硅酸盐学报

熔融沉积方法增材制造锆钛酸铅压电陶瓷

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刘月明 ¹ , 董浩霖 ¹ , 刘鹏 ¹ , 杨现锋 ¹ , 赵巍 ² , 谢志鹏 ³

硅酸盐学报 | 研究论文 2024,52(6): 1953-1961

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硅酸盐学报 |研究论文 2024 , 52 (6) : 1953 -1961

熔融沉积方法增材制造锆钛酸铅压电陶瓷

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刘月明¹, 董浩霖¹, 刘鹏¹, 杨现锋¹, 赵巍², 谢志鹏³

作者信息

^1．长沙理工大学材料科学与工程学院，长沙 410114

^2．天津城建大学材料科学与工程学院，天津 300384

^3．清华大学，新型陶瓷与精细工艺国家重点实验室，北京 100083

通讯作者:

杨现锋（1980—），男，博士，教授。

作者简介:

刘月明（1998—），男，硕士研究生。

Additive Manufacturing of Lead Zirconate Titanate Piezoelectric Ceramic by Fused Deposition Modeling

Yueming LIU¹, Haolin DONG¹, Peng LIU¹, Xianfeng YANG¹, Wei ZHAO², Zhipeng XIE³

Affiliations

^1.Changsha University of Science & Technology, College of Materials Science and Engineering, Changsha 410114, China

^2.Tianjin Chengjian University, School of Materials Science and Engineering, Tianjin 300384, China

^3.State Key Laboratory of New Ceramic and Fine Processing, School of Materials Science and Engineering, Tsinghua University, Beijing 100083, China

Corresponding Author:

YANG Xianfeng (1980-), Male, Ph.D., Professor. E-mail: yangxfcsust@csust.edu.cn

LIU Yueming (1998-), male, Master candidate. E-mail: liuyueming1998@foxmail.com

出版时间: 2024-06-20 doi: 10.14062/j.issn.0454-5648.20230821

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摘要

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采用基于螺杆挤出的熔融沉积成型方法结合两步脱脂工艺增材制造了PZT压电陶瓷，研究了固相含量对耗材流变性质、密度和收缩率的影响，以87%（质量分数）耗材为主，观察了显微形貌并测试了电学性能。结果表明，制备的高固相低黏度打印混合料呈现典型的剪切变稀流变学性质，具有优异的打印性能，成功打印了壁厚1 mm的环形阵列、阵元间距为0.25 mm的矩形阵列和30°倾角的环形薄壁生坯样品，且PZT陶瓷样品层间结合良好，成功制备了无支撑球壳结构的PZT陶瓷样品。随着固相含量的增加，PZT陶瓷的密度随之升高，固相含量为87%时，PZT陶瓷的密度为7.82 g/cm³，压电常数d₃₃达到316 pC/N，为制备复杂结构的PZT压电陶瓷提供了新的思路。

关键词

3D打印 / 锆钛酸铅 / 熔融沉积成型 / 压电陶瓷

Abstract

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Introduction

Lead zirconate titanate (PZT) piezoelectric ceramics are widely used in electronic components. With the continuous development of intelligent, integrated and lightweight piezoelectric devices, the shape and structure of piezoelectric ceramic components become more complex. 3D printing technology has potential advantages in the personalized manufacturing of complex ceramic parts, especially the fused deposition modeling (FDM) method, which has the advantages of high efficiency, low cost, and wide material adaptability. This paper was to prepare PZT piezoelectric ceramics by FDM. In addition, the process optimization, printing performance, sintering behavior, and electrical properties were also investigated.

Methods

A PZT powder with an average particle size of 2.85 μm was used. An organic binder was composed of 58% paraffin wax (PW, purity: 99% in mass fraction, the same below), 5% stearic acid (SA, 98%), 20% Polyethylene (PE, 99%), and 17% ethylene-vinyl acetate copolymer (EVA, 98%). The ceramic powder and organic binder were thoroughly mixed by a double-roller mixing machine at 130 ℃ for 60 min, and then crushed into granules of less than 5 mm. The solid loading of the feedstock was set to 83%, 85%, 87%, and 89%. A commercial extrusion printer (UP-R200, Shenzhen Uprise 3D Technology Co., Ltd., China) with the extrusion nozzle diameter of 0.5 mm, and the layer thickness of 0.2 mm for FDM was used in this study. The printing condition was printing temperature of 120 ℃, print speed of 40 mm/s, and printing platform temperature of 85 ℃. Some complex shaped parts like ring array, rectangular array, and thin-walled cylindrical structures were printed. The printed green bodies were firstly placed in kerosene for solvent debinding at 40 ℃ for 20 h and then dried in an oven at 40 ℃ for 15 h. The dried parts were heated at 600 ℃ for 2 h. After thermal debinding, the samples were put into a crucible with a lid, buried on PZT powder, and sintered in the furnace at 1 100 ℃ for 2 h. The PZT ceramics coated with silver electrodes were polarized in an electric field of 2.5 kV/mm in silicone oil at 120 ℃ for 20 min. The phase composition and structure of the sample were determined by a model D8 Advance X-ray diffractometer (XRD, Germany) with detect angles ranging from 10° to 80°. The rheological properties of the printing consumables were tested at 180 ℃ by a model Rosand RH2000 capillary rheometer (Malvern Co., UK). The microstructures of samples were analyzed by a model JSM-6700F field emission scanning electron microscope (SEM, JEOL Co., Japan). The density of the samples was measured by a drainage method. The dielectric constant ε_r and dielectric loss δ were measured by a model Agilent-4294A impedance analyzer (USA). The ferroelectric properties were analyzed by a model aix ACCT-TF Analyzer 2000 ferroelectric tester (Germany). The piezoelectric constant of the polarized sample was measured by a model ZJ-3AN quasi-static d₃₃ meter (Institute of Acoustics, Chinese Academy of Sciences, China).

