硅酸盐学报

煅烧温度对铌酸钾钠基铁电陶瓷压电性能的影响

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王孟丽 ¹ , 桑秀杰 ¹ , 周静 ¹ , 李芳 ¹ , 李敏 ²

硅酸盐学报 | 研究论文 2024,52(6): 1935-1941

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硅酸盐学报 |研究论文 2024 , 52 (6) : 1935 -1941

煅烧温度对铌酸钾钠基铁电陶瓷压电性能的影响

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王孟丽¹, 桑秀杰¹, 周静¹, 李芳¹, 李敏²

作者信息

^1．潍坊职业学院，山东潍坊 262737

^2．池州学院，安徽池州 247000

通讯作者:

李敏（1983—），女，硕士，副教授。

作者简介:

王孟丽（1984—），女，硕士，讲师。

Effect of Calcination Temperature on Strain Properties of Potassium Sodium Niobate Based Ferroelectric Ceramics

Mengli WANG¹, Xiujie SANG¹, Jing ZHOU¹, Fang LI¹, Min LI²

Affiliations

^1.Weifang Vocational College, Weifang 262737, Shandong, China

^2.Chizhou University, Chizhou 247000, Anhui, China

Corresponding Author:

LI Min (1983-), female, Master, Associate Professor. E-mail: 714821655@qq.com

WANG Mengli (1984-), female, Master, Lecturer. E-mail: 13516362561@163.com

出版时间: 2024-06-20 doi: 10.14062/j.issn.0454-5648.20230726

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摘要

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铁电陶瓷在电场下产生应变性能，是制备致动器的关键元件。多相共存结构的铁电陶瓷产生大应变，除了组成，混合料煅烧条件影响相结构和应变性能。采用传统固相烧结法制备0.97KNNS-0.03BNKZ（0.97（K_0.48Na_0.52）（Nb_0.97Sb_0.03）O₃-0.03Bi_0.5（K_0.48Na_0.52）_0.5ZrO₃）铁电陶瓷，研究混合料煅烧温度在600~950 ℃范围内对陶瓷的直径收缩率、微观形貌、晶体结构、介电性能、铁电性能和应变性能的影响。结果表明，随混合料煅烧温度的增加，陶瓷直径收缩率先增加至8.5%然后减小；陶瓷平均晶粒尺寸先减小后增加至0.48 μm；所有陶瓷晶体具有畸变的正交结构；Curie温度从280 ℃增加到320 ℃，相应地最大介电常数从4 520增加到7 769；最大极化强度先减小后增加，最高达到35 μC/cm²。煅烧温度为950 ℃时，陶瓷在40 kV/cm电场下其双极应变达到0.3%，原因在于铁电畴易翻转；其它煅烧温度制备的陶瓷其应变性能在0.25%左右，区别不大。

关键词

煅烧 / 铌酸钾钠陶瓷 / 压电性能

Abstract

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Introduction

Ferroelectric ceramics generate a strain property in electric field due to the inverse piezoelectric effect and ferroelectric domain swiching, and these ceramics can be made as key components of actuators. Lead-based ferroelectric ceramics are widely used in actuators, but their high lead level is harmful to human-being health and environment. (K_1-_xNa_x)NbO₃-based ceramics replace lead-based ceramics for actuators applications. (K_1-_xNa_x)NbO₃-based ceramics with a multi-phase coexistence structure at room temperature have a high strain due to the possible increasing polarization direction. The classical (1-x)(K_1-_yNa_y)(Nb_1-_zSb_z)O₃-xBi_0.5(Na_1-_wK_w)_0.5ZrO₃ (0≤x≤0.05, 0.40≤y≤0.68, 0≤z≤0.08, 0≤w≤1) (KNNS-BNKZ) system can be adjusted to have rhombohedral-tetragonal (R-T), rhombohedral-orthogonal-tetragonal (R-O-T), orthogonal-tetragonal (O-T) phases coexisted structures to increase the strain property. When the system is used to construct the coexistence structure, the composition and process need to be finely regulated, especially the raw material calcination or pre-firing process. Pre-firing is a solid-phase reaction of various raw materials at a certain temperature, and the purpose is to synthesize the crystal structure of the target component without raw material components. The activity, particle size and uniformity of the pre-fired powder have a great influence on the difficulty of green sintering and the electrical properties of ceramics. The pre-firing temperature affects the phase coexist structures of 0.96(K_0.5Na_0.5)(Nb_0.96Sb_0.04)O₃-0.04Bi_0.5(Na_0.5K_0.5)_0.5ZrO₃ ceramic coming from KNNS-BNKZ system, but the effect of the strain properties of ceramics is not reported yet. In this paper, 0.97(K_0.48Na_0.52)(Nb_0.97Sb_0.03)O₃-0.03Bi_0.5(K_0.48Na_0.52)_0.5ZrO₃ (0.97KNNS-0.03BNKZ) with R-T was designed according to KNNS-BNKZ system. KNN-based ceramics with multi-phase coexistence for improving their strain properties were constructed via adjusting the pre-firing temperature. In addition, the effect of pre-firing temperature on the phase structure, dielectric properties, ferroelectric properties and strain properties of 0.97KNNS-0.03BNKZ ferroelectric ceramics was investigated.

