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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 73 records · Page 4
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Weather aging effects on modified asphalt with rubber-polyethylene composites

Weather aging may cause more severe degradation on asphalt than thermal-oxidative aging due to the synergistic effect among oxygen, heat, ultraviolet (UV) radiation, and moisture. This study aimed to investigate weather aging effects and anti-aging mechanisms on asphalt modified with rubber-polyethylene (PE) composites. The modified binder blends and asphalt mixtures were subjected to outdoor weather aging. Dynamic shear rheometer (DSR), Fourier transform infrared spectroscopy (FTIR), Gel permeation chromatography (GPC), and optical microscopy tests were adopted to characterize the rheological properties, aging resistance, polymer degradation, and anti-aging mechanisms of modified binder blends, respectively. Mixture performance tests including Asphalt Pavement Analyzer (APA) and Ideal-CT tests were used to evaluate rutting and cracking resistance of asphalt mixtures. Results showed that weather aging can cause more severe aging to asphalt binders than pressure aging vessel (PAV) due to the severe degradation of PE particles. Rubber-PE composites alloyed with an extruder proved to stabilize PE particles in asphalt and significantly improve the aging resistance of modified binder blends. Furthermore, the enhanced aging resistance is attributed to the dispersion of PE particles and carbon black released by soluble rubbers.

Aging resistance↗
DOE OSTI2022

“Tailing” Phenomenon During Polymer Propagation at The Milne Point Polymer Flood

Chemical flooding simulators traditionally assume that polymer retention follows the Langmuir isotherm, while fractional-flow calculations assume concentration-independent retention. Both models predict a delay in propagation of the polymer front (in proportion to the retention value), followed by a rapid rise in produced polymer concentration to the injected level. In contrast, laboratory retention studies for the Milne Point polymer flood (North Slope of Alaska) consistently show virtually no delay in polymer propagation, a rapid rise in produced polymer to 70-90% of the injected concentration, followed by produced concentration gradually approaching the injected value over many pore volumes. From a practical viewpoint, this behavior means that retention causes no significant delay in propagation of the polymer bank (and therefore the oil bank), but the effective viscosity and displacement efficiency are less than originally planned. This paper explores why this polymer “tailing” phenomenon occurs. During core floods, effluent was analyzed for brine-tracer concentration, viscosity, total organic carbon, and total nitrogen. The latter three items allowed three independent measures of polymer concentration and polymer retention. Experiments were performed with Milne Point core material, oil, brine, and conditions. Mechanistic experiments were also performed with packs of glass beads with controlled levels of various minerals. In Milne Point cores, the presence of the tailing phenomenon was not sensitive to flow rate, polymer concentration, core heterogeneity, or whether the core was preserved, cleaned of oil, or cleaned and resaturated with oil, or cleaned, re-saturated and aged with oil. The three independent measures of polymer concentration confirmed that the tailing phenomenon was not an artifact associated with polymer degradation or detection interferences. Tailing was also observed during mechanistic floods using glassbead packs when sufficient levels of illite or kaolinite were present. This observation was consistent with high levels of illite noted in Milne Point cores. The tailing was not noted during mechanistic floods that contained beads with montmorillonite, chlorite, calcium carbonate, dolomite, siderite, pyrite, or calcium sulfate. A model is proposed to account for the tailing phenomenon. This work suggests that mineralogy analysis (especially for illite and kaolinite) may reveal whether tailing should be accounted for during simulations of polymer propagation/retention in a given field application.

Seright, Randy↗
DOE OSTI2021

Design, synthesis, and characterization of vinyl-addition polynorbornenes with tunable thermal properties

