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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 739 records · Page 41

Determining sulfur speciation in oxidatively crosslinked degradable polymers using sulfur K-edge X-ray absorption spectroscopy

A new family of water-degradable elastic polymers prepared by oxidative crosslinking of the parent polythionolactones shows promise in a broad range of applications, but the compositions of these materials elude conventional analytical methods. Here, in this work, we use sulfur K-edge X-ray absorption spectroscopy to quantify the amounts of thioether, disulfide, sulfone, sulfate ester, and thionoester in each polymer and to rule out the presence of several other functional groups, including sulfonate, thiosulfonate, sulfate, and sulfoxide. We rationalize this speciation as a function of linker flexibility in the context of sulfinyl cycloaddition reactions and propose a mechanism of aggregation for the oxidized polymers. Our results correlate with swelling ratios but not with porosity nor crosslink density measurements, demonstrating the importance of pairing mechanical and chemical techniques when characterizing heterogeneous organic polymers. Finally, we take advantage of the proximity of the gold M 4,5 -edges to the sulfur K-edge to analyze the binding and reactivity of Au(III) with the crosslinked polymers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Segmentation of RDX and TNT in X‐Ray Computed Tomography Reconstructions of Melt‐Cast Explosives

ABSTRACT Three‐dimensional mesoscale characterization of heterogeneous melt‐cast high explosives is challenging because of the difficulty differentiating binder from explosive crystals: two functionally different materials which are typically similar in density by design. Here, we report an algorithm which can differentiate hexahydro‐1,3,5‐trinitro‐1,3,5‐triazine (RDX) from 2,4,6‐trinitrotoluene (TNT) in x‐ray computed tomography (CT) volumes with tens of microns resolution. This method allows us to quantify RDX/TNT content, porosity, and RDX domain size. We calibrated the segmentation algorithm using simulated x‐ray CT volumes containing object models of RDX crystals within a TNT matrix. We then segmented and analyzed CT data for Composition B (Comp B), a 60/40 RDX/TNT mixture, and Cyclotol, a 75/25 RDX/TNT mixture. We examined melt‐cast samples fabricated with 100% theoretical maximum density (TMD) and 85% TMD. For the 100% TMD Comp B and Cyclotol samples, the RDX content values calculated by segmentation were 3% and 9% lower, respectively, than the values measured by high‐performance liquid chromatography on material from the same synthesis lots. This result is consistent with the expected underreporting of RDX content resulting from x‐ray CT resolution limits on RDX particles with diameters smaller than 25 µm. The 85% TMD samples were less accurately segmented with our algorithm due to the confounding presence of voids.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

High‐Loading Lithium‐Sulfur Batteries with Solvent‐Free Dry‐Electrode Processing

Abstract Lithium‐sulfur (Li‐S) batteries, with their high energy density, nontoxicity, and the natural abundance of sulfur, hold immense potential as the next‐generation energy storage technology. To maximize the actual energy density of the Li‐S batteries for practical applications, it is crucial to escalate the areal capacity of the sulfur cathode by fabricating an electrode with high sulfur loading. Herein, ultra‐high sulfur loading (up to 12 mg cm −2 ) cathodes are fabricated through an industrially viable and sustainable solvent‐free dry‐processing method that utilizes a polytetrafluoroethylene binder fibrillation. Due to its low porosity cathode architecture formed by the binder fibrillation process, the dry‐processed electrodes exhibit a relatively lower initial capacity compared to the slurry‐processed electrode. However, its mechanical stability is well maintained throughout the cycling without the formation of electrode cracking, demonstrating significantly superior cycling stability. Additionally, through the optimization of the dry‐processing, a single‐layer pouch cell with a loading of 9 mg cm −2 and a novel multi‐layer pouch cell that uses an aluminum mesh as its current collector with a total loading of 14 mg cm −2 are introduced. To address the reduced initial capacity of dry‐processed electrodes, strategies such as incorporating electrocatalysts or employing prelithiated active materials are suggested.

