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At least 1,531 records · Page 85

Understanding and Strategies for Controlled Interfacial Phenomena in Lithium-Ion Batteries and Beyond

Electrolyte chemistry and properties and electrode structure and chemical properties particularly at the interfaces are crucial for the development of advanced battery components. This project focused on elucidating the roles of the electrolyte and electrode on the formation and evolution of the SEI layer and cell electrochemical performance on silicon and on Li metal anodes. For Si nano/microstructures we evaluated lithiation, volume changes, reactivity, and chemo-mechanical transformations as functions of nanoparticle size, shape, presence of coatings, electrolyte composition, electron leakage to the electrolyte, and cycling. For Li metal anodes we provided detailed analyses of the electrode and electrolyte effects on interfacial reactivity and as a function of microstructural evolution and underlying stochasticity as dendrites nucleate and grow. We thoroughly investigated and simulated how the chemistry of the various components of the electrolyte and the electrode architecture may affect the electrochemical reactions as well as cell degradation. A multiscale modeling approach was utilized, where atomistic simulations informed about the microscopic behavior of the system, and intermediate time and length scales were investigated with mesoscopic models. Results were also tested against selected experiments from our collaborators. The combined theoretical-experimental strategy saves costs by utilizing predictions from computational analyses to guide experimentation.

25 ENERGY STORAGE↗

Enabling Multi-Material Structures of Co-Based Superalloy Using Laser Directed Energy Deposition Additive Manufacturing

Cobalt superalloys such as Tribaloys are widely used in environments that involve high temperatures, corrosion, and wear degradation. Additive manufacturing (AM) processes have been investigated for fabricating Co-based alloys due to design flexibility and efficient materials usage. AM processes are suitable for reducing the manufacturing steps and subsequently reducing manufacturing costs by incorporating multi-materials. Laser directed energy deposition (laser DED) is a suitable AM process for fabricating Co-based alloys. T800 is one of the commercially available Tribaloys that is strengthened through Laves phases and of interest to diverse engineering fields. However, the high content of the Laves phase makes the alloy prone to brittle fracture. In this study, a Ni-20%Cr alloy was used to improve the fabricability of the T800 alloy via laser DED. Different mixture compositions (20%, 30%, 40% NiCr by weight) were investigated. The multi-material T800 + NiCr alloys were heat treated at two different temperatures. These alloy chemistries were characterized for their microstructural, phase, and mechanical properties in the as-fabricated and heat-treated conditions. SEM and XRD characterization indicated the stabilization of ductile phases and homogenization of the Laves phases after laser DED fabrication and heat treatment. In conclusion, the NiCr addition improved the fabricability and structural integrity of the T800 alloy.

36 MATERIALS SCIENCE↗

Development of ductile high-strength chromium alloys, phase 2

Strength and ductility were evaluated for chromium alloys dispersion hardened with the putative TaC, TaB, CbC, and CbB compounds. TaC and TaB proved to be the most potent strengtheners, but when combined, their effect far outweighed that produced individually. Tests at 1422 K (2100 F) on an alloy containing these two compounds at the combined level of 0.5 m/o revealed a 495 MN/sq m (70 ksi) tensile strength for wrought material, and a 100 hour rupture strength of 208 MN/sq m (30 ksi) when solution annealed and aged to maximize creep resistance. These levels of high temperature strength greatly exceed that reported for any other chromium-base alloy. The ductile-to-brittle transition temperature (DBTT) of the two phase strengthened alloy occurred at approximately 588 K (600 F) when heat treated to optimize creep strength and was not improved by fabrication to produce a wrought and recovered microstructure. The lowest DBTT measured on any of the alloys investigated was 422 K (300 F). Strengthening phases actually formed in Cr-Ta-B and Cr-Cb-B compositions are probable M2CrB2 (M=Ta or Cb) compounds of tetragonal crystal structure. The likely habit relationship between these compounds and chromium is postulated. Cube habit coherency was identified for TaC precipitation in chromium by electron microscopy. In another study, the maximum solubility of carbon in chromium was indicated to lie between 3/4 and 1 a/o and that of boron to be 1/2 a/o.

