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Thermal shock resistance of multilayer silicon carbide receiver tubes for 800oC molten salt concentrating solar power application

AIP Conference Proceedings

Armijo, Kenneth M.; Walker, Matthew W.; Christian, Joshua M.; Madden, Dimitri A.; Stavig, Mark E.; Oliverio, Steven; Feinroth, Herbert

CSP power tower receiver systems during rapid transient weather periods can be vulnerable to thermal shock conditions from rain that which can facilitate the onset of leaks and failures that can have catastrophic consequences. Silicon carbide (SiC) materials have attractive receiver application characteristics for being light weight, having high-strength and excellent thermal shock resistance performance which make them a particularly good fit for receiver absorber materials in CSP. In this investigation, the performance characteristics of Ceramic Tubular Products (CTP) SiC ceramic matrix composite (CMC), multilayered tubes were explored with respect to thermal shock performance for solar receiver applications in next generation CSP plants. Here, thermal shock testing was performed at the Sandia National Laboratories (SNL) Solar Furnace facility using a dynamic stage and thermal shock tube test setup. The tubes tested under incident solar heat flux of 100 W/cm2 were heated with inner tube temperatures reaching approximately 800 °C, with outer temperatures exceeding or just reaching 1000 ℃ for the multilayer and monolithic SiC tubes respectively. The tubes were then quenched with simulated rain. The tubes were then cooled and subjected to hoop stress analysis using an Instron device to assess their subsequent mechanical strength. The on-sun study experimental results indicate an average of 24.2% and 97% higher hoop strength for the CMC tubes than those composed of monolithic SiC and aluminum oxide (Al2O3) respectively.

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Encapsulant Void Breakdown Voltage Modeling & Experiments

Moore, Christopher H.; Clem, Paul G.; Biedermann, Laura B.; Miller, William K.; Stavig, Mark E.; Turner, Christian T.

For high voltage electrical devices, prevention of high voltage breakdown is critical for device function. Use of polymeric encapsulation such as epoxies is common, but these may include air bubbles or other voids of varying size. The present work aimed to model and experimentally determine the size dependence of breakdown voltage for voids in an epoxy matrix, as a step toward establishing size criteria for void screening. Effects were investigated experimentally for both one-dimensional metal/epoxy/air/epoxy/metal gap sizes from 50 μm to 10 mm, as well as spherical voids of 250 μm, 500 μm, 1 mm and 2 mm sizes. These experimental results were compared to modified Paschen curve and particle-in-cell discharge models; minimum breakdown voltages of 6 - 8.5 kV appeared to be predicted by 1D models and experiments, with minimum breakdown voltage for void sizes of 0.2 - 1 mm. In a limited set of 3D experiments on 250 μm, 500 μm, 1 mm and 2 mm voids within epoxy, the minimum breakdown voltages observed were 18.5 - 20 kV, for 500 μm void sizes. These experiments and models are aimed at providing initial size and voltage criteria for tolerable void sizes and expected discharge voltages to support design of encapsulated high voltage components.

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Interfacial toughness: dependence on surface roughness and test temperature

International Journal of Fracture

Reedy, Earl D.; Stavig, Mark E.

Interfacial toughness quantifies resistance to crack growth along an interface and in this investigation the toughness of an aluminum/epoxy interface was measured as a function of surface roughness and test temperature. The large strain response of the relatively ductile epoxy adhesive used in this study was also characterized. This epoxy adhesive exhibits intrinsic strain-softening after initial compressive yield and then deforms plastically at a roughly constant flow stress until it rapidly hardens at large compressive strains. We find that interface toughness scales as the product of the temperature dependent epoxy yield strength and a length scale that characterizes surface roughness. The proposed scaling is based upon dimensional considerations of a model problem that assumes that the characteristic length scale of both the roughness and the crack-tip yield zone is small relative to the region dominated by the linear elastic asymptotic crack-tip stress field. Furthermore, the model assumes that interfacial failure occurs only after the epoxy begins to harden at large strains. The proposed relationship is validated by our interfacial toughness measurements.

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Evaluation of High Temperature Plastics as a Ceramic Replacement

Redline, Erica M.; Dial, Brent E.; Stavig, Mark E.; Sawyer, P.S.; Miller, Lance L.