Chemistry↗

A Versatile Approach to Stabilize Liquid–Liquid Interfaces using Surfactant Self-Assembly

Stabilizing liquid–liquid interfaces, whether between miscible or immiscible liquids, is crucial for a wide range of applications, including energy storage, microreactors, and biomimetic structures. Here, in this study, a versatile approach for stabilizing the water-oil interface is presented using the morphological transitions that occur during the self-assembly of anionic, cationic, and nonionic surfactants mixed with fatty acid oils. The morphological transitions underlying this approach are characterized and extensively studied through small-angle X-ray scattering (SAXS), rheometry, and microscopy techniques. Dissipative particle dynamics (DPD) as a simulation tool is adopted to investigate these morphological transitions both in the equilibrium ternary system as well as in the dynamic condition of the water-oil interface. Such a versatile strategy holds promise for enhancing applications such as liquid-in-liquid 3D printing. Moreover, it has the potential to revolutionize a wide range of fields where stabilizing liquid–liquid interfaces not only offers unprecedented opportunities for fine-tuning nanostructural morphologies but also imparts interesting practical features to the resulting liquid shapes. These features include perfusion capabilities, self-healing, and porosity, which could have significant implications for various industries.

36 MATERIALS SCIENCE↗

Micron Size NaCrO 2 Particles Enable High‐loading Dry‐processed Electrode for Sodium Ion Batteries

Dry-process fabrication using fibrillatable binder is emerging as a promising method to produce high-loading electrodes for energy storage applications, favored by its cost-efficiency and eco-friendliness. While previous studies have demonstrated the advantages of dry process over the traditional slurry method, there remains a gap in understanding how the particle size of active materials influences the mechanical and electrochemical performance of dry electrodes. In this study, four different particle size NaCrO 2 materials (Average size, S-NCO: 0.6 µm, M1-NCO 1.5 µm, M2-NCO: 4.4 µm, and L-NCO: 9.9 µm) are synthesized to investigate the effect of particle size on dry-processed high-loading electrodes. The findings reveal that the larger micron-sized (>4.4 µm) NCO dry films exhibit significantly improved tensile strength and electrochemical performance, primarily ascribed to the low film porosity, abundant inter-particle connection by the binder, comprehensive carbon coverage, and efficient percolation of the conductive pathway. Notably, a full cell incorporated with a high loading (5.2 mAh cm −2 ) and high active material ratio (96.5 wt.%) L-NCO film electrode demonstrates promising cycling stability and rate capability. Furthermore, these results provide valuable insights regarding the design and fabrication of dry-processed electrodes for future energy storage applications.

25 ENERGY STORAGE↗

Bioinspired Dry‐Steam Superinsulation Straw Foam

Abstract Cellulosic materials offer sustainable advantages for building energy conservation. However, their development has been hindered by reduced thermal performance, often caused by structural collapse during the transition from solution to solid. Inspired by natural goose down, a bio‐based, lightweight insulation foam derived from agricultural waste straw is presented. Through in situ synthesis, bio‐silica fibers with branched structures capable of supporting hollow silica microspheres are fabricated. After steam‐mediated processing, the resulting foam exhibit low density (95 mg cm − 3 ), high porosity (95.5%), low thermal conductivity (0.03 ± 0.003 W mK −1 ), and a cyclic compressive strength of 90 kPa at 50% strain. Owing to the synergistic microstructure formed by branched bio‐fibers and hollow silica spheres, the bio‐silica foam exhibit outstanding thermal insulation performance relative to other bio‐based foams prepared by ambient drying. A passivated insulation panel is further developed by incorporating this material as the core component, achieving a thermal conductivity of 0.0275 W mk −1 and flexural strength of 6.85 MPa. The panel demonstrated durability with stable thermal performance throughout a 60‐day outdoor test. Moreover, the bio‐silica foam shows a carbon footprint of 7.50 kgCO₂ kg −1 at 70.2 wt.% silica, highlighting its promise as a sustainable insulation solution for green buildings.