Unfunctionalized vinyl-addition polynorbornene (VAPNB) possesses many outstanding properties such as high thermal, chemical, and oxidative stability. These features make VAPNB a promising candidate for many engineering applications. However, VAPNB has a small service window between its glass transition temperature (T g ) and decomposition temperature (T d ), and it cannot be readily processed in a melt state. In this work, we demonstrate that the service window of VAPNBs can be tailored through the use of norbornene monomers bearing alkyl, aryl, and aryl ether substituents. The vinyl addition homopolymerization and copolymerization of these functionalized norbornyl-based monomers yielded VAPNBs with high T' g s (>150 °C) and large service windows (T d –T g > 100 °C), which are comparable to other commercial engineering thermoplastics. To further establish the feasibility of melt processing, a functionalized VAPNB material with T g = 209 °C and a service window of 170 °C was successfully extruded and molded into bars. Subsequent characterization of the bars by dynamic mechanical analysis (DMA), nuclear magnetic resonance spectroscopy (NMR), and gel permeation chromatography (GPC) revealed only minor signs of polymer degradation. Furthermore, these studies suggest that substituted VAPNBs could be developed into a new class of engineering thermoplastics that is compatible with workhorse melt processing techniques such as extrusion and injection molding, as well as emerging techniques such as extrusion-based 3D printing.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Understanding Recoverable vs Unrecoverable Voltage Losses and Long-Term Degradation Mechanisms in Anion Exchange Membrane Fuel Cells

Anion exchange membrane fuel cells (AEMFCs) have recently shown excellent progress in terms of their performance – e.g., achievable power and current density. However, very few AEMFCs have been demonstrated with the ability to operate for a long duration (>1000 h). In addition, it is unknown whether performance losses observed during operation are reversible, irreversible, or a combination of the two. In this study, a high-performance AEMFC operated continuously at 600 mA/cm 2 for 3600 h (150 days) at 80 °C with H 2 /O 2 reacting gases was demonstrated. Throughout testing, the electrochemical properties of the AEMFC were probed to provide information about performance degradation pathways and their degree of reversibility. It was found that a portion of the performance loss that occurs during AEMFC operation was due to suboptimal reaction conditions and can be recovered. At the end of the experiment, the cell was disassembled, and its structure and composition were evaluated at the nanoscale by aberration-corrected scanning transmission electron microscopy and energy-dispersive X-ray spectroscopy. The structure and composition of the electrode were compared to cells at the beginning of their operational life. It was found that the primary mechanism for long-term AEMFC performance loss was catalyst agglomeration. During the operational time, there was no evidence of significant polymer degradation, likely due to the high hydration state of the cell. By documenting the long-term changes in high-performing AEMFCs, this work provides important information for the systematic design of cell components and demonstrates the importance of controlling cell operation, which can aid in the commercialization and widespread deployment of low-cost, long-life AEMFCs.

30 DIRECT ENERGY CONVERSION↗
DOE OSTI2022

In Situ EXAFS-Based Nanothermometry of Heterodimer Nanocrystals under Induction Heating

The ability to heat nanocrystalline materials through magnetic induction has been used in the fields of catalysis, biomedical sciences, and polymer degradation. However, the working temperature to which the inductively coupled material rises is still poorly understood. Herein, we use extended X-ray absorption fine structure spectroscopy in conjunction with thermal imaging to improve the understanding of heating in inductively coupled systems. After extraction of the Debye–Waller factor from the spectroscopy, we obtain the temperature of inductively heated nanocrystals from the correlated Debye model. We combine carbon-supported iron oxide nanocrystals as induction heating agents with platinum nanocrystals as thermal probes. By testing these nanocrystal species as both unattached nanocrystals and heterodimers, we report that nanostructured systems show a significant temperature difference of up to 73.60 °C when compared to their local support environment. Furthermore, this result has implications for inductively heated catalysis, magnetic hyperthermia for targeted cell death, and polymer synthesis.

09 BIOMASS FUELS↗
DOE OSTI2024

Biocomposite thermoplastic polyurethanes containing evolved bacterial spores as living fillers to facilitate polymer disintegration

The field of hybrid engineered living materials seeks to pair living organisms with synthetic materials to generate biocomposite materials with augmented function since living systems can provide highly-programmable and complex behavior. Engineered living materials have typically been fabricated using techniques in benign aqueous environments, limiting their application. In this work, biocomposite fabrication is demonstrated in which spores from polymer-degrading bacteria are incorporated into a thermoplastic polyurethane using high-temperature melt extrusion. Bacteria are engineered using adaptive laboratory evolution to improve their heat tolerance to ensure nearly complete cell survivability during manufacturing at 135 °C. Furthermore, the overall tensile properties of spore-filled thermoplastic polyurethanes are substantially improved, resulting in a significant improvement in toughness. The biocomposites facilitate disintegration in compost in the absence of a microbe-rich environment. Finally, embedded spores demonstrate a rationally programmed function, expressing green fluorescent protein. This research provides a scalable method to fabricate advanced biocomposite materials in industrially-compatible processes.

