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通过两步固相反应烧结法制备了(1–x) Pb0.99Nb0.02[(Zr0.57Sn0.43)0.94Ti0.06]0.98O3:xAlN ((1–x)PNZST:xAlN, x = 0, 0.1, 0.2, 0.3, 0.4))复合陶瓷, 系统研究了复合陶瓷晶体结构、微观形貌、畴结构演变以及铁电、介电和热释电性能等. 实验结果表明: 基于两相之间热膨胀系数失配产生的局域应力场有效调控了畴结构组态和相结构演变, 在室温附近构建了铁电/反铁电相界, 继而在温度场作用下表现出优异的热释电性能; 当x = 0.1时, 在近人体温度37 ℃时其热释电系数p达到最大值3.30×10–3 C/(m2⋅K), 电流响应优值Fi = 3.16 × 10–9 m/V, 电压响应优值Fv = 0.613 m2/C, 探测率优值Fd = 4.40×10–4 Pa–1/2, 且其半峰宽为16.3 ℃, 在室温宽温域内表现出优异的热释电性能; 随着AlN含量的增多, 该复合陶瓷的热释电峰值温度在37—73 ℃宽温域内可调, 表现出良好的温度稳定性.In this work, composite ceramics (1–x)Pb0.99Nb0.02[(Zr0.57Sn0.43)0.94Ti0.06]0.98O3:xAlN (abbreviated (1–x)PNZST:xAlN, x = 0, 0.1, 0.2, 0.3 and 0.4) are prepared by a two-step solid phase synthesis method. The crystal structures, micromorphologies, domain structure evolutions, ferroelectric, dielectric and pyroelectric properties of those composite ceramics are systematically investigated. The results show that the difference in thermal expansion coefficient between PNZST and AlN creates compressive stresses in the PNZST matrix when cooling down from the sintering temperature, then a metastable ferroelectric (FE) phase is induced in the anti-FE matrix by the AlN component-induced internal stress, and in turn ferroelectric/antiferroelectric phase boundary is constructed near room temperature. As the temperature increases, the ferroelectric-to-antiferroelectric phase transition causes a larger pyroelectric current peak. In particular, the composition with x = 0.1 exhibits a high pyroelectric coefficient p = 3.3×10–3 C⋅m–2⋅K–1 and figure-of-merit with current responsivity Fi = 3.16×10–9 m⋅V–1, voltage responsivity Fv = 0.613 m2⋅C–1, and detectivity Fd = 4.4×10–4 Pa–1/2 around human body temperature. Moreover, the enhanced pyroelectric coefficient exists in a broad operation temperature range with a large full width at half maximums of 16.3 ℃ at 37 ℃. With the increase of AlN content, the pyroelectric peak temperature of the composite ceramic is adjustable in a wide temperature range of 37–73 ℃, showing good temperature stability.
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Keywords:
- pyroelectricity /
- composite ceramics /
- local stress field /
- ferroelectric domain
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图 1 不同组分的(1–x)PNZST:xAlN (x = 0.1, 0.2, 0.3, 0.4)复合陶瓷的XRD谱和(111)与(200)衍射峰的放大图谱
Fig. 1. XRD patterns of (1–x)PNZST:xAlN (x = 0.1, 0.2, 0.3, 0.4) ceramics, enlarged (111) and (200) diffraction peaks.
图 2 (1–x)PNZST:xAlN (x = 0, 0.1, 0.2, 0.3和0.4)陶瓷的(a)—(e) SEM图像和(f)晶粒尺寸分布 (a) x = 0; (b) x = 0.1; (c) x = 0.2; (d) x = 0.3; (e) x = 0.4; (f)平均晶粒尺寸随AlN含量变化的关系
Fig. 2. The SEM images (a)–(e) and grain size distribution (f) of (1–x)PNZST:xAlN: (a) x = 0; (b) x = 0.1; (c) x = 0.2; (d) x = 0.3; (e) x = 0.4; (f) the composition dependence of average grain size.
图 3 0.9PNZST:0.1ZnO的(a) SEM图像; (b)—(h) Pb, Nb, Zr, Ti, O, Al和N元素分布(比例尺: 2.5 µm)
Fig. 3. Typical SEM micrograph (a) and element distribution of Pb, Nb, Zr, Ti, O, Al and N (b)–(h) for 0.9PNZST:0.1ZnO (scale bar: 2.5 µm).
图 4 (1–x)PNZST:xAlN陶瓷在直流电压为0, 10, 20, 30和40 V极化后的室温振幅图和相位图 (a) x = 0; (b) x = 0.1
Fig. 4. Room temperature out-of-plane amplitude and phase images of (1–x)PNZST:xAlN ceramics after poling with the DC voltage of 0, 10, 20, 30 and 40 V: (a) x = 0; (b) x = 0.1.
