Growth and property characterization of relaxor ferroelectric PZN PT single crystals

GROWTH AND PROPERTY CHARACTERIZATION OF RELAXOR FERROELECTRIC PZN-PT SINGLE CRYSTALS KALIDINDI KOTAM RAJAN (M.Sc., NUS) A THESIS SUBMITTED FOR THE DEGREE OF DOCTOR OF PHILOSOPHY DEPARTMENT OF MECHANICAL ENGINEERING NATIONAL UNIVERSITY OF SINGAPORE 2007 Acknowledgements I would like to express my sincere gratitude to my supervisor Dr Lim Leong Chew He has been an excellent mentor and very supportive throughout I thank him for everything he has done for me, for devoting his valuable time to teach me both experimental and theoretical concepts with patience and understanding He is easily approachable for advice on both academic and non-academic matters which all added making my research a memorable stint in my life His dedication to work and his discipline are amazing and I just hope that some of it has rubbed off on to me I can never forget those long technical discussions even in flight when I traveled with him to several conferences Most importantly, he always knew when to be a teacher and when to be a friend I am really glad to have had the chance to be his student This thesis would have not existed without his expert guidance, inspiration, and support I sincerely thank him for all the help and guidance that he has rendered I owe a special thanks to Dr Jin Jing who helped me all the way during my course of work This thesis could not have been completed before time without the help and useful discussions with him I have had the privilege of working with Prof Z.G Ye group at SFU, the one worth mentioning from his group is Dr Alex Bokov with whom scientific discussions were excellent Special thanks to Microfine Materials Technologies Pte Ltd for supplying the crystals needed for my work I also must acknowledge Joy Chuah and Paul Lim for their help with sample preparation and the experimental part of this work I would like to thank my group members Wei Sea, Shanthi, Rahul for their help in discussions I would also like to thank all the staff of Materials Science Laboratory I especially, Thomas Tan, Ng Hong Wei, Abdul Khalim and Aye Thein for their continuous support I can never forget those people who are with me in ups and downs of my life in Singapore Yes, they are my friends; some are my undergraduate classmates (Madan, Bhasker, Ravi, Nandu) and some whom I met in Singapore (Saradhi, Ram, Venku, Sonti) I would also like to express my gratitude to Niranjan, Chava, for the excitement and pleasure I had with them during my stay in Singapore Finally, I would like to thank my parents for their love, support and continuous encouragement through out my studies I would like to thank my wife Sireesha, for her support and all the evenings she spent alone patiently waiting for me to finish my research II Table of Contents Acknowledgements I Table of Contents III Summary VII List of Figures IX List of Tables XV Chapter 1: Introduction Chapter 2: Literature Review 2.1 Background on Ferroelectricity 2.2 Normal & Relaxor Ferroelectrics 2.3 Perovskite Structure 10 2.4 Lead Zirconate Titanate Piezoceramics 13 2.5 Relaxor PZN-PT Single Crystals 2.5.1 18 2.5.2 2.6 Crystal Growth & Properties of PZN-PT Single Crystals Structural Characterization of PZN-PT Single Crystals 21 Domain Structures in Relaxor PZN-PT Single Crystals 28 Chapter 3: Growth and Longitudinal Properties of PZN-PT Single Crystals 3.1 Background 35 3.2 A Note on Flux Growth Mechanisms of PZN-PT Crystals 35 3.3 Improved Flux Growth of PZN-PT Crystals 39 3.4 Determination of Optimum Crystal Compositions 41 3.5 Homogeneity Check of Flux-grown PZN-(6-7)%PT 45 3.6 A Note on Dielectric Constant of Relaxor Single Crystals 54 III Chapter 4: Transverse-Mode Properties of [001]-Poled PZN-(6-7)%PT Single Crystals 4.1 Introduction 58 4.2 [001]-poled PZN-(6-7)%PT d31-Sensor/Actuators 59 4.2.1 Effect of Initial Domain