We demonstrate the ability to measure R-curves of brittle materials using a method adapted from Theo Fett et al. The method is validated with a NIST standard reference material and demonstrated using Si3N4 of two different microstructures; glass-ceramic, and PZT. As expected, each material's R-curve is seen to be slightly different with glass-ceramics showing the most pronounced R-curve effects. Plans for future applications and experimental efforts are discussed.
Glass-ceramic seals may be the future of hermetic connectors at Sandia National Laboratories. They have been shown capable of surviving higher temperatures and pressures than amorphous glass seals. More advanced finite-element material models are required to enable model-based design and provide evidence that the hermetic connectors can meet design requirements. Glass-ceramics are composite materials with both crystalline and amorphous phases. The latter gives rise to (non-linearly) viscoelastic behavior. Given their complex microstructures, glass-ceramics may be thermorheologically complex, a behavior outside the scope of currently implemented constitutive models at Sandia. However, it was desired to assess if the Simplified Potential Energy Clock (SPEC) model is capable of capturing the material response. Available data for SL 16.8 glass-ceramic was used to calibrate the SPEC model. Model accuracy was assessed by comparing model predictions with shear moduli temperature dependence and high temperature 3-point bend creep data. It is shown that the model can predict the temperature dependence of the shear moduli and 3- point bend creep data. Analysis of the results is presented. Suggestions for future experiments and model development are presented. Though further calibration is likely necessary, SPEC has been shown capable of modeling glass-ceramic behavior in the glass transition region but requires further analysis below the transition region.
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.