图 5 (a)—(e)不同组分(1–x)PNZST:xAlN (x = 0, 0.1, 0.2, 0.3, 0.4)陶瓷样品极化后的介电温谱和(f)铁电-反铁电相转变温度TFE-AFE
Fig. 5. Temperature-dependent dielectric properties (a)–(e) and the composition dependent TFE-AFE (f) of (1–x)PNZST:xAlN (x = 0, 0.1, 0.2, 0.3, 0.4) composite.
图 6 不同组分(1–x)PNZST:xAlN陶瓷样品在室温不同电场下的P-E (a)—(e)和J-E (f)—(j)曲线 (a), (f) x = 0; (b), (g) x = 0.1; (c), (h) x = 0.2; (d), (i) x = 0.3; (e), (j) x = 0.4
Fig. 6. Electric field-dependent P-E loops (a)–(e) and J-E (f)–(j) curves of (1–x)PNZST:xAlN composite at room temperature: (a), (f) x = 0; (b), (g) x = 0.1; (c), (h) x = 0.2; (d), (i) x = 0.3; (e), (j) x = 0.4.
图 7 不同组分(1–x)PNZST:xAlN陶瓷样品在不同电场下的P-E (a)—(d)和J-E (e)—(h)曲线 (a), (e) x = 0.1; (b), (f) x = 0.2; (c), (g) x = 0.3; (d), (h) x = 0.4
Fig. 7. Temperature-dependent P-E loops (a)–(d) and J-E curves (e)–(h) of (1–x)PNZST:xAlN composite at room temperature: (a), (e) x = 0.1; (b), (f) x = 0.2; (c), (g) x = 0.3; (d), (h) x = 0.4.
图 8 不同组分(1–x)PNZST:xAlN(x = 0, 0.1, 0.2, 0.3, 0.4)陶瓷样品随温度变化的热释电系数值
Fig. 8. Temperature-dependent pyroelectric coefficient of (1–x)PNZST:xAlN (x = 0, 0.1, 0.2, 0.3 and 0.4) composite.
表 1 PNZST:AlN复合陶瓷与其他已报道的无铅材料和PZT基材料的热释电性能参数比较
Table 1. Comparison of the pyroelectric parameters of PNZST:AlN ceramics, other reported lead-free materials and PZT-based materials.
材料组成 介电常数εr 介电损耗tanδ 热释电系数p/
(10–4 C·m–2·K–1)电流优值因子Fi/
(10–10 m·V–1)电压优值因子Fv/
(10–2 m2·C–1)探测率优值因子Fd/
(10–5 Pa–1/2)文献 TGS 55 0.025 5.5 2.12 43 6.1 [1] LiTaO3 crystal 47 0.0005 2.3 0.72 17 15.7 [1] PVDF 11 0.02 0.3 0.13 13.4 0.9 [35] BNT-BT 403 0.011 2.42 2.68 1.53 [2] BNT-BT-ST 1278 0.109 5.7 2.08 1.8 0.589 [2] PLZT 511 0.014 4.0 1.66 3.6 2.07 [36] KNN-BKT 980 0.035 2.18 0.994 1.14 0.57 [37] BNT-BA-KNN 514 0.029 3.7 1.32 2.89 1.15 [38] BCT-BST 3500 0.025 2.05 1 0.32 0.41 [39] CSBN 328 0.033 1.24 0.6 2.03 0.61 [40] PZT-based 290 0.0027 3.8 6.0 5.8 [2] KBT-BT-NBT 660 0.23 2.58 0.92 1.5 0.53 [34] PIMNT film 2824 0.004 8.5 3.40 1.4 1.03 [11] x = 0.1 583.6 0.01 33.0 31.6 61.3 44.0 本工作 
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[1] Liu Z, Lu T, Dong X, Wang G, Liu Y 2021 IEEE Trans. Ultrason. Ferr. 68 242
Google Scholar
[2] Jia J, Guo S, Yan S, Cao F, Yao C, Dong X, Wang G 2019 Appl. Phys. Lett. 114 032902
Google Scholar
[3] Whatmore R W 1986 Rep. Prog. Phys. 49 1135
Google Scholar
[4] Wang Y, Yuan G, Luo H, Li J, Viehland D 2017 Phys. Rev. Appl. 8 034032
Google Scholar
[5] Domingo N, Bagués N, Santiso J, Catalan G 2015 Phys. Rev. B 91 094111
Google Scholar
[6] Pandya S, Wilbur J, Kim J, Gao R, Dasgupta A, Dames C, Martin L W 2018 Nat. Mater. 17 432
Google Scholar
[7] Yang M M, Luo Z D, Mi Z, Zhao J, Sharel P E, Alexe M 2020 Nature 584 377
Google Scholar
[8] 郭少波, 闫世光, 曹菲, 姚春华, 王根水, 董显林 2020 69 127708
Google Scholar
Guo S B, Yan S G, Cao F, Yao C H, Wang G S, Dong X L 2020 Acta Phys. Sin. 69 127708
Google Scholar
[9] Xu Y Q, Wu N J, Ignatiev A 2000 J. Appl. Phys. 88 1004
Google Scholar
[10] Zhang S, Lebrun L, Jeong D Y, Randall C A, Zhang Q, Shrout T R 2003 J. Appl. Phys. 93 9257