Chemistry↗

Through‐Plane Conductive Hydrophobic Electrodes for CO 2 Electrolysis to Ethylene

Copper catalyst gas diffusion electrodes (GDEs) have demonstrated unique electrochemical selectivity converting CO 2 to C 2 -hydrocarbons such as ethylene and ethanol but have been challenged by their hydrophobic chemical stability and internal electrical resistance leading to low energy efficiency. Carbon-supported GDEs have low electrical resistance but lack sufficient stability at industrially relevant current densities. While polymer-supported GDEs have improved hydrophobicity, they also display high in-plane electrical resistance, particularly at industrial scales. Here, in this work, we demonstrate a composite gas diffusion layer that combines hydrophobic porous polymers with an electrically conductive backbone addressing these core gas diffusion electrode (GDE) scaling challenges. We investigate the material properties of standalone porous perfluoropolyether (PFPE) polymers, including porosity and surface morphology, under varying processing conditions and then incorporate these polymers into a porous copper foam. This composite enhances the mechanical rigidity necessary for cell assembly and provides a through-plane electrical conduction path to reduce electrical resistive losses. This enhanced PFPE composite GDE displays efficient CO 2 reduction, achieving 15% ethylene energy efficiency at 100 cm 2 . These findings contribute to the development of advanced catalyst materials and electrode architectures and promote scalable strategies for electrochemical conversion of CO 2 into high-value carbon products.

Chemistry↗

Elucidating Pore Network Evolution in Laboratory‐ and Shaft‐Furnace Hydrogen‐Reduced Iron Pellets Using Nanotomographic Characterization

Direct reduced iron (DRI) is an increasingly important feedstock for modern steelmaking. Fundamental research into DRI properties is limited by the discrepancy between the behavior of industrially produced pellets and laboratory‐produced pellets, leading to nongeneralizable conclusions from laboratory work. Here, in this study, a detailed nano‐computed tomographic characterization of ore pellets, hydrogen DRI reduced in a pilot‐scale shaft furnace, and laboratory‐reduced DRI is presented to better understand the microstructurally influenced property differences between the two. The shaft‐furnace‐reduced pellets show lower overall porosity but larger average pore volume thickness and solid volume thickness than the laboratory‐reduced pellets. This effect is attributed to increased sintering behavior in the shaft furnace case. All pellet types show almost entirely connected pore volumes. The tortuosity of the pores is shown to increase with a degree of reduction, though the shaft furnace pellets show lower tortuosity than the laboratory‐reduced pellets. Again, this difference is attributed to the larger pore volume thickness for shaft‐furnace‐reduced pellets.

36 MATERIALS SCIENCE↗

Mechanical and poroelastic behavior of porous tuff under drained and undrained conditions

A series of drained and undrained water-saturated constant mean-stress tests were performed to investigate the strength, elasticity, and poroelastic response of a water-saturated high porosity nonwelded tuff. Drained strengths are found to increase with increasing effective confining pressures. Elastic moduli increase with increasing mean stress. Undrained strengths are small due to development of high pore pressures that generate low effective confining pressures. Skempton’s values are pressure dependent and appear to reflect the onset of inelastic deformation. Permeabilities decrease after deformation from ~ 10 –14 to ~ 10 –16 m 2 and are a function of the applied confining pressure. Deformation is dominated by pore collapse, compaction, and intense microfracturing, with the undrained tests favoring microfracture-dominant deformation and the drained tests favoring compaction-dominant deformation. These property determinations and observations are used to develop/parameterize physics-based models for underground explosives testing.

58 GEOSCIENCES↗

Full-Strength Additive Manufacturing of Pure Aluminum Alloy 7075 Using Liquid Metal Jet Printing

