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At least 469 records · Page 26

Extended X-ray absorption fine structure of dynamically-compressed copper up to 1 terapascal

Abstract Large laser facilities have recently enabled material characterization at the pressures of Earth and Super-Earth cores. However, the temperature of the compressed materials has been largely unknown, or solely relied on models and simulations, due to lack of diagnostics under these challenging conditions. Here, we report on temperature, density, pressure, and local structure of copper determined from extended x-ray absorption fine structure and velocimetry up to 1 Terapascal. These results nearly double the highest pressure at which extended x-ray absorption fine structure has been reported in any material. In this work, the copper temperature is unexpectedly found to be much higher than predicted when adjacent to diamond layer(s), demonstrating the important influence of the sample environment on the thermal state of materials; this effect may introduce additional temperature uncertainties in some previous experiments using diamond and provides new guidance for future experimental design.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Dynamics Impact Tolerance of Shuttle RCC Leading Edge Panels Using LS-DYNA

This paper describes a research program conducted to enable accurate prediction of the impact tolerance of the shuttle Orbiter leading-edge wing panels using physics-based codes such as LS-DYNA, a nonlinear, explicit transient dynamic finite element code. The shuttle leading-edge panels are constructed of Reinforced-Carbon-Carbon (RCC) composite material, which is used because of its thermal properties to protect the shuttle during reentry into the Earth's atmosphere. Accurate predictions of impact damage from insulating foam and other debris strikes that occur during launch required materials characterization of expected debris, including strain-rate effects. First, analytical models of individual foam and RCC materials were validated. Next, analytical models of foam cylinders impacting 6- in. x 6-in. RCC flat plates were developed and validated. LS-DYNA pre-test models of the RCC flat plate specimens established the impact velocity of the test for three damage levels: no-detectable damage, non-destructive evaluation (NDE) detectable damage, or visible damage such as a through crack or hole. Finally, the threshold of impact damage for RCC on representative Orbiter wing panels was predicted for both a small through crack and for NDE-detectable damage.

Fasanella, Edwin L.↗

Dynamic Impact Tolerance of Shuttle RCC Leading Edge Panels using LS-DYNA

This paper describes a research program conducted to enable accurate prediction of the impact tolerance of the shuttle Orbiter leading-edge wing panels using 'physics-based- codes such as LS-DYNA, a nonlinear, explicit transient dynamic finite element code. The shuttle leading-edge panels are constructed of Reinforced-Carbon-Carbon (RCC) composite material, which issued because of its thermal properties to protect the shuttle during re-entry into the Earth's atmosphere. Accurate predictions of impact damage from insulating foam and other debris strikes that occur during launch required materials characterization of expected debris, including strain-rate effects. First, analytical models of individual foam and RCC materials were validated. Next, analytical models of individual foam cylinders impacting 6-in. x 6-in. RCC flat plates were developed and validated. LS-DYNA pre-test models of the RCC flat plate specimens established the impact velocity of the test for three damage levels: no-detectable damage, non-destructive evaluation (NDE) detectable damage, or visible damage such as a through crack or hole. Finally, the threshold of impact damage for RCC on representative Orbiter wing panels was predicted for both a small through crack and for NDE-detectable damage.

Fasanella, Edwin↗

Spectroscopic Behavior of Composite, Black Thermal Paint, Solar Cell, and Multi-layered Insulation Materials in a GEO Simulated Environment

Materials currently populating Earth orbital regimes can be distinguished by comparing remote observational data to that of optical material measurements obtained in the laboratory. Experimentation for this research primarily involved the acquisition of spectroscopic measurements on materials of interest to the telescopic observational community for enhanced space situational awareness. Common spacecraft materials worthy of preeminent analysis for this investigation include a carbon-carbon (c-c) matrix composite, various black thermal paints, a GPS solar cell and three different cover glass components. These materials were subjected to a simulated geosynchronous Earth orbit (GEO) space environment with the intent of observing material optical property behavior over quantitative exposure time. The aforementioned materials have been measured in their pristine and GEO simulated exposed conditions. A reflectance spectrometer and a bi-directional reflectance distribution function (BRDF) optical system have been operated to perform material characterization, optical property analysis, and to further compare such data to telescopic observational data acquired on equal materials.

