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At least 217 records · Page 12

Electrolyte Design for Fast‐Charging Lithium‐Based Batteries

Fast charging is essential for the widespread adoption of lithium (Li)-ion batteries, but it is fundamentally limited by sluggish interfacial kinetics, Li plating, and electrolyte instability at high current densities. Over the past decade, electrolyte engineering has emerged as a key strategy to address these challenges. This review summarizes the development of fast-charging electrolytes over the past ten years and outlines a design framework. Electrolyte formulations are first deconstructed into their main components—solvents, salts, and functional additives—and representative strategies for tuning solvation structure and interphase chemistry are discussed to suppress Li plating and improve interfacial kinetics. The discussion then extends to advanced electrolyte systems, particularly localized high-concentration electrolytes (LHCEs), and their compatibility with different anode chemistries. Advanced characterization techniques are also summarized and categorized based on destructiveness, spatial and temporal resolution, quantitative analysis, and the chemical species or processes probed across multiple length scales. Recent progress in AI-enabled electrolyte discovery and battery management system (BMS) strategies for optimized fast-charging protocols is further highlighted. Finally, perspectives are presented on translating electrolyte innovations from academic research to practical applications, with emphasis on cell format, realistic operating conditions, and manufacturability.

25 ENERGY STORAGE↗

Finding a needle in a haystack: quantitative HERFD-XRF imaging and HERFD-XANES characterization of trace platinum in gold solidi from the Late Roman and Byzantine Empires

High-Energy Resolution Fluorescence Detection X-Ray Fluorescence (HERFD-XRF) imaging and HERFD X-ray Absorption Near Edge Structure (XANES) spectroscopy are used to quantify and characterize trace platinum (Pt) in gold solidi from the Late Roman and Byzantine Empires. Historically, the elemental analysis of coins has been pivotal in distinguishing authentic artifacts from forgeries, elucidating minting practices, and understanding economic shifts. Notably, a new gold source with high platinum content appeared in the fourth century CE, transforming the Roman economy. Traditional methods struggled to detect platinum due to the overwhelming gold matrix. Here, this study demonstrates the effectiveness of HERFD techniques in resolving this challenge. Three gold solidi, minted between 654 and 659 CE, were analyzed alongside reference gold materials with known Pt concentrations. The HERFD-XRF imaging revealed spatial distributions of platinum, highlighting non-uniformities within the coins. Additionally, HERFD-XANES spectroscopy identified the oxidation states and chemical speciation of platinum. Results demonstrate that platinum in the solidi primarily exists as metallic Pt, with some surface oxidation. The findings align with previous measurements but reveal higher Pt concentrations and significant inhomogeneities. This research confirms the reliability of HERFD methods for quantifying trace elements and provides new insights into the raw material sources and minting techniques of ancient gold coins. The non-destructive nature of this approach allows for extensive analyses, offering valuable data for historical, economic, and archaeological studies. This innovative application of HERFD-XRF imaging and XANES in cultural heritage research underscores the potential for detailed material characterization and conservation, enhancing our understanding of ancient economies and trade patterns.

Van Loon, Lisa L.↗

New Instrumentation for Phase Partitioning

Cells and molecules can be purified by partitioning between the two immiscible liquid phases formed by aqueous solutions of poly/ethylene glycol and dextran. Such purification can be more selective, higher yielding, and less destructive to sensitive biological materials than other available techniques. Earth's gravitational field is a hindering factor as it causes sedimentation of particles to be purified and shear-induced particle randomization. The present proposal is directed toward developing new instrumentation for performing phase partitioning both on Earth and in microgravity.

Harris, J. M.↗

Identification and characterization of extraterrestrial non-chondritic interplanetary dust

