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(PZT) Piezoelectric Ceramics Ching-Chang Chung University of Connecticut - Storrs, [email protected]

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(PZT) Piezoelectric Ceramics Ching-Chang Chung University of Connecticut - Storrs, Ching-Chang.Chung@Uconn.Edu University of Connecticut OpenCommons@UConn Doctoral Dissertations University of Connecticut Graduate School 1-13-2014 Microstructural Evolution in Lead Zirconate Titanate (PZT) Piezoelectric Ceramics Ching-Chang Chung University of Connecticut - Storrs, [email protected] Follow this and additional works at: https://opencommons.uconn.edu/dissertations Recommended Citation Chung, Ching-Chang, "Microstructural Evolution in Lead Zirconate Titanate (PZT) Piezoelectric Ceramics" (2014). Doctoral Dissertations. 293. https://opencommons.uconn.edu/dissertations/293 Microstructural Evolution in Lead Zirconate Titanate (PZT) Piezoelectric Ceramics Ching-Chang Chung, Ph.D. University of Connecticut, 2014 Solid solutions of lead zirconate titanate [PbZr1-xTixO3 (PZT)] are extensively used in electromechanical transducers. A maximum in dielectric and piezoelectric response is observed near the morphotropic phase boundary (MPB) separating rhombohedral and tetragonal ferroelectric phases. The origin of the enhanced properties near the MPB remains controversial and has been variously attributed to coexisting rhombohedral and tetragonal ferroelectric phases, to the formation of nanodomains, and/or to lower symmetry monoclinic phases. Hence, the phase diagram of PZT in the region of the MPB remains open to debate. In this work, dense polycrystalline PZT ceramics prepared by chemical methods were subjected to different time-temperature histories to investigate the origins of the two-phase coexistence and to determine the influence of thermal history on structure, microstructure and dielectric properties. Long annealing (240 hours) above the Curie temperature (Tc) revealed a slow relaxation process that was manifested in changes of structural properties. The changes in structural properties were accompanied by changes in the behavior of the paraelectric to ferroelectric phase transition, the domain structure, and the extrinsic contributions to dielectric permittivity. The changes in all these properties were found to show maxima near the MPB. The combined results showed that PZT ceramics made by a normal ceramic processing were not in their equilibrium state near the MPB. However, no clear evidence of phase decomposition into an equilibrium mixture of tetragonal and rhombohedral phases was found. Instead, the changes in structural and dielectric properties observed on annealing were most consistent with a stress relief mechanism that provided for the coarsening of the domain structure and increased domain wall contributions to dielectric properties. The results provide evidence that the domain structures and electromechanical properties of PZT compositions near the MPB can be controlled without dopants by processing using differing thermal histories. In addition, results obtained for un-annealed PZT ceramics were used to resolve the long controversial issue of tricritical behavior at the paraelectric to ferroelectric phase transition, to separate intrinsic and extrinsic contributions to the dielectric response, and to quantify reversible and irreversible domain wall motion. Microstructural Evolution in Lead Zirconate Titanate (PZT) Piezoelectric Ceramics Ching-Chang Chung B.S., National Cheng Kung University, 2004 M.S., National Cheng Kung University, 2006 A Dissertation Submitted in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy at the University of Connecticut 2014 Copyright by Ching-Chang Chung 2014 APPROVAL PAGE Doctor of Philosophy Dissertation Microstructural Evolution in Lead Zirconate Titanate (PZT) Piezoelectric Ceramics Presented by Ching-Chang Chung, B.S., M.S. Major Advisor ______________________________________ George A. Rossetti, Jr. Associate Advisor ___________________________________ S. Pamir Alpay Associate Advisor ___________________________________ Pu-Xian Gao University of Connecticut 2014 ACKNOWLEDGEMENTS I would like to express my gratitude to Dr. George A. Rossetti, Jr. I could never have accomplished what I did over the last five years without his kind assistance, invaluable guidance, and support. I would also like to thank Dr. S. Pamir Alpay and Dr. Puxian Gao, my associate advisors, for their support, and constructive suggestions. I sincerely acknowledge the valuable feedback from my committee members Dr. Mark Aindow, Dr. Bryan D. Huey, and Dr. Harris L. Marcus. Also, I would like to thank Dr. Lichun Zhang for helping me with TEM measurements and data analysis. It has been an honor working with all of you. I want to thank all the present and past members of Dr. George A. Rossetti’s and Dr. S. Pamir Alpay’s groups for their company and