Filippi, A. M.↗

Sintering, crystallization, and breccia formation

The process of breccia formation by viscous sintering in the absence of pressure, advanced by Simonds (1973), is examined in detail. The limitations on the standard model for such sintering are considered. The competing process of crystallization is analyzed kinetically in terms of time-temperature-transformation curves corresponding to various degrees of crystallinity. The analysis is applied to Lunar Composition 15418 to illustrate the approach. The results indicate that close constraints can be placed on the thermal histories of lunar breccias, particularly breccias with modest degrees of crystallinity, from microstructural observations and kinetic measurements.

Uhlmann, D. R.↗

On the Cu-Nb Phase Diagram and Solidified Microstructures

Container and containerless processing was employed to determine liquidus temperatures and to examine microstructural development in the Cu-Nb system. The Cu-Nb phase diagram of an S-shaped, near-horizontal liquidus, has been confirmed by both the temperature-time profiles and resultant microstructures with only Nb dendrites in a Cu matrix, which were obtained from crucible experiments under clean conditions. However, the microstructural pathways of Cu-Nb alloys are particularly sensitive to processing variables. By the addition of oxygen impurities or rapid solidification, droplet-shaped morphology was observed for some compositions, implying occurrence of a liquid-phase separation. The effects of impurities and cooling rates are analyzed in connection with a stable and metastable liquid miscibility gap, respectively.

Li, D.↗

Some Novel Solidification Processing Techniques Being Investigated at MSFC: Their Extension for Study Aboard the ISS

The float-zone and the Bridgman techniques are two classical directional solidification processing methods that are used to improve materials properties. Unfortunately, buoyancy effects and gravity-driven convection due to unstable temperature and/or composition gradients still produce solidified products that exhibit segregation and, consequently, degraded properties. This presentation will briefly introduce how some novel processing applications can minimize detrimental gravitational effects and enhance microstructural uniformity. Discussion follows that to fully understand and model these procedures requires utilizing, in conjunction with a novel mixing technique, the facilities and quiescent microgravity environment available on the ISS.

Grugel, R. N.↗

In-Situ NDE Characterization of Kevlar and Carbon Composite Micromechanics for Improved COPV Health Monitoring

This project is a subtask of a multi-center project to advance the state-of-the-art by developing NDE techniques that are capable of evaluating stress rupture (SR) degradation in Kevlar/epoxy (K/Ep) composite overwrapped pressure vessels (COPVs), and damage progression in carbon/epoxy (C/Ep) COPVs. In this subtask, acoustic emission (AE) data acquired during intermittent load hold tensile testing of K/Ep and C/Ep composite tow materials-of-construction used in COPV fabrication were analyzed to monitor progressive damage during the approach to tensile failure. Insight into the progressive damage of composite tow was gained by monitoring AE event rate, energy, source location, and frequency. Source location based on arrival time data was used to discern between significant AE attributable to microstructural damage and spurious AE attributable to background and grip noise. One of the significant findings was the observation of increasing violation of the Kaiser effect (Felicity ratio < 1.0) with damage accumulation.

Waller, Jess M.↗

Experimental Investigation of Space Radiation Processing in Lunar Soil Ilmenite: Combining Perspectives from Surface Science and Transmission Electron Microscopy