Interplanetary dust particles (IDPs) are among the most pristine and primitive extraterrestrial materials available for direct study. Most of the stratospheric particles selected for study from the JSC Curatorial Collection were chondritic in composition (major element abundances within a factor of two of chondritic meteorites) because this composition virtually ensures that the particle is from an extraterrestrial source. It is likely that some of the most interesting classes of IDP's have not been recognized simply because they are not chondritic or do not fit established criteria for extraterrestrial origin. Indeed, mass spectroscopy data from the Giotto Flyby of comet Halley indicate that a substantial fraction of the dust is in the submicron size range and that a majority of these particles contain C, H, O, and/or N as major elements. The preponderance of CHON particles in the coma of Halley implies that similar particles may exist in the JSC stratospheric dust collection. However, the JSC collection also contains a variety of stratospheric contaminants from terrestrial sources which have these same characteristics. Because established criteria for extraterrestrial origin may not apply to such particles in individual cases, and integrated approach is required in which a variety of analysis techniques are applied to the same particle. Non-chondritic IDP's, like their chondritic counterparts, can be used to elucidate pre- and early solar system processes and conditions. The study of non-chondritic IDP's may additionally yield unique information which bears on the nature of cometary bodies and the processing of carbonaceous and other low atomic number materials. A suite of complementary techniques, including Low Voltage Scanning Electron Microscopy (LVSEM), Energy-Dispersive X-ray Microanalysis (EDX), Secondary Ion Mass Spectrometry (SIMS) isotope-ratio imaging and Analytical Electron Microscopy (AEM), were utilized to accomplish the following two objectives: (1) to develop criteria for the unequivocal identification of extraterrestrial non-chondritic IDP's; and (2) to infer IDP parent body, solar nebula, and pre-solar conditions through the study of phases, textures, and components contained within non-chondritic IDP's. The general approach taken is designed to maximize the total information obtained from each particle. Techniques will be applied in order from least destructive to most destructive.

Blake, D. F.↗

Creep and Environmental Durability of EBC/CMCs Under Imposed Thermal Gradient Conditions

Interest in SiC fiber-reinforced SiC ceramic matrix composite (CMC) environmental barrier coating (EBC) systems for use in high temperature structural applications has prompted the need for characterization of material strength and creep performance under complex aerospace turbine engine environments. Stress-rupture tests have been performed on SiC/SiC composites systems, with varying fiber types and coating schemes to demonstrate material behavior under isothermal conditions. Further testing was conducted under exposure to thermal stress gradients to determine the effect on creep resistance and material durability. In order to understand the associated damage mechanisms, emphasis is placed on experimental techniques as well as implementation of non-destructive evaluation; including electrical resistivity monitoring. The influence of environmental and loading conditions on life-limiting material properties is shown.

Appleby, Matthew↗

Environmental Durability and Stress Rupture of EBC/CMCs

This research focuses on the strength and creep performance of SiC fiber-reinforced SiC ceramic matrix composite (CMC) environmental barrier coating (EBC) systems under complex simulated engine environments. Tensile-strength and stress-rupture testing was conducted to illustrate the material properties under isothermal and thermal gradient conditions. To determine material durability, further testing was conducted under exposure to thermal cycling, thermal gradients and simulated combustion environments. Emphasis is placed on experimental techniques as well as implementation of non-destructive evaluation, including modal acoustic emission and electrical resistivity monitoring, to characterize strength degradation and damage mechanisms. Currently, little is known about the behavior of EBC-CMCs under these conditions; consequently, this work will prove invaluable in the development of structural components for use in high temperature applications.

Appleby, Matthew↗

Simulated Lunar Surface Hydration Measurements using Multispectral Lidar at 3 µm

Accurately measuring the variability of spectroscopic signatures of hydration (H2O + OH) on the illuminated lunar surface at 3 µm as a function of latitude, lunar time of day, and composition is crucial to determining the generation and destruction mechanisms of OH species and understanding the global water cycle. A prime complication in analysis of the spectroscopic feature is the accurate removal of thermal emission, which can modify or even eliminate the hydration feature depending on the data processing methods used and assumptions made. An orbital multispectral lidar, with laser illumination at key diagnostic wavelengths, would provide uniform, zero-phase geometry, complete latitude and time of day coverage from a circular polar orbit, and is agnostic to the thermal state of the surface. We have performed measurement simulations of a four-wavelength multispectral lidar using spectral mixtures of hydrated mid-ocean ridge basalt (MORB) glasses and lunar regolith endmembers to assess the lidar performance in measuring hydration signatures on the lunar surface. Our results show a feasible system with wavelengths at 1.5 µm, 2.65 µm, 2.8 µm, and 3.1 µm can measure lunar hydration with a precision of 52 ppm (1σ) or better. These results, combined with the uniform measurement capabilities of multispectral lidar make it a valuable spectroscopic technique for elucidating mechanisms of OH/H2O generation, migration, and destruction.

