Chapter 10 Conclusions Based on the results presented in the previous chapters, the following conclusions can be drawn concerning the phase and domain structures in unpoled (annealed) PZN(4.5-9)%PT single crystals (a) The surface layer of carefully-polished PZN-PT single crystals is covered with a deformed layer and is not suitable for typical XRD study A fracture technique has been devised which exposes the relatively strain-free crystal bulk for the XRD study (b) The present work shows that the observed HR-XRD (002) RSMs of PZN-xPT single crystals, 0.045 ≤ x ≤ 0.09, can be understood from the micro- and nanotwin structures of both R and T phases in the material (c) For PZN-xPT of lower PT contents (i.e x ≤ 0.07) at room temperature, the {100}R diffractions manifest as an extremely broad peak at 2θ = 44.50-44.65° Bragg’s position, being the convoluted peak of the four degenerated R microtwins In addition to the extremely broad convoluted R peak, nanotwin diffractions arising from {100}-type and {110}-type R nanotwins have also been 179 detected in selected samples, suggesting that the R phase exist in a mixture of micro and nanotwins in PZN-(4.5-8)%PT single crystals at room condition (d) In addition to the R diffractions, T micro- and nanotwin domains could also be detected in PZN-(6-8)%PT single crystals at room condition Our HR-XRD RSM results indicate that the T phase in these crystal compositions is likely to be a metastable phase stabilized by the cooling-cum-transformation stresses in the crystal This is manifested by the disappearing of the (100)T diffractions on the fracture surface, a result attributed to the stress relaxation effect in the surface layer of the fractured crystal Such stress relaxation effects are expected to be more pronounced for the R+T domains with their {110}R//{110}T interface lying at about 45° to the (100)pc diffraction planes (e) For PZN-9%PT, the dominant phase at room condition is the T phase of both micro- and nanotwin domains, although a small amount of the R phase may also be present (f) Strong evidence of T nanotwins, manifested by their streaked diffractions, has been detected in PZN-(4.5-8)%PT in the vicinity of TR-T phase transformation, suggesting that it presence being promoted by the transformation stress possibly as a means to relax the transformation stresses in the crystal 180 (g) A revised phase diagram for the PZN-PT system has been constructed Two new evident features of this revised phase diagram are: (a) the expanded (R+T) twophase MPB region, and (b) a (T+C) two-phase region at high temperature before the crystal transforms completely into the single C phase (h) The expanded (R+T) MPB region can be further divided into two regions In the lower PT region, 0.06 ≤ x ≤ 0.08, the T phase is metastable stabilized by the residual stress in the crystal In the high PT region, 0.09 ≤ x ≤ 0.10, both the (R+T) phase are thermodynamically stable phases at room temperature (i) The ease with which perovskite crystals may form micro- and nanotwins may play an important role in the reported superior piezoelectricity of PZN-PT and PMN-PT single crystals, especially near their MPBs (j) This present work does not support the existence of M phases in PZN-PT single crystals considering the transformations from M to C, R to MC, and MB to T are not allowed in perovskite structure as according to Landau theory In addition, experimental analysis involving polarization and structural characteristics suggests that the out-of-plane diffractions pertained to coherent diffraction phenomenon associated with micro/nanotwin of R and T 181 Chapter 11 Recommendations for Future Work The present work has shown that micro- and nanotwin domains in both the R and T phases serve to relax the transformation stresses leading to an expanded MPB across 0.06 ≤ x ≤ 0.10 in PZN-xPT single crystals This expanded (R+T) MPB region can be further divided into two different regions In the low PT region (i.e., 0.06 ≤ x ≤ ≈ 0.08), the room temperature T phase is metastable stabilized by the residual stresses in the material In the high PT region (i.e., 0.09 ≤ x ≤ 0.10), both the R and T are thermodynamically stable phases The presence of (R+T) micro- and nanotwin domains is believed to play a role in the superior piezoelectricity of relaxor ferroelectric single crystals In order to provide a better understanding of the structuralproperty relationship in relaxor ferroelectric single crystals, the following topics are recommended for future studies: (a) The fine (002) XRD spectra obtained from SSLS provide circumstantial evidence for the presence of R micro- and nanotwin domains in the PZN-PT single crystals Despite so, the ultra fine nanotwin structure in R, are difficult to resolve with high-synchrotron x-ray as available in SSLS Higher energy x-ray of improved 182 resolution is required to resolve these fine nanotwin diffractions and to decipher the detailed configurations of the R* domains, which 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(001)T domains in PZN( 6-8)%PT crystals, which are shadowed by the R domains upon fracturing (b) To investigate the effects of temperature and E-field on the R and T micro- and nanotwin domains in. ..detected in selected samples, suggesting that the R phase exist in a mixture of micro and nanotwins in PZN- (4. 5- 8)%PT single crystals at room condition (d) In addition to the R diffractions,