Mn掺杂对KNbO3和(K0.5Na0.5)NbO3无铅钙钛矿陶瓷铁电压电性能的影响

徐泽; 娄路遥; 赵纯林; 汤浩正; 刘亦轩; 李昭; 齐晓梅; 张波萍; 李敬锋; 龚文; 王轲

doi:10.7498/aps.69.20200277

摘要

(K_0.5Na_0.5)NbO₃基无铅压电陶瓷具有出色的综合铁电压电性能, 已经初步满足了部分实际应用场景的需求. 近期的研究发现, 某些元素的掺杂对优化(K_0.5Na_0.5)NbO₃基陶瓷的机电耦合性能起着至关重要的作用. 本文将MnO₂添加到KNbO₃和(K_0.5Na_0.5)NbO₃两种压电陶瓷中, 对比研究了Mn掺杂对两种陶瓷微观结构和宏观电学性能的不同影响, 分析了造成这些差异的微观物理机理. 实验结果表明, 掺杂后的两种陶瓷中均存在Mn²⁺. Mn掺杂会使KNbO₃陶瓷的铁电畴尺寸减小、居里温度降低、拉曼光谱中的振动峰宽化、相变过程变得弥散, 并呈现出束腰电滞回线和可回复的双极场致应变曲线; 在(K_0.5Na_0.5)NbO₃陶瓷中掺杂Mn后, 其性能变化却显著不同, 陶瓷的铁电畴尺寸无明显变化、居里温度未发生变化、拉曼光谱中的振动峰未发生宽化, 呈现出饱和的矩形电滞回线和不可回复的双极场致应变曲线. 这可能是因为, (K_0.5Na_0.5)NbO₃陶瓷相比KNbO₃陶瓷具有更大的离子无序度和晶格畸变, 从而使得Mn掺杂所产生的影响相对减小.

关键词:

Abstract

Potassium sodium niobate ((K_0.5Na_0.5)NbO₃)-based lead-free piezoelectric ceramics are excellent ferroelectric materials and have been demonstrated to have many practical applications. Recent studies have revealed that chemical doping plays a crucial role in optimizing the electromechanical coupling properties of (K_0.5Na_0.5)NbO₃-based piezoelectric ceramics. In this paper, MnO₂ is doped into potassium niobate (KNbO₃) and (K_0.5Na_0.5)NbO₃ piezoelectric ceramics prepared by the conventional solid-state reaction method. The influences of doped Mn cation on KNbO₃ and (K_0.5Na_0.5)NbO₃ piezoelectric ceramics including microstructure and macroscopic electrical properties are systematically investigated. The doping effects of Mn cation on the KNbO₃ and (K_0.5Na_0.5)NbO₃ piezoelectric ceramics are significantly different from each other. For the Mn-doped KNbO₃ piezoelectric ceramics, the sizes of ferroelectric domains are reduced. Meanwhile, the diffused orthorhombic-tetragonal phase transition is observed, which is accompanied by reducing dielectric loss and Curie temperature, and broadening vibration peaks in Raman spectrum. It is known that the oxygen vacancy can be formed to compensate for the charges created by the acceptor doping of Mn into the B site of perovskite, and thus forming a defect dipole with the acceptor center. From the ferroelectric measurement, a double hysteresis loop (P-E curve) and a recoverable electric-field-induced strain due to the formation of defect dipole are observed. On the contrary, for the Mn-doped (K_0.5Na_0.5)NbO₃ piezoelectric ceramics, the sizes of ferroelectric domains are not reduced. Meanwhile, the Curie temperature and vibration peaks in Raman spectrum are not changed. A rectangular hysteresis loop (P-E curve) and an unrecoverable electric-field-induced strain are observed in the ferroelectric measurement. The difference between these systems might originate from the greater ionic disorder and lattice distortion in (K_0.5Na_0.5)NbO₃ piezoelectric ceramics. The difference in ionic radius between Na⁺ and K⁺ can affect the migration and distribution of oxygen vacancies, which makes it difficult to form stable defect dipoles in the Mn-doped (K_0.5Na_0.5)NbO₃ piezoelectric ceramics. The results will serve as an important reference for preparing high-performance (K_0.5Na_0.5)NbO₃-based piezoelectric ceramics via chemical doping.

Keywords:

作者及机构信息

1.
清华大学材料学院, 新型陶瓷与精细工艺国家重点实验室, 北京　100084

2.
北京科技大学材料科学与工程学院, 北京　100083

3.
浙江清华长三角研究院, 先进陶瓷材料与器件研究中心, 嘉兴　314006

通信作者: 张波萍, bpzhang@ustb.edu.cn ; 龚文, gongwen@tsinghua-zj.edu.cn ; 王轲, wang-ke@tsinghua.edu.cn

基金项目: 国家级-国家自然科学基金优秀青年科学基金项目(51822206)

Authors and contacts

1.
State Key Laboratory of New Ceramics and Fine Processing, School of Materials Science and Engineering, Tsinghua University, Beijing 100084, China

2.
School of Materials Science and Engineering, University of Science and Technology Beijing, Beijing 100083, China

3.
Advanced Ceramic Materials & Devices Research Center, Yangtze Delta Region Institute of Tsinghua University, Zhejiang, Jiaxing 314006, China

Corresponding author: Zhang Bo-Ping, bpzhang@ustb.edu.cn ; Gong Wen, gongwen@tsinghua-zj.edu.cn ; Wang Ke, wang-ke@tsinghua.edu.cn

文章全文

参考文献

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施引文献

图 1 KN, KN-Mn, KNN和KNN-Mn陶瓷XRD图谱

Fig. 1. XRD patterns of KN, KN-Mn, KNN, and KNN-Mn ceramics.

