Publications

Abstract not provided.

Structural phase transformations between ferroelectric (FE), antiferroelectric (AFE), and paraelectric (FE) phases are frequently observed in the zirconia-rich phase region on the lead zirconate-titanate (PZT) phase diagram. Since the free energy difference among these phases is small, phase transformation can be easily induced by temperature, pressure and electric field. These induced transformation characteristics have been used for many practical applications. This study focuses on a hydrostatic pressure induced FE-to-AFE phase transformation in a tin modified PZT ceramic (PSZT). The relative phase stability between FE and AFE phases is determined by the dielectric permittivity measurement as a function of temperature from -60 C to 125 C. A pressure-temperature phase diagram for the PSZT system will be presented.

Phase transformation between the ferroelectric (FE) and the antiferroelectric (AFE) phases in tin modified lead zirconate titanate (PSZT) ceramics can be influenced by pressure and electric field. Increasing the pressure has the tendency to favor the AFE phase while electric field favors the FE phase. In this study, these phase transformations are studied as functions of external pressure, temperature, and dc bias. The shifting of transformation temperature and the relative phase stability between FE and AFE with respect to these external parameters will be presented. Results will be compared to a pressure-induced depoling behavior (or FE-to-AFE phase transformation) for the PSZT ceramic. Fundamental issues relates to the relative phase stability will be discussed from the perspective of lattice dynamics theory.

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.

The effect of composition on the elastic responses of alumina particle-filled epoxy composites is examined using isotropic elastic response models relating the average stresses and strains in a discretely reinforced composite material consisting of perfectly bonded and uniformly distributed particles in a solid isotropic elastic matrix. Responses for small elastic deformations and large hydrostatic and plane-strain compressions are considered. The response model for small elastic deformations depends on known elastic properties of the matrix and particles, the volume fraction of the particles, and two additional material properties that reflect the composition and microstructure of the composite material. These two material properties, called strain concentration coefficients, are characterized for eleven alumina-filled epoxy composites. It is found that while the strain concentration coefficients depend strongly on the volume fraction of alumina particles, no significant dependence on particle morphology and size is observed for the compositions examined. Additionally, an analysis of the strain concentration coefficients reveals a remarkably simple dependency on the alumina volume fraction. Responses for large hydrostatic and plane-strain compressions are obtained by generalizing the equations developed for small deformation, and letting the alumina volume fraction in the composite increase with compression. The large compression plane-strain response model is shown to predict equilibrium Hugoniot states in alumina-filled epoxy compositions remarkably well.

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Alumina-filled epoxies are composites having constituents with highly dissimilar mechanical properties, resulting in complex behavior during shock compression and release. Two distinguishing characteristics are amplitude-dependent wave structures and high release wave velocities. Recent studies examined the effects of various compositional changes on these shock properties. As expected, the strongest effects were observed when the total alumina volume fraction was reduced in steps from a nominal 43% to 0%. In the present study, compositions prepared over the same range of alumina loadings were examined at initial temperatures that were nominally -55 °C or 70 °C. Experimental configurations were identical to previous room-temperature experiments. Laser interferometry and wave timing were used to obtain transmitted wave profiles, Hugoniot states, and release wave velocities. Initial densities were determined from thermal expansion coefficients measured for each composition. Although initial density changes are very small, significant temperature effects on shock properties were observed. © 2007 American Institute of Physics.

A strong electric field can be generated when the shock-induced depoling current from a normally poled PZT 95/5 sample is passed through a large resistive load. The portion of total depoling current that is retained on the sample electrodes to account for capacitance is governed by the dynamic dielectric properties of both unshocked and shocked material. Early studies used measured load currents from single samples to assess models for dielectric response. In more recent studies, we used shock-driven circuits in which multiple PZT 95/5 elements were displaced both parallel and perpendicular to the shock motion. This allowed both load and charging currents to be measured for individual elements that are subjected to shock compression and release at different times. In the present study, these techniques have been utilized to examine dielectric properties in PZT 95/5 samples at initial temperatures from -56 to 74 °C. Significant changes in permittivity with temperature are observed in both unshocked and shocked samples. Measured currents show a complex dielectric response which can only be partially predicted using a simple dielectric relaxation model. © 2007 American Institute of Physics.

Specimens of poled and unpoled ''chem-prep'' PNZT ceramic from batch HF1035 were tested under hydrostatic, uniaxial, and constant stress difference loading conditions at -55, 25, and 75 C. The objective of this experimental study was to characterize the mechanical properties and conditions for the ferroelectric (FE) to antiferroelectric (AFE) phase transformations of this ''chem-prep'' PNZT ceramic to aid grain-scale modeling efforts in developing and testing realistic response models for use in simulation codes. As seen from a previously characterized material (batch HF803), poled ceramic from HF1035 was seen to undergo anisotropic deformation during the transition from a FE to an AFE phase. Also, the phase transformation was found to be permanent for the two low temperature conditions, whereas the transformation can be completely reversed at the highest temperature. The rates of increase in the phase transformation pressures with temperature were practically identical for both unpoled and poled PNZT HF1035 specimens. We observed that temperature spread the phase transformation over mean stress analogous to the observed spread over mean stress due to shear stress. Additionally, for poled ceramic samples, the FE to AFE phase transformation was seen to occur when the normal compressive stress, acting perpendicular to a crystallographic plane about the polar axis, equals the hydrostatic pressure at which the transformation otherwise takes place.

