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Constitutive Model Development for Aging Polymer Encapsulants (ASC P&EM FY2021 L2 Milestone 7836)

Cundiff, Kenneth N.; Long, Kevin N.; Kropka, Jamie M.; Carroll, Shianne C.; Groves, Catherine G.

This SAND report fulfills the completion requirements for the ASC Physics and Engineering Modeling Level 2 Milestone 7836 during Fiscal Year 2021. The Sandia Simplified potential energy clock (SPEC) non-linear viscoelastic constitutive model was developed to predict a whole host of polymer glass physical behaviors in order to provide a tool to assess the effects of stress on these materials over their lifecycle. Polymer glasses are used extensively in applications such as electronics packaging, where encapsulants and adhesives can be critical to device performance. In this work, the focus is on assessing the performance of the model in predicting material evolution associated with long-term physical aging, an area that the model has not been fully vetted in. These predictions are key to utilizing models to help demonstrate electronics packaging component reliability over decades long service lives, a task that is very costly and time consuming to execute experimentally. The initiating hypothesis for the work was that a model calibration process can be defined that enables confidence in physical aging predictions under ND relevant environments and timescales without sacrificing other predictive capabilities. To test the hypothesis, an extensive suite of calibration and aging data was assembled from a combination of prior work and collaborating projects (Aging and Lifetimes as well as the DoD Joint Munitions Program) for two mission relevant epoxy encapsulants, 828DGEBA/DEA and 828DGEBA/T403. Multiple model calibration processes were developed and evaluated against the entire set of data for each material. A qualitative assessment of each calibration's ability to predict the wide range of aging responses was key to ranking the calibrations against each other. During this evaluation, predictions that were identified as non-physical, i.e., demonstrated something that was qualitatively different than known material behavior, were heavily weighted against the calibration performance. Thus, unphysical predictions for one aspect of aging response could generate a lower overall rating for a calibration process even if that process generated better quantitative predictions for another aspect of aging response. This insurance that all predictions are qualitatively correct is important to the overall aim of utilizing the model to predict residual stress evolution, which will depend on the interplay amongst the different material aging responses. The DSC-focused calibration procedure generated the best all-around aging predictions for both materials, demonstrating material models that can qualitatively predict the whole host of different physical aging responses that have been measured. This step forward in predictive capability comes from an unanticipated source, utilization of calorimetry measurements to specify model parameters. The DSC-focused calibration technique performed better than compression-focused techniques that more heavily weigh measurements more closely related to the structural responses to be predicted. Indeed, the DSC-focused calibration procedure was only possible due to recent incorporation of the enthalpy and heat capacity features into SPEC that was newly verified during this L2 milestone. Fundamentally similar aspects of the two material model calibrations as well as parametric studies to assess sensitives of the aging predictions are discussed within the report. A perspective on the next steps to the overall goal of residual stress evolution predictions under stockpile conditions closes the report.

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Limited Characterization of Wind Turbine Adhesives [EPIKOTE Resin MGS BPR 135G3/EPIKURE Curing Agent MGS RIMH 134 (H134i) and MGS BP20/EPIKURE Curing Agent MGS BPH 20 (rework adhesive)] and Root Insert Exterior Surface

Kropka, Jamie M.; Baca, Ana B.; Brumbach, Michael T.; Chow, Rebecca C.

The National Rotor Testbed (NRT) is a wind turbine blade research program in the Sandia National Laboratories (SNL) Wind Department that has developed a new blade design. Each blade includes bonded-in, threaded metal root inserts that enable the blades to be bolted onto the wind turbine hub. Prior to installing the flight blades on the turbine, root insert strength verification tests exhibited a subset of failures below the design load on one (NRT-02) of four blades. As part of a root cause analysis for the failures, this work analyzes "scraps" of the epoxy adhesive used to bond the metal inserts into the blade and uses surface topography and x-ray fluorescence (XRF) measurements to characterize the exterior surface of the root insert. Samples were taken from inserts that exhibited both high and low loads at failure, as well as some "control inserts" to monitor the state of the surface throughout the manufacturing process. Differences in the calorimetric response of the adhesive from the separate root inserts are apparent but none of them appear to relate to the pull load required to dislodge the inserts. Two takeaways of note include: In the way that the adhesive is processed, it does not reach full cure; and, Something occurred to sample#10 such that the fully-cured adhesive has a significantly lower Tg.

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Predictions of Yield Strength Evolution Due to Physical Aging of 828 DGEBA/DEA using the Simplified Potential Energy Clock Model

Tenney, Craig M.; Long, Kevin N.; Kropka, Jamie M.

The capability of the Simplified Potential Energy Clock Model (SPEC) to represent the uniaxial compression yield strength evolution under isothermal aging conditions is evaluated for a widely used epoxy thermoset encapsulation material, 828 DGEBA/DEA. A baseline model calibration is used. We note that this calibration did not consider yield strength behavior close to the glass transition temperature (Tg), but in this work, the model is exercised in this temperature range to evaluate the ability to predict changes in material response with aging as equilibrium is approached. Some model alterations were needed to remove negative Prony weights in the thermal and bulk relaxation function (f1), which is chiefly responsible for aging in this analysis, but otherwise, the model was not altered. Model predictions of yield stress evolution are quantitatively different compared with experiments, but the rate of change of yield stress with respect to aging time is in reasonable agreement with respect to experiments for the first 1000 hours of aging. After this aging time, the measured yield stress stops evolving, but the model continues to evolve for several more decades in time. Parametric studies and model alterations are considered to investigate how yield strength evolution predictions are affected by modeling choices. It is clear that the baseline calibration must be re-examined in order to represent the aging data quantitatively.

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Reactions of DGEBA epoxy cured with diethanolamine: Isoconversional kinetics and implications to network structure

Thermochimica Acta

Kropka, Jamie M.; McCoy, John D.; Ancipink, Windy B.; Maestas, Salomon R.; Draelos, Lara R.; Devries, David B.

The curing of diglycidyl ether of bisphenol A (DGEBA) epoxy with diethanolamine (DEA) is studied. DEA has three reactive groups, a secondary amine hydrogen and two hydroxyls. The secondary amine reacts rapidly, forming an adduct containing tertiary amines, epoxides and hydroxyls. The epoxides and hydroxyls then react in the presence of the amines to crosslink and vitrify the epoxy in the “gelation” reaction. The gelation reaction, the subject of this study, is not simple. The reaction exhibits unusual dependencies on both temperature and degree of cure. Previously, the general mechanisms of this curing process were explored by a number of us. In the present paper, both differential scanning calorimetry (DSC) and isothermal microcalorimetry (IMC) are used to determine a number of characteristic times associated with the reaction. The characteristic times show that the reaction rate has different functional forms at different temperatures and extents of reaction. This results from the reaction rate not depending solely upon the temperature and over-all extent-of-reaction. The concentration of a number of auxiliary reactive species that are generated in the course of the reaction (as well as their mobility and steric hindrance) appear to be key factors in defining the reaction kinetics. The dependence of the final network structure on cure schedule for this type of tertiary amine activated reaction is then discussed in the context of the literature. Finally, in the Supplementary Material, Kamal-like functions are fit to the isothermal reaction kinetics, with the reader cautioned in applying the functions to non-isothermal cures.

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Results 1–25 of 120
Results 1–25 of 120