Switching behavior of 90° domains in epitaxial Pb(Zr0.32Ti0.68)O3 thin films under applied bias voltage was investigated in situ using synchrotron x-ray diffraction, and contribution of the switching to ferroelectric P–E hysteresis curve could be estimated. The electric field in the region illuminated by x ray was made confined exactly normal to the film/substrate interface by patterning an isolated capacitor (1×1 mm2) and etching off the remainder in order to eliminate mechanical constraint from nonswitching region. The portion of polarization taken up by 90° domain reversal was separated from 180° domain switching after measuring the changes in relative intensity ratio of PZT (001) and (100) reflections, which exhibited hysteresis behavior depending on applied voltage. Within the experimental region of electric field up to 24 kV/mm, maximum 27.8% of 90° domains were reoriented, which corresponds to ∼2% contribution to total polarization.
Epitaxial (Pb1−xSrx)TiO3 (PST, x = 4 0.0–0.24) thin films were grown on MgO(001) single-crystal substrates by pulsed laser deposition. General x-ray diffraction techniques including θ–2θ scan and rocking curve were used to determine lattice constants, degree of c-axis orientation, and crystal quality of the tetragonal thin films. The degree of c-axis orientation in the epitaxial PST films increased as Sr concentration (x) increased, which in turn induces the systematic change in the Curie temperature as well as the transformation strain at and below the Curie temperature. An inverse relation between the c-domain abundances and the transformation strains is established.
Epitaxial Pb(Zr x Ti 12x )O 3 (x 0.0-0.32) ferroelectric thin films of 500 nm thickness were grown on MgO(001) single crystal substrates by in situ rf magnetron sputtering, and evolution of their domain structures is characterized by employing various x-ray diffraction techniques. X-ray u-2u scan showed the films were grown highly c-axis oriented with a tetragonal perovskite structure. 90 ± domain configuration was investigated using the x-ray rocking curve analysis for PZT 100 peaks in two different f angles. The rocking curve analysis showed that the degree of c-axis orientation and the crystalline quality of the films were improved continuously with increasing Zr concentration. The c-domain abundance as a function of Zr concentration was quantified using the x-ray rocking curves of PZT 001 and 100, taking account of structural factors and Lorentz-polarization factors. High temperature x-ray technique was also employed to quantify the domain structure as a function of temperature during cooling after reheating the samples to 650 ± C. During the cooling process, c-domain abundance was found to increase continuously while the crystalline quality of the films was deteriorated below the Curie temperature. The results led us to conclude that the transformation strain of the film at and below the Curie temperature plays a significant role in the final domain structure and abundance of epitaxial PZT thin films.132
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