D. R. Cremons↗

Multimodal Defect Imaging of Pure Tungsten Components Fabricated via Electron Beam Powder Bed Fusion

The utilization of additive manufacturing (AM) techniques for refractory materials in high-temperature environments has significantly expanded because of the ability to fabricate geometrically complex components. Electron beam powder bed fusion (EB-PBF), which provides lower residual stress, a cleaner vacuum environment, and better efficiency for high melting point, is one of the best-suited AM methods to produce advanced refractory components. However, the property variation attributed to the heterogeneous microstructure and process-induced defects has hindered the widespread adoption of EB-PBF-produced material like tungsten. While numerous in-situ monitoring and defect detection methods have been demonstrated for EB-PBF, a workflow that compares and evaluates process-induced abnormalities from different imaging perspectives is still limited. This study examines a feature-embedded tungsten component manufactured via the EB-PBF process to demonstrate the defect detection capabilities of a multimodal defect imaging workflow. The predefined and process-induced defects are evaluated by harnessing various imaging techniques, including in-situ electron imaging, layerwise near-infrared (NIR) imaging, post-build high-energy x-ray computed tomography (CT), and conventional destructive metallography. The results highlight the strengths and limitations of distinctive defect imaging techniques concerning specific defect types, sizes, and conditions. It was found that electron imaging can provide more abnormal detection capabilities while maintaining a higher measuring accuracy, against the conventional metallography in this case study, compared with NIR and CT imaging techniques.

36 MATERIALS SCIENCE↗

Determining the Oxygen Fugacity of Lunar Pyroclastic Glasses Using Vanadium Valence - An Update

We have been developing an oxygen barometer based on the valence state of V (V(2+), V(3+), V(4+), and V(5+)) in solar system basaltic glasses. The V valence is determined by synchrotron micro x-ray absorption near edge structure (XANES), which uses x-ray absorption associated with core-electronic transitions (absorption edges) to reveal a pre-edge peak whose intensity is directly proportional to the valence state of an element. XANES has advantages over other techniques that determine elemental valence because measurements can be made non-destructively in air and in situ on conventional thin sections at a micrometer spatial resolution with elemental sensitivities of approx. 100 ppm. Recent results show that fO2 values derived from the V valence technique are consistent with fO2 estimates determined by other techniques for materials that crystallized above the IW buffer. The fO2's determined by V valence (IW-3.8 to IW-2) for the lunar pyroclastic glasses, however, are on the order of 1 to 2.8 log units below previous estimates. Furthermore, the calculated fO2's decrease with increasing TiO2 contents from the A17 VLT to the A17 Orange glasses. In order to investigate these results further, we have synthesized lunar green and orange glasses and examined them by XANES.

Karner, J. M.↗

Agile Allocation in the Tundra: A Single Growing Season of Warming Increases Nutrient Availability While Decreasing Fine-Root Length

The majority of plant biomass is located belowground in Arctic ecosystems and plant roots are responsible for the uptake of the nutrients that constrain plant growth in these infertile ecosystems. Despite performing a crucial role connecting primary producers to the soil, roots are relatively understudied in the Arctic and their functional response to a rapidly warming and increasingly variable climate is unknown. Here, we assessed whether one growing season with elevated temperatures would have an impact on nutrient uptake and allocation by applying a warming technique that increased daily air temperatures by 3.2 °C. Destructive sampling was performed at the peak of the growing season to quantify biomass pools of carbon (C) and nitrogen (N), root traits, and uptake of a 15 N tracer ( 15 NH 4 + ) for the dominant plant species, Arctagrostis latifolia. We found that soil nutrient availability increased with short-term warming, but A. latifolia NH 4 + uptake remained unchanged. Fine-root length density and root biomass within the soil profile, however, were both reduced by warming. N allocation patterns across plant tissues were also altered by warming. NH 4 + uptake was best fit with a logistic model that captured the spatial relationship between roots and soil (NH 4 + uptake expressed per length fine root and NH 4 + availability expressed per unit soil volume) rather than a traditional Michaelis–Menten model. Our results indicate that short-term experimental warming can shift plant–soil interactions, suggesting that the tundra’s belowground response to elevated temperatures may be more dynamic than previously recognized.

15N tracer↗

Sterilization of space hardware.

Discussion of various techniques of sterilization of space flight hardware using either destructive heating or the action of chemicals. Factors considered in the dry-heat destruction of microorganisms include the effects of microbial water content, temperature, the physicochemical properties of the microorganism and adjacent support, and nature of the surrounding gas atmosphere. Dry-heat destruction rates of microorganisms on the surface, between mated surface areas, or buried in the solid material of space vehicle hardware are reviewed, along with alternative dry-heat sterilization cycles, thermodynamic considerations, and considerations of final sterilization-process design. Discussed sterilization chemicals include ethylene oxide, formaldehyde, methyl bromide, dimethyl sulfoxide, peracetic acid, and beta-propiolactone.