Energetic ions mostly from the solar wind play a major role in lunar space weathering because they contribute structural and chemical changes to the space-exposed surfaces of lunar regolith grains. In mature mare soils, ilmenite (FeTiO3) grains in the finest size fraction have been shown in transmission electron microscope (TEM) studies to exhibit key differences in their response to space radiation processing relative to silicates [1,2,3]. In ilmenite, solar ion radiation alters host grain outer margins to produce 10-100 nm thick layers that are microstructurally complex, but dominantly crystalline compared to the amorphous radiation-processed rims on silicates [1,2,3]. Spatially well-resolved analytical TEM measurements also show nm-scale compositional and chemical state changes in these layers [1,3]. These include shifts in Fe/Ti ratio from strong surface Fe-enrichment (Fe/Ti >> 1), to Fe depletion (Fe/Ti < 1) at 40-50 nm below the grain surface [1,3]. These compositional changes are not observed in the radiation-processed rims on silicates [4]. Several mechanism(s) to explain the overall relations in the ilmenite grain rims by radiation processing and/or additional space weathering processes were proposed by [1], and remain under current consideration [3]. A key issue has concerned the ability of ion radiation processing alone to produce some of the deeper- penetrating compositional changes. In order to provide some experimental constraints on these questions, we have performed a combined X-ray photoelectron spectroscopy (XPS) and field-emission scanning transmission electron (FE-STEM) study of experimentally ion-irradiated ilmenite. A key feature of this work is the combination of analytical techniques sensitive to changes in the irradiated samples at depth scales going from the immediate surface (approx.5 nm; XPS), to deeper in the grain interior (5-100 nm; FE-STEM).

Christoffersen, R.↗

Relationship of Powder Feedstock Variability to Microstructure and Defects in Selective Laser Melted Alloy 718

Powder-bed additive manufacturing processes use fine powders to build parts layer by layer. For selective laser melted (SLM) Alloy 718, the powders that are available off-the-shelf are in the 10-45 or 15-45 micron size range. A comprehensive investigation of sixteen powders from these typical ranges and two off-nominal-sized powders is underway to gain insight into the impact of feedstock on processing, durability and performance of 718 SLM space-flight hardware. This talk emphasizes an aspect of this work: the impact of powder variability on the microstructure and defects observed in the as-fabricated and full heated material, where lab-scale components were built using vendor recommended parameters. These typical powders exhibit variation in composition, percentage of fines, roughness, morphology and particle size distribution. How these differences relate to the melt-pool size, porosity, grain structure, precipitate distributions, and inclusion content will be presented and discussed in context of build quality and powder acceptance.

Characterization↗

Time at Temperature Abstract and Intern Poster

Current NRC regulations for BWR operations dictate that any occurrence reaching the point of Departure from Nucleate Boiling (DNB) disqualifies the use of the fuel rod for further reactor operation. That criteria does not account for duration of rate of the power increase, the corresponding effects on material properties or rewetting that may occur. Previous Anticipated Operational Occurrences (AOOs) show short durations power increase that may require limited amounts of heat removal. Industrial experience has shown evidence that fuel can reach dryout yet continue to safely operate in regular reactor conditions. The gap in research into such occurrences is the motivation for a series of experiments, including this current work. Time-at-Temperature experiments aim to identify and characterize the microstructural changes in Zircaloy-2 under oxygen-free high temperatures. This work uses the FlashDSC instrument to rapidly ramp up and down the temperature of a focus ion beam (FIB) prepared large area lift-out (LALO) of Zircaloy-2 at a rate of 10,000 K/s to desired values. The focus is to characterize the microstructure evolution, if any, of Zircaloy-2 that may impact its performance under typical BWR conditions. This characterization includes analyzing grain structure and size, secondary phase particle (SPPs) size, shape, composition, and location using Transmission Electron Microscopy (TEM). Further data collection and analysis is in progress including diffraction pattern indexing and 4D STEM processing. While current results focus on the testing and characterizing unirradiated material, future plans include expansion to irradiated material to explore the effects of rapid transition rates seen in DNB and dryout conditions on irradiationg damage and defect annealing.

