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Register a new userSymmetry of high-piezoelectric Pb-based complex perovskites at the morphotropic phase boundary I. Neutron diffraction study on Pb(Zn1/3Nb2/3)O3 -9%PbTiO3
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Yoshiaki Uesu
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The symmetry was examined using neutron diffraction method on Pb(Zn1/3Nb2/3)O3 -9%PbTiO3 (PZN/9PT) which has a composition at the morphotropic phase boundary (MPB) between Pb(Zn1/3Nb2/3)O3 and PbTiO3. The results were compared with those of other specimens with same composition but with different prehistory. The equilibrium state of all examined specimens is not the mixture of rhombohedral and tetragonal phases of the end members but exists in a new polarization rotation line Mc# (orthorhombic-monoclinic line). Among examined specimens, one exhibited tetragonal symmetry at room temperature but recovered monoclinic phase after a cooling and heating cycle.
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The temperature dependence of elastic, dielectric, and piezoelectric properties of (65-x)Pb(Mg1/3Nb2/3)O3-xBaTiO335-PbTiO3 ceramics with x=0, 1, 2, 3, and 4 was investigated. Compound with x=2 was found to exhibit a large piezoelectric response (d31=-170 pC/N, d33=530 pC/N at 300 K). Particularly, its d31 value was nearly a constant over a temperature range from 185 to 360 K. A broad ferroelectric phase transition tuned by BaTiO3 doping was deduced from the dielectric constant, elastic compliance constant and Raman spectra. The temperature-stable piezoelectric response was attributed to the counter-balance of contributions from the dielectric and elastic responses.
Single crystals of Pb(In1/2Nb1/2)O3-Pb(Mg1/3Nb2/3)O3-PbTiO3 (PIN-PMN-PT) poled along [001] were investigated by dielectric, x-ray, and polarized light (PLM) and piezo-force microscopy (PFM) methods. PLM revealed {100} macro-domain plates that formed after poling, whose size increased on heating between room temperature and a rhombohedral rightarrow tetragonal phase transition, above which point a break-up of the macro-domain plates was observed. Corresponding PFM studies demonstrated that poling reduced the size of stripe-like domains that were internal to the macro-domain plates, whose size also increased on heating to TR-T. The temperature dependence of both the size of the macro-domain plates and internal sub-domains followed the Arrhenius relation with the activation energy of 0.4-0.5eV. The coercive field displays an abnormal increase on heating below TR-T, different than that for PMN-PT. The anomalously increased coercive field can be ascribed to the Arrhenius-type domain growth, indicating a simple thermally activated process and an important role of hierarchial domains in the improved performance of PIN-PMN-PT.
Single crystals of the relaxor PZN-xPT display an enormously strong piezoelectric character. Recent x-ray scattering studies have revealed novel electric-field induced phase transitions in PZN-8%PT. As-grown crystals exhibit a rhombohedral structure that, under application of an electric field oriented along [001], transforms into a monoclinic (MA) phase, and then irreversibly to another monoclinic (MC) phase with increasing field strength. Since the latter phase change is very unusual, its transition sequence has been investigated by using triple-axis neutron scattering techniques so that the ``skin effect observed by x-ray scattering can be avoided, and the entire crystal bulk is probed. Contour maps of the elastic scattering have been mapped out in each phase in the (HOL) zone with high q-resolution. Increasing the field strength within the MC phase induces a sharp c-axis jump around 15 kV/cm. This jump was observed easily with x-rays in previous studies, but it was not observed in 5 different crystals examined with neutrons. A subsequent high-energy x-ray study of the same crystals showed that the c-axis jump is distributed within the crystal volume, thereby washing out the jump. The observed R-MA-MC transformational path is in perfect accord with very recent first principles calculations by Bellaiche, Garcia, and Vanderbilt in the PZT system.
Neutron and x-ray diffraction techniques have been used to study the competing long and short-range polar order in the relaxor ferroelectric Pb(Mg$_{1/3}$Nb$_{2/3}$)O$_{3}$ (PMN) under a [111] applied electric field. Despite reports of a structural transition from a cubic phase to a rhombohedral phase for fields E $>$ 1.7 kV/cm, we find that the bulk unit cell remains cubic (within a sensitivity of 90$^{circ}$-$alpha$ =0.03$^{circ}$)for fields up to 8 kV/cm. Furthermore, we observe a structural transition confined to the near surface volume or `skin of the crystal where the cubic cell is transformed to a rhombohedral unit cell at T$_{c}$=210 K for E $>$ 4 kV/cm, for which 90$^{circ}$-$alpha$=0.08 $pm$ 0.03$^{circ}$ below 50 K. While the bulk unit cell remains cubic, a suppression of the diffuse scattering and concomitant enhancement of the Bragg peak intensity is observed below T$_{c}$=210 K, indicating a more ordered structure with increasing electric field yet an absence of a long-range ferroelectric ground state in the bulk. The electric field strength has little effect on the diffuse scattering above T$_{c}$, however below T$_{c}$ the diffuse scattering is reduced in intensity and adopts an asymmetric lineshape in reciprocal space. The absence of hysteresis in our neutron measurements (on the bulk) and the presence of two distinct temperature scales suggests that the ground state of PMN is not a frozen glassy phase as suggested by some theories but is better understood in terms of random fields introduced through the presence of structural disorder. Based on these results, we also suggest that PMN represents an extreme example of the two-length scale problem, and that the presence of a distinct skin maybe necessary for a relaxor ground state.
Temperature dependent structural changes in a nearly pure monoclinic phase composition (x=0.525) of Pb(Zr_xTi_1-x)O_3 (PZT) have been investigated using Rietveld analysis of high-resolution synchrotron powder x-ray diffraction data and correlated with changes in the dielectric constant and planar electromechanical coupling coefficient. Our results show that the intrinsic piezoelectric response of the tetragonal phase of PZT is higher than that of the monoclinic phase. It is also shown that the high piezoelectric response of PZT may be linked with an anomalous softening of the elastic modulus (1/S_11) of the tetragonal compositions closest to the morphotropic phase boundary.
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