Preparation and magnetic properties of (Ln0.2La0.2Nd0.2Sm0.2Eu0.2)MnO3 (Ln = Dy, Ho, Er) high-entropy perovskite ceramics containing heavy rare earth elements

QIN Jiedong; FENG Xingmin; WEN Zhiqin; TANG Li; LONG Defeng; ZHAO Yuhong

doi:10.7498/aps.74.20250256

Abstract

Equimolar ratio high-entropy perovskite ceramics (HEPCs) have attracted much attention due to their excellent magnetization intensity. To further enhance their magnetization intensities, (Ln_0.2La_0.2Nd_0.2Sm_0.2Eu_0.2)MnO₃ (Ln = Dy, Ho and Er, labeled as Ln-LNSEMO) HEPCs are designed based on the configuration entropy S_config, tolerance factor t, and mismatch degree σ². Single-phase HEPCs are synthesized by the solid-phase method in this work, in which the effects of the heavy rare-earth elements Dy, Ho and Er on the structure and magnetic properties of Ln-LNSEMO are systematically studied. The results show that all Ln-LNSEMO HEPCs exhibit high crystallinity and maintain excellent structural stability after sintering at 1250 ℃ for 16 h. Ln-LNSEMO HEPCs exhibit significant lattice distortion effects, with smooth surface morphology, clearly distinguishable grain boundaries, and irregular polygonal shapes. In the present work, the influences of A-site average ion radius, grain size and lattice distortion on the magnetic interactions of Ln-LNSEMO HEPCs are investigated. The three high-entropy ceramic samples exhibit hysteresis behavior at T = 5 K, with the Curie temperature T_C decreasing as the radius of the introduced rare-earth ions decreases, while the saturation magnetization and coercivity increase accordingly. When the average ionic radius of A-site decreases, the interaction between their valence electrons and local electrons in the crystal increases, thereby enhancing the conversion of electrons to oriented magnetic moments under an external magnetic field. Thus, Er-LNSEMO HEPC shows a higher saturation magnetization strength (42.8 emu/g) and coercivity (2.09 kOe) than the other samples, which is attributed to the strong magnetic crystal anisotropy, larger lattice distortion σ² (6.52×10^–3), smaller average grain size (440.49 ± 22.02 nm), unit cell volume (229.432 Å³) and A-site average ion radius (1.24 Å) of its magnet. The Er-LNSEMO HEPC has potential applications in magnetic recording materials.

Keywords:

Authors and contacts

1.
Guangxi Key Laboratory of Optoelectronic Materials and Devices, School of Materials Science and Engineering, Guilin University of Technology, Guilin 541004, China
2.
Department of Special Technology, Army Special Operations Academy, Guilin 541002, China
3.
School of Materials Science and Engineering, North University of China, Taiyuan 030051, China

Corresponding author: WEN Zhiqin, wenzhiqin@glut.edu.cn

Funds: Project supported by the Natural Science Foundation of Guangxi Province, China (Grant No. 2024GXNSFAA010415) and the Science and Technology Plan Project of Guangxi Province, China (Grant No. GuikeAD25069100).

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References

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[16]	Krawczyk P A, Salamon W, Marzec M, Szuwarzynski M, Pawlak J, Kanak J, Dziubaniuk M, Kubiak W W, Zywczak A 2023 Materials 16 4210 Google Scholar
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[29]	Alonso J A, Martinez-Lope M J, Casais M T, Fernández-Díaz M T 2000 Inorg. Chem. 39 917 Google Scholar
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Cited By

图 1 1250 ℃下煅烧所得Ln-LNSEMO陶瓷的性质　(a) A位平均离子半径; (b)容差因子t、构型熵S_config和失配度σ²的理论计算值; (c) XRD图谱; (d)—(f) Rietveld精修图谱

Figure 1. Characteristics of Ln-LNSEMO ceramics sintered at 1250 ℃: (a) Average ionic radius of A-site; (b) theoretical calculation values of tolerance factor t, configuration entropy S_config and mismatch degree σ²; (c) X-ray diffraction patterns; (d)–(f) rietveld refinement.