support- Richard, Nasser, Adam, Thevika, Jialan, Claire, Liang, Fu-Chang, Hamidreza and Tumerkan. Also, a special thank you also goes to my friends in the Institute of Materials Science (IMS) and the Taiwanese Student Association (TSA) at UCONN. I really enjoyed my time here. I would like to thank the IMS and the Army Research Office (ARO) for their financial support. This work also benefited from the Office of Naval Research (ONR). Lastly, I offer my most heartfelt thanks to my parents, Muyung and Chunming, aunt Meiyu, my brother Keen, my sister Carolina, my in-laws Melissa and Uri, and other family members for their unending encouragement and love throughout the years. Their unconditional support helped me to never lose optimism and motivation during my time at UCONN. Without them, this thesis would never have been written. I would like to dedicate this work to them. Page | iv TABLE OF CONTENTS ACKNOWLEDGEMENTS ............................................................................................ iv LIST OF FIGURES ......................................................................................................... xi LIST OF TABLES ....................................................................................................... xxiii CHAPTER 1 TECHNICAL BACKGROUND .......................................................................................1 1.1 Ferroelectric Materials .............................................................................................. 1 1.2 Ferroelectric Domains ............................................................................................... 6 1.3 Intrinsic and Extrinsic Contribution to Dielectric Response ..................................... 8 1.4 Field Amplitude Dependence Dielectric Properties and Rayleigh Law ................. 15 1.5 Lead Titanate Zirconate (PZT) ................................................................................ 18 1.6 Phase Coexistence in PZT ....................................................................................... 22 1.6.1 Conventional Diffusionless Phase Diagram ......................................................25 1.6.2 Metastable Coexistence .....................................................................................25 1.6.3 Equilibrium Coexistence ...................................................................................26 1.6.4 Heterogeneity (Composition Fluctuation) .........................................................27 1.6.5 Thermal Fluctuation (Statistical Distribution Model) .......................................28 1.7 Kinetics of Forming PZT Solid Solution ................................................................ 30 1.8 Monoclinic Phase in PZT ........................................................................................ 32 1.9 Domain Miniaturization around MPB..................................................................... 34 1.10 References ............................................................................................................. 37 Chapter 2 OBJECTIVES AND THESIS OVERVIEW .................................................................45 2.1 Statement of Problem and Objectives ..................................................................... 45 2.2 Thesis Overview ...................................................................................................... 47 Page | v 2.3 References ............................................................................................................... 51 CHAPTER 3 SYNTHESIS OF PZT POWDER AND SAMPLE PREPARATION .........................53 3.1 Synthesis of PZT Powder ........................................................................................ 53 3.2 Synthesis of Polycrystalline PZT Dense Pellets ..................................................... 59 3.3 Phase Purity ............................................................................................................. 60 3.3.1 Phase purity of PZT powder ..............................................................................60 3.3.2 Phase purity of dense PZT ceramics ..................................................................66 3.4 Summary ................................................................................................................. 68 3.5 References ............................................................................................................... 69 CHAPTER 4 CHARACTERIZATION OF STRUCTURE, MICROSTRUCTURE AND DOMAIN STRUCTURE .................................................................................................70 4.1 Structural Characterization ...................................................................................... 70 4.1.1 Lattice Parameters .............................................................................................71 4.1.2 Ferroelastic
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