36 - MATERIALS SCIENCE↗

Particle interspacing effects on the mechanical behavior of a Fe–TiB 2 metal matrix composite using FFT-based mesoscopic field dislocation mechanics

This paper presents an application to metal matrix composites (MMCs) of an enhanced elasto-viscoplastic Fast Fourier Transform (EVP-FFT) formulation coupled with a phenomenological continuum Mesoscale Field Dislocation Mechanics (MFDM) theory. Contrary to conventional crystal plasticity, which only accounts for plastic flow and hardening induced by statistically stored dislocations (SSDs), MFDM-EVP-FFT also describes the evolution of polarized geometrically necessary dislocation (GND) density and its effect on both plastic flow and hardening. Numerical results for a Fe–TiB 2 MMC made of a ferrite matrix (α-Fe) and elastic ceramic particles (TiB 2 ) are presented. Full-field simulations are performed using synthetic periodic unit cells representative of the MMC, with single-crystalline and polycrystalline matrix, for different particle interspacing distances. A strong dependence of the predicted equivalent stress, cumulated plastic strain and GND density fields with particle interspacing distance is observed, in contrast with conventional crystal plasticity. Correlations between these mechanical fields and microstructural features, and their influence on local and global mechanical behavior are examined for the different MMC microstructures.

42 ENGINEERING↗

Influence of Molybdenum on Rapid Solidification Microstructure and Microsegregation in Primary Ferrite Solidified Stainless Steel

Due to the widespread use and familiarity of austenitic stainless steels in many industries these alloys are often the first materials used when adapting new processing techniques. The rapid cooling and solidification rates that occur during fusion based additive manufacturing processes like powder bed fusion cause a fundamental shift in the solidification behavior of the material. While the effects that Cr and Ni have on the microstructure have been fairly well documented across a range of solidification conditions, the impact of alloying elements like Mo are not as well understood at rapid solidification rates. For this study, four custom stainless steel alloy feedstocks were made with targeted modification of the Cr and Mo concentrations to maintain a constant Cr/Ni eq ratio of ~1.7. Two-piston splat quenching was used to produce rapidly solidified samples and the solidification mode, phase, and cell size were investigated. Solidification rates were estimated to be between 0.4 and 1.5m/s. A comparison of the microsegregation and partitioning behavior of Cr, Ni and Mo in ferrite solidified material was also performed for the different alloy compositions. Variations of the Mo concentration between each feedstock showed no measurable influence on the solidification/cooling rates, solidification morphology, or the partitioning of Mo. Furthermore, higher concentrations of Mo were found to significantly increase the amount of ferrite phase in the microstructure by suppressing the ferrite to austenite massive transformation.

36 MATERIALS SCIENCE↗

Micromechanics Based Design/Analysis Codes for Advanced Composites

Advanced high temperature Ceramic Matrix Composites (CMC) hold an enormous potential for use in aero and space related applications specifically for propulsion system components. Consequently, this has led to a multitude of research activities pertaining to fabrication, testing and modeling of these materials. The efforts directed at the development of ceramic matrix composites have focused primarily on improving the properties of the constituents as individual phases. It has, however, become increasingly clear that for CMC to be successfully employed in high temperature applications, research and development efforts should also focus on optimizing the synergistic performance of the constituent phases within the as-produced microstructure of the complex shaped CMC part. Despite their attractive features, the introduction of these materials in a wide spectrum of applications has been excruciatingly slow. The reasons are the high costs associated with the manufacturing and a complete experimental testing and characterization of these materials. Often designers/analysts do not have a consistent set of necessary properties and design allowables to be able to confidently design and analyze structural components made from these composites. Furthermore, the anisotropy of these materials accentuates the burden both on the test engineers and the designers by requiring a vastly increased amount of data/characterization compared to conventional materials.

