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Lead loss during processing of solution-derived Pb(Zr,Ti)O3 (PZT)-based thin-films can result in the formation of a Pb-deficient, nonferroelectric fluorite phase that is detrimental to dielectric properties. It has recently been shown that this nonferroelectric fluorite phase can be converted to the desired perovskite phase by postcrystallization treatment. Here, quantitative standard-based energy-dispersive x-ray spectrometry (EDS) in a scanning transmission electron microscope (STEM) is used to study cation distribution before and after this fluorite-to-perovskite transformation. Single-phase perovskite PbZr0.53Ti0.47O3 (PZT 53/47) and Pb0.88La0.12Zr0.68Ti0.29O3 (PLZT 12/70/30) specimens that underwent this treatment were found to be chemically indistinguishable from the perovskite present in the multiphase specimens prior to the fluorite-to-perovskite transformation. Significant Zr–Ti segregation is found in PLZT 12/70/30, but not in PZT 53/47. Slight La-segregation was seen in rapidly crystallized PLZT, but not in more slowly crystallized PLZT.
Chemical solution deposition has been used to fabricate continuous ultrathin lead lanthanum zirconate titanate (PLZT) films as thin as 20 nm. Further, multilayer capacitor structures with as many as 10 dielectric layers have been fabricated from these ultrathin PLZT films by alternating spin-coated dielectric layers with sputtered platinum electrodes. Integrating a photolithographically defined wet etch step to the fabrication process enabled the production of functional multilayer stacks with capacitance values exceeding 600 nF. Such ultrathin multilayer capacitors offer tremendous advantages for further miniaturization of integrated passive components.
A facile solution-based processing route using standard spin-coating deposition techniques has been developed for the production of reliable capacitors based on lead lanthanum zirconate titanate (PLZT) with active areas of ⩾1 mm2 and dielectric layer thicknesses down to 50 nm. With careful control of the dielectric phase development through improved processing, ultrathin capacitors exhibited slim ferroelectric hysteresis loops and dielectric constants of >1000, similar to those of much thicker films. Thus, it has been demonstrated that chemical solution deposition is a viable route to the production of capacitor films which are as thin as 50 nm but are still macroscopically addressable with specific capacitance values >160 nF/mm2.
Chemically prepared zinc oxide powders were processed for the production of high aspect ratio varistor components (length/diameter >5). Near-net-shape casting methods including slip casting and agarose gelcasting were evaluated for effectiveness in achieving a uniform green microstructure that densifies to near theoretical values during sintering. The structure of the green parts was examined by mercury porisimetry. Agarose gelcasting produced green parts having low solids loading values and did not achieve high fired density. Isopressing the agarose cast parts after drying raised the fired density to greater than 95%, but the parts exhibited catastrophic shorting during electrical testing. Slip casting produced high green density parts, which exhibit high fired density values. The electrical characteristics of slip-cast parts are comparable with dry-pressed powder compacts.
Lanthanide (Ln) doping of lead zirconate titanate (PLnZT 4/30/70) thin films was conducted to investigate effects on structural and electrical properties. Films were spin-coat deposited from precursor solutions made using a previously reported “basic route to PZT” chemistry. The remanent polarization (Pr), dielectric constant (ε), dielectric loss (tan δ), and lattice parameter values were obtained for each of the doped PLnZT films. Films doped with amphoteric cations (Tb, Dy, Y, and Ho) displayed high Pr values, square hysteresis loops, and enhanced fatigue resistance. Smaller radius Ln-doped films display an increased tendency toward (100) orientation in otherwise (111)-oriented films.
Pb(Zr,Ti)O3 (PZT) thin films are being developed for use in optical and electronic memory devices. To study ferroelectric switching behavior, we have produced relatively untextured PZT thin films on Si substrates. We have developed a method for using x-ray diffraction to observe domain switching in situ. Our study involved the use of a micro-diffractometer to monitor the switching behavior in relatively small (0.7mm diameter) electroded areas. Diffraction analyses were done while DC voltages were applied and removed, representing several places in the hysteresis loop. In particular, we were looking for relative intensity changes in the [h 00],[00l] diffraction peaks as a function of position in the hysteresis loop. Our study indicates that the 90° domain switching exhibited by bulk ferroelectrics, is very limited in films on Si when grain sizes are less than about 1 μm.
Switchable polarization can be significantly suppressed in ferroelectric (FE) materials by optical, thermal, and electrical processes. The thermal process can occur by either annealing the FE in a reducing environment or by heating it in air to 100°C while impressing a bias near the switching threshold. The optical process occurs while biasing the FE near the switching threshold and illuminating with bandgap light. And the electrical suppression effect occurs by subjecting the FE to repeated polarization reversals. Using electron paramagnetic resonance, polarization-vol tage measurements, and charge injection scenarios, we have been able to elucidate both electronic and ionic trapping effects that lead to a suppression in the amount of switchable polarization in FE materials. The relative roles of electronic and ionic effects in the same material can depend on the stress condition. For instance, in oxidized BaTiO3 crystals, optical and thermal suppressions occur by electronic domain pinning; electrical fatigue in the BaTiO3 crystals also appears to involve electronic charge trapping, however, it is suggested that these electronic traps are further stabilized by nearby ionic defects. In sol-gel PZT thin films with either Pt, RuO2, or La-Sr-Co-O electrodes it appears that the polarization suppression induced by electrical fatigue, a temperature/bias combination, or a light/bias combination are all primarily due to the trapping of electronic charge carriers to first order.
