Accelerated Testing of the Mechanical and Thermal Integrity of Polymeric Materials
Long time mechanical and thermal stability of polymeric materials predicted from accelerated testing at increased temperature-time relations
THERMAL INSTABILITY↗
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Accelerated Testing of the Mechanical and Thermal Integrity of Polymeric Materials
Long time mechanical and thermal stability of polymeric materials predicted from accelerated testing at increased temperature-time relations
Hamaker, F. M.↗
The Qualification of Sealability and Creep Relaxation of Additively Manufactured Zytel Gaskets for PEM Fuel Cells
The purpose of this thesis is to study the feasibility of low-cost additive manufacturing of gaskets for proton exchange membrane fuel cells exposed to extreme temperature conditions ranging from -55°C to 100°C. With the growing popularity and decreasing costs of additive manufacturing technologies, specifically Material Extrusion (ME), research is being conducted to determine the feasibility of ME components. Thermally cycled PEMFCs may exhibit accelerated gasket deterioration, therefore, the mechanical stability of material extruded gaskets following a harsh thermal cycle must be assessed. The feasibility of the material extruded gaskets will be proven by manufacturing optimization and mechanical testing. The target material for this study is Zytel by DuPont Chemical. The mechanical stability will be assessed via sealability and creep relaxation testing according to ASTM F37B and ASTM F38B respectively. Because the capabilities to conduct sealability testing at temperature were not available, each specimen was thermally soaked and allowed to return to room temperature prior to testing. As a result of sealability experiments, the 100°C-soaked specimens resulted in lower leak rates with a higher precision when compared to specimens soaked at -55°C and 22°C at across all compressive loads. It was observed from results from creep relaxation testing that there is thermal contraction and expansion occurring at 55°C and 100°C respectively, which can be observed by the resultant graphs. The recoverability of thermally cycled specimens are better than those that just experienced a high temperature hold. After the seven-day thermal cycle, the samples stabilized and maintained their structure.
Lazarin, Robert↗
Protonation Stimulates the Layered to Rock Salt Phase Transition of Ni‐Rich Sodium Cathodes
Abstract Protonation of oxide cathodes triggers surface transition metal dissolution and accelerates the performance degradation of Li‐ion batteries. While strategies are developed to improve cathode material surface stability, little is known about the effects of protonation on bulk phase transitions in these cathode materials or their sodium‐ion battery counterparts. Here, using NaNiO 2 in electrolytes with different proton‐generating levels as model systems, a holistic picture of the effect of incorporated protons is presented. Protonation of lattice oxygens stimulate transition metal migration to the alkaline layer and accelerates layered‐rock‐salt phase transition, which leads to bulk structure disintegration and anisotropic surface reconstruction layers formation. A cathode that undergoes severe protonation reactions attains a porous architecture corresponding to its multifold performance fade. This work reveals that interactions between electrolyte and cathode that result in protonation can dominate the structural reversibility/stability of bulk cathodes, and the insight sheds light for the development of future batteries.
