硅酸盐学报

（1-x）（0.75K_0.5Bi_0.5TiO₃-0.25BiFeO₃）-xNa_0.73Bi_0.09NbO₃电介质陶瓷的微观结构与储能性能

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盛林生 ¹ , 沈超 ² , 姜梦琦 ¹ , 杨光 ¹ , 郑鹏 ³ , 白王峰 ⁴

硅酸盐学报 | 电介质储能材料专刊—研究论文 2024,52(4): 1335-1344

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硅酸盐学报 |电介质储能材料专刊—研究论文 2024 , 52 (4) : 1335 -1344

（1-x）（0.75K_0.5Bi_0.5TiO₃-0.25BiFeO₃）-xNa_0.73Bi_0.09NbO₃电介质陶瓷的微观结构与储能性能

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盛林生¹, 沈超², 姜梦琦¹, 杨光¹, 郑鹏³, 白王峰⁴

作者信息

^1．嘉兴南湖学院信息工程学院，浙江嘉兴 314001

^2．嘉兴南湖学院机电工程学院，浙江嘉兴 314001

^3．杭州电子科技大学，电子科学与技术系纳米电子学与纳电子器件实验室，杭州 310018

^4．杭州电子科技大学，传感器新型材料浙江省重点实验室，杭州 310012

通讯作者:

郑鹏（1983—），男，博士，副教授。

白王峰（1985—），男，博士，副教授。

作者简介:

盛林生（1993—），男，硕士研究生。

Microstructure and Energy Storage Performance of (1-x)(0.75K_0.5Bi_0.5TiO₃-0.25BiFeO₃)-xNa_0.73Bi_0.09NbO₃ Ceramics

Linsheng SHENG¹, Chao SHEN², Mengqi JIANG¹, Guang YANG¹, Peng ZHENG³, Wangfeng BAI⁴

Affiliations

^1.College of Information Engineering, Jiaxing Nanhu University, Jiaxing 314001, Zhejiang, China

^2.School of Mechanical and Electrical Engineering, Jiaxing Nanhu University, Jiaxing 314001, Zhejiang, China

^3.Lab for Nanoelectronics and Nanoelectronic Devices, Department of Electronics Science and Technology, Hangzhou Dianzi University, Hangzhou 310018, China

^4.Key Laboratory of Novel Materials for Sensor of Zhejiang Province, Hangzhou Dianzi University, Hangzhou 310012, China

Corresponding Author:

ZHENG Peng (1983-), male, Ph.D., Associate Professor; E-mail: zhengpeng@hdu.edu.cn;

BAI Wangfeng (1985-), male, Ph.D., Associate Professor. bwf@hdu.edu.cn

SHENG Linsheng (1993-), male, Master candidate. E-mail: shenglinsheng@jxnhu.edu.cn

出版时间: 2024-04-20 doi: 10.14062/j.issn.0454-5648.20230751

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摘要

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为满足不断增长的高性能储能设备需求，亟需研发能量存储性能出众的电介质电容器。采用传统固相反应法制备了（1-x）（0.75Bi_0.5K_0.5TiO₃-0.25BiFeO₃）-xNa_0.73Bi_0.09NbO₃（x=0~0.4）（简称BKT-BF-xNBN）样品。在380 kV/cm电场下，样品表现出良好的储能性能，可实现可回收能量密度W_rec=4.23 J/cm³和效率η=81.2%。NBN的引入对BKT基陶瓷的微观结构与弛豫性产生了显著影响，导致晶粒尺寸减小、陶瓷更加致密，并诱导促使极性纳米区域的形成。此外，样品还具有出色的充放电性能（放电时间t_0.9<75 ns，放电电流密度C_D=757.9 A/cm²，放电功率P_D=94.7 MW/cm³）。这些结果表明BKT-BF-xNBN无铅铁电体在超级（电介质）储能电容器领域具有广阔的前景。

关键词

钛酸铋钾 / 无铅 / 介电陶瓷 / 弛豫铁电体 / 储能电容器

Abstract

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Introduction

Lead-free dielectric capacitors have attacted recent attention due to the super power density, fast charge-discharge rate and outstanding thermal stability. However, the recoverable energy density of lead-free ferroelectric ceramic is relatively lower, compared to ceramics containing lead. The introduction of strong relaxor ferroelectrics can realize the excellent energy storage performance via decreasing remanent polarization as well as enhancing impedance. Bi_0.5K_0.5TiO₃ (BKT) is a promising candidate for dielectric capacitor due to the unique lone pair electronic 6s² configuration about Bi, leading to a large spontaneous polarization (i.e., P = 52 μC/cm²). Nevertheless, the energy storage properties of BKT-based ceramics are poor (i.e., W_rec < 3 J/cm³, η < 80%) because of the large remanent polarization and negative breakdown strength. Chen et al. reported that the recoverable energy storage density reached 7.5 J/cm³ through adding the BaTiO₃ and NaNbO₃ into BKT, indicating that BKT-based ceramics had a substantial prospect. The long-range ferroelectric order is broken to obtain a slim hysteresis loop, which can improve the energy storage performance. Simultaneously, the uniform small grain and compact microstructure of ceramic are essential, which can upgrade the breakdown strength for ferroelectric material. Thus, reducing grain size and breaking ferroelectric long-range order to generate polar nano-regions (PNRs) could improve the BKT-based specimens energy storage properties. In this paper, a relaxor ferroelectric material of Na_0.73Bi_0.09NbO₃ (NBN) was induced into 0.75Bi_0.5K_0.5TiO₃-0.25BiFeO₃(0.75BKT-0.25BF) to reinforce the ESP of ceramics. BF and NBN were selected to optimize ESP. The morphotropic phase boundary (MPB) of BKT-BF binary system was constructed.