Pflug, I. J.↗

Fault Injection Techniques and Tools

Dependability evaluation involves the study of failures and errors. The destructive nature of a crash and long error latency make it difficult to identify the causes of failures in the operational environment. It is particularly hard to recreate a failure scenario for a large, complex system. To identify and understand potential failures, we use an experiment-based approach for studying the dependability of a system. Such an approach is applied not only during the conception and design phases, but also during the prototype and operational phases. To take an experiment-based approach, we must first understand a system's architecture, structure, and behavior. Specifically, we need to know its tolerance for faults and failures, including its built-in detection and recovery mechanisms, and we need specific instruments and tools to inject faults, create failures or errors, and monitor their effects.

Hsueh, Mei-Chen↗

NASA Glenn/AADC-Rolls Royce Collaborated to Measure Erosion Resistance on Coated Polymer Matrix Composites

Polymer matrix composites (PMCs) are increasingly used in aerospace and automotive applications because of their light weight and high strength-to-weight ratio relative to metals. However, a major drawback of PMCs is poor abrasion resistance, which restricts their use, especially at high temperatures. Simply applying a hard coating on PMCs to improve abrasion and erosion resistance is not effective since coating durability is short lived (ref. 1). Generally, PMCs have higher coefficients of thermal expansion than metallic or ceramic coatings have, and coating adhesion suffers because of poor interfacial adhesion strength. One technique commonly used to improve coating adhesion or durability is the use of bond coats that are interleaved between a coating and a substrate with vastly different coefficients of thermal expansion. An example of this remedy is the use of bondcoats for ceramic thermal barrier coatings on metallic turbine components (ref. 2). Prior collaborative research between the NASA Glenn Research Center and the Allison Advanced Development Company (AADC) demonstrated that bond coats sandwiched between PMCs and high-quality plasma-sprayed, erosion-resistant coatings substantially improved the erosion resistance of PMCs (ref. 3). One unresolved problem in this earlier collaboration was that there was no easy, accurate way to measure the coating erosion wear scar. Coating wear was determined by both profilometry and optical microscopy. Both techniques are time consuming. Wear measurement by optical microscopy requires sample destruction and does not provide a comprehensive measure of the entire wear volume. An even more subtle, yet critical, problem is that these erosion coatings contain two or more materials with different densities. Therefore, simply measuring specimen mass loss before and after erosion will not provide an accurate gauge for coating and/or substrate volume loss. By using a noncontact technique called scanning optical interferometry, which was recently developed at Glenn, researchers can accurately determine the wear performance of erosion-coated PMCs while preserving the sample. An example of this interferometry technique is shown in the preceding figure for an erosion-coated inlet guide vane from a Rolls Royce AE3007 regional gas turbine jet engine. Erosion was conducted with coated and uncoated PMC vanes, with the abrasive material moving at a velocity of 229 m/s at impingement angles of 20 and 90 degrees. The coatings for PMCs remarkably reduced the erosion volume loss by a factor of approximately 10. Currently, several erosion coatings for PMCs are being compared and downselected for engine testing at Rolls Royce.

Miyoshi, Kazuhisa↗

New Techniques in Characterization of Ferroelectric Materials

Two new techniques have been developed to characterize Pb(Mg1/3Nb2/3)O3-PbTiO3 (PMN-PT) based ferroelectric single crystals: (i) electro-thermal imaging, and (ii) single crystal x-ray diffraction in the transmission mode. (i) Electro-thermal imaging is a remote sensing technique that can detect the polarization direction and poling state of a whole crystal slice. This imaging technique utilizes an IR camera to determine the field induced temperature change and does not require any special or destructive sample preparation. In the resulting images it is possible to distinguish regions of 180 deg domains. This powerful technique can be used remotely during poling to determine the poling state of the crystal to avoid over-poling that can result in inferior properties and/or cracking of the crystals. Electro-thermal imaging produced the first direct observations of polarization rotation. Under bipolar field, the domains near the corners were the first to switch direction. As the field increased above the coercive field, domains at the center part of the crystals switched direction. (ii) X-ray diffraction in the transmission mode has long been used in structure determination of organic crystals and proteins; however, it is not used much to characterize inorganic systems. 0.7Pb(Mg1/3Nb2/3)O3-0.3PbTiO3 single crystals were examined by this XRD technique for the first time, and a never-before-seen super-lattice was revealed with a doubling of the unit cell in all three directions, giving a cell volume eight times that of a traditional perovskite unit cell. The significance of the super-lattice peaks increased with poling, indicating a structural contribution to ordering. Lack of such observations by electron diffraction in the transmission electron microscope examinations suggests the presence of a bulk effect.