25 ENERGY STORAGE↗
Passive Water Assurance Delivery System
This report provides an analysis and evaluation of proposed design improvements to the internal water delivery system of NASA’s passive vegetable growing system. The VEGGIE system is designed to provide fresh vegetables and psychological benefits for astronauts aboard the International Space Station. Preliminary testing conducted by NASA for the VEGGIE system revealed flaws in the water delivery system. In these tests, the interface between the plants and the water reservoir failed to provide passive water delivery through the system both in microgravity experiments and experiments conducted on Earth. Our team’s goal was to fix this interface such that water can be passively delivered from the water reservoir to the plant rooting pillows to grow vegetative crops from seed to harvest. The system requirements outlined by NASA include: minimal total mass, on-demand passive water delivery, same dimensions as existing fixtures, minimal pressure on system to prevent leaking, zero mold growth, minimal swelling or clogging for non-flammable capillary materials, pressure stabilization between the water reservoir and plant pillow bags, even dispersal of water during initial priming, minimal bubble obstruction of capillary interface, maximum gas availability to plant roots, growth in a mixed artificial media (50:50 Arcillite:Fafard #2), and to avoid overwatering and drought conditions for plants. The major proposed design improvements are to use a single-interface capillary cord design to directly connect the water reservoir to the plant-rooting pillows, and to alter the water reservoir to model a propellant management device (PMD) in order to ensure consistent and long term watering for the VEGGIE system. The plant rooting pillow required minimal changes outside of replacing the capillary mat on the bottom of the pillow with O-ring insertion points the single-interface capillary system. - Research was conducted to determine which materials are able to uptake water through capillary action to grow Outredgeous Lettuce plants from seed to harvest. The primary requirements to be met by the team's design and evaluation of the capillary interface were: continuous passive watering for 90 days using non-flammable capillary materials and a peak water delivery rate of 30 mL/hr./0.15 m 2 . The results of the team's experimentation showed that the capillary material Nomex displayed the highest capillary water delivery potential with a maximum flow rate of 3.6 mL/hr. The Nomex capillary systems were the only capillary material to consistently grow Outredgeous Lettuce plants from seed to harvest, and displayed the highest average flow rate for multiple experiment sets. The Nomex material was previously incorporated into the VEGGIE system using a matted version of the capillary material, though the team recommends using a cord configuration in the single-interface capillary system for greater system stability. Nomex has proven to be a promising material, as it has passed both health and fire standards for use aboard the International Space Station. PMDs are made of materials that utilize surface tension and adhesive forces to overcome adverse accelerations to improve stability and ensure fluid delivery. PMDs are typically used in fuel tanks to ensure fuel delivery. The team recommends using a sponge PMD in order to mitigate bubble obstruction, decrease system weight, and ensure reliable water delivery to the capillary interface. The PMD water reservoir requires a rigid water reservoir and a vent tube for pressure stabilization. Since PMD’s cannot be tested in 1-G (Earth conditions), further theoretical modeling and testing is required for the proposed water reservoir design. The intent of this proposed system is to passively water plants in microgravity, though the technology is not limited to microgravity applications. The testing at The Ohio State University has proven that the design is highly effective on Earth, demonstrating that it could serve as a simple water delivery system in home and office applications. This would make vegetative crops more accessible in all indoor applications, thereby improving indoor air quality and occupant comfort. Additionally, this technology has great potential to be utilized in greenhouse plant production, cutting back on more sophisticated watering system energy and time requirements.
Alexandria Jensen↗
Insights into the Enhanced Oxidative Thermal Stability of Nanoparticle Organic Hybrid Materials Developed for Carbon Capture and Energy Storage
Due to the growing need for Direct Air Capture (DAC) and integrated carbon capture and conversion technologies, CO 2 capture materials that can withstand a wide range of environmental conditions, including fluctuating ambient temperatures and high concentrations of oxidizing agents (i.e., oxygen and moisture), are critically needed. Liquid-like Nanoparticle Organic Hybrid Materials (NOHMs) have been proposed as candidates for DAC and electrolyte additives enabling sustainable energy storage (i.e., integrated CO 2 capture and conversion and flow batteries). Liquid-like NOHMs functionalized with an ionic bond have been shown to display greatly enhanced oxidative thermal stability compared to the untethered polymer. However, these studies were limited in terms of reaction conditions and the detailed mechanisms of the oxidative thermal degradation were not reported. In this work, a kinetic thermal degradation analysis was performed on NOHM-I-HPE and the neat polymer, Jeffamine M2070 (HPE), in both non-oxidative and oxidative conditions. NOHM-I-HPE displayed similar thermal stability to the untethered polymer in a nitrogen environment, but interestingly, the thermal stability of the ionically tethered polymer was significantly enhanced in the presence of air. This observed enhancement of oxidative thermal stability is attributed to the orders of magnitude larger viscosity of the liquid-like NOHMs compared to untethered polymer and the bond stabilization of the ionically tethered polymer in the NOHMs canopy. Further, spectroscopic analyses of the liquid residue revealed that in the presence of oxygen, the degradation of HPE and NOHM-I-HPE occurs through the formation of trace amounts of carbonyls. This study illustrated that NOHMs can serve as functional materials for sustainable energy storage applications because of their excellent oxidative thermal stability.