Methods

For the preparation of 0.97KNNS-0.03BNKZ ferroelectric ceramics by a solid-phase sintering method, the ingredients were made according to the chemical formula, and various raw materials were mixed and ground with absolute ethanol in a ball mill with zirconia balls. After 12_h milling, the slurry was dried. The mixture of 0.97KNNS-0.03BNKZ components of 20.0 g in a crucible was calcined at 600-950 ℃ for 3 h. After milling and drying, the powder was pressed into green discs with the diameter of 13 mm. The upper and lower surfaces of the green discs were buried with the same calcination powder, covered with alumina crucible then sealed with alumina powder. Finally, the green discs were sintered in a high-temperature furnace at 1 180 ℃ for 3 h. The ceramic samples were obtained after cooling in the furnace.

The samples were not polished and thermally corroded. The surface morphology of the ceramics was determined by a model Smartlab 3 kW scanning electron microscope after direct cleaning and drying. The density of the samples was analyzed by the Archimedes drainage method. After grinding the surface of samples, the phase structure of the ceramics was characterized by X-ray diffracometer (XRD). Their ferroelectric and strain properties were determined at 10 Hz by a model Precision Premier II ferroelectric system. Their permittivity was measured at 10 kHz by a model TZDM permittivity instrument.

Results and discussion

The effect of calcination temperature (i.e., 600-950 ℃) on the diameter shrinkage, density, relative density, microstructure, crystal structure, dielectric properties, ferroelectric properties and strain properties of 0.97KNNS-0.03BNKZ ceramics was analyzed. The results show that the diameter shrinkage density and relative density of these ceramics firstly increase and then decrease with the increase of the calcination temperature. The ceramics calcinated at 800 ℃ have the maximum relative density (i.e., 94.9%), while the ceramics calcinated at 600 ℃ and 950 ℃ have the minimum relative density (i.e., 80.3% and 80.4%). All of the ceramics have the same distorted orthogonal crystal structure based on the XRD patterns and temperature-dependence of dielectric constant. Their Curie temperature increases from 280 ℃ to 320 ℃, while their dielectric constant increases from 4 520 to 7 769. The maximum polarization strength (P_max) of the ceramics at 600, 800 ℃ and 950 ℃ is obtained due to the easy domain swiching for the high or small relative density of ceramics. At 950 ℃, the bipolar strain of the ceramics reaches 0.5% at 60 kV/cm because the ferroelectric domain is easy to swiching, and the interacts between defect dipoles and domain swiching. At 600-900 ℃, the strain properties of the ceramics change slightly (i.e., 0.2%-0.3% strain). The unipolar strain properties of ceramics calcinated at different temperatures are similar.

Conclusions

The pre-firing had little effect on the crystal structure of 0.97KNNS-0.03BNKZ ceramics, but had a great effect on the density and strain performance of the ceramics. When the calcination temperature was 950 ℃, the bipolar strain of the ceramics reached 0.5% at 60 kV/cm, because the ferroelectric domain was easy to swiching and the interacts between defect dipoles and domain swiching.

Key words

calcination / potassium sodium niobatebceramics / Piezoelectric property

引用本文

王孟丽, 桑秀杰, 周静, 李芳, 李敏. 煅烧温度对铌酸钾钠基铁电陶瓷压电性能的影响. 硅酸盐学报, 2024 , 52 (6) : 1935 -1941 . DOI: 10.14062/j.issn.0454-5648.20230726

Mengli WANG, Xiujie SANG, Jing ZHOU, Fang LI, Min LI. Effect of Calcination Temperature on Strain Properties of Potassium Sodium Niobate Based Ferroelectric Ceramics[J]. Journal of the Chinese Ceramic Society, 2024 , 52 (6) : 1935 -1941 . DOI: 10.14062/j.issn.0454-5648.20230726

基金

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材料加工实验实训中心(2021ZSXZX01)
安徽省高活性微纳粉体工程研究中心

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2024年第52卷第6期

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文章信息

doi: 10.14062/j.issn.0454-5648.20230726

接收时间：2023-09-18
首发时间：2026-10-22
出版时间：2024-06-20

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收稿日期：2023-09-18
修回日期：2024-01-04

基金

材料加工实验实训中心(2021ZSXZX01)

安徽省高活性微纳粉体工程研究中心

作者信息

^1．潍坊职业学院，山东潍坊 262737

^2．池州学院，安徽池州 247000

通讯作者:

李敏（1983—），女，硕士，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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