This report describes the 2015-2017 fiscal year research efforts to evaluate high temperature plastics as replacement materials for ceramics in electrical contact assemblies. The main objective of this work was to assess the feasibility of replacing existing high-price ceramic inserts with a polymeric material. Current ceramic parts are expensive due to machining costs and can suffer brittle failure. Therefore, replacing the ceramic with a more cost-effective material -- in this case a plastic -- is highly desirable. Not only are plastics easier to process, but they can also eliminate final tooling and are less brittle than ceramics. This effort used a three-phase approach: selection of appropriate materials determined by a comprehensive literature review, performance of an initial thermal stability screening, understanding of aging behavior under normal and off-normal conditions, and evaluation of performance at elevated temperatures. Two polymers were determined to meet the desired criteria: polybenzimidazole, and Vespel(r) SP-1 polyimide. Polymer derived ceramics may also be useful but will require further development of molding capabilities that were beyond the scope of this program. This page intentionally left blank.

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Assessing the Validity of the Simplified Potential Energy Clock Model for Modeling Glass-Ceramics

Jamison, Ryan D.; Grillet, Anne M.; Stavig, Mark E.; Strong, Kevin T.; Dai, Steve X.

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.

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Validation Assessment of a Glass-to-Metal Seal Finite-Element Model

Jamison, Ryan D.; Buchheit, Thomas E.; Emery, John M.; Romero, Vicente J.; Stavig, Mark E.; Newton, Clay S.; Brown, Arthur B.

Sealing glasses are ubiquitous in high pressure and temperature engineering applications, such as hermetic feed-through electrical connectors. A common connector technology are glass-to-metal seals where a metal shell compresses a sealing glass to create a hermetic seal. Though finite-element analysis has been used to understand and design glass-to-metal seals for many years, there has been little validation of these models. An indentation technique was employed to measure the residual stress on the surface of a simple glass-to-metal seal. Recently developed rate- dependent material models of both Schott 8061 and 304L VAR stainless steel have been applied to a finite-element model of the simple glass-to-metal seal. Model predictions of residual stress based on the evolution of material models are shown. These model predictions are compared to measured data. Validity of the finite- element predictions is discussed. It will be shown that the finite-element model of the glass-to-metal seal accurately predicts the mean residual stress in the glass near the glass-to-metal interface and is valid for this quantity of interest.

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Predictive Modeling of Polymer Mechanical Behavior Coupled to Chemical Change/ Technique Development for Measuring Polymer Physical Aging

Kropka, Jamie M.; Stavig, Mark E.; Arechederra, Gabriel A.; McCoy, John D.

Develop an understanding of the evolution of glassy polymer mechanical response during aging and the mechanisms associated with that evolution. That understanding will be used to develop constitutive models to assess the impact of stress evolution in encapsulants on NW designs.

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Stress Mapping in Glass-to-Metal Seals using Indentation Crack Lengths

Strong, Kevin T.; Buchheit, Thomas E.; Diebold, Thomas W.; Newton, Clay S.; Bencoe, Denise N.; Stavig, Mark E.; Jamison, Ryan D.

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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Stress Relaxation in Epoxy Thermosets via a Ferrocene-Based Amine Curing Agent

Macromolecules

Jones, Brad H.; Wheeler, David R.; Black, Hayden T.; Stavig, Mark E.; Sawyer, P.S.; Giron, Nicholas H.; Celina, Mathias C.; Lambert, Timothy N.; Alam, Todd M.

Physical stress relaxation in rubbery, thermoset polymers is limited by cross-links, which impede segmental motion and restrict relaxation to network defects, such as chain ends. In parallel, the cure shrinkage associated with thermoset polymerizations leads to the development of internal residual stress that cannot be effectively relaxed. Recent strategies have reduced or eliminated such cure stress in thermoset polymers largely by exploiting chemical relaxation processes, wherein temporary cross-links or otherwise transient bonds are incorporated into the polymer network. Here, we explore an alternative approach, wherein physical relaxation is enhanced by the incorporation of organometallic sandwich moieties into the backbone of the polymer network. A standard epoxy resin is cured with a diamine derivative of ferrocene and compared to conventional diamine curing agents. The ferrocene-based thermoset is clearly distinguished from the conventional materials by reduced cure stress with increasing cure temperature as well as unique stress relaxation behavior above its glass transition in the fully cured state. The relaxation experiments exhibit features characteristic of a physical relaxation process. Furthermore, the cure stress is observed to vanish precipitously upon deliberate introduction of network defects through an increasing imbalance of epoxy and amine functional groups. We postulate that these beneficial properties arise from fluxional motion of the cyclopentadienyl ligands on the polymer backbone.

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Residual Stress Developed During the Cure of Thermosetting Polymers: Optimizing Cure Schedule to Minimize Stress

Kropka, Jamie M.; Stavig, Mark E.; Jaramillo, Rex J.