25 ENERGY STORAGE↗
Grain Boundary Plane Measurement Using Transmission Electron Microscopy Automated Crystallographic Orientation Mapping for Atom Probe Tomography Specimens
Abstract Grain boundaries are critical in determining the properties of materials, including mechanical stability, conductivity, and corrosion resistance. The specific properties of materials depend not only on the misorientation of the crystals, the three most commonly characterized parameters, but also on the angle of the grain boundary plane between the two crystals, the final two parameters in the five-parameter macroscopic description of the grain boundary. The method presented here allows for the direct measurement of all five parameters of the grain boundary in a transmission electron microscopy specimen of various morphologies. This is especially applicable to atom probe specimens, where only a single-tilt axis is generally available, allowing the crystallographic description to be matched to the detailed chemical data available in the atom probe tomography. This method provides a platform for efficient grain boundary analysis in unique samples, saving operator time and allowing for ease of acquisition and interpretation in comparison with traditional electron diffraction methods.
Materials Science↗
Status of Solar Sail Material Characterization at NASA's Marshall Space Flight Center
Near term solar sail propelled science missions are targeting the Lagrange point 1 (Ll) as well as locations sunward of L1 as destinations. These near term missions include the Solar Polar Imager' and the L1 Diamond '. The Environmental Effects Group at NASA's Marshall Space Flight Center (MSFC) continues to actively characterize solar sail material in preparation for these near term solar sail missions. Previous investigations indicated that space environmental effects on sail material thermo-optical properties were minimal and would not significantly affect the propulsion efficiency of the sail. These investigations also indicated that the sail material mechanical stability degrades with increasing radiation exposure. This paper will further quantify the effect of space environmental exposure on the mechanical properties of candidate sail materials. Candidate sail materials for these missions include Aluminum coated Mylar(TradeMark), Teonex(TraeMark), and CP1 (Colorless Polyimide). Experimental data will be presented on sail material response to charged particle radiation and subsequent Hypervelocity Impact (HVI). Data will also be presented indicating mechanical property variations in sail material resulting from electron exposure, proton exposure, and a combined electron and proton exposure. Tabular data consisting of areal density, thickness, thermo-optical, mechanical, and electrical properties, vacuum stability and outgassing will be presented.
Edwards, David L.↗
Solution-processed tungsten diselenide as an inorganic hole transport material for moisture-stable perovskite solar cells in the n-i-p architecture
Some of the obstacles to the commercialization of perovskite solar cells (PSCs) are their long-term moisture stability and material cost of the constituent layers, such as the commonly used spiro-OMeTAD hole transport layer (HTL). Replacing the spiro-OMeTAD with low-cost inorganic hole transport materials (HTMs) are important to further elevate the attractiveness of PSCs for commercialization. Perovskite-compatible, solution-exfoliated two-dimensional (2D) transition metal dichalcogenides (TMDCs) are being considered as viable candidates for inorganic HTMs. We consider one such TMDC, WSe 2 which was chemically exfoliated using dichlorobenzene (DCB), a perovskite-compatible solvent, as it was integrated with triple cation perovskite absorbers within the solar cell stack. Here, the WSe 2 HTL required heat treatment processes to be maintained below 100°C in order to preserve the integrity of the underlying perovskite; despite this lower temperature post treatment process, the structural morphology of the film revealed its dense and pinhole-free nature. Temperature-dependent transport studies conducted on the WSe 2 film provided evidence of its semiconducting character and its ability to extract holes well from the underlying triple-cation Cs 0.05 FA 0.79 MA 0.16 PbI 2.45 Br 0.55 absorber. The inorganic HTL offered better environmental stability in moisture-rich environments of up to 60% relative humidity, in comparison to spiro-OMeTAD HTL-based devices which degraded faster as a result of pinholes
14 SOLAR ENERGY↗
Microcalorimetric Measurements of Hydrogen Peroxide Stability