DownLoad: Full-Size Img PowerPoint

图 2 Ln-LNSEMO陶瓷Rietveld精修后的晶格参数(a)、晶胞体积(b)以及样品的晶体结构(c)

Figure 2. Lattice parameters (a), cell volume (b) of Ln-LNSEMO ceramics after Rietveld refinement and crystal structure of samples (c)

DownLoad: Full-Size Img PowerPoint

图 3 1250 °C下烧结的Ln-LNSEMO HEPCs的SEM图、粒度分布、EDS图谱和化学成分(%) (a), (a1) Dy-LNSEMO; (b), (b1) Ho-LNSEMO; (c), (c1) Er-LNSEMO

Figure 3. SEM micrographs, particle size distribution, EDS mapping and chemical composition (%) of Ln-LNSEMO HEPCs sintered at 1250 °C: (a), (a1) Dy-LNSEMO; (b), (b1) Ho-LNSEMO; (c), (c1) Er-LNSEMO.

DownLoad: Full-Size Img PowerPoint

图 4 Ln-LNSEMO HEPCs的高分辨率XPS光谱　(a) O 1s; (b) Mn 2p; (c) Dy 3d; (d) Ho 4d; (e) Er 4d

Figure 4. High-resolution XPS spectra of Ln-LNSEMO HEPCs: (a) O 1s; (b) Mn 2p; (c) Dy 3d; (d) Ho 4d; (e) Er 4d.

DownLoad: Full-Size Img PowerPoint

图 5 Ln-LNSEMO HEPCs的M-T曲线(a)和dM/dT-T曲线(b)

Figure 5. M-T curves (a) and dM/dT-T curves (b) of Ln-LNSEMO HEPCs.

DownLoad: Full-Size Img PowerPoint

图 6 Ln-LNSEMO HEPCs的T = 5 K时的磁滞回线(a)和低磁场区域(b)的磁化曲线

Figure 6. Hysteresis loops at T = 5 K (a), the magnified magnetization curves in the low magnetic field region (b) of Ln-LNSEMO HEPCs.

DownLoad: Full-Size Img PowerPoint

图 7 Ln-LNSEMO HEPCs的磁性能参数

Figure 7. Magnetic properties parameters of Ln-LNSEMO HEPCs.

DownLoad: Full-Size Img PowerPoint

DownLoad: Full-Size Img PowerPoint

表 1 氧化态、配位数(CN)和相应的离子半径(r)^[23]

Table 1. Oxidation state, co-ordination number (CN) and corresponding ionic radius (r)^[23].

Element Oxidation CN r/Å

La 3⁺ XII 1.36
Nd 3⁺ XII 1.27
Sm 3⁺ XII 1.24
Eu 3⁺ XII 1.22
Dy 3⁺ XII 1.19
Ho 3⁺ XII 1.18
Er 3⁺ XII 1.11
Mn 3⁺ VI 0.64
O 2^– VI 1.40

DownLoad: CSV

表 2 三组样品Rietveld精修后的键长d和键角θ

Table 2. Bond length d and bond angle θ of three groups of Rietveld refined samples.

Samples ${d _\text{Mn—O}} $/Å ${\theta _\text{Mn—O—Mn}} $/(°)

Dy-LNSEMO 1.9157(3) 148.167(6)

Ho-LNSEMO 1.9357(2) 141.748(6)

Er-LNSEMO 1.9500(3) 152.118(4)