Mital, Subodh K.↗

Segmentation method comparison for residual fiber length measurement across tiled microscopy images

Fiber length distribution (FLD), in part, governs mechanical properties in discontinuous fiber composites, yet manual measurement methods limit the high-throughput characterization needed for materials design optimization. This study compares deep learning segmentation approaches for automated FLD measurement in large-field microscopy, evaluating how method choice affects the microstructural descriptors used in structure-property-processing relationships. A critical challenge is that high-resolution microscopy images (10,000×10,000 pixels) must be tiled for deep learning analysis, fragmenting fibers at boundaries. We demonstrate that segmentation method proves crucial for measurement accuracy. For example, instance segmentation with Slicing Aided Hyper Inference (SAHI) preserves individual fiber integrity across tiles while semantic segmentation prioritizes speed. Comparing against manual measurement of extracted carbon fibers, YOLOv11-SAHI matched manual ground truth (238 μm weighted mean) with 40x speedup (4.5 vs 167 minutes per image). U-Net provides rapid quantification although it is at the cost of reduced accuracy due only reliably measuring stand-alone fibers. Our comparative analysis reveals that instance segmentation with SAHI better preserves length measurements while semantic segmentation prioritizes speed, providing empirical guidance for method selection. The characterization provides essential inputs for mechanical property prediction models and inverse design workflows, accelerating composite materials development cycles.

Additive manufacturing↗

Polyethylene Blends for Improved Oxygen Barrier: Processing-Dependent Microstructure and Gas Permeability

Here this work demonstrates a greater than expected enhancement of oxygen barrier properties in linear low-density polyethylene (LLDPE)-based materials by blending LLDPE with high-density polyethylene (HDPE). The films made by melt pressing the LLDPE/HDPE blends had a greater reduction in oxygen permeability coefficients (PO 2 ) than predicted using common permeability reduction models, i.e., the harmonic average model and zero-permeability nanofiller model. The reduction of PO 2 was attributed to the presence of spherulite crystal structures, as revealed by atomic force microscopy combined with infrared spectroscopy (AFM-IR). The LLDPE matrix exhibited significant spherulite formation even at a relatively low addition of HDPEs, which likely formed tortuous pathways for diffusing oxygen molecules. Transport results from melt-pressed films contrast with the results from films with similar compositions prepared by film blowing, which did not show barrier enhancement beyond expectation. AFM-IR revealed that the blown films lacked spherulite crystals likely due to stretching in the machine direction followed by rapid cooling. These findings demonstrate the role of processing in controlling microstructures and thus the oxygen barrier performance. This work offers the possibility of achieving easily recyclable LLDPE-based packaging materials by simple blending of polyethylenes with different crystalline content.

36 MATERIALS SCIENCE↗

Microstructural Evaluations of Baseline HSR/EPM Disk Alloys

Six alloys representing two classes of powder metallurgy nickel-based superalloys were examined by transmission electron microscopy (TEM) and phase extraction. Alloys KM4, CH98, IN-100 and 456 are based on a Ni-18Co-12Cr composition while alloys Rene' 88 DT and SR 3 have lower Al and Co and higher Cr contents. The lambda size distributions were determined from quantitative image analysis of the TEM images. The volume fraction of lambda and carbides and the composition of the phases were determined by a combination of phase extraction and TEM. The results showed many similarities in lambda size distributions, grain boundary serrations, and grain boundary carbide frequencies between alloys KM4, CH98, 456, Rene' 88 DT and SR 3 when heat treated to give an approximate grain size of ASTM 6. The density of grain boundary carbides in KM4 was shown to substantially increase as the grain size increased. IN-100 and 456 subjected to a serration cooling heat treatment had much more complex lambda size distributions with very large intergranular and intragranular secondary lambda as well as finer than average cooling and aging lambda. The grain boundary carbides in IN-100 were similar to the other alloys, but 456 given the serration cooling heat treatment had a more variable density of grain boundary carbides. Examination of the phases extracted from the matrix showed that there were significant differences in the phase chemistries and elemental partitioning ratios between the various alloys.