Recent interest in propellants with nontoxic reaction products has led to a resurgence of interest in hydrogen peroxide for various propellant applications. Because hydrogen peroxide is sensitive to contaminants and materials interactions, stability and shelf life are issues. A relatively new, ultrasensitive heat measurement technique, isothermal microcalorimetry, is being used at the White Sands Test Facility to monitor the decomposition of hydrogen peroxide at near ambient temperatures. Isothermal microcalorimetry measures the beat flow from a reaction vessel into a surrounding heat sink. In these applications, microcalorimetry is approximately 1,000 times more sensitive than accelerating rate calorimetry or differential scanning calorimetry for measuring thermal events. Experimental procedures have been developed for the microcalorimetric measurement of the ultra-small beat effects caused by incompatible interactions of hydrogen peroxide. The decomposition rates of hydrogen peroxide at the picomole/sec/gram level have been measured showing the effects of stabilizers and peroxide concentration. Typical measurements are carried out at 40 C over a 24-hour period, This paper describes a method for the conversion of the heat flow measurements to chemical reaction rates based on thermochemical considerations. The reaction rates are used in a study of the effects of stabilizer levels on the decomposition of propellant grade hydrogen peroxide.
Davis, Dennis D.↗
Oxygen Mass Flow Rate Generated for Monitoring Hydrogen Peroxide Stability
Recent interest in propellants with non-toxic reaction products has led to a resurgence of interest in hydrogen peroxide for various propellant applications. Because peroxide is sensitive to contaminants, material interactions, stability and storage issues, monitoring decomposition rates is important. Stennis Space Center (SSC) uses thermocouples to monitor bulk fluid temperature (heat evolution) to determine reaction rates. Unfortunately, large temperature rises are required to offset the heat lost into the surrounding fluid. Also, tank penetration to accomodate a thermocouple can entail modification of a tank or line and act as a source of contamination. The paper evaluates a method for monitoring oxygen evolution as a means to determine peroxide stability. Oxygen generation is not only directly related to peroxide decomposition, but occurs immediately. Measuring peroxide temperature to monitor peroxide stability has significant limitations. The bulk decomposition of 1% / week in a large volume tank can produce in excess of 30 cc / min. This oxygen flow rate corresponds to an equivalent temperature rise of approximately 14 millidegrees C, which is difficult to measure reliably. Thus, if heat transfer were included, there would be no temperature rise. Temperature changes from the surrounding environment and heat lost to the peroxide will also mask potential problems. The use of oxygen flow measurements provides an ultra sensitive technique for monitoring reaction events and will provide an earlier indication of an abnormal decomposition when compared to measuring temperature rise.
Ross, H. Richard↗
Solar Sail Material Performance Property Response to Space Environmental Effects
The National Aeronautics and Space Administration's (NASA) Marshall Space Flight Center (MSFC) continues research into the utilization of photonic materials for spacecraft propulsion. Spacecraft propulsion, using photonic materials, will be achieved using a solar sail. A solar sail operates on the principle that photons, originating from the sun, impart pressure to the sail and therefore provide a source for spacecraft propulsion. The pressure imparted to a solar sail can be increased, up to a factor of two if the sun-facing surface is perfectly reflective. Therefore, these solar sails are generally composed of a highly reflective metallic sun-facing layer, a thin polymeric substrate and occasionally a highly emissive back surface. Near term solar sail propelled science missions are targeting the Lagrange point 1 (L1) as well as locations sunward of L1 as destinations. These near term missions include the Solar Polar Imager' and the L1 Diamond '. The Environmental Effects Group at NASA's Marshall Space Fliglit Center (MSFC) continues to actively characterize solar sail material in preparation for these near term solar sail missions. Previous investigations indicated that space environmental effects on sail material thermo-optical properties were minimal and would not significantly affect the propulsion efficiency of the sail3-'. These investigations also indicated that the sail material mechanical stability degrades with increasing radiation exposure. This paper will further quantify the effect of space environmental exposure on the mechanical properties of candidate sail materials. Candidate sail materials for these missions include Aluminum coated Mylar TM, Teonexm, and CP1 (Colorless Polyimide). These materials were subjected to uniform radiation doses of electrons and protons in individual exposures sequences. Dose values ranged from 100 Mrads to over 5 Grads. The engineering performance property responses of thermo-optical and mechanical properties were characterized. The contribution of Near Ultraviolet (NUV) radiation combined with electron and proton radiation was also investigated. Conclusions will be presented providing a gauge of measure for engineering performance stability for sails operating in the L1 space environment.