Results and discussion

At a constant solid loading, the shear viscosity of the feedstock at 180 ℃ decreases with the increase of shear rate, and has obvious shear thinning characteristics, which is beneficial to the extrusion process. At a constant shear rate, the higher the solid loading is, the higher the measured shear viscosity will be. At a shear rate of 100 s^-1, the shear viscosity is 30.30, 45.07, 47.08 Pa·s and 655.21 Pa·s respectively as the solid loading increases. Annular arrays with a wall thickness of 1 mm, rectangular arrays with an element spacing of 0.25 mm, and annular thin-wall blank samples with an inclination angle of 30° are printed, indicating that the prepared feedstock has a good printing performance. The SEM images show that the prepared PZT ceramic samples have a good interlayer bonding. Each layer is straight, uniform and continuous. After debinding and sintering, the interior of the material is uniform and dense without obvious pore defects, which shows that PZT ceramics with a good interlayer bonding can be obtained by the FDM method. The density of both green body and sintered body increases with the increase of solid loading, and the density of sintered body increases from 7.55 g/cm³ to 7.84 g/cm³. The results show that the sintering shrinkage in the Z direction is higher than that in the X-Y direction. The SEM images of PZT samples at each stage show that the two-step debinding process of solvent debinding + thermal debinding is beneficial to eliminating organic binders without causing defects. PZT piezoelectric ceramic sheets with a diameter of 17.5 mm and a thickness of 1.35 mm are prepared using a feedstock with a solid loading of 87%. The electrical property analysis indicates that the Curie temperature reaches 295℃, the coercive electric field E is 7.57 kV/cm, the remnant polarization P_r reaches 3.66 μC/cm², and the piezoelectric constant d₃₃ reaches 316 pC/N.

Conclusions

The prepared feedstock with a high solid content and a low viscosity exhibited a typical shear thinning rheology and an excellent printing performance. A PZT spherical shell structure without support was prepared. The PZT ceramic samples had good interlayer bonding and no interlayer cracks. The density of PZT ceramics increased with increasing the solid loading. At a solid loading of 87%, the density of PZT ceramic reached 7.82 g/cm³, and the piezoelectric constant d₃₃ was 316 pC/N. This study provided an effective approach for the preparation of complex structure PZT piezoelectric ceramics.

Key words

3D printing / lead zirconate titanate / fused deposition modeling / piezoelectric ceramic

引用本文

刘月明, 董浩霖, 刘鹏, 杨现锋, 赵巍, 谢志鹏. 熔融沉积方法增材制造锆钛酸铅压电陶瓷. 硅酸盐学报, 2024 , 52 (6) : 1953 -1961 . DOI: 10.14062/j.issn.0454-5648.20230821

Yueming LIU, Haolin DONG, Peng LIU, Xianfeng YANG, Wei ZHAO, Zhipeng XIE. Additive Manufacturing of Lead Zirconate Titanate Piezoelectric Ceramic by Fused Deposition Modeling[J]. Journal of the Chinese Ceramic Society, 2024 , 52 (6) : 1953 -1961 . DOI: 10.14062/j.issn.0454-5648.20230821

基金

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国家自然科学基金(52172063)
湖南省研究生科研创新项目(CX20210830)

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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.0454-5648.20230821

接收时间：2023-10-25
首发时间：2026-10-22
出版时间：2024-06-20

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收稿日期：2023-10-25
修回日期：2023-12-27

基金

国家自然科学基金(52172063)

湖南省研究生科研创新项目(CX20210830)

作者信息

^1．长沙理工大学材料科学与工程学院，长沙 410114

^2．天津城建大学材料科学与工程学院，天津 300384

^3．清华大学，新型陶瓷与精细工艺国家重点实验室，北京 100083

通讯作者:

杨现锋（1980—），男，博士，教授。

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https://castjournals.cast.org.cn/joweb/gsyxb/CN/10.14062/j.issn.0454-5648.20230821

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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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