Reyes, Jacqueline A.↗

NASA Research Center Contributions to Space Shuttle Return to Flight (SSRTF)

Contributions provided by the NASA Research Centers to key Space Shuttle return-to-flight milestones, with an emphasis on debris and Thermal Protection System (TPS) damage characterization, are described herein. Several CAIB recommendations and Space Shuttle Program directives deal with the mitigation of external tank foam insulation as a debris source, including material characterization as well as potential design changes, and an understanding of Orbiter TPS material characteristics, damage scenarios, and repair options. Ames, Glenn, and Langley Research Centers have performed analytic studies, conducted experimental testing, and developed new technologies, analysis tools, and hardware to contribute to each of these recommendations. For the External Tank (ET), these include studies of spray-on foam insulation (SOFI), investigations of potential design changes, and applications of advanced non-destructive evaluation (NDE) technologies to understand ET TPS shedding during liftoff and ascent. The end-to-end debris assessment included transport analysis to determine the probabilities of impact for various debris sources. For the Orbiter, methods were developed, and validated through experimental testing, to determine thresholds for potential damage of Orbiter TPS components. Analysis tools were developed and validated for on-orbit TPS damage assessments, especially in the area of aerothermal environments. Advanced NDE technologies were also applied to the Orbiter TPS components, including sensor technologies to detect wing leading edge impacts during liftoff and ascent. Work is continuing to develop certified TPS repair options and to develop improved methodologies for reinforced carbon-carbon (RCC) damage progression to assist in on-orbit repair decision philosophy.

Cockrell, Charles E., Jr.↗

Evaluation of Delamination Onset and Growth Characterization Methods under Mode I Fatigue Loading

Double-cantilevered beam specimens of IM7/8552 graphite/epoxy from two different manufacturers were tested in static and fatigue to compare the material characterization data and to evaluate a proposed ASTM standard for generating Paris Law equations for delamination growth. Static results were used to generate compliance calibration constants for reducing the fatigue data, and a delamination resistance curve, GIR, for each material. Specimens were tested in fatigue at different initial cyclic GImax levels to determine a delamination onset curve and the delamination growth rate. The delamination onset curve equations were similar for the two sources. Delamination growth rate was calculated by plotting da/dN versus GImax on a log-log scale and fitting a Paris Law. Two different data reduction methods were used to calculate da/dN. To determine the effects of fiber-bridging, growth results were normalized by the delamination resistance curves. Paris Law exponents decreased by 31% to 37% after normalizing the data. Visual data records from the fatigue tests were used to calculate individual compliance constants from the fatigue data. The resulting da/dN versus GImax plots showed improved repeatability for each source, compared to using averaged static data. The Paris Law expressions for the two sources showed the closest agreement using the individually fit compliance data.

Murri, Gretchen B.↗

Precise Identification and Characterization of Catalytically Active Sites on the Surface of γ-Alumina

γ-alumina is one of the oldest and most important commercial catalytic materials with high surface area and stability. These attributes enabled its use as the first commercial large-scale heterogeneous catalyst for ethanol dehydration. Despite progress in materials characterization the nature of the specific sites on the surface of γ-alumina that are responsible for its unique catalytic properties has remained obscure and controversial. By using combined infrared spectroscopy, electron microscopy and solid-state nuclear magnetic resonance measurements we identify the octahedral, amphoteric (O) 5 Al(VI)-OH sites on the (100) segments of massively restructured (110) facets on typical rhombus-platelet γ-alumina as well as the (100) segments of irrational surfaces (invariably always present in all γ-alumina samples) responsible for its unique catalytic activity. Such (O) 5 Al(VI)-OH sites are also present on the macroscopically defined (100) facets of γ-alumina with elongated/rod-like geometry. The mechanism by which these sites lose -OH groups upon thermal dehydroxylation resulting in coordinatively unsaturated penta-coordinate Al +3 O 5 sites is clarified. These coordinatively unsaturated penta-coordinate Al sites produce well-defined thermally stable Al-carbonyl complexes. Overall, our findings contribute to the understanding of the nature of coordinatively unsaturated Al sites on the surface of γ-alumina and their role as catalytically active sites.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Coupled Gel/Seeded Growth of Cs2AgBiBr6 Single Crystals for Radiation Detection