Detailed statistical analysis of the experimental data from testing of alumina-loaded epoxy (ALOX) composites was conducted to better understand influences of the selected compositional properties on the compressive strength of these ALOX composites. Analysis of variance (ANOVA) for different models with different sets of parameters identified the optimal statistical model as, y{sub l} = -150.71 + 29.72T{sub l} + 204.71D{sub l} + 160.93S{sub 1l} + 90.41S{sub 2l}-20.366T{sub l}S{sub 2l}-137.85D{sub l}S{sub 1l}-90.08D{sub l}S{sub 2l} where y{sub l} is the predicted compressive strength, T{sub l} is the powder type, D{sub l} is the density as the covariate for powder volume concentration, and S{sub il}(i=1,2) is the strain rate. Based on the optimal statistical model, we conclude that the compressive strength of the ALOX composite is significantly influenced by the three main factors examined: powder type, density, and strain rate. We also found that the compressive strength of the ALOX composite is significantly influenced by interactions between the powder type and the strain rate and between the powder volume concentration and the strain rate. However, the interaction between the powder type and the powder volume concentration may not significantly influence the compressive strength of the ALOX composite.

Abstract not provided.

Abstract not provided.

Specimens of poled 'chem-prep' PNZT ceramic from batch HF803 were tested under hydrostatic, uniaxial, and constant stress difference loading conditions at three temperatures of -55, 25, and 75 C and pressures up to 500 MPa. 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 so that grain-scale modeling efforts can develop and test models and codes using realistic parameters. The poled ceramic undergoes anisotropic deformation during the transition from a FE to an AFE structure. The lateral strain measured parallel to the poling direction was typically 35 % greater than the strain measured perpendicular to the poling direction. The rates of increase in the phase transformation pressures per temperature changes were practically identical for both unpoled and poled PNZT HF803 specimens. We observed that the retarding effect of temperature on the kinetics of phase transformation appears to be analogous to the effect of shear stress. We also observed that the FE-to-AFE phase transformation occurs in poled ceramic when the normal compressive stress, acting perpendicular to a crystallographic plane about the polar axis, equals the hydrostatic pressure at which the transformation otherwise takes place.

Sandia is currently developing a lead-zirconate-titanate ceramic 95/5-2Nb (or PNZT) from chemically prepared ('chem-prep') precursor powders. Previous PNZT ceramic was fabricated from the powders prepared using a 'mixed-oxide' process. The specimens of unpoled PNZT ceramic from batch HF803 were tested under hydrostatic, uniaxial, and constant stress difference loading conditions within the temperature range of -55 to 75 C and pressures to 500 MPa. The objective of this experimental study was to obtain mechanical properties and phase relationships so that the grain-scale modeling effort can develop and test its models and codes using realistic parameters. The stress-strain behavior of 'chem-prep' PNZT under different loading paths was found to be similar to that of 'mixed-oxide' PNZT. The phase transformation from ferroelectric to antiferroelectric occurs in unpoled ceramic with abrupt increase in volumetric strain of about 0.7 % when the maximum compressive stress, regardless of loading paths, equals the hydrostatic pressure at which the transformation otherwise takes place. The stress-volumetric strain relationship of the ceramic undergoing a phase transformation was analyzed quantitatively using a linear regression analysis. The pressure (P{sub T1}{sup H}) required for the onset of phase transformation with respect to temperature is represented by the best-fit line, P{sub T1}{sup H} (MPa) = 227 + 0.76 T (C). We also confirmed that increasing shear stress lowers the mean stress and the volumetric strain required to trigger phase transformation. At the lower bound (-55 C) of the tested temperature range, the phase transformation is permanent and irreversible. However, at the upper bound (75 C), the phase transformation is completely reversible as the stress causing phase transformation is removed.

Aluminum oxide (ALOX) filled epoxy is the dielectric encapsulant in shock driven high-voltage power supplies. ALOX encapsulants display a high dielectric strength under purely electrical stress, but minimal information is available on the combined effects of high voltage and mechanical shock. We report breakdown results from applying electrical stress in the form of a unipolar high-voltage pulse of the order of 10-{micro}s duration, and our findings may establish a basis for understanding the results from proposed combined-stress experiments. A test specimen geometry giving approximately uniform fields is used to compare three ALOX encapsulant formulations, which include the new-baseline 459 epoxy resin encapsulant and a variant in which the Alcoa T-64 alumina filler is replaced with Sumitomo AA-10 alumina. None of these encapsulants show a sensitivity to ionizing radiation. We also report results from specimens with sharp-edged electrodes that cause strong, localized field enhancement as might be present near electrically-discharged mechanical fractures in an encapsulant. Under these conditions the 459-epoxy ALOX encapsulant displays approximately 40% lower dielectric strength than the older Z-cured Epon 828 formulation. An investigation of several processing variables did not reveal an explanation for this reduced performance. The 459-epoxy encapsulant appears to suffer electrical breakdown if the peak field anywhere reaches a critical level. The stress-strain characteristics of Z-cured ALOX encapsulant are measured under high triaxial pressure and we find that this stress causes permanent deformation and a network of microscopic fractures. Recommendations are made for future experimental work.

In the present study, 10 impact tests were conducted on unpoled PZT 95/5, with 9% porosity and 2 at% Nb doping. These tests were instrumented to obtain time-resolved loading, unloading and span signatures. As well, PVDF gauges allowed shock timing to be established explicitly. The ferroelectric/antiferroelectric phases transition was manifested as a ramp to 0.4 GPa. The onset of crushup produced the most visible signature: a clear wave separation at 2.2 GPa followed by a highly dispersive wave. The end states also reflected crushup, and are consistent with earlier data and with related poled experiments. A span strength value of 0.17 GPa was measured for a shock stress of 0.5 GPa, this decreased to a very small value (no visible pullback signature) for a shock strength of 1.85 GPa.