Sehirlioglu, Alp↗

Quantitative non-destructive evaluation of porous composite materials based on ultrasonic wave propagation

Two complementary ultrasonic techniques for characterizing porosity in fiber-reinforced composite laminates are evaluated. Five uniaxial graphite-fiber/epoxy-matrix composites having a range of 1 to 8 percent volume fraction of solid glass inclusions to model porosity were investigated. In one technique, signal loss was measured in transmission mode and slope of attenuation, obtained from the first order coefficient of a two-parameter polynomial fit about the center frequency of the useful bandwidth, was used as the ultrasonic parameter to characterize the porosity. The results of these transmission mode measurements displayed a good correlation between the volume fraction of porosity and the slope of attenuation. Integrated polar backscatter was used as a second ultrasonic parameter for the characterization of the porosity in these samples. A single transducer insonified the samples and measured the resulting backscatter at a polar angle of 30 deg with respect to the normal of the sample surface with the azimuthal angles centered at 0 deg with respect to the fiber orientation (i.e., along the fibers). Integrated polar backscatter also displayed good correlation with the volume fraction of porosity.

Miller, James G.↗

Wire Crimp Termination Verification Using Ultrasonic Inspection

The development of a new ultrasonic measurement technique to quantitatively assess wire crimp terminations is discussed. The amplitude change of a compressional ultrasonic wave propagating through the junction of a crimp termination and wire is shown to correlate with the results of a destructive pull test, which is a standard for assessing crimp wire junction quality. Various crimp junction pathologies such as undercrimping, missing wire strands, incomplete wire insertion, partial insulation removal, and incorrect wire gauge are ultrasonically tested, and their results are correlated with pull tests. Results show that the nondestructive ultrasonic measurement technique consistently (as evidenced with destructive testing) predicts good crimps when ultrasonic transmission is above a certain threshold amplitude level. A physics-based model, solved by finite element analysis, describes the compressional ultrasonic wave propagation through the junction during the crimping process. This model is in agreement within 6% of the ultrasonic measurements. A prototype instrument for applying this technique while wire crimps are installed is also presented. The instrument is based on a two-jaw type crimp tool suitable for butt-splice type connections. Finally, an approach for application to multipin indenter type crimps will be discussed.

Perey, Daniel F.↗

Spot size measurement of a deuterium–tritium dense plasma focus using neutron radiography

Neutron radiography is a technique uniquely suited to applications in nuclear diagnostics, non-destructive testing, and subcritical experiments. The spatial resolution of neutron radiographs is degraded by optical blur in the imaging system and the neutron source size, where the ideal source is point-like to optimize the point-spread function. A potential neutron source for radiography is the dense plasma focus (DPF), a coaxial Z-pinch that produces thermonuclear and beam-target neutrons. To assess if the source size is suitable for radiography, a neutron imaging system was used to measure the source size of the 4 MA Sodium DPF at the Nevada National Security Site operating with deuterium–tritium gas-fill. The source size was measured using the edge-spread function of tungsten objects, each having a rolled (convex) edge. The spot size was found to be 7–12 mm full-width at half-max (FWHM) assuming a Gaussian source, though comparison is presented for Lorentzian and Bennett distributions. The average FWHM was found to be 8.6 ± 1.2 mm vertically and 10.8 ± 1.2 mm horizontally with respect to the image plane, averaging over varied edges and alignments. The results were sensitive to source alignment and edge metrology, which introduced notable uncertainties. These results are consistent with separate experimental measurements as well as magnetohydrodynamics simulations of this DPF, which suggest that neutron production can originate from pinches ∼5–7 mm off-axis. These results suggest that the DPF should be used for radiography at low magnification (M < 1) where spot size does not dominate spatial blur.

47 OTHER INSTRUMENTATION↗

Scanning microscopy in microcircuit failure analysis

A three-phase microcircuit failure analysis procedure is presented. In the first phase, the device is nondestructively tested and the data obtained is correlated with the circumstances surrounding the failure event. The device is then subjected to a limited nondestructive analysis dominated by optical and scanning electron microscopy (SEM). Knowing that microcircuits usually fail from manufacturing defects or misuse, the analyst looks for one of the probable mechanisms. The SEM has two special operating modes that provide unique data for nondestructive analysis: voltage contrast and conductive current. These are used with other SEM modes and surface analysis techniques to analyze complicated microcircuits. The last phase includes the destructive procedures. The end product of these analyses is a corrective action that will yield a highly reliable system.

Nicolas, D. P.↗