Abstract— The all-inorganic lead free Cs2AgBiBr6 perovskite represents a highly promising environment-friendly radiation detector material. The first attempt to grow Cs2AgBiBr6 single crystals using the unique gel growth method is reported in this study. This technique enables controlled reagent diffusion in a gel medium at room temperature, fostering the growth of visible single crystals. It offers advantages over conventional methods, leading to fewer equilibrium and non-equilibrium defects and simplified execution. Interestingly, the as-grown crystals exhibited variations in size and colors within the gel matrix, indicating the influence of Bi solutes in Bi-poor and Bi-rich Cs2AgBiBr6 crystals. Once the crystals were confirmed by powder xray diffraction, a series of comprehensive material characterizations was performed. The resistivity of Cs2AgBiBr6 single crystals was measured at 1.12x107 Ω•cm. Trap density analysis yielded a value of 2.82 x1010 cm-3. The charge carrier mobility was determined to be 32.9 cm2V-1S-1, suggesting the suitability for radiation detector applications. Additional growth optimization is going on and further characterization will be reported during the presentation. Our work helps accelerate the development of lead-free perovskite materials toward radiation detector applications.

James, Ralph B.↗

Mechanical Impact Testing: A Statistical Measurement

In the decades since the 1950s, when NASA first developed mechanical impact testing of materials, researchers have continued efforts to gain a better understanding of the chemical, mechanical, and thermodynamic nature of the phenomenon. The impact mechanism is a real combustion ignition mechanism that needs understanding in the design of an oxygen system. The use of test data from this test method has been questioned due to lack of a clear method of application of the data and variability found between tests, material batches, and facilities. This effort explores a large database that has accumulated over a number of years and explores its overall nature. Moreover, testing was performed to determine the statistical nature of the test procedure to help establish sample size guidelines for material characterization. The current method of determining a pass/fail criterion based on either light emission or sound report or material charring is questioned.