Google Scholar
[11] Huang X, Tang Y, Wang F, Ming Leung C, Zhao X, Qin X, Wang T, Duan Z, Wu Y, Wang J, Shi W 2022 J. Am. Ceram. Soc. 105 327
Google Scholar
[12] He H, Lu X, Hanc E, Chen C, Zhang H, Lu L 2020 J. Mater. Chem. C 8 1494
Google Scholar
[13] Song K, Ma N, Mishra Y K, Adelung R, Yang Y 2019 Adv. Electron. Mater. 5 1800413
Google Scholar
[14] Srikanth K S, Singh V P, Vaish R 2017 J. Eur. Ceram. Soc. 37 3943
Google Scholar
[15] Patel S, Weyland F, Tan X, Novak N 2018 Energy Technology 6 865
Google Scholar
[16] Li L, Liu H, Wang R X, Zhang H, Huang H, Lu M H, Zhang S T, Jiang S, Wu D, Chen Y F 2020 J. Mater. Chem. C 8 7820
Google Scholar
[17] Liu B, Li L, Zhang S T, Zhou L, Tan X 2022 J. Am. Ceram. Soc. 105 794
Google Scholar
[18] Riemer L M, Lalitha K V, Jiang X, Liu N, Dietz C, Stark R W, Groszewicz P B, Buntkowsky G, Chen J, Zhang S T, Rodel J, Koruza J 2017 Act. Mater. 136 271
Google Scholar
[19] Yin J, Wang Y, Zhang Y, Wu B, Wu J 2018 Act. Mater. 158 269
Google Scholar
[20] Tabary P, Servant C, Alary J A 2000 J. Eur. Ceram. Soc. 20 913
Google Scholar
[21] 田野, 靳立, 冯玉军, 庄永勇, 徐卓, 魏晓勇 2017 物理学进展 37 155
Tian Y, Jin L, Feng Y J, Zhuang Y Y, Xu Z, Wei X 2017 Prog. Phys. 37 155
[22] Wang H, Jiang B, Thomas R S, Cao W 2004 IEEE Trans. Ultrason. Ferr. 51 908
Google Scholar
[23] Lee H J, Zhang S, Luo J, Li F, Shrout T R 2010 Adv. Funct. Mater. 20 3154
Google Scholar
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Google Scholar
[25] You D, Tan H, Yan Z, Gao H, Chen S, Ma W, Fan P, Tran N M, Liu Y, Salamon D, Zhang H 2022 ACS Appl. Mater. Inter. 14 17652
Google Scholar
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Google Scholar
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Google Scholar
[28] Frederick J, Tan X, Jo W 2011 J. Am. Ceram. Soc. 94 1149
Google Scholar
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Google Scholar
[30] Tan X, Frederick J, Ma C, Jo W, Rodel J 2010 Phys. Rev. Lett. 105 255702
Google Scholar
[31] Yang X, Zhuo F, Wang C, Liu Y, Wang Z, He C, Long X 2020 Act. Mater. 186 523
Google Scholar
[32] Li S, Nie H, Wang G, Liu N, Zhou M, Cao F, Dong X 2019 J. Mater. Chem. C 7 4403
Google Scholar
[33] Zhou M, Liang R, Zhou Z, Dong X 2019 J. Am. Ceram. Soc. 103 193
Google Scholar
[34] Thakre A, Maurya D, Kim D Y, Kim Y, Sriboriboon P, Yoo I R, Priya S, Cho K H, Song H C, Ryu J 2021 J. Eur. Ceram. Soc. 41 2524
Google Scholar
[35] Whatmore R W 2021 Encyclopedia Mater. Tech. Ceram. Glasses 3 139
[36] Qiao P, Zhang Y, Chen X, Zhou M, Wang G, Dong X 2019 Ceram. Int. 45 7114
Google Scholar
[37] Jiang X P, Chen Y, Lam K H, Choy S H, Wang J 2010 J. Alloys Compd. 506 323
Google Scholar
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Google Scholar
[39] Srikanth K S, Patel S, Steiner S, Vaish R 2018 Scr. Mater. 146 146
Google Scholar
[40] Chen H, Guo S, Dong X, Cao F, Mao C, Wang G 2017 J. Alloys Compd. 695 2723
Google Scholar
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