Publications

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Polymeric materials are commonplace in the natural gas infrastructure as distribution pipes, coatings, seals, and gaskets. Under the auspices of the U.S. Department of Energy HyBlend program, one of the means to reduce greenhouse gas emissions is with replacing natural gas, either partially or completely, with hydrogen. This approach makes it imperative that we conduct near-term and long-term materials compatibility research in these relevant environments. Insights into the effects of hydrogen and hydrogen gas blends on polymer integrity can be gained through both ex-situ and in-situ analytical methods. Our work represented here highlights a study of the behavior of pipeline polyethylene (PE) materials, including HDPE (Dow 2490 and GDB50) and MDPE (Ineos and legacy Dupont Aldyl A), when exposed to hydrogen by means of in-situ X-ray scattering and ex-situ Raman spectroscopy techniques. These methods complement each other in analyzing polymer microstructure. Data collected revealed that the aforementioned polymers did not show significant changes in crystallinity or morphology under the exposure conditions tested. These studies help establish techniques to study real-time effects of hydrogen gas on polymer structure and chemistry, which is directly related to pipeline mechanical strength and longevity of service.

Polymers used in hydrogen transportation, production, storage, and dispensing operations of the hydrogen infrastructure are subject to demanding performance temperatures (-60°C to +140°C) and pressures (0.9 MPa to 87 MPa), under static and cycling conditions of hydrogen exposure. Cycling exposures which include pressurization and depressurization stages can particularly affect properties of these soft materials. Other factors such temperature of exposure in hydrogen environments can also play an influential role on polymer degradation behaviors. In this work, we evaluated the influence of varying rates of depressurization (1, 10, 20, 40 MPa/min and uncontrolled) with model elastomer compounds exposed to high-pressure hydrogen cycling (17 MPa to 87 MPa) at ambient temperature. The goal was to develop an understanding of factors that affect rapid gas decompression in elastomers, which is a phenomenon common in hydrogen fueling operations. Cycling was followed by ex-situ characterization for changes in properties. Dynamic Mechanical Thermal Analysis (DMTA), density, compression set, Attenuated Total Reflectance-FTIR (ATR-FTIR), nanoindentation, and X-ray computer tomography were characterization techniques used to compare polymers before and after cycling. Polymer degradation in the form of internal damage was found to increase with rate of depressurization. EPDM showed the most dependence on rates of depressurization, compared to FKM and HNBR formulations. Additionally, filled, and unfilled model compounds of EPDM, FKM, HNBR, and NBR were tested in high-pressure (17 MPa to 87 MPa) and low-pressure (10 MPa to 31 MPa) cycling conditions at -40°C and +85°C. These experiments were performed at a fixed depressurization rate. The goal of these experiments was to better understand temperature effects under pressure cycling conditions for elastomeric polymer seals. Filled formulations of EPDM, HNBR, and NBR exhibited increased compression set and decreased storage modulus under cold cycling exposures to a greater extent than when cycled at ambient. For filled polymers cycled at low pressures at 85°C and -40°C, FKM showed the most resistance to blistering. HNBR and NBR showed heavy swelling and blistering under both these conditions. Micro CT imaging of one of the polymers (EPDM) subjected to high-pressure cycling at 85°C showed great damage in the form of cracks in the center of the sample. Filled formulations exhibited decreased compression set and storage modulus under hot cycling exposures to a greater extent than with cold and ambient cycling. The findings from these studies will help build a strong understanding of polymer behaviors in cycling hydrogen under rapid gas decompression and thermal conditions encountered in fueling operations and storage. Proper material selection for appropriate use-conditions within components is also enabled.

Additive manufacturing (AM) is a relatively new technological advancement that allows for rapid prototyping, development of intricate shapes, and reduction in manufacturing time. The materials of interest for this project are Ultem 1010, ABS M30, FDM Nylon 12, PC, and PPSF. However, little is known regarding the aging behavior of these AM materials. The limited aging study outlined herein was designed to compare the chemical, physical, and mechanical properties of AM parts as they experience accelerated aging at 70 °C for a total of 24 weeks. In general, ABS M30 stood out as it appeared to undergo chemical and physical changes leading to increase in density and an overall more brittle material, making this commonly used material not attractive for long-term use.

