Giant electrocaloric effect enhancement due to the polarization flip and influence of Mn4+ doping on the dielectric, ferroelectric properties in 0.7BiFeO3-0.3BaTiO3 ceramics

Tang Hui; Niu Xiang; Yang Zhi-Peng; Peng Xiao-Cao; Zhao Xiao-Bo; Yao Ying-Bang; Tao Tao; Liang Bo; Tang Xin-Gui; Lu Sheng-Guo

doi:10.7498/aps.71.20220280

Abstract

As a kind of ferroelectric and antiferromagnetic coexistent multi-ferroic material, BiFeO₃ (BFO) has a theoretical saturation polarization over 100 μC/cm², and a Curie temperature of 830 ℃, which may offer a huge electrocaloric effect. However, owing to the evaporation of Bi₂O₃ in the sintering process at high temperatures and the variation of chemical valence of iron ions, there are lots of point defects and also a large leakage current existing in BFO, making the ferroelectricity of BFO hard to develop and measure. Although the forming of solid solution with BaTiO₃ (BTO) or other oxide ferroelectrics may mitigate the leakage current, high loss tangent is still existent. This work tries to address this issue by adding manganese ions into the BFO-BTO solid solution. The 0.7(BFO)-0.3(BTO)+x%MnO₂ ceramics are prepared through using the conventional solid-state reaction at high temperature. The microstructure, dielectric characteristic and ferroelectric characteristic are investigated by doping different Mn⁴⁺ ions. Results indicate that the crystallographic structure is of rhombohedral and pseudocubic phase coexistence. It is observed that a certain content of Mn⁴⁺ ions may lead both the loss tangent and the leakage current for BFO-BTO ceramic to decrease, which is due to the compensation of dopant Mn⁴⁺ ions for the oxygen vacancies. In addition, the 0.7BFO-0.3BTO+0.5%MnO₂ ceramic arrives at a maximum polarization of 50.53 μC/cm² at 100 kV/cm. Finally, a direct approach is used to measure the electrocaloric effect. It is found that using the polarization flip method, the ECE temperature change is observed to increase almost 8 times when the electric field changes from 0 to –30 kV/m with respect to that when the electric field decreases from 30 kV/cm to 0. This verifies that the Lu et al’s method is also applicable to polycrystalline first-order phase transition ferroelectrics.

Keywords:

Authors and contacts

1.
Guangdong Provincial Key Laboratory of Functional Soft Condensed Matter, Guangdong Provincial Research Center on Smart Materials and Energy Conversion Devices, School of Materials and Energy, Guangdong University of Technology, Guangzhou 510006, China
2.
School of Physics and Optoelectronic Engineering, Guangdong University of Technology, Guangzhou 510006, China

Corresponding author: Lu Sheng-Guo, sglu@gdut.edu.cn

Funds: Project supported by the National Natural Science Foundation of China (Grant Nos. 51372042, 51872053), the Guangdong Provincial Natural Science Foundation, China (Grant No. 2015A030308004), the NSFC-Guangdong Joint Fund, China (Grant No. U1501246), the Dongguan City Frontier Research Project, China (Grant No. 2019622101006), and the Advanced Energy Science and Technology Guangdong Provincial Laboratory Foshan Branch-Foshan Xianhu Laboratory Open Fund-Key Project, China (Grant No. XHT2020-011).

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References

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图 1 BFO-BTO+x%MnO₂陶瓷的XRD图谱　(a) x = 0; (b) x = 0.05; (c) x = 0.10; (d) x = 0.20; (e) x = 0.50; (f) x = 1.00

Figure 1. XRD patterns of BFO-BTO+x%MnO₂ samples: (a) x = 0; (b) x = 0.05; (c) x = 0.10; (d) x = 0.20; (e) x = 0.50; (f) x = 1.00.

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图 2 BFO-BTO+x%MnO₂陶瓷的Mn 2pXPS图谱　(a) x = 0.20; (b) x = 0.50; (c) x = 1.00

Figure 2. Mn 2p XPS spectrums of BFO-BTO+x%MnO₂ samples: (a) x = 0.20; (b) x = 0.50; (c) x = 1.00.

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图 3 BFO-BTO+x%MnO₂陶瓷的SEM形貌图　(a) x = 0; (b) x = 0.05; (c) x = 0.10; (d) x = 0.20; (e) x = 0.50; (f) x = 1.00

Figure 3. SEM images of BFO-BTO+x%MnO₂ samples: (a) x = 0; (b) x = 0.05; (c) x = 0.10; (d) x = 0.20; (e) x = 0.50; (f) x = 1.00.

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图 4 BFO-BTO+x%MnO₂陶瓷在不同频率不同温度下的介电常数和介电损耗　(a) x = 0; (b) x = 0.05; (c) x = 0.10; (d) x = 0.20; (e) x = 0.50; (f) x = 1.00

Figure 4. Permittivity and loss tangent as a function of temperature and frequency for BFO-BTO+x%MnO₂ samples: (a) x = 0; (b) x = 0.05; (c) x = 0.10; (d) x = 0.20; (e) x = 0.50; (f) x = 1.00.