Additive manufacturing (AM) of high-strength aluminum alloys can produce high-performance aerospace and biomedical parts with unique geometries and functions. However, many high-performance alloy systems such as AA 7075 pose challenges during AM due to thermal cycles that cause hot cracking, limiting AM to casting-friendly alloys. Stock AA 7075 alloy poses additional challenges due to the excessive growth of insoluble precipitates during casting and needs to be thermomechanically processed to obtain acceptable mechanical properties. Here, this work uses liquid metal jet printing to produce high-resolution pure AA 7075 parts at high strength (593 MPa) and ductility (10 pct), surpassing the specific strength of any type of steel. The parts are printed by depositing fine droplets on a high-temperature substrate that reduces cooling rates, preventing hot cracking. The results show that fully dense, crack-free parts can only be printed at substrate temperatures of 500 °C with a cooling rate threshold of < 2000 K/s to prevent cracking and < 500 K/s to eliminate porosity. The tensile strength, microhardness, and ductility of the parts matched or were beyond the wrought alloy specifications after heat treatment, possibly due to high solidification rates that produce finer insoluble precipitates. Our results indicate that many challenging high-performance alloy systems can now be 3D printed based on the critical thresholds for cooling rates using any AM method that can satisfy these conditions.

36 MATERIALS SCIENCE↗

Micro-cold Spray Deposition of YSZ Films from Ultrafine Powders Using a Pressure Relief Channel Nozzle

Abstract The use of ultrafine powders in the micro-cold spray (MCS) process, also referred to as the aerosol deposition method, typically results in porous and/or poorly adhering films because the particles do not impact at a high enough velocity for sufficient plastic deformation and interparticle bonding to occur. Under typical operating conditions, particles < 100 nm accelerate to high velocities but then are slowed by the stagnant gas in the bow shock that forms just upstream of the substrate. Using larger particles reduces particle slowing, but large particles can cause erosion of the film at high impact velocity, decreasing deposition efficiency. In this study, a pressure relief channel nozzle using helium as a carrier gas is proposed such that high-velocity deposition of yttria-stabilized zirconia particles as small as 10 nm in diameter is possible. This is well below the size range of powders previously used for MCS. The proposed nozzle design increases impact velocities for 10, 20, and 50 nm particles by ~ 880, 560, and 160 m/s, respectively, when compared to a conventional nozzle. Experimental deposition of ultrafine 8YSZ powder shows that the pressure relief channel nozzle results in lower porosity and more uniform deposits, with a ∼ 186% increase in deposition efficiency.

Materials Science↗

Creep Deformation and Damage Mechanisms in an Advanced High-Temperature Additively Manufactured Nickel-Base Superalloy

Abstract This research investigates the processing–structure–properties–performance relationship in a novel nickel-base superalloy, ABD ® -900AM, designed for extreme environments. Specifically tailored for additive manufacturing (AM), ABD ® -900AM maintains mechanical integrity at high temperatures and is comparable to other nickel-based superalloys with a 30–40% gamma-prime volume fraction. A comprehensive study was conducted using laser-beam powder bed fusion and electron-beam powder bed fusion methods. Factors such as heat treatment, porosity, build orientation, and hot isostatic pressing were evaluated to understand their effects on microstructure and mechanical performance. Microstructural characterization revealed significant differences in grain size and orientation across build processes and heat treatments. High-temperature mechanical testing indicated that grain size, heat treatment, and orientation significantly influence creep behavior. A super-solvus heat treatment led to recrystallization and grain growth, significantly improving creep properties compared to a near-solvus heat treatment. Various creep mechanisms were identified across different conditions, and creep rupture models were developed for each build process. Post-test microstructural analysis showed grain boundary damage, with differences in creep cavitation morphology under varying stress conditions. It was shown that MC carbides grow at the expense of gamma-prime near grain boundaries, leading to precipitate-free zones in specimens tested at higher temperatures. This study fills a significant gap in fundamental research by offering a deeper insight into the high-temperature mechanical behavior of additively manufactured nickel-base superalloys. It also explores critical research questions regarding the role of carbides and the significance of heat treatment. The insights gained enhance confidence in the industry adoption of ABD ® -900AM and similar alloys for high-temperature applications, bridging the knowledge gap and supporting the development of reliable AM processes for extreme environments.