36 MATERIALS SCIENCE↗
DOE OSTI2022

The Bacteroidetes Aequorivita sp. and Kaistella jeonii Produce Promiscuous Esterases With PET-Hydrolyzing Activity

Certain members of the Actinobacteria and Proteobacteria are known to degrade polyethylene terephthalate (PET). Here, we describe the first functional PET-active enzymes from the Bacteroidetes phylum. Using a PETase-specific Hidden-Markov-Model- (HMM-) based search algorithm, we identified several PETase candidates from Flavobacteriaceae and Porphyromonadaceae. Among them, two promiscuous and cold-active esterases derived from Aequorivita sp. (PET27) and Kaistella jeonii (PET30) showed depolymerizing activity on polycaprolactone (PCL), amorphous PET foil and on the polyester polyurethane Impranil ® DLN. PET27 is a 37.8 kDa enzyme that released an average of 174.4 nmol terephthalic acid (TPA) after 120 h at 30°C from a 7 mg PET foil platelet in a 200 μl reaction volume, 38-times more than PET30 (37.4 kDa) released under the same conditions. The crystal structure of PET30 without its C-terminal Por-domain (PET30ΔPorC) was solved at 2.1 Å and displays high structural similarity to the Is PETase. PET30 shows a Phe-Met-Tyr substrate binding motif, which seems to be a unique feature, as Is PETase, LCC and PET2 all contain Tyr-Met-Trp binding residues, while PET27 possesses a Phe-Met-Trp motif that is identical to Cut190. Microscopic analyses showed that K. jeonii cells are indeed able to bind on and colonize PET surfaces after a few days of incubation. Homologs of PET27 and PET30 were detected in metagenomes, predominantly aquatic habitats, encompassing a wide range of different global climate zones and suggesting a hitherto unknown influence of this bacterial phylum on man-made polymer degradation.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

Diffusion-limited hydrolysis in polymeric materials

Polymer degradation under aggressive environmental stressors often develops heterogeneities due to diffusion-limited reaction phenomena. This is well established for diffusion-limited oxidation (DLO), which is known to occur for most polymeric materials at elevated temperatures but has been less summarized for the conditions of diffusion-limited hydrolysis (DLH). Here, an overview of hydrolysis for several materials and a computational model, analogous to the underlying equations for DLO, able to define this diffusion-reaction system is presented. A systematic study of the influence of various parameters, such as water diffusivity, reaction rate and order, and a more in-depth focus on residual isocyanate hydrolysis in a polymeric methylene diphenyl diisocyanate (pMDI) based polyurethane (PU) foam is given. For this system, we present experimental data for model ‘input’ parameters and discuss predictions for different conditions. We conceptually compare the behavior of diffusion-limited oxidation to that of diffusion-limited hydrolysis (DLH). With the mathematical framework and key material properties presented herein, any DLH phenomena following Fickian diffusion behavior can be understood, modeled, and predicted.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Opinion to address the personal protective equipment shortage in the global community during the COVID-19 outbreak

The current COVID-19 pandemic is stretching both the global supply for face masks and personal protective equipment (PPE). Production capacity is severely limited in many countries. This is a call for the R&D community, particularly to those in the polymer degradation and stability field. We have not only an opportunity but an obligation to engage and collaborate with virology and bio-medical experts. We require comparative R&D for extended, reuse and recyclability options. Additionally, there is urgent need for large scale institutional approaches and methods that can be quickly applied locally by non-experts with limited resources.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Oxidative instability of ionomers in hydroxide-exchange-membrane water electrolyzers