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图 5 (a) BFO-BTO+x%MnO₂陶瓷在不同频率的介电损耗; (b) BFO-BTO+x%MnO₂陶瓷在50 kV/cm 时的漏电流

Figure 5. (a) $\varepsilon_{\rm{r}} $ and tanδ as a function of frequency for BFO-BTO+x%MnO₂ samples; (b) the leakage current for BFO-BTO+x%MnO₂ samples at 50 kV/cm.

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图 6 BFO-BTO+x%MnO₂陶瓷在不同电场下的室温电滞回线　(a) x = 0; (b) x = 0.05; (c) x = 0.10; (d) x = 0.20; (e) x = 0.50; (f) x = 1.00

Figure 6. The P-E hysteresis loops for BFO-BTO+x%MnO₂ samples with different electric fields at room temperature: (a) x = 0; (b) x = 0.05; (c) x = 0.10; (d) x = 0.20; (e) x = 0.50; (f) x = 1.00.

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图 7 (a) Mn0陶瓷在直测电卡时的电压变化; (b) Mn0陶瓷在电场从+30 kV/cm至0 kV/cm和0 kV/cm至–30 kV/cm过程中的直测电卡; (c) BFO-BTO+x%MnO₂陶瓷在不同电场直测电卡和电场转变从+30—–30 kV/cm时电畴翻转的直测电卡; (d) BFO-BTO陶瓷在电场40 kV/cm和50 kV/cm 时不同温度下直测电卡; (e) Mn0陶瓷在电场40 kV/cm和50 kV/cm 时不同温度下直测电卡电卡强度ΔT/E; (f) Mn0陶瓷理论计算的电卡强度ΔT/E

Figure 7. (a) The change of electric field when the electrocaloric of Mn0 ceramics measured; (b) the direct measurement electrocaloric ΔT of Mn0 ceramics during the electric field changes from +30 kV/cm to 0 kV/cm and 0 kV/cm to –30 kV/cm; (c) the ΔT of BFO-BTO + x% MnO₂ ceramics at different electric field and the ΔT of BFO-BTO + x% MnO₂ ceramics with polarization flip during the electric field changes from +30 kV/cm to –30 kV/cm; (d) the ΔT of BFO-BTO ceramics at different temperatures under 40 kV/cm and 50 kV/cm; (e) the ΔT/E of Mn0 ceramics at different temperatures under 40 kV/cm and 50 kV/cm; (f) the theoretical ΔT/E of Mn0 ceramics.

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表 1 BFO-BTO+x%MnO₂样品的精修参数

Table 1. The refined retrieved lattice parameters, volumes and R factors for BFO-BTO+x%MnO₂ ceramics.

x	相成分/%		晶格参数/Å			晶胞体积/Å³		R 因子
	相成分/%		a	c	a	晶胞体积/Å³		R 因子
	R	PC	R		PC	R	PC	R_wp/%	R_wp/%	χ²
0	75.64	24.36	5.6400(2)	13.8964(0)	3.9893(6)	382.92	63.49	6.98	4.65	2.37
0.05	72.97	27.03	5.6411(7)	13.8983(8)	3.9902(5)	383.03	63.53	5.91	4.06	1.45
0.10	72.70	27.30	5.6390(5)	13.8909(8)	3.9938(5)	382.54	63.71	5.23	3.81	1.24
0.20	68.48	31.62	5.6398(2)	13.8962(4)	3.9911(4)	382.79	63.58	6.39	4.49	1.85
0.50	67.21	32.79	5.6458(1)	13.8768(6)	3.9898(0)	383.07	63.51	5.80	4.09	1.50
1.00	66.41	33.59	5.6487(1)	13.8299(8)	3.9914(5)	382.17	63.59	5.88	4.35	1.36

