Publications

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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.

Chemically prepared zinc oxide powders are fabricated for the production of high aspect ratio varistor components. Colloidal processing was performed to reduce agglomerates to primary particles, form a high solids loadingslurry, and prevent dopant migration. The milled and dispersed powder exhibited a viscoelastic to elastic behavioral transition at a volume loading of 43-46%. The origin of this transition was studied using acoustic spectroscopy, zeta potential measurements, and oscillatory rheology. The phenomenon occurs due to a volume fraction solids dependent reduction in the zeta potential of the solid phase. It is postulated to result from divalent ion binding within the polyelectrolyte dispersant chain and was mitigated using a polyethylene glycol plasticizing additive. This allowed for increased solids loading in the slurry and a green body fabrication study to be presented in our companion paper.

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Calculations of the Hamaker constants representing the van der Waals interactions between conductor, resistor and dielectric materials are performed using Lifshitz theory. The calculation of the parameters for the Ninham-Parsegian relationship for several non-aqueous liquids has been derived based on literature dielectric data. Discussion of the role of van der Waals forces in the dispersion of particles is given for understanding paste formulation. Experimental measurements of viscosity are presented to show the role of dispersant truncation of attractive van der Waals forces.

Embedded resistor circuits have been generated with the use of a Micropen system Ag conductor paste (DuPont 6142D), a new experimental resistor ink from DuPont (E84005-140), and Low Temperature Co-fired Ceramic (LTCC) green tape (DuPont A951). Sample circuits were processed under varying peak temperature ranges (835 C-875 C) and peak soak times (10 min-720 min). Resistors were characterized by SEM, TEM, EDS, and high-temperature XRD. Results indicate that devitrification of resistor glass phase to Celcian, Hexacelcian, and a Zinc-silicate phase occurred in the firing ranges used (835-875 C) but kinetics of divitrification vary substantially over this temperature range. The resistor material appears structurally and chemically compatible with the LTCC. RuO{sub 2} grains do not significantly react with the devitrifying matrix material during processing. RuO{sub 2} grains coarsen significantly with extended time and temperature and the electrical properties appear to be strongly affected by the change in RuO{sub 2} grain size.

The System of Labs Direct Fabrication Technology program was intended to foster cooperation and development in a cooperative effort between Sandia National Labs, Idaho National Energy and Environment Lab and Oak Ridge National Lab. The goal of this program was to bring together LENS (Laser Engineered Net Shaping) from Sandia, INEEL's spray forming process and the alloy development expertise of ORNL. This program investigated the feasibility of combining the LENS and spray forming processes to exploit the best features of both approaches. Further, since both processes were thought to result in a rapidly solidified structure, the alloy design expertise of ORNL offered the opportunity for alloy design or processing options which could more fully utilize the unique capabilities of the processes.

The electrical properties were investigated for ruthenium oxide based devitrifiable resistors embedded within low temperature co-fired ceramics. Special attention was given to the processing conditions and their affects on resistance and temperature coefficient of resistance (TCR). Results indicate that the conductance for these buried resistors is limited by tunneling of charge carriers through the thin glass layer between ruthenium oxide particles. A modified version of the tunneling barrier model is proposed to more accurately account for the microstructure ripening observed during thermal processing. The model parameters determined from curve fitting show that charging energy (i.e., the energy required for a charge carrier to tunnel through the glass barrier) is strongly dependent on particle size and particle-particle separation between ruthenium oxide grains. Initial coarsening of ruthenium oxide grains was found to reduce the charging energy and lower the resistance. However, when extended ripening occurs, the increase in particle-particle separation increases the charging energy, reduces the tunneling probability and gives rise to a higher resistance. The trade-off between these two effects results an optimum microstructure with a minimum resistance and TCR. Furthermore, the TCR of these resistors has been shown to be governed by the magnitude of the charging energy. Model parameters determined by our analysis appear to provide quantitative physical interpretations to the microstructural change in the resistor, which in turn, are controlled by the processing conditions.

High temperature XRD has been employed to monitor the devitrification of Dupont 951 low temperature co-fired ceramic (LTCC) and Dupont E84005 resistor ink. The LTCC underwent devitrification to an anorthite phase in the range of 835-875 C with activation energy of 180 kJ/mol as calculated from kinetic data. The resistor paste underwent devitrification in the 835-875 C range forming monoclinic and hexagonal celcian phases plus a phase believed to be a zinc-silicate. RuO{sub 2} appeared to be stable within this devitrified resistor matrix. X-ray radiography of a co-fired circuit indicated good structural/chemical compatibility between the resistor and LTCC.

The need for advanced (electronic) ceramic components with smaller size, greater functionality, and enhanced reliability requires the ability to integrate electronic ceramics in complex 3-D architectures. However, traditional tape casting and screen printing approaches are poorly suited to the requirements of rapid prototyping and smalI-lot manufacturing. To address this need, we are developing a direct-write approach for fabricating highly integrated, multilayer components using a micropen to deposit slurries in precise patterns. This approach provides the ability to fabricate multifunctional, multimaterial integrated ceramic components (MMICCs) in an agile and rapid way, and has been used to make integrated passive devices such RC filters, inductors, and voltage transformers.

