441 Google Scholar
[2]	张虎, 邢成芬, 龙克文, 肖亚宁陶坤, 王利晨, 龙毅 2018 物理学报 67 207501 Google Scholar Zhang H, Xing C F, Long K W, Xiao Y N, Tao K, Wang L C, Long Y 2018 Acta Phys. Sin. 67 207501 Google Scholar
[3]	Zhou H, Tao K, Chen B, Chen H D, Qiao K M, Yu Z Y, Cong J Z, Huang R J, Taskaev S V, Zhang H 2022 Acta Mater. 229 117830 Google Scholar
[4]	Chmielus M, Zhang X X, Witherspoon C, Dunand D C, Müllner P 2009 Nature Mater. 8 863 Google Scholar
[5]	Zhang H, Li Y W, Liu E K, Tao K, Wu M L, Wang Y X, Zhou H B, Xue Y J, Cheng C, Yan T, Long K W, Long Y 2017 Mater. Design 114 531 Google Scholar
[6]	Guo W H, Miao X F, Cui J Y, Torii S K, Qian F J, Bai Y Q, Kou Z D, Zha J J, Shao Y Y, Zhang Y J, Xu F, Caron L 2024 Acta Mater. 263 119530 Google Scholar
[7]	Imaizumi K, Fujita A, Suzuki A, Kobashi M, Ozaki K 2022 Acta Mater. 227 117726 Google Scholar
[8]	Beckmann B, Taubel A, Gottschall T, Pfeuffer L, Koch D, Staab F, Bruder E, Scheibel F, Skokov K P, Gutfleisch O 2025 Acta Mater. 282 120460 Google Scholar
[9]	Çakır A, Righi L, Albertini F, Acet M, Farle M 2015 Acta Mater. 99 140 Google Scholar
[10]	Fries M, Pfeuffer L, Bruder E, Gottschall T, Ener S, Diop L V B, Gröb T, Skokov K P, Gutfleisch O 2017 Acta Mater. 132 222 Google Scholar
[11]	Dan’kov S Y, Tishin A M, Pecharsky V K, Gschneidner K A 1998 Phys. Rev. B 57 3478 Google Scholar
[12]	Zhang H, Sun Y J, Niu E, Hu F X, Sun J R, Shen B G 2014 Appl. Phys. Lett. 104 062407 Google Scholar
[13]	Zhang H, Shen B G, Xu Z Y, Zheng X Q, Shen J, Hu F X, Sun J R, Long Y 2012 J. Appl. Phys. 111 07A909 Google Scholar
[14]	Miao X F, Wang C X, Liao T W, Ju S H, Zha J J, Wang W Y, Liu J, Zhang Y J, Ren Q Y, Xu F, Caron L 2023 Acta Mater. 242 118453 Google Scholar
[15]	Kang K H, Lee A Y, Ahn H, Lee W, Kim J W 2025 J. Magn. Magn. Mater. 614 172753 Google Scholar
[16]	Liu J, Gottschall T, Skokov K P, Moore J D, Gutfleisch O 2012 Nature Mater. 11 620 Google Scholar
[17]	Gottschall T, Gràcia-Condal A, Fries M, Taubel A, Pfeuffer L, Mañosa L, Planes A, Skokov K P, Gutfleisch O 2018 Nature Mater. 17 929 Google Scholar
[18]	Qiao K M, Cui Z, Hao X W, Zhao Q, Xu Y X, Wang D K, Liu J Y, Wang D D, Xia Y G, Yin W, Hao J Z, He L H, Romero-Muñiz C, Law J Y, Franco V, Ren Q Y, Zhang H 2025 Acta Mater. 297 121344 Google Scholar
[19]	Li Y, Zeng Q Q, Wei Z Y, Liu E K, Han X L, Du Z W, Li L W, Xi X K, Wang W H, Wang S G, Wu G H 2019 Acta Mater. 174 289 Google Scholar
[20]	郑新奇, 沈俊, 胡凤霞, 孙继荣, 沈保根 2016 物理学报 65 217502 Google Scholar Zheng X Q, Shen J, Hu F X, Sun J R, Shen B G 2016 Acta Phys. Sin. 65 217502 Google Scholar
[21]	Onuike B, Heer B, Bandyopadhyay A 2018 Addit. Manuf. 21 133