When thermosetting polymers are used to bond or encapsulate electrical, mechanical or optical assemblies, residual stress, which often affects the performance and/or reliability of these devices, develops within the structure. The Thin-Disk-on-Cylinder structural response test is demonstrated as a powerful tool to design epoxy encapsulant cure schedules to reduce residual stress, even when all the details of the material evolution during cure are not explicitly known. The test's ability to (1) distinguish between cohesive and adhesive failure modes and (2) demonstrate methodologies to eliminate failure and reduce residual stress, make choices of cure schedules that optimize stress in the encapsulant unambiguous. For the 828/DEA/GMB material in the Thin-Disk-on-Cylinder geometry, the stress associated with cure is significant and outweighs that associated with cool down from the final cure temperature to room temperature (for measured lid strain, IεcureI > IεthermalI). The difference between the final cure temperature and the temperature at which the material gels, Tf-Tgel, was demonstrated to be a primary factor in determining the residual stress associated with cure. Increasing Tf-Tgel leads to a reduction in cure stress that is described as being associated with balancing some of the 828/DEA/GMB cure shrinkage with thermal expansion. The ability to tune residual stress associated with cure by controlling Tf-Tgel would be anticipated to translate to other thermosetting encapsulation materials, but the times and temperatures appropriate for a given material may vary widely.

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Viscoelasticity of glass-forming materials: What about inorganic sealing glasses?

Conference Proceedings of the Society for Experimental Mechanics Series

Chambers, Robert S.; Stavig, Mark E.; Tandon, Rajan T.

Glass forming materials like polymers exhibit a variety of complex, nonlinear, time-dependent relaxations in volume, enthalpy and stress, all of which affect material performance and aging. Durable product designs rely on the capability to predict accurately how these materials will respond to mechanical loading and temperature regimes over prolonged exposures to operating environments. This cannot be achieved by developing a constitutive framework to fit only one or two types of experiments. Rather, it requires a constitutive formalism that is quantitatively predictive to engineering accuracy for the broad range of observed relaxation behaviors. Moreover, all engineering analyses must be performed from a single set of material model parameters. The rigorous nonlinear viscoelastic Potential Energy Clock (PEC) model and its engineering phenomenological equivalent, the Simplified Potential Energy Clock (SPEC) model, were developed to fulfill such roles and have been applied successfully to thermoplastics and filled and unfilled thermosets. Recent work has provided an opportunity to assess the performance of the SPEC model in predicting the viscoelastic behavior of an inorganic sealing glass. This presentation will overview the history of PEC and SPEC and describe the material characterization, model calibration and validation associated with the high Tg (~460 °C) sealing glass.

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Characterization and calibration of a viscoelastic simplified potential energy clock model for inorganic glasses

Journal of Non-Crystalline Solids

Chambers, Robert S.; Tandon, Rajan T.; Stavig, Mark E.

To analyze the stresses and strains generated during the solidification of glass-forming materials, stress and volume relaxation must be predicted accurately. Although the modeling attributes required to depict physical aging in organic glassy thermosets strongly resemble the structural relaxation in inorganic glasses, the historical modeling approaches have been distinctly different. To determine whether a common constitutive framework can be applied to both classes of materials, the nonlinear viscoelastic simplified potential energy clock (SPEC) model, developed originally for glassy thermosets, was calibrated for the Schott 8061 inorganic glass and used to analyze a number of tests. A practical methodology for material characterization and model calibration is discussed, and the structural relaxation mechanism is interpreted in the context of SPEC model constitutive equations. SPEC predictions compared to inorganic glass data collected from thermal strain measurements and creep tests demonstrate the ability to achieve engineering accuracy and make the SPEC model feasible for engineering applications involving a much broader class of glassy materials.

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Cracking in a flame-sprayed epoxy

Materials Performance and Characterization

Ford, K.R.; Stavig, Mark E.; Chambers, Robert S.

The objective of this work was to understand the cracking of aluminum flame spray on an epoxy thermoset. In the experiments presented here, epoxy cylinders were uniformly coated with flame spray. The cylinders were put into a state of tensile stress by taking them to elevated temperatures and similarly put into a state of compression by taking them down to cold temperatures. Surface cracks on the outside of the cylinders were photographed and compared. The cylinders were cross-sectioned at room temperature to study how the aluminum surface cracks propagate into the epoxy. It was shown that thicker aluminum generates observable surface cracks at a lower temperature than a thinner coating does. The surface cracks cannot be seen at room temperature. However, some of the coating cracks propagate into the substrate and can be seen at room temperature when the cylinder is crosssectioned. The substrate cracks tend to be deeper with a larger coating thickness. Similarly, cracks are deeper when the substrate with a given thickness is taken to higher temperature. Supplementary examples that contain the addition of a hard inclusion (copper strip) between the aluminum and epoxy substrate at elevated temperatures were discussed, as well as delamination of the aluminum film at cold temperature.

