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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
All sourcesNASA NTRSDOE OSTI
NASA NTRS2000

Characterizing the Use of Ultrasonic Energy in Promoting Uniform Microstructural Dispersions in Immiscible Mixtures

Gravity driven separation and preferential wetting precludes uniform microstructural distributions during solidification processing of immiscible, liquid-liquid mixtures. Historically, it is, however, established that liquid/liquid suspensions can be established and maintained by utilizing ultrasound. Following a brief introduction the results of experiments on immiscible mixtures subjected to ultrasonic energy during solidification processing will be compared and evaluated in view of a recently developed mathematical model. The presentation continues by discussion of scaling the model to commercial viability and concludes with the implications of such processing in a microgravity environment.

Grugel, R. N.↗
NASA NTRS2001

Characterizing the Use of Ultrasonic Energy in Promoting Uniform Microstructural Dispersions in Immiscible Mixtures

Gravity driven separation and preferential wetting precludes uniform microstructural distributions during solidification processing of immiscible, liquid-liquid mixtures. Historically, it is, however, established that liquid/liquid suspensions can be established and maintained by utilizing ultrasound. Following a brief introduction the results of experiments on immiscible mixtures subjected to ultrasonic energy during solidification processing will be compared and evaluated in view of a recently developed mathematical model. The presentation continues by discussion of scaling the model to commercial viability and concludes with the implications of such processing in a microgravity environment.

Grugel, R. N.↗
DOE OSTI2022

USE OF TWO-PISTON SPLAT QUENCHING TO INVESTIGATE & CHARACTERIZE THE IMPACT OF COMPOSITIONAL VARIATIONS ON RAPID SOLIDIFICATION MICROSTRUCTURES & SUB-MICROSCALE FEATURES IN STAINLESS STEEL ALLOY.

The objective of this dissertation was to use two-piston splat quenching (SQ) to investigate the impact of compositional modifications on the solidification and microstructure of rapidly solidified austenitic stainless steels (SS) and to demonstrate the ability of SQ to quickly and effectively simulate rapid solidification conditions similar to those found in powder bed fusion (PBF) additive techniques. PBF techniques like laser powder bed fusion (LPBF) are being implemented across a breadth of research and industrial applications to create parts with complex geometries and performance capabilities while pushing the current limits of processing conditions and understanding of material systems. In this work, SQ was used to experimentally produce rapid solidification in 20+ unique austenitic SS compositions with systematic variations of the chrome and nickel equivalency ratio (Cr/Nieq) through targeted compositional modifications. From the targeted change of Cr, Ni, and Mo concentrations in rapidly solidified SS alloys, the ferrite solidification mode was found to be the primary solidification mode at significantly lower Cr/Nieq than previously predicted for RS. Also, decreasing concentrations of Fe at a constant Cr/Nieq ratio (i.e., different Fe isopleths), or increased Mo concentrations at a constant Cr/Nieq ratio were found to suppress the ferrite to austenite massive transformation when compared to alloys with lower concentrations at the same Cr/Nieq. Using an established empirical relationship between cell size and cooling rate, the SQ technique was estimated to produce cooling rates between 106 and 108 K/s. Thermal gradients were extracted from 2-D heat transfer simulations of the SQ solidification event and used with these cooling rates to produce solidification rate estimates for SQ which were between 0.4-1.6m/s. The primary solidification mode was observed to be the determining factor in which elements segregated to the cell boundaries during RS, for which Cr and Mo were the main elements to segregate during primary austenite solidification and Ni during primary ferrite solidification. Finally, the solidification rates and conditions produced by SQ experiments resulted in similar microstructures, features, and microsegregation to what was found in LPBF samples of the same feedstock.

Hasenbusch, Zachary↗
DOE OSTI2021

High Entropy Alloys: Irradiation

High entropy alloys (HEAs) have been considered as structural materials for nuclear applications due to their promising mechanical properties and radiation resistance. For this purpose, irradiation-induced defect evolution and microstructure change have been characterized to evaluate the irradiation performance of different HEAs. This article reviews recent advances in understanding the irradiation response of HEAs, including the effect of disordered states on the defect energy landscape and defect evolution, irradiation-induced microstructure changes, void swelling, phase stability, mechanical properties under irradiation, as well as the He irradiation effects.