Edwards, David L.↗
Thermophysical properties of plasma sprayed coatings
Thermophysical properties of plasma sprayed materials were determined for the following plasma sprayed materials: CaO - stabilized ZrO2, Y2O3 - stabilized ZerO2, Al2O3, HfO2 Mo, nichrome, NiAl, Mo-ZrO2, and MoAl2O3 mixtures. In all cases the thermal conductivity of the as-sprayed materials was found to be considerably lower than that of the bulk material. The flash-laser thermal diffusivity technique was used both for diffusivity determination of single-layer materials and to determine the thermal contact resistance at the interface of two-layer specimens.
Wilkes, K. E.↗
Space Environmental Effects on Candidate Solar Sail Materials
The National Aeronautics and Space Administration's (NASA) Marshall Space Flight Center (MSFC) continues research into the utilization of photonic materials for spacecraft propulsion. Spacecraft propulsion, using photonic materials, will be achieved using a solar sail. A solar sail operates on the principle that photons, originating from the sun, impart pressure to the sail and therefore provide a source for spacecraft propulsion. The pressure imparted ot a solar sail can be increased, up to a factor of two, if the sun-facing surface is perfectly reflective. Therefore, these solar sails are generally composed of a highly reflective metallic sun-facing layer, a thin polymeric substrate and occasionally a highly emissive back surface. Near term solar sail propelled science missions are targeting the Lagrange point 1 (L1) as well as locations sunward of L1 as destinations. These near term missions include the Solar Polar Imager and the L1 Diamond. The Environmental Effects Group at NASA's Marshall Space Flight Center (MSFC) continues to actively characterize solar sail material in preparation for these near term solar sail missions. Previous investigations indicated that space environmental effects on sail material thermo-optical properties were minimal and would not significantly affect the propulsion efficiency of the sail. These investigations also indicated that the sail material mechanical stability degrades with increasing radiation exposure. This paper will further quantify the effect of space environmental exposure on the mechanical properties of candidate sail materials. Candidate sail materials for these missions include Aluminum coated Mylar, Teonex, and CP1 (Colorless Polyimide). These materials were subjected to uniform radiation doses of electrons and protons in individual exposures sequences. Dose values ranged from 100 Mrads to over 5 Grads. The engineering performance property responses of thermo-optical and mechanical properties were characterized. The contribution of Near Ultraviolet (NUV) radiation combined with electron and proton radiation was also investigated.
Edwards, David L.↗
Solar Sail Material Performance Property Response to Space Environmental Effects
The National Aeronautics and Space Administration's (NASA) Marshall Space Flight Center (MSFC) continues research into the utilization of photonic materials for spacecraft propulsion. Spacecraft propulsion, using photonic materials, will be achieved using a solar sail. A solar sail operates on the principle that photons, originating from the sun, impart pressure to the sail and therefore provide a source for spacecraft propulsion. The pressure imparted to a solar sail can be increased, up to a factor of two, if the sun-facing surface is perfectly reflective. Therefore, these solar sails are generally composed of a highly reflective metallic sun-facing layer, a thin polymeric substrate and occasionally a highly emissive back surface. Near term solar sail propelled science missions are targeting the Lagrange point 1 (Ll) as well as locations sunward of L1 as destinations. These near term missions include the Solar Polar Imager and the L1 Diamond. The Environmental Effects Group at NASA s Marshall Space Flight Center (MSFC) continues to actively characterize solar sail material in preparation for these near term solar sail missions. Previous investigations indicated that space environmental effects on sail material thermo-optical properties were minimal and would not significantly affect the propulsion efficiency of the sail. These investigations also indicated that the sail material mechanical stability degrades with increasing radiation exposure. This paper will further quantify the effect of space environmental exposure on the mechanical properties of candidate sail materials. Candidate sail materials for these missions include Aluminum coated Mylar[TM], Teonex[TM], and CPl (Colorless Polyimide). These materials were subjected to uniform radiation doses of electrons and protons in individual exposures sequences. Dose values ranged from 100 Mrads to over 5 Grads. The engineering performance property responses of thermo-optical and mechanical properties were characterized. The contribution of Near Ultraviolet (NUV) radiation combined with electron and proton radiation was also investigated.