Gabb, Timothy P.↗

Characterization of Al-Cu-Mg-Ag Alloy RX226-T8 Plate

Aluminum-copper-magnesium-silver (Al-Cu-Mg-Ag) alloys that were developed for thermal stability also offer attractive ambient temperature strength-toughness combinations, and therefore, can be considered for a broad range of airframe structural applications. The current study evaluated Al-Cu-Mg-Ag alloy RX226-T8 in plate gages and compared performance with sheet gage alloys of similar composition. Uniaxial tensile properties, plane strain initiation fracture toughness, and plane stress tearing resistance of RX226-T8 were examined at ambient temperature as a function of orientation and thickness location in the plate. Properties were measured near the surface and at the mid-plane of the plate. Tensile strengths were essentially isotropic, with variations in yield and ultimate tensile strengths of less than 2% as a function of orientation and through-thickness location. However, ductility varied by more than 15% with orientation. Fracture toughness was generally higher at the mid-plane and greater for the L-T orientation, although the differences were small near the surface of the plate. Metallurgical analysis indicated that the microstructure was primarily recrystallized with weak texture and was uniform through the plate with the exception of a fine-grained layer near the surface of the plate. Scanning electron microscope analysis revealed Al-Cu-Mg second phase particles which varied in composition and were primarily located on grain boundaries parallel to the rolling direction. Fractography of toughness specimens for both plate locations and orientations revealed that fracture occurred predominantly by transgranular microvoid coalescence. Introduction High-strength, low-density Al-Cu-Mg-Ag alloys were initially developed to replace conventional 2000 (Al-Cu-Mg) and 7000 (Al-Zn-Cu-Mg) series aluminum alloys for aircraft structural applications [1]. During the High Speed Civil Transport (HSCT) program, improvements in thermal stability were demonstrated for candidate aircraft wing and fuselage skin materials through the addition of silver to Al-Cu-Mg alloys based on Al 2519 chemistry [2]. Thermal stability of the resulting Al-Cu-Mg-Ag alloys, C415-T8 and C416-T8, was due to co-precipitation of the thermally stable . (AlCu) and ' (Al2Cu) strengthening phases [1-4]. The strength and toughness behavior was investigated for these alloys produced as 0.090-inch thick rolled sheet in the T8 condition and after various thermal exposures. The mechanical properties were shown to be competitive with conventional aircraft alloys, 2519-T8 and 2618-T8 [2]. During the Integral Airframe Structure (IAS) program, advanced aluminum alloys were examined for use in an integrally stiffened airframe structure where the skin and stiffeners would be machined from plate and extruded frames would be mechanically attached (see Figure 1) [5]. Advantages of integrally stiffened structure include reduced part count, and reduced assembly times compared to conventional built-up airframe structure. The near-surface properties of a thick plate are of significance for a machined integrally stiffened airframe structure since this represents the skin location. Properties measured at the mid-plane of the plate are more representative of the stiffener web. RX226 was developed to exploit strength-toughness improvements and thermal stability benefits of Al-Cu-Mg-Ag alloys in plate gages. This study evaluated the microstructure and properties of three gages of plate produced in the T8 condition.

Lach, Cynthia L.↗

Crystalline Loading of Lipophilic Coenzyme Q10 Pharmaceuticals within Conjugated Carbon Aerogel Derivatives

Low-density aerogel materials currently are being considered for applications in controlling the rate of release for small-molecule pharmaceuticals in vivo. In particular, silica (SiO2) aerogels are an intriguing platform for controlling both the absolute amount of drug loading, but also the crystalline state of small molecule pharmaceuticals has been shown to affect drug release kinetics. To date, loading silica aerogel materials with crystalline pharmaceuticals typically require dissolving small molecules in a supercritical solvent (i.e., CO2) before drying to recover the aerogel/drug composite. Here we demonstrate a simple and low-cost method for controlling the crystallinity of the model drug coenzyme Q10 (CoQ10) within carbon aerogel materials by rationally controlling the chemical microstructure of the aerogel to exhibit ?-conjugated (sp2) chemical bonding. In particular, both pyrolyzed graphene and nanodiamond aerogels exhibit enhanced intrinsic drug loading capacity and CoQ10 crystallinity over a broad range of sp2 surface-curvature. In contrast, amorphous carbon aerogel materials are observed to load CoQ10 pharmaceuticals with strictly amorphous microstructure.

Lim, Mathew↗