Zhao, Shijun↗
NASA NTRS1993

The influence of a microgravity environment on the dendritic morphology during directional solidification of hypoeutectic Al-Si alloys

NASA grant NAGW-2540 provided the opportunity to evaluate and extend ongoing studies of directionally solidified Al-Si alloys. Microstructural development was further characterized in terms of solidification processing parameters; novel relationships between processing and development of dendrite trunk diameters and tertiary dendrite arm spacings were found. This has resulted in three publications (one in print, one in press, and one in review). Microstructural development under conditions of controlled acceleration during directional solidification has been investigated; this has culminated in a Master's degree and will be submitted for publication. The above work not only contributes to our understanding of solidification phenomena but also defines the processing parameters for a successful microgravity experiment while providing a data base to which mu g samples can be unequivocally compared and evaluated.

Grugel, Richard N.↗
NASA NTRS1999

Higher-Order Theory for Functionally Graded Materials

This paper presents the full generalization of the Cartesian coordinate-based higher-order theory for functionally graded materials developed by the authors during the past several years. This theory circumvents the problematic use of the standard micromechanical approach, based on the concept of a representative volume element, commonly employed in the analysis of functionally graded composites by explicitly coupling the local (microstructural) and global (macrostructural) responses. The theoretical framework is based on volumetric averaging of the various field quantities, together with imposition of boundary and interfacial conditions in an average sense between the subvolumes used to characterize the composite's functionally graded microstructure. The generalization outlined herein involves extension of the theoretical framework to enable the analysis of materials characterized by spatially variable microstructures in three directions. Specialization of the generalized theoretical framework to previously published versions of the higher-order theory for materials functionally graded in one and two directions is demonstrated. In the applications part of the paper we summarize the major findings obtained with the one-directional and two-directional versions of the higher-order theory. The results illustrate both the fundamental issues related to the influence of microstructure on microscopic and macroscopic quantities governing the response of composites and the technologically important applications. A major issue addressed herein is the applicability of the classical homogenization schemes in the analysis of functionally graded materials. The technologically important applications illustrate the utility of functionally graded microstructures in tailoring the response of structural components in a variety of applications involving uniform and gradient thermomechanical loading.

Aboudi, Jacob↗
NASA NTRS2014

Producing Zirconium Diboride Components with Complex, Near-Net Shape Geometries by Aqueous Room-Temperature Injection Molding

Room-temperature injection molding is proposed as a novel, low-cost and more energy efficient manufacturing process capable of forming complex-shaped zirconium diboride (ZrB2) parts. This innovative processing method utilized aqueous suspensions with high powder loading and a minimal amount (5 vol.) of water-soluble polyvinylpyrrolidone (PVP), which was used as a viscosity modifier. Rheological characterization was performed to evaluate the room-temperature flow properties of ZrB2-PVP suspensions. ZrB2 specimens were fabricated with high green body strength and were machinable prior to binder removal despite their low polymer content. After binder burnout and pressureless sintering, the bulk density and microstructure of specimens were characterized using Archimedes technique and scanning electron microscopy. X-Ray Diffraction was used to determine the phase compositions present in sintered specimens. Ultimate strength of sintered specimens will be determined using ASTM C1323-10 compressive C-ring test.

Near-Net Shape Forming↗
NASA NTRSDate not supplied

Zircon (U-Th)/He Impact Crater Thermochronometry and the Effects of Shock Microstructures on Helium Diffusion Kinetics