DownLoad: CSV

map

[1]	George E P, Ritchie R O 2022 MRS Bull. 47 145 Google Scholar
[2]	Rost C M, Sachet E, Borman T, Moballegh A, Dickey E C, Hou D, Jones J L, Curtarolo S, Maria J P 2015 Nat. Commun. 6 8485 Google Scholar
[3]	Hai W X, Wu Z H, Zhang S B, Chen H, Hu L, Zhang H, Sun W Z, Liu M L, Chen Y H 2023 Int. J. Refract. Met. Hard Mater. 112 106114 Google Scholar
[4]	Zhou Q, Xu F, Gao C Z, Zhao W X, Shu L, Shi X Q, Yuen M F, Zuo D W 2023 Ceram. Int. 49 25964 Google Scholar
[5]	Zhang Y, Guo W M, Jiang Z B, Zhu Q Q, Sun S K, You Y, Plucknett K, Lin H T 2019 Scr. Mater. 164 135 Google Scholar
[6]	李汪国, 刘佃光, 王珂玮, 马百胜, 刘金铃 2022 无机材料学报 37 1289 Google Scholar Li W G, Liu D G, Wang K W, Ma B S, Liu J L 2022 J. Inorg. Mater. 37 1289 Google Scholar
[7]	Gautam A, Das S, Ahmad M I 2024 Surf. Interfaces 46 104054 Google Scholar
[8]	Xie M, Lai Y, Xiang P, Liu F, Zhang L, Liao X, Huang H, Liu Q, Wu C, Li Y 2024 Biochem. Eng. J. 496 154132 Google Scholar
[9]	Xiong W, Zhang H F, Cao S Y, Gao F, Svec P, Dusza J, Reece M J, Yan H X 2021 J. Eur. Ceram. Soc. 41 2979 Google Scholar
[10]	郭猛, 张丰年, 苗洋, 刘宇峰, 郁军, 高峰 2021 无机材料学报 36 431 Google Scholar Guo M, Zhang F N, Miao Y, Liu Y F, Yu J, Gao F 2021 J. Inorg. Mater. 36 431 Google Scholar
[11]	Sang X H, Grimley E D, Niu C N, Irving D L, LeBeau J M 2015 Appl. Phys. Lett. 106 061913 Google Scholar
[12]	Ning Y T, Pu Y P, Zhang Q W, Zhou S Y, Wu C H, Zhang L, Shi Y, Sun Z X 2023 Ceram. Int. 49 12214 Google Scholar
[13]	Medarde M L 1997 J. Phys. : Condens. Matter 9 1679 Google Scholar
[14]	史镇华, 胡新哲, 周厚博, 田正营, 胡凤霞, 陈允忠, 孙志刚, 沈保根 2025 74 027501 Google Scholar Shi Z H, Hu X Z, Zhou H B, Tian Z Y, Hu F X, Chen Y Z, Sun Z G, Shen B G 2025 Acta. Phys. Sin. 74 027501 Google Scholar
[15]	Zhao W J, Zhang M, Xue L Y, Wang K X, Yang F, Zhong J P, Chen H 2024 J. Rare Earths 42 1937 Google Scholar
[16]	Krawczyk P A, Salamon W, Marzec M, Szuwarzynski M, Pawlak J, Kanak J, Dziubaniuk M, Kubiak W W, Zywczak A 2023 Materials 16 4210 Google Scholar
[17]	Witte R, Sarkar A, Velasco L, Kruk R, Brand R A, Eggert B, Ollefs K, Weschke E, Wende H, Hahn H 2020 J. Appl. Phys. 127 185109 Google Scholar
[18]	Qin J D, Wen Z Q, Ma B, Wu Z, Lü Y, Yu J, Zhao Y H 2024 J. Magn. Magn. Mater. 597 172010 Google Scholar
[19]	Qin J D, Wen Z Q, Ma B, Wu Z Y, Yu J J, Tang L, Lu T Y, Zhao Y H 2024 Ceram. Int. 50 26040 Google Scholar
[20]	Stoica I, Abraham A R, Haghi A 2023 Modern Magnetic Materials: Properties and Applications (CRC Press