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A Process and Environment Aware Sierra/SolidMechanics Cohesive Zone Modeling Capability for Polymer/Solid Interfaces

Reedy, Earl D.; Hughes, Lindsey G.; Kropka, Jamie M.; Stavig, Mark E.; Stevens, Mark J.; Chambers, Robert S.

The performance and reliability of many mechanical and electrical components depend on the integrity of po lymer - to - solid interfaces . Such interfaces are found in adhesively bonded joints, encapsulated or underfilled electronic modules, protective coatings, and laminates. The work described herein was aimed at improving Sandia's finite element - based capability to predict interfacial crack growth by 1) using a high fidelity nonlinear viscoelastic material model for the adhesive in fracture simulations, and 2) developing and implementing a novel cohesive zone fracture model that generates a mode - mixity dependent toughness as a natural consequence of its formulation (i.e., generates the observed increase in interfacial toughness wi th increasing crack - tip interfacial shear). Furthermore, molecular dynamics simulations were used to study fundamental material/interfa cial physics so as to develop a fuller understanding of the connection between molecular structure and failure . Also reported are test results that quantify how joint strength and interfacial toughness vary with temperature.

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Multilayer Coextrusion of Polymer Composites to Develop Organic Capacitors

International Polymer Processing

Mondy, L.A.; Bieg, Lothar F.; Spangler, Scott W.; Stavig, Mark E.; Schroeder, John L.; Rao, Rekha R.; DiAntonio, Christopher D.

Multilayer coextrusion is applied to produce a tape containing layers of alternating electrical properties to demonstrate the potential for using coextrusion to manufacture capacitors. To obtain the desired properties, we develop two filled polymer systems, one for conductive layers and one for dielectric layers. We describe numerical models used to help determine the material and processing parameters that impact processing and layer stability. These models help quantify the critical ratios of densities and viscosities of the two layers to maintain stable layers, as well as the effect of increasing the flow rate of one of the two materials. The conducting polymer is based on polystyrene filled with a blend of low-melting-point eutectic metal and nickel particulate filler, as described by Mrozek et al. (2010). The appropriate concentrations of fillers are determined by balancing measured conductivity with processability in a twin screw extruder. Based on results of the numerical models and estimates of the viscosity of emulsions and suspensions, a dielectric layer composed of polystyrene filled with barium titanate is formulated. Despite the fact that the density of the dielectric filler is less than the metallic filler of the conductive phase, as well as rheological measurements that later showed that the dielectric formulation is not an ideal match to the viscosity of the conductive material, the two materials can be successfully coextruded if the flow rates of the two materials are not identical. A measurable capacitance of the layered structure is obtained.

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Residual internal stress optimization for EPON 828/DEA thermoset resin using fiber Bragg grating sensors

Proceedings of SPIE - The International Society for Optical Engineering

Rohr, Garth R.; Rasberry, Roger D.; Kaczmarowski, Amy K.; Stavig, Mark E.; Gibson, Cory S.; Udd, Eric; Roach, R.A.; Nation, Brendan

Internal residual stresses and overall mechanical properties of thermoset resins are largely dictated by the curing process. It is well understood that fiber Bragg grating (FBG) sensors can be used to evaluate temperature and cure induced strain while embedded during curing. Herein, is an extension of this work whereby we use FBGs as a probe for minimizing the internal residual stress of an unfilled and filled Epon 828/DEA resin. Variables affecting stress including cure cycle, mold (release), and adhesion promoting additives will be discussed and stress measurements from a strain gauge pop-off test will be used as comparison. Sandia National Laboratories is a multi-program laboratory managed and operated by Sandia Corporation, a wholly owned subsidiary of Lockheed Martin Corporation, for the U.S. Department of Energy's National Nuclear Security Administration under contract DE-AC04-94AL85000.

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Proposed Testing to Assess the Accuracy of Glass-To-Metal Seal Stress Analyses

Chambers, Robert S.; Emery, John M.; Tandon, Rajan T.; Antoun, Bonnie R.; Stavig, Mark E.; Newton, Clay S.; Gibson, Cory S.; Bencoe, Denise N.

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.