Engel, Carl D.↗

Sample Curation in Support of the OSIRIS-REx Asteroid Sample Return Mission

The OSIRIS-REx asteroid sample return mission launched to asteroid Bennu Sept. 8, 2016. The spacecraft will arrive at Bennu in late 2019, orbit and map the asteroid, and perform a touch and go (TAG) sampling maneuver in July 2020. After sample is stowed and confirmed the spacecraft will return to Earth, and the sample return capsule (SRC) will land in Utah in September 2023. Samples will be recovered from Utah [2] and then transported and stored in a new sample cleanroom at NASA Johnson Space Center in Houston [3]. The materials curated for the mission are described here. a) Materials Archive and Witness Plate Collection: The SRC and TAGSAM were built between March 2014 and Summer of 2015, and instruments (OTES,OVIRS, OLA, OCAMS, REXIS) were integrated from Summer 2015 until May 2016. A total of 395 items were received for the materials archive at NASA-JSC, with archiving finishing ~30 days after launch (with the final archived items being related to launch operations)[4]. The materials fall into several general categories including metals (stainless steel, aluminum, titanium alloys, brass and BeCu alloy), epoxies, paints, polymers, lubricants, non-volatile-residue samples (NVR), sapphire, and various miscellaneous materials. All through the ATLO process (from March 2015 until late August 2016) contamination knowledge witness plates (Si wafer and Al foil) were deployed in the various cleanrooms in Denver and KSC to provide an additional record of particle counts and volatiles that is archived for current and future scientific studies. These plates were deployed in roughly monthly increments with each unit containing 4 Si wafers and 4 Al foils. We archived 128 individual witness plates (64 Si wafers and 64 Al foils); one of each witness plate (Si and Al) was analyzed immediately by the science team after archiving, while the remaining 3 of each are archived indefinitely. Information about each material archived is stored in an extensive database at NASA-JSC, and key summary information for each will be presented in an online catalog. b) Bulk Asteroid sample: The Touch and Go Sampling Mechanism (TAGSAM) head will contain up to 1.5 kg of asteroid material. Upon return to Earth, the TAGSAM head with the sample canister will be subjected to a nitrogen purge and then opened in a nitrogen cabinet in Houston. Once the TAGSAM head is removed from the canister, it will be dis-assembled slowly and carefully under nitrogen until the sample can be removed for processing in a dedicated nitrogen glovebox. Bennu surface samples are expected to be sub-cm sized, based on thermal infrared and radar polarization ratio measurements [1]. The upper limit on material collected by the TAGSAM head is ~2 cm. Therefore, we will be prepared to handle, subdivide, and characterize materials of a wide grain size (from ~10 m to 2 cm), and for both organic (UV fluorescence) and inorganic (SEM, FTIR, optical) properties. Representative portions of the bulk sample will be prepared for JAXA (0.5 %; see also [5]) and Canadian Space Agency (4%), with the remaining divided between the science team (<25%) and archived for future studies (NASA) (>75%). c) Contact Pad samples: The base of the TAGSAM head contains 24 contact pads that are designed to trap the upper surface layer of material and thus offer an opportunity to study asteroid samples that have resided at the very top surface of the regolith. Asteroid material is trapped on the pads in spring steel Velcro hooks, and material will have to be removed from these pads by curation specialists in the lab. d) Hardware: Some canister and SRC hardware items will contain information that will be important to understanding the collected samples, including the canister gas filter, temperature strips, flight witness plates, and the TAGSAM and canister parts that might have adhering dust grains. Some challenges remaining for both bulk sample and contact pad samples include: i) working with intermediate size range (200 to 500 micron) samples - a size range NASA has not previously worked in such detail; ii) techniques for removal of contact pad material from the spring steel hooks, iii) static electrical effects of dust sized particles during sample handling and curation is likely to be significant, and iv) the TAGSAM head and associated canister hardware will undoubtedly be coated with fine adhering dust grains from Bennu. In the case of collection of a large bulk sample mass, the adhering dust grains may be of lower priority. If a small sample mass is returned, the adhering dust may attain a higher priority, so recovery of adhering dust grains is an additional challenge to consider. In the year leading up to sample return we plan a variety of sample handling rehearsals that will enables the curation team to be prepared for many new aspects posed by this sample suite.

Righter, Kevin↗

Effects of Neutron Irradiation on the Micro/Nano Scale Structure and Fission Product Distribution of TRISO Coated Particle Fuel Kernels from AGR Experiments

The Advanced Reactor Technologies (ART) Program at Idaho National Laboratory (INL) includes the Advanced Gas Reactor (AGR) fuel development and qualification program that consists of fuel fabrication, experiment irradiations, post-irradiation examination (PIE) and safety testing to assess tristructural isotropic (TRISO) fuel performance during normal irradiation and under potential accident conditions. Advanced microscopy work on selected AGR-1 and AGR-2 unirradiated and irradiated fuel specimens is performed as part of the PIE effort. PIE work on fuel from the first experiment irradiation, AGR-1, began at INL in April 2010, and AGR-2 PIE began at INL in July 2014. This work scope includes University of Florida (UF) performing advanced electron microscopy examination and analysis using facilities at the Center for Advanced Energy Studies (CAES), INL or UF’s electron microscopy facilities. Electron microscopic examination and analysis may include scanning transmission electron microscopy (STEM), transmission electron microscopy (TEM), selected area diffraction (SAD), electron energy loss spectroscopy (EELS), electron dispersive spectroscopy (EDS) and atom probe tomography (APT) on the fuel kernels of TRISO-coated fuel particles. The electron microscopy lamellae will be provided by INL and will be available at CAES or Irradiated Materials Characterization Laboratory (IMCL).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Experimental Steps toward a Density Law for Chlorine-Crediting Criticality Models of Aqueous Plutonium solutions