[22]	Wen Y J, Wu X K, Huang A K, Narayan R L, Wang P, Zhang L J, Zhang B C, Ramamurty U, Qu X H 2024 Acta Mater. 264 119572 Google Scholar
[23]	Wen Y J, Zhang B C, Narayan R L, Wang P, Song X, Zhao H, Ramamurty U, Qu X H 2021 Addit. Manuf. 40 101926
[24]	Wen Y J, Gao Y, Narayan R L, Cai W, Wang P, Wei X D, Zhang B C, Ramamurty U, Qu X H 2025 Int. J. Plasticity 189 104342 Google Scholar
[25]	Liu J, He C, Zhang M X, Yan A R 2016 Acta Mater. 118 44 Google Scholar
[26]	Shao Y Y, Liu J, Zhang M X, Yan A R, Skokov K P, Karpenkov D Y, Gutfleisch O 2017 Acta Mater. 125 506 Google Scholar
[27]	Sun Y, Lv W J, Liang Y, Gao Y, Cui W J, Yan Y J, Zhao W Y, Zhang Q J, Sang X H 2023 Scripta Mater. 223 115068 Google Scholar
[28]	Krautz M, Skokov K, Gottschall T, Teixeira C S, Waske A, Liu J, Schultz L, Gutfleisch O 2014 J. Alloys Compd. 598 27 Google Scholar
[29]	Eggert B, Lill J, Günzing D, Terwey A, Radulov I A, Wilhelm F, Rogalev A, Rovezzi M, Skokov K, Ollefs K, Gutfleisch O, Gruner M E, Wende H 2025 J. Alloys Compd. 1031 180586 Google Scholar
[30]	Zhang X, Wang K, Huang K L, Yao Q R, Lu Z, Long Q X, Deng J Q, Wang J, Zhou H Y 2024 J. Magn. Magn. Mater. 607 172379 Google Scholar
[31]	Miao L Y, Lu X, Wei Z Y, Zhang Y F, Zhang Y X, Liu J 2023 Acta Mater. 245 118635 Google Scholar
[32]	Lovell E, Pereira A M, Caplin A D, Lyubina J, Cohen L F 2014 Adv. Energy Mater. 5 1401639 Google Scholar
[33]	Lai J W, Sepehri-Amin H, Tang X, Li J, Matsushita Y, Ohkubo T, Saito A T, Hono K 2021 Acta Mater. 220 117286 Google Scholar
[34]	Liu J, Krautz M, Skokov K, Woodcock T G, Gutfleisch O 2011 Acta Mater. 59 3602 Google Scholar
[35]	杨静洁, 赵金良, 许磊, 张红国, 岳明, 刘丹敏, 蒋毅坚 2018 物理学报 67 077501 Google Scholar Yang J J, Zhao J L, Xu L, Zhang H G, Yue M, Liu D M, Jiang Y J 2018 Acta Phys. Sin. 67 077501 Google Scholar

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Magnetocaloric properties of additively manufacturing La(Fe, Si)₁₃-based gradient alloys with wide temperature range

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Corresponding author: LIU Jian, liujian@shu.edu.cn ; ZHANG Hu, zhanghu@ustb.edu.cn

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Magnetocaloric properties of additively manufacturing La(Fe, Si)13-based gradient alloys with wide temperature range

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Corresponding author: LIU Jian, liujian@shu.edu.cn ; ZHANG Hu, zhanghu@ustb.edu.cn

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Magnetocaloric properties of additively manufacturing La(Fe, Si)₁₃-based gradient alloys with wide temperature range