软模板法制备高频超声换能器用1-3复合压电材料

doi:10.15541/jim20210282

无机材料学报 ›› 2022, Vol. 37 ›› Issue (5): 507-512.DOI: 10.15541/jim20210282 CSTR: 32189.14.10.15541/jim20210282

软模板法制备高频超声换能器用1-3复合压电材料

田俊亭¹(), 李晓兵¹(), 丁伟艳¹, 聂生东¹, 梁柱²

1. 上海理工大学健康科学与工程学院, 上海 200093
2. 中国科学院上海硅酸盐研究所, 上海 200050

收稿日期:2021-05-06 修回日期:2021-10-14 出版日期:2022-05-20 网络出版日期:2021-10-21
通讯作者: 李晓兵, 副教授. E-mail: xiaobing@usst.edu.cn
作者简介:田俊亭(1997-), 女, 硕士研究生. E-mail: 1195309903@qq.com
基金资助:
上海市自然科学基金(19ZR1436200);上海市港澳台合作项目(19440760800)

Fabrication of 1-3 Piezocomposites via Soft Mold Method for High-frequency Ultrasound Transducer

TIAN Junting¹(), LI Xiaobing¹(), DING Weiyan¹, NIE Shengdong¹, LIANG Zhu²

1. School of Health Science and Engineering, University of Shanghai for Science and Technology, Shanghai 200093, China
2. Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China

Received:2021-05-06 Revised:2021-10-14 Published:2022-05-20 Online:2021-10-21
Contact: LI Xiaobing, associate professor. E-mail: xiaobing@usst.edu.cn
About author:TIAN Junting (1997-), female, Master candidate. E-mail: 1195309903@qq.com
Supported by:
Natural Science Foundation of Shanghai(19ZR1436200);Science and Technology Commission of Shanghai Municipality(19440760800)

摘要/Abstract

摘要：

医用高频超声成像技术广泛应用于皮肤、眼睛及血管壁等人体组织的精细结构成像。1-3复合压电材料因具有较高的机电耦合系数而成为高频超声换能器的核心材料。传统的机械切割-填充、等离子蚀刻等1-3复合材料制备方法成本高、效率低, 难以实现工业化制备。本研究提出一种新的基于软模板的高频复合材料制备方法, 在获得高机电耦合系数的同时, 实现高性能1-3复合压电材料的低成本制备。研究采用微米孔径的软模板实现PZT粉的浆料填充, 通过热压烧结获得均匀竖立的PZT陶瓷微柱阵列, 进而制备出PZT/环氧1-3复合材料。对复合材料进行系统的机电性能测试, 并利用不同方法对复合材料的微结构及其均匀性进行表征。结果表明, 软模板法可使压电微柱具有完整的相结构和较高的成分均匀性, 能够实现较高的胚体压缩率, 提高陶瓷微柱的致密度, 同时形成了微柱阵列且微柱直径可控制在70 μm。软模板法有利于在提高复合材料超声频率(30~50 MHz)的同时获得64%的高机电耦合系数, 为医用高频超声成像以及超声生物显微镜等应用提供了一种高效的1-3复合压电材料工业化制备方法。

关键词: 1-3复合压电材料, 软模板法, 高频超声换能器, 压电陶瓷

Abstract:

The high-frequency ultrasonic technology has been widely used for the fine structures medical imaging of skin, eye and vessel as its high spatial resolution. 1-3 piezocomposite plays an important part in the high frequency transducer owing to the excellent electromechanical coupling properties of this material even at high frequency. However, its industrial applications were limited by the inefficient fabrication methods and expensive equipment, such as mechanical cutting-filling and plasma/laser etching. In this work, a low-cost and novel soft mold method was developed to fabricate 1-3 piezoelectric composites with high electromechanical coupling coefficient k_t for high frequency ultrasound transducers. The process of soft mold filling, hot-pressed sintering PZT pillars and epoxy curing was ruly carried out. Then, a series of samples with different thicknesses were fabricated and characterized. It demonstrates that the fabricated PZT pillars with pure rhombohedral phase are homogeneous. Besides, the length to diameter ratio of sintered pillars is 10 : 1 and the k_t of the 1-3 piezocomposite reaches as high as 64% for the 30-50 MHz high frequency transducer. The result indicates that the soft mold method is an economical and effective way to fabricate the 1-3 piezoelectric composites for medical and biological imaging in high frequency ultrasound applications.