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[1]	Nan C W 2015 Sci. Sin. Tech. 45 339 Google Scholar
[2]	Meng K, Li W, Tang X G, Liu Q X, Jiang Y P 2021 ACS Appl. Electron. Mater. 4 9216 Google Scholar
[3]	Khasbulatov S, Kallaev S, Gadjiev H, Omarov Z, Bakmaev A, Verbenko I, Pavelko A, Reznichenko L 2020 J. Adv. Dielectr. 10 2060019 Google Scholar
[4]	Wang D W, Wang G, Murakami S, Fan Z, Feteira A, Zhou D, Sun S, Zhao Q, Reaney I M 2018 J. Adv. Dielectr. 8 1830004 Google Scholar
[5]	Xun B, Song A, Yu J, Yin Y, Li J F, Zhang B P 2021 ACS Appl. Mater. Interfaces 13 4192 Google Scholar
[6]	Kim A Y, Lee Y J, Kim J S, Han S H, Kang H W, Lee H G, Cheon C I 2012 J. Korean Phys. Soc. 60 83 Google Scholar
[7]	Wang D, Wang M, Liu F, Cui Y, Zhao Q, Sun H, Jin H, Cao M 2015 Ceram. Int. 41 8768 Google Scholar
[8]	Neaton J B, Ederer C, Waghmare U V, Spaldin N A, Rabe K M 2005 Phys. Rev. B 71 014113 Google Scholar
[9]	Lebeugle D, Colson D, Forget A, Vire M 2007 Appl. Phys. Lett. 91 022907 Google Scholar
[10]	Khesro A, Boston R, Sterianou I, Sinclair D C, Reaney I M 2016 J. Appl. Phys. 119 054101 Google Scholar
[11]	Leontsev S O, Eitel R E 2009 J. Am. Ceram. Soc. 92 2957 Google Scholar
[12]	Kumar M M, Srinivas A, Suryanarayana S V 2000 J. Appl. Phys. 87 855 Google Scholar
[13]	Chaudhary P, Shukla R, Dabas S, Thakur O P 2021 J. Alloys Compd. 869 159228 Google Scholar
[14]	Wan Y, Li Y, Li Q, Zhou W, Zheng Q, Wu X, Xu C, Zhu B, Lin D, Jones J 2014 J. Am. Ceram. Soc. 97 1809 Google Scholar
[15]	Chen Z, Bai X, Wang H, Du J, Bai W, Li L, Wen F, Zheng P, Wu W, Zheng L, Zhang Y 2020 Ceram. Int. 46 11549 Google Scholar
[16]	Lu Z, Wang G, Bao W, Li J, Li L, Mostaed A, Yang H, Ji H, Li D, Feteira A, Xu F, Sinclair D C, Wang D, Liu S Y, Reaney I M 2020 Energy Environ. Sci. 13 2938 Google Scholar
[17]	Calisir I, Amirov A A, Kleppe A K, Hall D A 2018 J. Mater. Chem. A 6 5378 Google Scholar
[18]	Liu X H, Xu Z, Qu S B, Wei X Y, Chen J L 2008 Ceram. Int. 34 797 Google Scholar
[19]	Yang H, Zhou C, Liu X, Zhou Q, Chen G, Li W, Wang H 2013 J. Eur. Ceram. Soc. 33 1177 Google Scholar
[20]	Li Q, Wei J X, Cheng J R, Chen J G 2017 J. Mater. Sci. 52 229 Google Scholar
[21]	Li Q, Cheng J R, Chen J G 2017 J. Mater. Sci. :Mater. Electron. 28 1370 Google Scholar
[22]	Alpay S P, Mantese J, Trolier-McKinstry S, Zhang Q, Whatmore R W 2014 MRS Bull. 39 1099 Google Scholar
[23]	Jian X D, Lu B, Li D D, Yao Y B, Tao T, Liang B, Guo J H, Zeng Y J, Chen J L, Lu S G 2018 ACS Appl. Mater. Interfaces 10 4801 Google Scholar
[24]	Neese B, Chu B, Lu S G, Wang Y, Furman E, Zhang Q M 2008 Science 321 821 Google Scholar
[25]	鲁圣国, 李丹丹, 林雄威, 简晓东, 赵小波, 姚英邦, 陶涛, 梁波 2020 物理学报 69 127701 Google Scholar Lu S G, Li D D, Lin X W, Jian X D, Zhao X B, Yao Y B, Tao T, Liang B 2020 Acta Phys. Sin. 69 127701 Google Scholar
[26]	Larson A C, Von Dreele R B 2004 General Structure Analysis System (GSAS) Los Alamos: Los Alamos National Laboratory Report LAUR p86
[27]	Toby H 2001 J. Appl. Crystallogr. 34 210 Google Scholar
[28]	Niu X, Jian X, Chen X, Li H, Liang W, Liang B, Lu S G 2021 J. Adv. Ceram. 10 482 Google Scholar
[29]	Dicastro V, Polzobetti G 1989 J. Electron Spectrosc. Relat. Phenom. 48 117 Google Scholar
[30]	Allen G C, Harris S J, Jutson J A 1989 Appl. Surf. Sci. 37 111 Google Scholar
[31]	Zhang X, Hu D, Pan Z, Lv X, He Z, Yang F, Li P, Liu J, Zhai J 2021 Chem. Eng. J. 406 126818 Google Scholar
[32]	Basso V, Gerard J F, Pruvost S 2014 Appl. Phys. Lett. 105 052907 Google Scholar
[33]	Lu B, Jian X, Lin X, Yao Y, Tao T, Liang B, Luo H, Lu S G 2020 Crystals 10 451 Google Scholar

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Giant electrocaloric effect enhancement due to the polarization flip and influence of Mn⁴⁺ doping on the dielectric, ferroelectric properties in 0.7BiFeO₃-0.3BaTiO₃ ceramics

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Corresponding author: Lu Sheng-Guo, sglu@gdut.edu.cn

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