Hydroxide-exchange membrane (HEM) electrolyzers can produce green H 2 with only earth-abundant catalysts and electrolyte-free (nominally pure) water feed, significantly decreasing system cost and complexity. However, HEM technology suffers from short lifetimes, attributed in part to poor stability of anion-exchange polymers used in the membrane and catalyst layers. We use electrochemical analysis and ex situ characterization techniques to study anion-exchange-polymer degradation in electrolyzers. Using multiple ionomers, catalyst-layer additives, and electrolyte feed, we show how anode-ionomer oxidation is the dominant degradation mechanism for all HEM-based electrolyzer cells tested. Here, we find improved device stability using oxidation-resistant catalyst-layer binders and propose new design strategies for advanced ionomer and catalyst-layer development.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Organocatalysis in ring opening copolymerization as a means of tailoring molecular weight dispersity and the subsequent impact on physical properties in 4D printable photopolymers

Vat photopolymerization 3D printing has traditionally relied on free radical crosslinking between alkenes to produce non-degradable parts, which may have limited use in the biomedical and clinical spaces. Photopolymer resins containing functionalized degradable polymers, specifically polyesters, are greatly interesting for 3D printing tissue scaffolds and medical devices. Unfortunately, most polyesters produced for these applications have been made using metal-containing catalysts, which are not without risk for medical applications. Organocatalysis is a viable alternative route to achieving the same types of polyesters. Here, ring opening copolymerization (ROCOP) of allyl and cyclohexene-containing polyesters is examined using bipyridine and a guanidine-containing catalyst. The role of the catalysts, initiators, and cocatalysts are examined for bulk, open air ROCOP reactions. Unlike previous efforts with organocatalysis, the examined catalysts here could be used to tailor the dispersity of the polyesters, with ~10 kDa polyesters with dispersity ranging from 1.3 to 2.5 examined for the impact on rheological and thermomechanical properties related to resin/part behavior. The bipyridine catalysts and a thiourea cocatalyst further are shown, through the introduction of new fluorescence emissions of the purified polyesters. As a result, this work demonstrates that tuning the dispersity of polyester photopolymers provides a direct method of tailoring physical and optical properties in 3D/4D printable materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Processing behavior evolution of recycled polypropylene: An integrated experimental and Computer-Aided engineering simulation study

Polypropylene (PP) comprises 21% of global plastics production and 18% of plastics waste, yet less than 1% of solid-waste PP is recycled in the United States (U.S.), representing significant environmental and economic challenges. Mechanical recycling, the most prevalent recycling method, subject's materials to thermomechanical stresses, which typically degrade polymer properties, affecting the quality of polymer products. This study replicates the impact of mechanical recycling through multiple extrusion cycles to examine the effects on PP's processing behavior. Dynamic scanning calorimetry (DSC) measurements showed stable melting behavior across all processing conditions, while crystallization analysis exhibited consistent shifts in kinetic parameters. Rheological characterization demonstrated progressive viscosity reductions through successive cycles, particularly pronounced at elevated reprocessing temperatures. Here, the integration of this experimental data into injection molding simulations showed that recycled PP maintains viable processing characteristics. Our findings establish quantitative correlations between processing history and material behavior, enabling optimization of processing parameters directly rather than relying on trial-and-error approaches. While these results reflect idealized recycling conditions with minimal contamination, they provide a framework for understanding fundamental property evolution during mechanical recycling.

42 ENGINEERING↗
DOE OSTI2024

Epoxy Coating of Biofiber: An Effective Modifier of Biofiber Physical and Flow Properties for Improved Tensile Behavior of Biofiber-Reinforced Biocomposite