Key words: 1-3 piezoelectric composite, soft mold method, high frequency ultrasonic, piezoelectric ceramics

中图分类号:

TQ174

田俊亭, 李晓兵, 丁伟艳, 聂生东, 梁柱. 软模板法制备高频超声换能器用1-3复合压电材料[J]. 无机材料学报, 2022, 37(5): 507-512.

TIAN Junting, LI Xiaobing, DING Weiyan, NIE Shengdong, LIANG Zhu. Fabrication of 1-3 Piezocomposites via Soft Mold Method for High-frequency Ultrasound Transducer[J]. Journal of Inorganic Materials, 2022, 37(5): 507-512.

图/表 7

图1 软模板法制备1-3复合压电材料的过程示意图

Fig. 1 Sketch of soft mold method for 1-3 piezocomposites fabrication

图2 软模板法制备的PZT微柱

Fig. 2 PZT ceramic pillars prepared via soft mold method (a) SEM image of PZT ceramic pillars; (b) SEM image of the details for local pillars; (c) Distribution of Pb, Zr, Ti elements contents along the radial direction of a pillar; (d) XRD pattern of the PZT pillars

图3 不同厚度的PZT陶瓷1-3复合材料阻抗谱

Fig. 3 Frequency dependent impedances and phase angles of the PZT/Epoxy 1-3 piezocomposites with different thicknesses

表1 不同厚度1-3复合材料的电阻抗性能

Table 1 Electrical impedance property of 1-3 piezocomposites of the samples with different thicknesses

Sample	l/mm	d/mm	ā/mm	f_r/MHz	f_a/MHz	N/(Hz·m)
1#	0.20	0.30	0.03	6.269	5.493	1254
2#	0.25	0.30	0.03	5.902	5.28	1476
3#	0.30	0.30	0.03	5.549	4.99	1665
4#	0.35	0.30	0.03	5.143	4.62	1800
5#	0.40	0.30	0.03	4.849	4.306	1940
6#	0.45	0.30	0.03	4.18	3.65	1881

图4 1-3复合材料的谐振、反谐振频率和机电耦合系数随厚度的变化

Fig. 4 Thickness dependent resonant, anti-resonance frequencies and electromechanical coupling factors for 1-3 piezocomposite

图5 软模法制备的高频超声换能器用1-3复合材料阻抗谱

Fig. 5 Frequency dependent impedances and phase angles of the 1-3 piezocomposite in medical high-frequency ultrasound transducer

表2 高频超声换能器用压电材料的压电、声学性能

Table 2 Piezoelectric and acoustic property of the piezoelectric materials for high-frequency transducers

Material	f_a/MHz	k_t	Q_m	Z_a/MRayl
PMNT crystal^[20]	45.0	0.55	100	37
PZT composite^[20]	57.5	0.68	-	15.3
PZT-5H	43.7	0.52	65	34
This work	31.6	0.64	72	10.8