Sandia National Laboratories is developing a new technology to fabricate three-dimensional metallic components directly from CAD solid models. This process, called Laser Engineered Net Shaping (LENS{trademark}), exhibits enormous potential to revolutionize the way in which metal parts, such as complex prototypes, tooling, and small lot production parts, are produced. To perform the process, metal powder is injected into a molten pool created by a focused, high powered laser beam. Simultaneously, the substrate on which the deposition is occurring is scanned under the beam/powder interaction zone to fabricate the desired cross-sectional geometry. Consecutive layers are sequentially deposited, thereby producing a three-dimensional metal component.

The need for advanced (electronic) ceramic components with smaller size, greater functionality, and enhanced reliability requires the ability to integrate electronic ceramics in complex 3-D architectures. For rapid prototyping and small-lot manufacturing, traditional tape casting and screen printing approaches are poorly suited. To address this need, the authors are developing a direct-write approach for fabricating highly integrated, multilayer components using a micropen to deposit slurries in precise patterns. With this technique, components can be constructed layer by layer, simplifying fabrication. It can also be used to produce structures combining several materials in a single layer. The parts are either cofired or sequentially fired, after each layer is deposited. Since differential shrinkage can lead to defects in these multilayer structures, they are characterizing the sintering behavior of individual layers. This technique has been used to fabricate devices such integrated RC filters, multilayer voltage transformers, and other passive components. The direct-write approach provides the ability to fabricate multifunctional, multimaterial integrated ceramic components (MMICCs) in an agile and rapid way.

Thin-film decoupling capacitors based on ferroelectric (Pb,La)(Zr,Ti)O3 films are being developed for use in advanced packaging applications. The increased integration that can be achieved by replacing surface-mount capacitors should lead to decreased package volume and improved high-speed performance. For this application, chemical solution deposition is an appropriate fabrication technique since it is a low-cost, high-throughput process. The use of relatively thick Pt electrodes (approximately 1 μm) to minimize series resistance and inductance is a unique aspect to fabricating these devices. In addition, the important electrical properties are discussed, with particular emphasis on lifetime measurements, which suggest that resistance degradation will not be a severe limitation on device performance. Finally, some of the work being done to develop methods of integrating these thin-film capacitors with ICs and MCMs is presented.

Epitaxial SrRuO{sub 3} thin films were deposited by RF sputtering on SrTiO{sub 3} or MgO substrates for use as underlying electrodes. On these conductive substrates, epitaxial Pb(Zr{sub 0.35}Ti{sub 0.65})O{sub 3} (PZT) and PbTiO{sub 3} (PT) thin films were, deposited by metalorganic chemical vapor deposition (MOCVD). X-ray diffraction (XRD), RBS channeling (RBS), transmission electron microscopy (TEM) and optical waveguiding were used to characterize phase, microstructure, defect structure, refractive index, and film thickness of the deposited films. The PZT and PT films were epitaxial and c-axis oriented. 90{degree} domains, interfacial misfit dislocations and dislocations and threading dislocations were the primary structural defects, and the films showed a 70% RBS channeling reduction. Hysteresis and dielectric measurements of epitaxial PZT ferroelectric capacitor structures formed using evaporated Ag or ITO glass top electrode showed: a remanent polarization of 46.2 mC/cm{sup 2}, a coercive field of 54.9 KV/cm, a dielectric constant of 410, a bipolar resistivity of {approximately}5.8 {times} 10{sup 9} {Omega}-cm at a field of 275 KV/cm, and a breakdown strength of >400 KV/cm.

The photocurrent response, photo-induced changes in hysteresis behavior, and electrooptic (birefringence) effects of sol-gel derived PZT film have been characterized as part of an effort to evaluate ferroelectric films for image storage and processing applications.

Although the feasibility of using PZT and PLZT films for optical data processing applications, such as optical storage disks, image comparators, and spatial light modulators, has clearly been established, most of the critical parameters related to the storage and readout processes still need to be evaluated. Optical readout techniques capable of nondestructively determining the value of polarization are based either on the quadratic electrooptic effect or on a photocurrent response. In reflection, large electrooptic retardations (>60{degrees}) have now been achieved with thin PZT films ({approx equal} 0.5 {mu}m) under conditions that optimize interference effects. These results are quite attractive for device applications. Model calculations, based on the equations of reflection ellipsometry, have been used to develop a framework for understanding those results. The magnitude of the photocurrent response has also been used to determine the polarization state. However, the photocurrent always has the same sign, regardless of the sign of the polarization, which suggests the presence of a strong bias field due to at least one of the interfaces. In addition, the accumulation of space charge after a succession of measurements suppresses the photocurrent transient, which severely limits the utility of a photocurrent based readout. 7 refs., 9 figs.