Criticality accident prevention is an essential safety consideration for all operations involving fissionable and fissile materials. Predictive criticality calculations using advanced neutron transport codes, such as Monte Carlo N-Particle Transport (MCNP), are invaluable tools for designing and implementing operational limits. While indispensable, these tools are limited by the quality and accuracy of the inputs that the user provides to define the modeled system. Parameters such as atomic composition, shape, and material density must be accurately defined to obtain a meaningful result. In the case of material property details for a plutonium model, accurate material characterization data is sometimes sparse. Thus limitations in calculation accuracy can be reduced by improving our knowledge of material properties in the targeted fissile systems. One of the biggest remaining challenges to accurately defining fissile systems is the description of aqueous fissile solutions. Even simple properties, such as density, are not well-known for fissile solutions relevant to nuclear energy and security. Described here are initial efforts undertaken to improve criticality calculation inputs for fissile plutonium chloride solutions in water. This effort is focused on experimentally determining accurate solution characteristics for ternary plutonium chloride/hydrochloric acid/water systems, by measurement of water activity and solution density. The effect of inputting experimental densities for these solutions into MCNP criticality calculations is compared to the traditional approach of modeling an idealized (and fictitious) plutonium-water mixture. Expansion of these efforts to a working density law for aqueous plutonium chloride solutions is also discussed.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Carbon fiber classification using raman spectroscopy

Carbon fiber characterization processes are described that include multi-condition Raman spectroscopy-based examination combined with multivariate data analyses. Methods are a nondestructive material characterization approach that can provide predictions as to carbon fiber bulk physical properties, as well as identification of unknown carbon fiber materials for quality control purposes. The framework of the multivariate analysis methods includes a principal component-based identification protocol including comparison of Raman spectral data from an unknown carbon fiber with a data library of multiple principal component spaces.

Houk, Amanda L.↗

Electrochemical Characterization of Degradation Modes of High-Voltage Li x Ni 0.33 Mn 0.33 Co 0.33 O 2 Electrodes

While deeply charged high-voltage cathodes can improve battery energy density, understanding and preventing any accelerated cell degradation is crucial to practical success. Here, to analyze the degradation of LiNi x Mn y Co 1–x–y O 2 (NMC) type material charged to 4.3 and 4.5 V, a physics-based model is applied to cycling data to obtain parameter estimates indicative of degradation modes, which are validated by simple electrochemical measurements and further interpreted by materials characterization. Growth rates of interfacial impedance and active material loss are greater at 4.5 V, as might be expected. However, when charged to 4.5 V, degradation rates are initially lower at a cycling C-rate of 1.0 C than at 0.5 C. Once degradation mode changes are quantified, simulations evaluate the contribution of individual degradation mode to performance losses and provide estimates of the energy-power correlation (Ragone plots) of cells after cycling.

25 ENERGY STORAGE↗

Electrochemically-assisted removal of cadmium ions by redox active Cu-based metal-organic framework

An electrochemically-assisted wastewater treatment using Faradaic materials offers a promising technique for the selective removal of hazardous substances. Here, we demonstrate the reversible capture and release of cadmium ions in aqueous solutions, using a redox-active metal-organic framework (MOF) electrode. As-synthesized copper-based MOF (Cu-MOF-74; copper 2,5-dihydroxyterephthalate) is a highly attractive candidate for Faradaic electrosorption due to its large surface area, water stability, and redox-active metal nodes. Our work demonstrates the reversible capture and release of Cd 2+ ions assisted by the electrochemical redox reaction of Cu 2+ /Cu + within the MOF structure. Combined material characterization and electrosorption tests were carried out to determine the operational conditions for maximizing adsorption capacity, energy efficiency, and material stability, thus leading to excellent electrosorption (>100 mg g -1 ) and regeneration efficiency (>90%). This study demonstrates the feasibility of leveraging MOFs containing redox-active metal nodes for the selective separation of toxic cations, and paves the way for promising future applications of these 3-D porous structures for wastewater treatment and environmental remediation.