Bridges, Alex (ORCID:000000030338759X)↗

Effects of an External Magnetic Field on Keyhole Mode Laser Melting of 316 Stainless Steel

Keyhole-mode laser melting is an efficient method for joining or cutting large, thick components, but controlling keyhole depth and fluctuations has remained challenging. Applying an external magnetic field can control melt pool flows and indirectly influence keyhole morphology and dynamics. The induced Lorentz force, comprising Seebeck and damping components, plays a crucial role in the melt pool dynamics, depending on temperature gradient, flow rates, and magnetic field orientation and magnitude. This research investigates the effects of an external magnetic field on keyhole behavior during laser spot melting of 316 stainless steel using synchronized high-speed synchrotron X-ray and thermal imaging. Findings revealed that a longitudinal magnetic field (120 mT) increased keyhole depth but exacerbated lateral fluctuations, resulted in a 20% increase in the melt pool temperature gradient and a 27% decrease in cooling rate. Conversely, a transverse magnetic field (760 mT) reduced keyhole depth and improved porosity formation. The findings suggest that a decrease in keyhole depth correlates with a decrease in fluctuations, and vice versa. These insights enhance understanding of external magnetic fields’ impact on laser melting, with implications for improving part quality.

Alamdari, Aslan Bafahm [The Ohio State Univ., Colu↗

A Review of the Influence of Processing Parameters on ODS Steels Produced via Additive Manufacturing Techniques

Abstract This paper reviews current observations regarding processing conditions for oxide dispersion-strengthened steels consolidated through additive manufacturing techniques. Variations in ODS steels observed across process parameters include changes in grain size, grain texture, oxide size, density of oxides, porosity, melt pool characteristics, and mechanical properties. These properties were then compared across techniques to understand which techniques and processing conditions lead to the highest strength, ductility, and oxide density. Current literature suggests that a mix of grain types, in the form of either morphology or phase, can significantly increase the strength of printed ODS steels. Meanwhile, the most ductile samples, regardless of consolidation technique or matrix material, were made from feedstock with oxide additions located on the powder surface. Reported grain and oxide sizes were plotted against the ratio of laser power to scan speed, volumetric energy density, and normalized enthalpy. No strong correlation between these values and microstructural features was observed. The plots that were made suggest that a larger data set, more in-depth representative equations, and more defined material properties as a function of specific feedstock used are necessary to determine a value that can be correlated to the printed ODS steel microstructure.

deJong, Matthew↗

Understanding poromechanical response of a biogenic coalbed methane reservoir

Abstract Biogenic coalbed methane (BCBM) reservoirs aim to produce methane from in situ coal deposits following microbial conversion of coal. Success of BCBM reservoirs requires economic methane production within an acceptable timeframe. The work reported here quantifies the findings of previously published qualitative work, where it was found that bioconversion induces strains in the pore, matrix and bulk scales. Using imaging and dynamic strain monitoring techniques, the bioconversion induced strain is quantified here. To understand the effect of these strains from a reservoir geomechanics perspective, a corresponding poromechanical model is developed. Furthermore, findings of imaging experiments are validated using core-flooding flow experiments. Finally, expected field-scale behavior of the permeability response of a BCBM operation is modeled and analyzed. The results of the study indicated that, for Illinois coals, bioconversion induced strains result in a decrease in fracture porosity, resulting in a detrimental permeability drop in excess of 60% during bioconversion, which festers itself exponentially throughout its producing life. Results indicate that reservoirs with high initial permeability that will support higher Darcian flowrates, would be better suited for coal bioconversion, thereby providing a site-selection criteria for BCBM operations.

Pandey, Rohit (ORCID:0009000415483436)↗

Biochar–polymer composites for 3D printing: a review

Biochar, a bio-based co-product of biofuel production via thermochemical conversion, holds potential as a filler for polymer composites to reduce costs, improve thermomechanical properties, and aid in environmental remediation. 3D-printed biochar composites have received growing interest over the past few years but have experienced difficulties such as poor layer adhesion and nozzle clogging. Currently, no literature review examines 3D-printed biochar composites and related biochar properties in-depth. This work summarizes and discusses recent studies on 3D-printed polymer and biochar composites and examines their mechanical, thermal, and additional properties that result from each study. Technical challenges in printability, such as nozzle clogging from particle size and biochar aggregation, are also discussed. Furthermore, this work discusses the variability of biochar properties resulting from the pyrolysis conditions and feedstock choice in relation to potential 3D printing outcomes. In particular, several studies reported that high lignin feedstocks could be candidates for 3D printing. The post-processing approaches of the biochar via physical and chemical methods are also introduced. Ball milling appears to hold the most promise for physical treatments due to its tunability of particle size, surface area, and functional groups, while chemical treatments with acids or alkalis are used to tailor biochar porosity and wettability. Overall, it was determined that future research needs to be done relating biochar production and post-processing methods to resulting 3D printing parameters as the number of studies is limited.