参考文献 20

[1]	MA X W, CAO W W. Single crystal high frequency intravascular ultrasound transducer with 40 micron axial resolution. IEEE Transactions on Ultrasonics Ferroelectrics and Frequency Control, 2020,67(4):810-816.
[2]	LI S, TIAN J, JIANG X. A micromachined PMN-PT single crystal composite circular array for intravascular ultrasound imaging. Journal of Engineering and Science in Medical Diagnostics and Therapy, 2019,2(2):021001.
[3]	XU J L, ZHANG Z, LIU S X, et al. Optimizing the piezoelectric vibration of Pb(Mg_1/3Nb_2/3)O₃-0.25PbTiO₃ single crystal by alternating current polarization for ultrasonic transducer. Applied Physics Letters, 2020,116(20):202903.
[4]	SMITH W A, AULD B A. Modeling 1-3 composite piezoelectrics: thickness-mode oscillations. IEEE Transactions on Ultrasonics, Ferroelectrics, and Frequency Control, 1991,38(1):40-47.
[5]	LEE J S, MOON J Y, CHANG J H. A 35 MHz/105 MHz dual-element focused transducer for intravascular ultrasound tissue imaging using the third harmonic. Sensors, 2018,18(7):2290.
[6]	ZHOU D, CHEUNG K F, CHEN Y, et al. Fabrication and performance of endoscopic ultrasound radial arrays based on PMN-PT single crystal/epoxy 1-3 composite. IEEE Transactions on Ultrasonics, Ferroelectrics, and Frequency Control, 2011,58(2):477-484.
[7]	WANG J S, CHEN M Z, ZHAO X Y, et al. Fabrication and high acoustic performance of high frequency needle ultrasound transducer with PMN-PT/Epoxy 1-3 piezoelectric composite prepared by dice and fill method. Sensors and Actuators A: Physical, 2021,318:112528.
[8]	CHEN R H, LAN C L. Fabrication of high-aspect-ratio ceramic microstructures by injection molding with the altered lost mold technique. Journal of Microelectromechanical Systems, 2001,10(1):62-68.
[9]	CERTON D, PATAT F, LEVASSORT F,et al. Lateral resonances in 1-3 piezoelectric periodic composite: modeling and experimental results. Journal of the Acoustical Society of America, 1997,101(4):2043-2051.
[10]	BENT A A, HAGOOD N W. Piezoelectric fiber composites with interdigitated electrodes. Journal of Intelligent Material Systems and Structures, 1997,8(11):903-919.
[11]	WANG S N, LI J F, WATANABE R, et al. Fabrication of lead zirconate titanate microrods for 1-3 piezocomposites using hot isostatic pressing with silicon molds. Journal of the American Ceramic Society, 2004,82(1):213-215.
[12]	WANG S N, LI J F, LI X H,et al. Processing of PZT microstructures. Sensors and Materials, 1998,10(6):375-384.
[13]	DONG Y Z, ZHOU Z Y, LIANG R H, et al. Correlation between the grain size and phase structure, electrical properties in BiScO₃-PbTiO₃-based piezoelectric ceramics. Journal of the American Ceramic Society, 2020,103(9):4785-4793.
[14]	PENG J, LUO H S, HE T H, et al. Elastic, dielectric, and piezoelectric characterization of 0.70Pb(Mg_1/3Nb_2/3)O₃-0.30PbTiO₃ single crystals. Materials Letters, 2005,59(6):640-643.
[15]	LIU C G, DJUTH F, ZHOU Q F,et al. Micromachining techniques in developing high-frequency piezoelectric composite ultrasonic array transducers. IEEE Transactions on Ultrasonics, Ferroelectrics, and Frequency Control, 2013,60(12):2615-2625.
[16]	CANNATA J M, RITTER T A, CHEN W H,et al. Design of efficient, broadband single-element (20-80 MHz) ultrasonic transducers for medical imaging applications. IEEE Transactions on Ultrasonics, Ferroelectrics, and Frequency Control, 2003,50(11):1548-1557.
[17]	FANG R R, ZHOU Z Y, LIANG R H, et al. Effects of CuO addition on the sinterability and electric properties in PbNb₂O₆- based ceramics. Ceramics International, 2020,46(15):23505-23509.
[18]	ZIPPARO M, SHUNG K K, SHROUT T R. Piezoceramics for high-frequency (20 to 100 MHz) single-element imaging transducers. IEEE Transactions on Ultrasonics, Ferroelectrics, and Frequency Control, 1997,44(5):1038-1048.
[19]	KRIMHOLTZ R, LEEDOM D A, MATTHAEI G L. New equivalent circuits for elementary piezoelectric transducers. Electronics Letters, 1907,6(13):398-399.
[20]	ZHOU Q F, XU X C, GOTTLIEB E J,et al. PMN-PT single crystal, high-frequency ultrasonic needle transducers for pulsed- wave Doppler application. IEEE Transactions on Ultrasonics, Ferroelectrics, and Frequency Control 2007,54(3):668-675.

软模板法制备高频超声换能器用1-3复合压电材料

Fabrication of 1-3 Piezocomposites via Soft Mold Method for High-frequency Ultrasound Transducer

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