42 ENGINEERING↗

Morphological Degradation of Oxygen Evolution Reaction-Electrocatalyzing Nickel Selenides at Industrially Relevant Current Densities

We investigated electrodeposited nanoparticulate nickel selenide (pre)catalysts that transform into nickel oxides/ oxyhydroxides under oxygen evolution reaction conditions in alkaline solutions. Previous studies of this transformation were conducted at lower current densities than those of industrial relevance (≥1 A cm −2 ). We used ultramicroelectrodes (UMEs) to achieve such current densities, benefiting from their small size, ensuring low absolute currents and low ohmic drop but high current densities. Morphological degradation of the catalyst material was only observed at current densities exceeding 1 A cm −2 but not for smaller ones. Using X-ray absorption, Xray photoemission spectroscopy, and X-ray diffraction, we confirmed that the degradation was accompanied by the literature-known transformation of nanoparticulate Ni 3 Se 2 (bulk)/NiSe (surface) into nickel oxyhydroxide. The transformation of the precatalyst goes along with a significant improvement in the charge transfer kinetics observed by decreasing Tafel slopes with ongoing experimental time extracted from cyclic voltammetry (CV) experiments and electrochemical impedance spectroscopy (EIS) in the high-frequency range. However, these kinetic improvements are accompanied by limitations in mass transport concluded from decreasing current responses at high overpotentials in CVs and increasing impedance in the low-frequency range of the EIS spectra after extended CV cycling. These mass transport limitations originated from morphological degradations at the UME exceeding 1 A cm −2 which we proved by applying identical location scanning electron microscopy. This has not been reported in studies that have been limited to lower current densities before. Our findings showcase how UMEs can be used to study (pre)catalysts (herein nickel selenides) under current densities of industrial relevance in the absence of ohmic drop-related ambiguities, combined with in-depth materials characterization studies, e.g., identical location microscopy and advanced spectroscopic methods. This approach enables direct evaluation and comparison of catalyst materials and thus demonstrates how to overcome long-standing limitations of electrocatalyst design and testing.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Modelling and Experimental Validation of Improved Performance of Lithium-Ion Batteries Having Thick Electrodes with Laser-Ablated Micro-Structures

For widespread adoption of electric vehicles, lithium-ion batteries (LiBs) need to achieve energy densities of >275 Wh/kg, cost less than $100/Wh, and charge to more than 80% capacity within 15 minutes. Increasing the battery electrode thicknesses is one way to increase cell energy densities while also saving on cell manufacturing cost by increasing the ratio of electrode active material to inactive material within each cell. However, increased electrode loading is often accompanied by decreased Li+-ion diffusion across the full thick electrodes. This leads to significant cell polarization that prevents full capacity utilization and accelerates cell degradation, especially at fast charging/discharging rates. The introduction of secondary pore networks in thick battery electrodes alleviates some of the trade-offs between energy and power performance. These microstructures provide low tortuosity pathways for facile Li+-ion diffusion deep into the thick electrodes, diminishing detrimental concentration gradients within the cell. Ultrafast-pulsed laser ablation is a promising method to introduce micro pores or channels in thick battery electrodes as it allows for precise control of pattern geometries, results in minimal damage to the electrode and can be introduced into existing roll-to-roll electrode manufacturing lines. Herein, the limitations of thick planer electrodes and the advanced predictive models to identify optimal electrode patterns for improved cycling performance will be presented. The impact of electrode laser patterning to create secondary pore networks also will be discussed. Materials characterization techniques (SEM-EDS, XRD) were used to explore the affect ultrafast laser ablation had on the electrode materials’ morphology and structure. The improvements in the patterned electrodes’ electrochemical cycling performances and degrees of wetting will be compared to a pristine baseline case. Finally, the discrepancies between experimentally obtained data and model predictions will be explained.

DIRECT ENERGY CONVERSION,ENERGY STORAGE↗