Structures, Length Orientation & E-Field 4.2.2 Dielectric Permittivity Vs Temperature 70 4.2.3 Determination of Depolarization Temperature 72 Chapter 5: Transverse-Mode Properties of [011]-Poled PZN-7%PT Single Crystals 5.1 Introduction 76 5.2 Effect of Length Orientation 77 5.3 Effect of Crystal Composition and Poling Conditions 77 5.4 Structural and Phase Studies 81 5.4.1 Dielectric permittivity Vs Temperature 82 5.4.2 Polarized light microscopy 82 5.4.3 X-ray Diffraction 87 5.4.4 Resonance Technique 89 Field-Induced-Phase-Transformation 92 5.5 Chapter 6: Shear Resonance Behavior of Single-Domain PZN-(6-7)%PT Single Crystals 6.1 Introduction 96 6.2 Experimental Details 98 6.3 Shear Characterization of Single Domain PZN-7%PT Single Crystals 6.3.1 Length-Shear Excitation with Electrodes on Minor Faces 6.3.2 Thickness-Shear Excitation with Electrodes on Major Surfaces (a) Electrodes on Major (11 ) Crystal Faces (b) 6.4 − Electrodes on Major (1 0) Crystal Faces Summary 103 108 110 115 IV Chapter 7: Measured Property Matrices of Differently-Poled PZN-(6-7)%PT Single Crystals 7.1 Introduction 116 7.2 Measured Property Matrix of [111]-Poled Single Domain Crystals 117 7.3 Measured Property Matrix of [001]-Poled Multi-Domain Crystals 127 Chapter 8: Deduced Property Matrices of [001]-Poled PZN-(6-7)%PT Single Crystals and Effects of Metastable Low-Symmetry Phases 8.1 Introduction 132 8.2 Assumptions Made 132 8.3 Deduced Property Matrix of [001]-Poled Single Crystals 136 8.4 Comparison between measured and deduced property values and effects of Metastable Low-Symmetry Phases 138 Chapter 9: Discussion 9.1 Relaxor Single Crystals of Superior Piezoelectric Properties 9.2 141 Properties of Rhombohedral Single Crystals 9.2.1 For Crystals of Compositions Away From MPBs 142 9.2.2 For Crystals of Near-MPB Compositions 145 9.3 Properties of Monoclinic /Orthorhombic Single Crystals 146 9.4 Remarks on Reported Property Values of [001] and [011]-Poled Single Crystals 147 9.5 Shear Properties of PZN-(6-7)%PT Single Domain Crystals 147 9.6 Full Property Matrices of Multi-domain PZN-7%PT Single Crystals149 9.7 Comparison with Reported Properties of PMN-PT Single Crystals 150 Chapter 10: Conclusions 155 V Chapter 11: Recommendations for Future Work 158 References 160 VI Summary Lead zinc niobate-lead titanate [Pb(Zn1/3Nb2/3)O3-PbTiO3 or PZN-PT] solid solution single crystals exhibit extremely high dielectric and piezoelectric properties, with KT > 5000, d33 ≥ 2000 pC/N and k33 ≥ 0.92, but the reported properties show large scatters and inconsistencies In this work, extensive experiments were performed to shed light on the effects of crystal composition, orientation and poling field condition on the phases present and domain structures and the ensuing properties of these single crystals The results show that monoclinic and/or orthorhombic phases can be induced by poling in the [001] and [011] crystal direction, respectively In moderate quantities, these metastable phases are responsible for the superior dielectric and electromechanical properties observed However, when present in sufficiently high quantities, they cause property degradation of the material, i.e., the crystals become overpoled with inferior properties Our results also show that the poled properties of transverse mode crystals depend sensitively on the length orientation of the plate and to certain extent, on the domain structure in the crystal Specifically, [011]poled PZN-PT single crystals of [001]-length-cut give superior dielectric and piezoelectric − properties compared to those of [ 011 ]-length-cut While [001]-poled plates of [110]length-cut display higher k31 values, they exhibit lower d31 values And, [001]-poled d31 plates of only braid-like initial domain structure have superior dielectric and piezoelectric to those of stripe-like domains or a mixed domain structure The present work