Biocomposites combine renewable, plant-based fibers with degradable polymers and are an attractive option for sustainable, lightweight, and cost-effective materials with a low carbon footprint, especially for large-scale additive manufacturing. One of the major challenges in the widespread adoption of biocomposites is that their mechanical performance is significantly inferior to that of synthetic composites. Surface treatment is a common and effective technique to improve the mechanical properties of the biofibers used in biocomposites. This study aims to investigate the physical and flow properties of surface-treated biofibers, as well as the tensile properties of their PLA-based biocomposite, to gain insights into how surface treatment changes the fiber‘s characteristics and biocomposite‘s mechanical properties. Surface treatment was created using a two-component epoxy system by reacting poly(bisphenol A-co-epichlorohydrin) glycidyl end-capped (PBG) and dicyandiamide (DICY). The treatment was tested on two different biofibers (loblolly pine and corn stover fibers) with three different PBG/DICY molar ratios (0.25, 0.5, and 2). Results showed that surface-treated fibers improved the tensile strength and Young‘s modulus of the biocomposites. Loblolly pine biocomposites from fibers treated with a PBG/DICY ratio of 0.25 exhibited the best tensile properties. The surface treatment resulted in a more loosely dispersed fiber bulk structure, as evidenced by less fiber agglomeration into smaller particle sizes, higher fiber sphericity, and lower loose bulk density. This can enhance stress distribution and the overall mechanical performance of the biocomposites. Additionally, surface-treated fibers exhibited better dynamic flow properties.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Volumetric Subtractive Manufacturing

Manufacturing small negative features has been extremely challenging in whole additive manufacturing (AM) field. Due to overcuring, diffusion and refractive index increase, the achievable smallest negative feature and fidelity is always worse than the smallest positive one using AM methods. Additionally, attempting to print multi-scale feature sizes in the same exposure has proven to be challenging in DLP printing due to diffusion and inhibition. To address these challenges, we have developed a hybrid additive and subtractive manufacturing approach on a DLP platform with a dual-wavelength photopolymers to be able to print multi-scale features and small negative features with accuracy. And we also have demonstrated a first-of-its-kind Volumetric Subtractive Manufacturing by fabricating non-planar double helix fluidics by photo-degrading polymers. This work has the potential to shift the paradigm of DLP AM techniques by incorporating subtractive manufacturing as a new degree of freedom for enhancing the achievable print resolution and enabling corrective and adaptive manufacturing.

42 ENGINEERING↗
NASA NTRS1988

Decrease in the etch rate of polymers in the oxygen afterglow with increasing gas flow rate

This paper reports the variation of the etch rate of polymers in the afterglow of a radio frequency discharge in oxygen as a function of total flow rate in the range 2-10 cu cm (STP)/min. The measurements were made at ambient temperature with the O(P-3) concentration held essentially constant. Results are reported on three polymers: cis-polybutadiene, a polybutadiene with 33 percent 1,2 double bonds, and a polybutadiene with 40 percent 1,2 double bonds. It has been observed that the etch rate of these polymers decreases significantly with increasing flow rate, strongly suggesting that the vapor-phase products of polymer degradation contribute to the degradation process.

Lerner, N. R.↗
NASA NTRS1994

Chemical and Thermal Analysis

Thermal decomposition activation energies have been determined using two methods of Thermogravimetric Analysis (TGA), with good correlation being obtained between the two techniques. Initial heating curves indicated a two-component system for Coflon (i.e. polymer plus placticizer) but a single component system for Tefzel. Two widely differing activation energies were for Coflon supported this view, 15 kcl/mol being associated with plasticizer, and 40 kcal/mol with polymer degradation. With Tefzel, values were 40-45 kcal/mol, the former perhaps being associated with a low molecular weight fraction. Appropriate acceleration factors have been determined. Thermomechanical Analysis (TMA) has shown considerable dimensional change during temperature cycles. For unaged pipe sections heating to 100 C and then holding the temperature resulted in a stable thickness increase of 2%, whereas the Coflon thickness decreased continuously, reaching -4% in 2.7 weeks. Previously strained tensile bars of Tefzel expanded on cooling during TMA. SEM performed on H2S-aged Coflon samples showed significant changes in both physical and chemical nature. The first may have resulted from explosive decompression after part of the aging process. Chemically extensive dehydrofluorination was indicated, and sulfur was present as a result of the aging. These observations indicate that chemical attack of PVDF can occur in some circumstances.

