Chemically prepared Pb(Zr0.95Ti0.05)O3 (PZT 95/5) ceramics were fabricated with a range of different porosity levels, while grain size was held constant, by systematic additions of added organic pore former (Avicel). Use of Avicel in amounts ranging from 0 to 4.0 wt% resulted in fired ceramic densities that ranged from 97.3% to 82.3%. Hydrostatic‐pressure‐induced ferroelectric (FE) to antiferroelectric (AFE) phase transformations were substantially more diffuse and occurred at lower hydrostatic pressures with increasing porosity. An ∼12 MPa decrease in hydrostatic transformation pressure per volume percent added porosity was observed. The decrease in transformation pressure with decreasing density was quantitatively consistent with the calculated macroscopic stress required to achieve a specific volumetric macrostrain (0.40%). This strain was equivalent to experimentally measured macrostrain for FE‐to‐AFE transformation. The macroscopic stress levels were calculated using measured bulk modulus values that decreased from 84 to 46 GPa as density decreased from 97.3% to 82.3%. Good agreement between calculated and measured values of FE‐to‐AFE transformation stress was obtained for ceramics fired at 1275° and 1345°C.
Robocasting, which is a computer-controlled slurry-deposition technique, was used to fabricate ceramic monoliths and composites of chemically prepared Pb(Zr 0.95 Ti 0.05 )O 3 ceramics. The densities and electrical properties of the robocast samples were equivalent to those obtained for cold isostatically pressed parts formed under a pressure of 200 MPa. Three-layer robocast composites that consisted of alternating layers of different sintered densities-93.9%/96.1%/93.9%-were fabricated using different levels of organic pore-former additions. Modification from a single-material to a multiple-material deposition robocaster was essential for the fabrication of composites that could withstand repeated cycles of saturated polarization switching under fields of 30 kV/cm. Furthermore, these composites withstood a poled ferroelectric-to-antiferroelectric phase transformation that was induced by a hydrostatic pressure of 500 MPa, during which strain differences on the order of 0.8% occurred between the composite elements.
The hydrostatically induced ferroelectric(FE)-to-antiferroelectric(AFE) phase transformation for chemically prepared niobium modified PZT 95/5 ceramics was studied as a function of density and pore former type (Lucite or Avicel). Special attention was placed on the effect of different pore formers on the charge release behavior associated with the FE-to-AFE phase transformation. Within the same density range (7.26 g/cm 3 to 7.44 g/cm 3), results showed that ceramics prepared with Lucite pore former exhibit a higher bulk modulus and a sharper polarization release behavior than those prepared with Avicel. In addition, the average transformation pressure was 10.7% greater and the amount of polarization released was 2.1% higher for ceramics with Lucite pore former. The increased transformation pressure was attributed to the increase of bulk modulus associated with Lucite pore former. Data indicated that a minimum volumetric transformational strain of-0.42% was required to trigger the hydrostatically induced FEto-AFE phase transformation. This work has important implications for increasing the high temperature charge output for neutron generator power supply units.
Specimens of poled and unpoled PZST ceramic were tested under hydrostatic loading conditions at temperatures of -55, 25, and 75°C. The objective of this experimental study was to obtain the electro-mechanical properties of the ceramic and the criteria of FE (Ferroelectric) to AFE (Antiferroelectric) phase transformations of the PZST ceramic to aid grain-scale modeling efforts in developing and testing realistic response models for use in simulation codes. As seen in previous studies, the poled ceramic from PZST undergoes anisotropic deformation during the transition from a FE to an AFE phase at -55°C. Warmer temperature tests exhibit anisotropic deformation in both the FE and AFE phase. The phase transformation is permanent at -55°C for all ceramics tests, whereas the transformation can be completely reversed at 25 and 75°C. The change in the phase transformation pressures at different temperatures were practically identical for both unpoled and poled PZST specimens. Bulk modulus for both poled and unpoled material was lowest in the FE phase, intermediate in the transition phase, and highest in the AFE phase. Additionally, bulk modulus varies with temperature in that PZST is stiffer as temperature decreases. Results from one poled-biased test for PZST and four poled-biased tests from PNZT 95/5-2Nb are presented. A bias of 1kV did not show noticeable differences in phase transformation pressure for the PZST material. However, with PNZT 95/5-2Nb phase transformation pressure increased with increasing voltage bias up to 4.5kV. 3 AcknowledgementsThe authors would like to acknowledge Thomas Pfeifle for his critical review of this report. The authors also thank Tim Scofield for overseeing fabrication of the PZST specimens.
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