下载: 全尺寸图片幻灯片

图 2 经热腐蚀的表面SEM形貌图　(a) KN陶瓷; (b) KN-Mn陶瓷; (c) KNN陶瓷; (d) KNN-Mn陶瓷

Fig. 2. SEM images of the thermally etched surface: (a) KN, (b) KN-Mn, (c) KNN, (d) KNN-Mn ceramics.

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图 3 (a)−(d)纵向压电响应模式(VPFM)、(e)−(h)横向压电响应模式(LPFM)下测试的未极化KN, KN-Mn, KNN, KNN-Mn陶瓷的铁电畴形貌图

Fig. 3. Domain images of unpoled KN, KN-Mn, KNN, KNN-Mn ceramics tested in (a)−(d) vertical piezoresponse force microscopy (VPFM) and (e)−(h) lateral piezoresponse force microscopy (LPFM).

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图 4 X波段ESR谱图　(a) KN-Mn陶瓷; (b) KNN-Mn陶瓷

Fig. 4. X-band ESR spectra: (a) KN-Mn ceramics; (b) KNN-Mn ceramics.

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图 5 (a) KN, KN-Mn, KNN和KNN-Mn陶瓷的拉曼散射光谱图; (b) NbO₆八面体三种内部振动模的示意图, 其中V₁和V₂为拉伸振动模、V₅为弯曲振动模

Fig. 5. (a) Raman spectra of KN, KN-Mn, KNN, KNN-Mn ceramics; (b) schematic illustration of three internal vibrational modes of NbO₆ octahedra. V₁ and V₂ are stretching modes, and V₅ is bending mode.

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图 6 陶瓷的相对介电常数和介电损耗随温度的变化　(a) KN, KN-Mn陶瓷; (b) KNN, KNN-Mn陶瓷

Fig. 6. Temperature dependence of dielectric permittivity and dielectric loss of unpoled for ceramics: (a) KN, KN-Mn ceramics; (b) KNN, KNN-Mn ceramics.

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图 7 (a) KN, (b) KN-Mn, (e) KNN, (f) KNN-Mn陶瓷的电滞回线; (c) KN, (d) KN-Mn, (g) KNN, (h) KNN-Mn陶瓷的双极场致应变曲线

Fig. 7. Polarization hysteresis loops of (a) KN, (b) KN-Mn, (e) KNN, (f) KNN-Mn ceramics; bipolar piezoelectric strain curves of (c) KN, (d) KN-Mn, (g) KNN, (h) KNN-Mn ceramics.

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表 1 KN, KN-Mn, KNN和KNN-Mn陶瓷的相对密度、压电性能和介电性能

Table 1. Relative density, piezoelectric and dielectric properties of KN, KN-Mn, KNN, and KNN-Mn ceramics.

d₃₃/pC·N^–1 Relative density/% k_p Q_m θ_max/(°) tanδ ε_r (1 kHz)

KN 90 92.0 0.26 177 66 0.042 576
KN-Mn 83 95.1 0.27 185 77 0.015 526
KNN 115 94.9 0.29 85 64 0.060 393
KNN-Mn 109 94.3 0.32 330 83 0.024 355

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[26]	Standards Committee of the IEEE Ultrasonics, Ferroelectrics, and Frequency Control Society 1988 IEEE Standard on Piezoelectricity (New York: IEEE) ANSI/IEEE Std. 176-1987
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[39]	刘霄, 徐小敏, 杜慧玲 2018 无机材料学报 33 683 Google Scholar Liu X, Xu X M, Du H L 2018 J. Inorg. Mater. 33 683 Google Scholar
[40]	Lee D, Jeon B C, Baek S H, Yang J S, Kim T H, Kim Y S, Yoon J G, Eom C B, Noh T W 2012 Adv. Mater. 24 6490 Google Scholar
[41]	Ren X 2004 Nat. Mater. 3 91 Google Scholar
[42]	Feng Z, Ren X 2007 Appl. Phys. Lett. 91 032904 Google Scholar
[43]	Voas B K, Usher T M, Liu X, Li S, Jones J L, Tan X, Cooper V R, Beckman S P 2014 Phys. Rev. B 90 024105 Google Scholar
[44]	Steiner S, Seo I T, Ren P, Li M, Keeble D J, Frömling T 2019 J. Am. Ceram. Soc. 102 5295 Google Scholar
[45]	Herber R P, Schneider G A, Wagner S, Hoffmann M J 2007 Appl. Phys. Lett. 90 252905 Google Scholar
[46]	Nakamura K, Tokiwa T, Kawamura Y 2002 J. Appl. Phys. 91 9272 Google Scholar
[47]	Qin Y, Zhang J, Yao W, Wang C, Zhang S 2015 J. Am. Ceram. Soc. 98 1027 Google Scholar

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Mn掺杂对KNbO₃和(K_0.5Na_0.5)NbO₃无铅钙钛矿陶瓷铁电压电性能的影响