further shows that for improved property consistency, the crystal compositions should be kept sufficiently away from the MPB composition to avoid overpoling of the crystals (6-7)%PT is thus selected as the optimum composition for PZN-PT single crystals This present work also involves the property characterization of [111]-single domain, [001] and [011] multi-domain PZN-(6-7)%PT single crystals Their complete property matrices are generated experimentally using resonance technique Also, [001] and VII [011] property matrices are predicted from [111]-single domain data, using axis transformation Results show that, [111]-single domain crystals exhibits extremely high piezoelectric coefficients (d15= 6000 pC/N) [001]-poled multi-domain crystals show high longitudinal and transverse piezoelectric coefficients but very low shear coefficients On the other hand, [011]-poled multi-domain crystals exhibits extremely high transverse (d32 = 3000 pC/N) piezoelectric coefficients Discrepancies between the measured and predicted materials constants of multi-domain crystals are discussed in view of extrinsic contributions Results show that the effect of extrinsic contribution to the piezoelectric properties in [001]-poled multi-domain crystals is negligible however they play a significant role in [011]-poled multi-domain crystals Finally, the measured properties of PZN-PT single crystals are discussed in view of previously reported properties in comparison with their similar counter part PMN-PT single crystals VIII List of Figures 2.1 A classification for the 32 crystallographic point groups………………………….4 2.2 Dielectric polarization hysteresis loop of a ferroelectric material…………………7 2.3 Basic relaxor characteristics (a) Dielectric properties, (b) Polarization -Electric field curve behaviour [23]……………………………………………… 11 2.4 Perovskite structures of various crystallographic crystal structures…………… 12 2.5 Ferroelectric domain orientational states of Rhombohedral, tetragonal, Orthorhombic, Monoclinic Cm and Pm phases…………………………………….14 2.6 Standard coordinates of different point group symmetries……………………… 15 2.7 Phase diagram of PZT FT-FM and PC-FT transition temperatures for x=0.48 and x=0.50 are plotted as solid symbols [26]…………………………………….17 2.8 Phase diagram of Pb(Zn1/3 Nb2/3)O3- PbTiO3 system [17]……………………… 19 2.9 (a) New phase diagram of PZN-xPT, (b) Sketch of the perovskite unit cell with the polarization vector (solid arrow) in the monoclinic MA phase, rotating between the rhombohedral (R) and tetragonal (T) phases in the (1 0) plane (shaded) (c) Sketch of the Perovskite unit cell with polarization vectors (solid arrows) in the monoclinic MC and orthorhombic (O) phases, rotating in the (010) plane (shaded)…………………………………………………………………………….24 2.10 Domain structures and phase transition of a (001) PZN91/9 crystal platelet (48µm thick): (a) Coexistence of the rhombohedral domains (R, with extinction // cub) and the tetragonal domains (T, with extinction // cub); (b) Morphotropic phase transitions from the rhombohedral (in extinction) to the tetragonal phase at 70ºC……………………………………………………………31 IX References J Valasek, “Piezo-electricity and allied phenomena in Rochelle salt”, Physical Review, 17, (1921), 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Single Crystals Structural Characterization of PZN- PT Single Crystals 21 Domain Structures in Relaxor PZN- PT Single Crystals 28 Chapter 3: Growth and Longitudinal Properties of PZN- PT Single Crystals. .. Properties of PZN- (6-7) %PT Single Domain Crystals 147 9.6 Full Property Matrices of Multi-domain PZN- 7 %PT Single Crystals1 49 9.7 Comparison with Reported Properties of PMN -PT Single Crystals 150 Chapter... during cycling of applied fields 2.5 Relaxor PZN- PT Single Crystals 2.5.1 Crystal Growth and Properties of PZN- PT Single Crystals Lead zinc niobate, Pb(Zn1/3Nb2/3)O3 (PZN) , is a relaxor ferroelectric