Bulluck, J. W.↗
NASA NTRS2003

Fragmentation under the Scaling Symmetry and Turbulent Cascade with Intermittency

Fragmentation plays an important role in a variety of physical, chemical, and geological processes. Examples include atomization in sprays, crushing of rocks, explosion and impact of solids, polymer degradation, etc. Although each individual action of fragmentation is a complex process, the number of these elementary actions is large. It is natural to abstract a simple 'effective' scenario of fragmentation and to represent its essential features. One of the models is the fragmentation under the scaling symmetry: each breakup action reduces the typical length of fragments, r (right arrow) alpha r, by an independent random multiplier alpha (0 < alpha < 1), which is governed by the fragmentation intensity spectrum q(alpha), integral(sup 1)(sub 0) q(alpha)d alpha = 1. This scenario has been proposed by Kolmogorov (1941), when he considered the breakup of solid carbon particle. Describing the breakup as a random discrete process, Kolmogorov stated that at latest times, such a process leads to the log-normal distribution. In Gorokhovski & Saveliev, the fragmentation under the scaling symmetry has been reviewed as a continuous evolution process with new features established. The objective of this paper is twofold. First, the paper synthesizes and completes theoretical part of Gorokhovski & Saveliev. Second, the paper shows a new application of the fragmentation theory under the scale invariance. This application concerns the turbulent cascade with intermittency. We formulate here a model describing the evolution of the velocity increment distribution along the progressively decreasing length scale. The model shows that when the turbulent length scale gets smaller, the velocity increment distribution has central growing peak and develops stretched tails. The intermittency in turbulence is manifested in the same way: large fluctuations of velocity provoke highest strain in narrow (dissipative) regions of flow.

Gorokhovski, M.↗
NASA NTRS2003

Mechanical Testing of PMCs under Simulated Rapid Heat-Up Propulsion Environments: In-Plane Compressive Behavior - II

Carbon fiber thermoset polymer matrix composites (PMC) with high temperature polyimide based in-situ polymerized monomer reactant (PMR) resin has been used for some time in applications which can see temperatures up to 550 F. Currently, graphite fiber PMR based composites are used in several aircraft engine components including the outer bypass duct for the GE F-404, exit flaps for the P&W F-100-229, and the core cowl for the GE/Snecma CF6-80A3. Newer formulations, including PMR-II-50 are being investigated as potential weight reduction replacements of various metallic components in next generation high performance propulsion rocket engines that can see temperatures which exceed 550 F. Extensive FEM thermal modeling indicates that these components are exposed to rapid heat-up rates (up to -200 F/sec) and to a maximum temperature of around 600 F. Even though the predicted maximum part temperatures were within the capability of PW-II-50, the rapid heat-up causes significant through-thickness thermal gradients in the composite part and even more unstable states when combined with moisture. Designing composite parts for such extreme service environments will require accurate measurement of intrinsic and transient mechanical properties and the hygrothermal performance of these materials under more realistic use conditions. The mechanical properties of polymers degrade when exposed to elevated temperatures even in the absence of gaseous oxygen. Accurate mechanical characterization of the material is necessary in order to reduce system weight while providing sufficient factors of safety. Historically, the testing of PMCs at elevated temperatures has been plagued by the antagonism between two factors. First, moisture has been shown to profoundly affect the mechanical response of these materials at temperatures above their glass transition temperature while concurrently lowering the material's Tg. Moisture phenomena is due to one or a combination of three effects, i.e., plastization of polymeric material by water, the internal pressure generated by the volatilization of water at elevated temperatures, and hydrolytic chemical decomposition. However, moisture is lost from the material at increasing rates as temperature increases. Second, because PMCs are good thermal insulators, when they are externally heated at even mild rates large thermal gradients can develop within the material. At temperatures where a material property changes rapidly with temperature the presence of a large thermal gradient is unacceptable for intrinsic property characterization purposes. Therefore, long hold times are required to establish isothermal conditions. However, in the service environments high-heating-rates, high temperatures, high-loading rates are simultaneous present along with residual moisture. In order to capture the effects of moisture on the material, holding at- temperature until isothermal conditions are reached is unacceptable particularly in materials with small physical dimensions. Thus, the effects due to moisture on the composite's mechanical characteristics, ie., their so-called analog response, may be instructive. One approach employed in this program was rapid heat-up (approx. 200 F/sec.) and loading of both dry and wet in-plane compressive specimens to examine the effects of moisture on this resin dominated mechanical property of the material.

Stokes, Eric H.↗