Day, Rachel [Auburn University, Auburn, AL]↗

Electrochemical grand potential-based phase-field simulation of electric field-assisted sintering

Here, an electrochemical grand potential functional was proposed to describe the sintering of an ionic ceramic green body. The resultant phase-field description enables simulation of the consolidation of an arbitrary number of granular particles and their interactions with the surrounding void phase. The model includes the effects of charged vacancies and the associated interactions between internal and applied electric fields. Defect segregation to grain boundaries is also accounted for, as well as enhanced interfacial defect mobilities. The model was parameterized for Y 2 O 3 . Simulations of two-particle systems showed that the applied electric field had an increasingly important impact on neck growth as particle size increased. A sudden rapid increase in temperature occurred for larger field strengths, which has been reported to be correlated to the onset of a flash event in flash sintering. Simulations of many particles showed that internal heat generation by Joule heating was localized at particle–particle contacts (grain boundaries), even though their conductivities were lower than nearby internal particle-void interfaces. A percolative path for ionic charge across the green body and the ceramic sintered solid was thus defined, accelerating the Joule heating process as the porosity of the green body is removed.

36 MATERIALS SCIENCE↗

Scaling microstructural processes in the sintering of ionic ceramics

A multi-scale framework, combining a multiphase field formulation and large deformation mechanics, was developed as a stepping stone to perform the data analytics of the microstructural level kinetics of a sintering solid. Relevant microstructural information from this framework, such as grain, stress, and porosity statistics, was scaled up to describe the macroscopic level sintering kinetics. Here, the developed formulation was applied to describe the electric field assisted sintering of Y 2 O 3 . Microstructural inhomogeneities in a multi-granular solid result in the formation of a field of compressive stress networks, which interleave with low compression and weakly tensile regions, defining a scaffolding for sintering concentration regions to develop. A Poisson effect-induced lateral stress network is also naturally self-induced as a result of the mechanical constraints imposed by the sintering apparatus. For long sintering times, localized shear stresses enhancing mass flow along grain boundaries and internal surfaces develop. Three-sided pores are removed by either vacancy transport to the surrounding pores, or move towards the external surfaces through grain boundary diffusion. Four- and higher order-sided pores stabilize because an equal amount of vacancies are gained and lost through the connecting grain boundaries. Grain dewetting contributes to pore coalescence, suggesting that pore kinetics and grain growth are coupled and should be analyzed in concert. The combined sintering and grain growth kinetics define six regimes of sintering behavior: (1) T, the transient regime; (2) E$_Υ$, the surface energy dominated, early sintering regime, where the grain growth exponent, p = 1, and the stress concentration factor, $f$ ~ $1/\hat{ρ}^{4.6}$; (3) E S , the stress dominated, early sintering regime, where p = 1 and $f$ ~ $1/\hat{ρ}^{4}$; (4) I$_Υ$, the surface energy dominated, intermediate sintering regime, where p = 2 and $f$ ~ $1/\hat{ρ}^{4.6}$; (5) I S , the stress dominated, intermediate sintering regime, where p = 2 and $f$ ~ $1/\hat{ρ}^{4}$; and (6) L, the late sintering regime, where p = 3 and $f$ ~ 1. At the macroscopic level, the rapid densification and suppression of grain growth observed in the electric field assisted sintering process is a consequence of the compounding effects of the underlying stress-, transport-, and interfacial-energy-induced energy minimization kinetics, as predicted by the multi-scale framework.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