Prototype ferroelectric thin film, nonvolatile memory, nondestructive readout (NDRO), semiconductor devices have been fabricated. The “1” and “0” logic states of these prototype devices are in principle determined by the modulation of the conductivity of a semiconductor film channel by the polarization state of the underlying ferroelectric thin film layer. Programmed resistance ratios of the two logic states of 5:1 are demonstrated. While the best performance to date has been achieved for devices that have a 40 nm ln2O3 film covering a 300 nm thick PZT 20/80 layer, we also develop criteria for selecting semiconductor films that will improve performance for this NDRO device design. Among the other semiconductor films that are characterized with respect to this criteria are boron doped Ge, ZnO and aluminum doped ZnO. It is demonstrated that by appropriate donor doping of ZnO films the effects of intrinsic defects are masked and that process temperatures can be extended by 300×C.
Ferroelectric polycrystalline thin films are being pursued as materials for use in the next generation of radiation hardened nonvolatile semiconductor memories, optical switches and optical computers. Of particular interest are PZT films with a composition near the morphotropic phase boundary. In order to fully understand the the difference in electrical properties as a function of processing parameters it is necessary to fully characterize phase composition and crystallographic properties of these films. Since some films are produced by either spinning or dipping successive layers to obtain the desired thickness it was necessary to compare the properties of each layer.
X-ray diffraction techniques employing parallel beam optics with grazing incidence angle geometry were used to characterize the films. Experimental procedures using sealed tube xray diffraction systems to determine differences in crystallite size and microstrain as a function of depth into the films are a rather unique application of this technique. Discerning the contribution to line broadening due to phase changes, grazing incident angle geometry, crystallite size and microstrain are key to the success of this technique.
This paper discusses the experimental techniques employed and will demonstrate how we were able to successfully determine microstrain as a function of depth into the film. We use transmission electron microscopy (TEM) to aid in the characterization of the films. A brief description of the processing procedures used to produce the films is also provided.
The use of grazing incidence parallel beam x-ray diffraction (GIXRD) in the characterization of lead zirconate titanate (PZT) films is described. This tool has enabled us to depth profile the films. The transmission electron microscopy (TEM) results obtained from a cross section of one film are shown to compliment the GIXRD results. The variation in crystallographic structure versus depth in the film was the primary focus of this study.
The insults from three PZT films having Zr/Ti ratios of 25/75, 48/52, and 75/25 are given. TEM results are reported from the sample with a Zr/Ti ratio of 48/52.
We have systematically varied processing parameters to fabricate PZT 53/47 thin films. Polycrystalline PZT thin films were fabricated by spin depositing Pt coated Sio2/Si substrates with alkoxide solutions. Our study focused on two process parameters: 1) heating rate and 2) excess Pb additions. We used rapid thermal processing techniques to vary heating rates from 3°C/min to 8400°C/min. Films were characterized with the following excess Pb additions: 0, 3, 5, and 10 mol% For all process variations, films with greater perovskite content had better ferroelectric properties. Our best films were fabricated using the following process parameters: an excess Pb addition of 5 mol%, a heating rate of 8400°C/min and annealing conditions of 700°C for 1 min. Films fabricated using these process conditions had a remanent polarization of 0.27 C/m2and a coercive field of 3.4 MV/m.
Electronic ceramic materials research is one of the fastest growing, most highly publicized areas of materials science. Subjects receiving considerable attention include high temperature superconductors, multilayer ceramic composites for high density microelectronics packaging, and ferroelectric electro-optic thin films. A complete review of all aspects of electronic ceramics research is beyond the scope of this article, which will focus on two general topics whose development is representative of recent contributions to the field. These two areas are synthesis and characterization of electronic ceramic films,1 and controlled use of low level dopants (1,000 ppm or less) in bulk polycrystalline ceramics, thin films, and single crystals to achieve desired properties. Perspective of the progress in ceramic film development is given by a review of single-crystal synthesis and properties.
Several examples of the impact that low level dopants and thin film synthesis have on electronic ceramics development are presented. Dopant concentrations of 1,000 ppm or less can have a dramatic effect on microstructural, optical, and electrical properties. For example, a decrease in aluminum content of 150 ppm resulted in an increase in grain size from 1 to 25 microns in otherwise identical ZnO varistors. Background aluminum concentrations for these varistors were less than 10 ppm. In another example, the photorefractive effect, the change in refractive index with optical light intensity, has been shown to be altered by orders of magnitude with ppm doping levels in ferroelectric electro-optic materials.
Several electronic ceramic devices have recently been developed due to improvements in ceramic film processing. Examples of these devices include: 1. multilayer PZT transformers, which allow fabrication of complex monolithic passive multicom-ponent networks, 2. liquid cooled multilayer ceramic substrates, with 400×800 micron liquid transfer capillaries integrated into the multilayer structure via ceramic processing techniques for high density VLSI packaging, and 3. ferroelectric electrooptic thin films that are compatible with silicon or III-V technology. For all the above applications, synthesis of electronic ceramic materials into high purity films is essential.
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