Methods

For the synthesis of BKT-BF-xNBN (x=0, 0.1, 0.2, 0.3 and 0.4) ceramics, Bi₂O₃ (99.5%, in mass fraction, the same below), K₂CO₃ (99.5%), TiO₂ (99.5%), Fe₂O₃ (99.5%), Na₂CO₃ (99.8%) and Nb₂O₅ (99.5%) were used as raw materials. The dried oxides were weighted and mixed according to stoichiometric ratios in a polyethylene container, and then the mixed materials with alcohol were ground in a ball mill for 12 h. After drying, the mixture was calcined at 850 ℃ for 5 h, and the powder was further ground under the same condition. Sequentially, the dried powder with 0.5% (in mass fraction) polyvinyl alcohol (PVA) was pressed into discs with a thickness of 0.8 mm and a diameter of 12 mm. Finally, the green plates were sintered at 1 000-1 035 ℃ for 3 h.

Results and discussion

The results show that an optimum recoverable energy storage density (W_rec) of 4.23 J/cm³ and an improved energy storage efficiency (η) of 81.2% at 380 kV/cm are achieved. The microstructure of the specimens is compact due to the refined size of grain, leading to a boosted breakdown strength (E_b). In addition, an enhanced efficiency of the specimen with x of 0.3 can be obtained, which arose from the negligible remanent polarization (P_r). Based on the analysis of dielectric relaxation, the dispersion coefficient (γ) of the BKT-BF-0.3NBN is 2.2, implying a short-range ferroelectric order, which can increase the polar nanometer regions. To better understand the reason for the decreased P_r, the first order reversal curve (FORC) distribution of ceramics was measured. The optimized composition has a distinguished dielectric thermal stability and a superior charge-discharge performance (i.e., t_0.9 (the time for releasing 90% of all storage energy) < 75 ns, current density (C_D) of 757.9 A/cm² and power density (P_D) of 94.7 MW/cm³), indicating a promising prospect in the applications for high-power dielectric capacitors. These results illustrate that the composition design for BKT-BF-xNBN is effective to refine the energy storage performance of ceramic.

Conclusions

Lead-free BKT-BF-xNBN ceramics with x of 0, 0.1, 0.2, 0.3 and 0.4 were synthesized. The introduction of Na_0.73Bi_0.09NbO₃ improved the microstructure of ceramics, boosted the breakdown strength, enhanced the ceramics relaxtion and resulted in the appearance of PNRs. As a result, the BKT-based ceramic with x of 0.3 had the optimum properties (i.e., W_rec of 4.23 J/cm³ and η of 81.2%). Moreover, the superior dielectric thermal stability as well as charge-discharge performance (i.e., t_0.9<75 ns, C_D=757.9 A/cm², P_D=94.7 MW/cm³) were achieved. This work indicated that BKT-BF-0.3NBN ceramic could have a promising application potential in cutting-edge performance dielectric capacitor.

Key words

bismuth potassium titanate / lead-free / dielectric ceramics / relaxor ferroelectrics / energy-storage capacitor

引用本文

盛林生, 沈超, 姜梦琦, 杨光, 郑鹏, 白王峰. （1-x）（0.75K_0.5Bi_0.5TiO₃-0.25BiFeO₃）-xNa_0.73Bi_0.09NbO₃电介质陶瓷的微观结构与储能性能. 硅酸盐学报, 2024 , 52 (4) : 1335 -1344 . DOI: 10.14062/j.issn.0454-5648.20230751

Linsheng SHENG, Chao SHEN, Mengqi JIANG, Guang YANG, Peng ZHENG, Wangfeng BAI. Microstructure and Energy Storage Performance of (1-x)(0.75K_0.5Bi_0.5TiO₃-0.25BiFeO₃)-xNa_0.73Bi_0.09NbO₃ Ceramics[J]. Journal of the Chinese Ceramic Society, 2024 , 52 (4) : 1335 -1344 . DOI: 10.14062/j.issn.0454-5648.20230751

基金

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浙江省自然科学基金(LY22E020006; LQ22A040012)
浙江省属高校基础研究基金

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2024年第52卷第4期

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文章信息

doi: 10.14062/j.issn.0454-5648.20230751

接收时间：2023-09-29
首发时间：2026-10-22
出版时间：2024-04-20

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收稿日期：2023-09-29
修回日期：2023-10-30

基金

浙江省自然科学基金(LY22E020006; LQ22A040012)

浙江省属高校基础研究基金

作者信息

^1．嘉兴南湖学院信息工程学院，浙江嘉兴 314001

^2．嘉兴南湖学院机电工程学院，浙江嘉兴 314001

^3．杭州电子科技大学，电子科学与技术系纳米电子学与纳电子器件实验室，杭州 310018

^4．杭州电子科技大学，传感器新型材料浙江省重点实验室，杭州 310012

通讯作者:

郑鹏（1983—），男，博士，副教授。

白王峰（1985—），男，博士，副教授。

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

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