[21]	李梅, 柳召刚, 吴锦绣, 胡艳宏 2009 稀土元素及其分析化学(北京: 化学工业出版社) 第49—55页 Li M, Liu Z G, Wu J X, Hu Y H 2009 Rare Earth Elements and Their Analytical Chemistry (Beijing: Chemical Industry Press) pp49–55
[22]	Zhivulin V E, Trofimov E A, Gudkova S A, Punda A Y, Valiulina A N, Gavrilyak A M, Zaitseva O V, Tishkevich D I, Zubar T I, Sun Z, Zhou D, Trukhanov S V, Vinnik D A, Trukhanov A V 2022 Ceram. Int. 48 9239 Google Scholar
[23]	Sarkar A, Djenadic R, Wang D, Hein C, Kautenburger R, Clemens O, Hahn H 2018 J. Eur. Ceram. Soc. 38 2318 Google Scholar
[24]	Goldschmidt V M 1926 Naturwiss 14 477 Google Scholar
[25]	Shannon R D 1976 Acta Crystallogr. Sect. A 32 751 Google Scholar
[26]	Han X, Yang Y, Fan Y, Ni H, Guo Y M, Chen Y, Ou X M, Ling Y H 2021 Ceram. Int. 47 17383 Google Scholar
[27]	Liu J M, Jiang Y, Zhang W C, Cheng X, Zhao P Y, Zhen Y C, Hao Y N, Guo L M, Bi K, Wang X H 2024 Nat. Commun. 15 8651 Google Scholar
[28]	Zhang P, Gong L Y, Xu X, Lou Z H, Wei Z Y, Chen P H, Wu Z Z, Xu J, Gao F 2023 Chem. Eng. J. 472 144974 Google Scholar
[29]	Alonso J A, Martinez-Lope M J, Casais M T, Fernández-Díaz M T 2000 Inorg. Chem. 39 917 Google Scholar
[30]	Shirley D A 1972 Phys. Rev. B 5 4709 Google Scholar
[31]	Wei S Y, Chen X, Dong G Z, Liu L J, Zhang Q, Peng B L 2022 Ceram. Int. 48 15640 Google Scholar
[32]	Lin J L, Wu S, Sun K T, Li H F, Chen W, Zhang Y K, Li L W 2024 Ceram. Int. 50 51269 Google Scholar
[33]	Li A S, Wei J J, Lin J L, Zhang Y K 2024 Ceram. Int. 50 13732 Google Scholar
[34]	Pashchenko A V, Pashchenko V P, Prokopenko V K, Revenko Y F, Mazur A S, Sychova V Y, Burkhoveckiy V V, Kisel N G, Sil'cheva A G, Liedienov N A 2014 Low Temp. Phys. 40 717 Google Scholar
[35]	Kim M, Yang J, Cai Q, Zhou X, James W J, Yelon W B, Parris P E, Buddhikot D, Malik S K 2005 Phys. Rev. B: Condens. Matter 71 014433 Google Scholar
[36]	Zener C 1951 Phys. Rev. 82 403 Google Scholar
[37]	Benelli C, Gatteschi D 2002 Chem. Rev. 102 2369 Google Scholar
[38]	Majetich S A, Scott J H, Kirkpatrick E M, Chowdary K, Gallagher K, McHenry M E 1997 Nanostruct. Mater. 9 291 Google Scholar
[39]	Jiao Y T, Dai J, Fan Z H, Cheng J Y, Zheng G P, Grema L, Zhong J W, Li H F, Wang D W 2024 Mater. Today 77 92 Google Scholar
[40]	Shen J Y, Mo J J, Lu Z Y, Tao Y C, Gao K Y, Liu M, Xia Y F 2022 Physica B 644 414213 Google Scholar
[41]	Chatterjee S, Das K, Das I 2022 J. Magn. Magn. Mater. 557 169473 Google Scholar

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Preparation and magnetic properties of (Ln_0.2La_0.2Nd_0.2Sm_0.2Eu_0.2)MnO₃ (Ln = Dy, Ho, Er) high-entropy perovskite ceramics containing heavy rare earth elements