Edwards, David L.↗
Voltage and Temperature Limits of Advanced Electrolytes for Lithium-Metal Batteries
Several advanced electrolytes (mainly ether-based) have recently demonstrated excellent electrochemical performance in high energy density lithium (Li)-metal batteries. However, the safety of these ether-based electrolytes is still unknown. This work evaluates the thermal stability of these new formulations to understand their safety limits of operation in comparison to carbonate electrolytes typically used in Li-ion batteries. Electrolyte stability is assessed in conjunction with LiNi 0.8 Mn 0.1 Co 0.1 O 2 cathode and Li-metal anode at ultra-high voltages (≤ 4.8 V) and temperatures (≤ 300°C) to trigger thermal runaway, where onset and extent of heat release are monitored via isothermal microcalorimetry and differential scanning calorimetry Most ether-based electrolytes show improved thermal resilience over commercial carbonate formulations when heated up to 300°C. The thermal behavior in presence of charged cathode and Li-metal suggests that the new electrolytes may be better at stabilizing active material surfaces than carbonate electrolytes. Although extreme voltages severely destabilize the ether-based formulations, prompting thermal runaway, a phosphate based localized high concentration electrolyte exhibits superior stability over commercial carbonate electrolytes at all tested temperatures (32°C, 45°C, and 60°C). Although thermal analysis during the first charge process (as adopted in this preliminary study) may be insufficient to conclude the long-term advantages of these electrolytes, a more stable electrolyte identified under extreme voltage and temperature conditions will provide valuable guidance for the safety of future electrolyte designs.
25 ENERGY STORAGE↗
Technical Routes to Achieve High Circular Polarized Luminescence in Chiral Perovskites: A Mini‐Review
Chiral hybrid organic-inorganic perovskites (HOIPs) have emerged as promising materials for optoelectronic and spintronic applications, leveraging unique properties such as circularly polarized luminescence (CPL), circularly polarized nonlinear optical (NLO) emission, and chiral-induced spin selectivity (CISS). However, challenges remain in stabilizing these materials under environmental stresses and precisely controlling chirality for scalable use. This review summarizes five main strategies to induce chirality in HOIPs, i.e., direct incorporation of chiral cations, surface modification with chiral ligands, ion doping, template-induced chirality, and chiral metasurfaces. Each approach offers distinct advantages for optimizing CPL efficiency and device stability, paving the way for next-generation applications in CPL detectors, information encryption, spintronic devices, etc.
14 SOLAR ENERGY↗
The stability of new transparent polymeric materials: The epoxy trimethoxyboroxine system. Part 1: The preparation, characterization and curing of epoxy resins and their copolymers
The effects of resin composition, curing conditions fillers, and flame retardant additives on the flammability of diglycidyl ether of bisphenol-A (DGEBA) as measured by the oxygen index is examined. The oxygen index of DGEBA cured with various curing agents was between 0.198 to 0.238. Fillers and flame retardant additives can increase the oxygen index dependent on the material and the amount used. Changes in the basic cured resin properties can be anticipated with the addition of noncompatible additives. High flame resistant epoxy resins with good stability and mechanical properties are investigated.
Pearce, E.↗