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Polymers such as PTFE (polytetrafluorethylene or Teflon), EPDM (ethylene propylene diene monomer) rubber, FKM fluoroelastomer (Viton), Nylon 11, Nitrile butadiene (NBR) rubber, hydrogenated nitrile rubber (HNBR) and perfluoroelastomers (FF_202) are commonly employed in super critical CO₂ (sCO2) energy conversion systems. O-rings and gaskets made from these polymers face stringent performance conditions such as elevated temperatures, high pressures, pollutants, and corrosive humid environments. In FY 2019, we conducted experiments at high temperatures (100°C and 120°C) under isobaric conditions (20 MPa). Findings showed that elevated temperatures accelerated degradation of polymers in sCO2, and that certain polymer microstructures are more susceptible to degradation over others. In FY 2020, the focus was to understand the effect of sCO2 on polymers at low (10 MPa) and high pressures (40 MPa) under isothermal conditions (100°C). It was clear that the same selectivity was observed in these experiments wherein certain polymeric functionalities showed more propensity to failure over others. Fast diffusion, supported by higher pressures and long exposure times (1000 hours) at the test temperature, caused increased damage in sCO2 environments to even the most robust polymers. We also looked at polymers under compression in sCO2 at 100°C and 20 MPa pressure to imitate actual sealing performance required of these materials in sCO2 systems. Compression worsened the physical damage that resulted from chemical attack of the polymers under these test conditions. In FY 2021, the effect of cycling temperature (from 50°C to 150°C to 50°C) for polymers under a steady sCO2 pressure of 20 MPa was studied. The aim was to understand the influence of cycling temperatures of sCO2 for typical polymers under isobaric (20 MPa) conditions. Thermoplastic polymers (Nylon, and PTFE) and elastomers (EPDM, Viton, Buna N, Neoprene, FF202, and HNBR) were subjected to 20 MPa sCO2 pressure for 50 cycles and 100 cycles in separate experiments. Samples were extracted for ex-situ characterization at 50 cycles and upon the completion of 100 cycles. Each cycle constituted of 175 minutes of cycling from 50°C to 150°C. The polymer samples were examined for physical and chemical changes by Dynamic Mechanical and Thermal Analysis (DMTA), Fourier Transform Infrared (FTIR) spectroscopy, and compression set. Density and mass changes immediately after removal from test were measured for degree of swell comparisons. Optical microscopy techniques and micro computer tomography (micro CT) images were collected on select specimens. Evaluations conducted showed that exposures to super-critical CO2 environments resulted in combinations of physical and/or chemical changes. For each polymer, the dominance of cycling temperatures under sCO2 pressures, were evaluated. Attempts were made to qualitatively link the permanent sCO2 effects to polymer micro- structure, free volume, backbone substitutions, presence of polar groups, and degree of crystallinity differences. This study has established that soft polymeric materials are conducive to failure in sCO2 through mechanisms of failure that are dependent on polymer microstructure and chemistry. Polar pendant groups, large atom substitutions on the backbone are some of the factors that are influential structural factors.

Conathane EN-7 (referred to as EN-7) has been used for decades to pot electrical connectors, providing mechanical support for solder joints in cables. Unfortunately, the EN-7 formulation contains a suspect carcinogen and chemical sensitizer, toluene diisocyanate (TDI). Because of this, various groups have been formulating replacement materials, but all have come up short in final properties or in processing. We propose Arathane 5753 HVB as a replacement for EN-7. The properties compare very well with EN-7 and the processing has both advantages and disadvantages over EN-7 as discussed in detail below.

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A copolymer of maleic anhydride and styrene is functionalized with Diels–Alder (DA) capable pendant groups to enable the study of this material with different crosslink densities. This constituent is synthesized using commercially available starting materials and relatively simple and uncomplicated chemistries which open the possibility for its use in large-scale applications. The 10%, 25%, 50%, and 100% DA nominal crosslinking based on available pendant furan groups on the polymeric component is investigated. The reaction kinetics are monitored using infrared spectroscopy and rheology. Based on the rheological results, carbon nanotube (CNT) incorporation into the DA matrix is explored in order to determine its effects on the complex modulus of the material. This work is meant as a proof of concept for this DA material with the possibility of its incorporation into other commonly used bulk materials and/or adhesives to allow for an easily reversible product formulation.

This work is to characterize the mechanical properties of the selected composites along both on- and off- fiber axes at the ambient loading condition (+25°C), as well as at the cold (-54°C), and high temperatures (+71°C). A series of tensile experiments were conducted at different material orientations of 0°, 22.5°, 45°, 67.5°, 90° to measure the ultimate strength and strain $σ_{f}, ϵ_{f}$, and material engineering constants, including Young's modulus Ε and Poisson's ratio ν. The composite materials in this study were one carbon composite carbon (AS4C/UF3662) and one E-galss (E-glass/UF3662) composite. They both had the same resin of UF 3362, but with different fibers of carbon AS4C and E-glass. The mechanical loading in this study was limited to the quasi-static loading of 2 mm/min (1.3x10^{^(-3)} in/s), which was equivalent to 5x10^(-4) strain rate. These experimental data of the mechanical properties of composites at different loading directions and temperatures were summarized and compared. These experimental results provided database for design engineers to optimize structures through ply angle modifications and for analysts to better predict the component performance.

This report describes the mechanical characterization of six types of woven composites that Sandia National Laboratories are interested in. These six composites have various combinations of two types of fibers (Carbon-IM7 and Glass-S2) and three types of resins (UF-3362, TC275-1, TC350-1). In this work, two sets of experiments were conducted: quasi-static loading with displacement rate of 2 mm/min (1.3x10^{^(-3)} in/s) and high rate loading with displacement of 5.08 m/s (200 in/s). Quasi-static experiments were performed at three loading orientations of 0°, 45°, 90° for all the six composites to fully characterize their mechanical properties. The elastic properties Young's modulus and Poisson's ratio, as well as ultimate stress and strain were obtained from the quasi-static experiments. The high strain rate experiments were performed only on glass fiber composites along 0° angle of loading. The high rate experiments were mainly to study how the strain rate affects the ultimate stress of the glass-fiber composites with different resins.

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An investigation of polyurethane foam filled with known flame retardant fillers including hydroxides, melamine, phosphate-containing compounds, and melamine phosphates was carried out to produce a low-cost material with high flame retardant efficiency. The impact of flame retardant fillers on the physical properties such a s composite foam density, glass transition temperature, storage modulus, and thermal expansion of composite foams was investigated with the goal of synthesizing a robust rigid foam with excellent flame retardant properties.

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