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Characterization & Modeling of Materials in Glass-To-Metal Seals: Part I

Chambers, Robert S.; Emery, John M.; Tandon, Rajan T.; Antoun, Bonnie R.; Stavig, Mark E.; Newton, Clay S.

To support higher fidelity modeling of residual stresses in glass-to-metal (GTM) seals and to demonstrate the accuracy of finite element analysis predictions, characterization and validation data have been collected for Sandia’s commonly used compression seal materials. The temperature dependence of the storage moduli, the shear relaxation modulus master curve and structural relaxation of the Schott 8061 glass were measured and stress-strain curves were generated for SS304L VAR in small strain regimes typical of GTM seal applications spanning temperatures from 20 to 500 C. Material models were calibrated and finite element predictions are being compared to measured data to assess the accuracy of predictions.

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Multilayer co-extrusion technique for developing high energy density organic devices

Mondy, L.A.; Rao, Rekha R.; Bieg, Lothar F.; Schneider, Duane A.; Stavig, Mark E.; Schroeder, John L.; Winter, Michael R.

The purpose of this project is to develop multi-layered co-extrusion (MLCE) capabilities at Sandia National Laboratories to produce multifunctional polymeric structures. Multi-layered structures containing layers of alternating electrical, mechanical, optical, or structural properties can be applied to a variety of potential applications including energy storage, optics, sensors, mechanical, and barrier applications relevant to the internal and external community. To obtain the desired properties, fillers must be added to the polymer materials that are much smaller than the end layer thickness. We developed two filled polymer systems, one for conductive layers and one for dielectric layers and demonstrated the potential for using MLCE to manufacture capacitors. We also developed numerical models to help determine the material and processing parameters that impact processing and layer stability.

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Materials-based process tolerances for neutron generator encapsulation

Adolf, Douglas B.; Stavig, Mark E.; Berry, Ryan S.

Variations in the neutron generator encapsulation process can affect functionality. However, instead of following the historical path in which the effects of process variations are assessed directly through functional tests, this study examines how material properties key to generator functionality correlate with process variations. The results of this type of investigation will be applicable to all generators and can provide insight on the most profitable paths to process and material improvements. Surprisingly, the results at this point imply that the process is quite robust, and many of the current process tolerances are perhaps overly restrictive. The good news lies in the fact that our current process ensures reproducible material properties. The bad new lies in the fact that it would be difficult to solve functional problems by changes in the process.

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Thermal Aging of the Polyurethane Foam for the H1616 Shipping Container

Stavig, Mark E.

A polyurethane foam used in the H1616 shipping container provides impact energy absorption and fire protection in hypothetical accident conditions. This study was undertaken to determine the estimated lifetime of the foam as a function of temperature. The foams were aged at temperatures ranging from 65°C to 95°C for periods of time ranging from 6 months to 6 years. Both destructive and nondestructive Dynamic Mechanical Analyses (DMA) were used to evaluate the performance of the foams as a function of time and temperature. In addition, color changes and weight loss were recorded. Three properties of the foam show a definite trend with aging time: weight loss, nondestructive G’ (measured at 100°C), and glassy G’. A time temperature superposition analysis shows a reasonable trend with temperature for both the weight loss and glassy G’. The acceleration factors for weight loss and glassy G’ did not correlate with each other, however. A prediction of the behavior of G’ as a function of aging time at 25°C was derived from an extrapolated value of the acceleration factor. In addition to providing a quantitative estimation of the aging process, the curve also provides a description of the qualitative features of the aging process. First, the aging process appears to proceed smoothly as a function of aging time. There are no discontinuities or sharp breaks in the glassy G’ as a function of aging time at any of the temperatures. Second, the rate of change of the glassy G’ appears to decrease as the aging time increases.

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Autonomic Healing of Epoxy Using Micro-Encapsulated Dicyclopentadiene

Giunta, Rachel K.; Thoma, Steven T.; Giunta, Rachel K.; Stavig, Mark E.; Emerson, John A.; Morales, Alfredo M.

The autonomic healing ability of an epoxy adhesive containing micro-encapsulated dicyclopentadiene (DCPD) was evaluated. The epoxy resin used was Epon 828 cured with either Versamid 140 or diethylenetriamine (DETA). Variables included total weight percent of microcapsules (MCs) and catalyst, as well as the catalyst to DCPD ratio. The degree of healing was determined by the fracture toughness before and after ''healing'' using double-cantilever beam analysis. It was found that the degree of self-healing was most directly related to the contact area (i.e. crack width) during healing. Temperature also played a significant role. Observed differences between the results of this study and those in literature are discussed.

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84 Results
84 Results