Publications

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Predicting the residual stress which develops during fabrication of a glass-to-metal compression seal requires material models that can accurately predict the effects of processing on the sealing glass. Validation of the predictions requires measurements on representative test geometries to accurately capture the interaction between the seal materials during a processing cycle required to form the seal, which consists of a temperature excursion through the glass transition temperature of the sealing glass. To this end, a concentric seal test geometry, referred to as a short cylinder seal, consisting of a stainless steel shell enveloping a commercial sealing glass disk has been designed, fabricated, and characterized as a model validation test geometry. To obtain data to test/validate finite element (FE) stress model predictions of this geometry, spatially-resolved residual stress was calculated from the measured lengths of the cracks emanating from radially positioned Vickers indents in the glass disk portion of the seal. The indentation crack length method is described, and the spatially-resolved residual stress determined experimentally are compared to FE stress predictions made using a nonlinear viscoelastic material model adapted to inorganic sealing glasses and an updated rate dependent material model for 304L stainless steel. The measurement method is a first to achieve a degree of success for measuring spatially resolved residual stress in a glass-bearing geometry and a favorable comparison between measurements and simulation was observed.

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The material characterization tests conducted on 304L VAR stainless steel and Schott 8061 glass have provided higher fidelity data for calibration of material models used in Glass - T o - Metal (GTM) seal analyses. Specifically, a Thermo - Multi - Linear Elastic Plastic ( thermo - MLEP) material model has be en defined for S S304L and the Simplified Potential Energy Clock nonlinear visc oelastic model has been calibrated for the S8061 glass. To assess the accuracy of finite element stress analyses of GTM seals, a suite of tests are proposed to provide data for comparison to mo del predictions.

A tape casting procedure for fabricating ceramic magnesium oxide tapes has been developed as a method to produce flat sheets of sintered MgO that are thin and porous. Thickness of single layer tapes is in the range of 200-400 {micro}m with corresponding surface roughness values in the range of 10-20 {micro}m as measured by laser profilometry. Development of the tape casting technique required optimization of pretreatment for the starting magnesium oxide (MgO) powder as well as a detailed study of the casting slurry preparation and subsequent heat treatments for sintering and final tape flattening. Milling time of the ceramic powder, plasticizer, and binder mixture was identified as a primary factor affecting surface morphology of the tapes. In general, longer milling times resulted in green tapes with a noticeably smoother surface. This work demonstrates that meticulous control of the entire tape casting operation is necessary to obtain high-quality MgO tapes.

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The ability to predict and control organic decomposition of a material under arbitrary thermal treatments is one of the main objectives of thermogravimetric studies. The development of this ability provides significant potential to ensure reliability and reproducibility for a given processing method and can be used in planning optimized thermal treatment strategies. Based on this report, the master sintering curve theory has been successfully extended to similar kinetically controlled phenomena. The theory has been applied to organic decomposition reaction kinetics to develop a master organic decomposition curve. The fundamental kinetics are assumed to be governed by an Arrhenius-type reaction rate, making master sintering and decomposition curves analogous to one another. The formulation and construction of a master decomposition curve are given in this paper. Simultaneous thermogravimetric and differential thermal analysis of a low-temperature co-fire glass/ceramic dielectric tape (Dupont 951 Green Tape™) is analyzed and used to demonstrate this new concept. The results reveal two independent organic decomposition reactions, the first occurring at ≈ 245° C and the second at ≈ 365°C. The analysis is used to produce a master decomposition curve and to calculate the activation energy for these reactions, at 86±6 and 142 ± 4 kJ/mol, respectively. In addition, the weight loss of product and the rate of decomposition can be predicted under varying thermal paths (time-temperature trajectories) following a minimal set of preliminary experiments. © 2005 The American Ceramic Society.

Low temperature co-fire ceramic (LTCC) materials technology offers a cost-effective and versatile approach to design and manufacture high performance and reliable advanced microelectronic packages (e.g., for wireless communications). A critical issue in manufacturing LTCC microelectronics is the need to precisely and reproducibly control shrinkage on sintering. Master Sintering Curve (MSC) theory has been evaluated and successfully applied as a tool to predict and control LTCC sintering. Dilatometer sintering experiments were designed and completed to characterize the anisotropic sintering behavior of green LTCC materials formed by tape casting. The resultant master sintering curve generated from these data provides a means to predict density as a function of sintering time and temperature. The application of MSC theory to DuPont 951 Green Tape™ will be demonstrated.

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Solid state {sup 31}P/{sup 27}Al and {sup 31}P/{sup 23}Na MAS NMR dipolar dephasing experiments have been used to investigate the spatial distribution of aluminum and sodium cations with respect to the phosphate backbone for a series of sodium aluminophosphate glasses, xAl{sub 2}O{sub 3}{center_dot}50Na{sub 2}O{center_dot}(50{minus}x)P{sub 2}O{sub 5} (0{le} x {le} 17.5). From the {sup 31}P/{sup 27}Al and {sup 31}P/{sup 23}Na connectivity data gathered, information about the medium range order in these glasses is obtained. The expanded connectivity data allows for better identification and interpretation of the new resonances observed in the {sup 31}P MAS NMR spectra with the addition of alumina. The results of the dipolar dephasing experiments show that the sodium-phosphate distribution remains relatively unchanged for the glass series, and that the addition of aluminum occurs primarily through the depolymerization of the phosphate tetrahedral backbone.

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