Absolute age determination of impact cratering events remains difficult and often controversial; a challenge that has resulted in < 50% of known impact craters regarded as accurately and precisely dated. Besides conventional 40Ar/39Ar and U-Pb methods, zircon (U-Th)/He (ZHe) dating of impactites has been applied to large- to medium-sized impact structures. ZHe dates can be fully reset in minutes at 1000°C, which is commonly reached in central sections of the melt sheet, whereas resetting of ZHe at <300°C, which might be encountered near the crater margins or persist in post-impact hydrothermal systems, may take >103-6 years. There is a critical need to quantify the effects of shock-induced microstructures and impact metamorphism on helium diffusion kinetics in well-characterized, variably shocked zircon to further establish the reliability of (U-Th)/He for dating impacts. For this purpose, we investigated suevite and impact melt samples from two impact structures, the Chicxulub multi-ring basin and the Ries complex crater, which enables us to compare zircon helium diffusion kinetics from impact structures with differing sizes, ages, and hydrothermal system longevities. Shock microstructures were characterized by backscattered-electron (BSE) imaging prior to diffusion step-heating fractional release experiments using light-bulb furnace with prograde and retrograde incremental 10°C steps from 250°C to 600°C. Afterward, we characterize the diffusion domain sizes and their interconnectivity within the shocked zircon grains using electron backscatter diffraction (EBSD). We find that zircon with few shock microstructures exhibit no significant deviation from helium diffusion kinetics of undamaged zircon. In contrast, zircon grains with planar deformation features (PDFs) and granular textures classified by BSE and EBSD are characterized by a dramatic decrease in helium retentivity, similar to radiation damaged grains, due to a reduction in the effective domain size and the introduction of interconnected fast diffusion pathways created by shock microstructures. A subset of grains were dated by ZHe after the external morphology of the grains was determined by BSE imaging. The euhedral grains yielded a weighted mean age within the uncertainty of the accepted impact ages, whereas the grains with PDFs or granular textures exhibited younger ages. Thus, these diffusion experiments and ZHe dates suggest that the dramatic decrease in domain size likely renders shocked grains more susceptible to impact-induced hydrothermal resetting and subsequent overprinting. Hence, characterization of shock microstructures is critical for determining accurate impact ages using ZHe methods especially when applied to previously unconstrained craters. The thermochronometer also offers the opportunity to determine the magnitude and duration of post-impact hydrothermal circulation.

zircon↗
DOE OSTI2024

The effect of neutron irradiation on conventional and nanocrystalline nickel: NSUF Work Package UA-22PN080501 Milestone M3UA-22PN0805012 (Final Report)

Even though nanocrystalline materials (20-100 nm) present an unprecedented potential, scientific knowledge related to the effect of neutron irradiation on the mechanical properties and microstructure is still scarce. Most of the past studies were conducted using ion irradiation which may not have the same effect as neutron irradiation because of the smaller irradiation volume and the higher dose rate. To reach a firm conclusion on the potential of nanocrystalline materials for nuclear reactor applications, extensive study of model metals with different stacking fault energy (SFE) is required to elucidate their behavior in radiation environments. Nanocrystalline copper and nickel are typically chosen because they are commonly used as model FCC metals in studies of radiation effects. Nickel is an FCC metal with a high stacking-fault energy (~125 mJ/m 2 ) compared to copper (~45 mJ/m 2 ). Hence, microcrystalline and nanocrystalline nickel samples were irradiated in the INL’s Advanced Test Reactor (ATR), as a part of FY08 North Carolina State University NSUF Irradiation Experiment# 96 to evaluate the irradiation behavior of these materials. The objective of this FY20 NSUF project# 19122 is to perform PIE (at PNNL NSUF facility) on previously ATR-neutron irradiated (1.2 and 2.6 dpa; 80-89°C) nanocrystalline and microcrystalline nickel samples to investigate the changes in mechanical properties and microstructures and evaluate whether nanocrystalline nickel is relatively more radiation resistant compared to conventional microcrystalline nickel. To perform PIE at PNNL, sixteen neutron irradiated specimens (microcrystalline and nanocrystalline) were transferred from the NSUF Nuclear Fuels and Materials Library at INL. Experimental techniques such as SEM/EBSD, XRD, TEM, Vickers microhardness and tensile testing were employed to characterize the effect of neutron irradiation on the microstructure and mechanical properties of nanocrystalline nickel and compared them with corresponding characteristics of microcrystalline nickel.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Influence of microstructure on replacement and porosity generation during experimental dolomitization of limestones

Replacement reactions commonly alter the multiscale pore structures of rocks during fluid-rock interactions. Analysis of these processes in various model fluid-rock systems during controlled laboratory experiments provides insights into the origins of microstructures found in natural materials. This study focused on understanding the effects of initial starting material permeability and resultant differences in transport pathways on porosity and mineralogical changes during limestone dolomitization.A series of replacement experiments (32–317 days in duration) have been conducted in which 1.59 cm (5/8 in.) diameter cores of two different limestones were reacted with saturated MgCl2 solutions at 200 °C. The Texas Cream (Austin Chalk) is a high-porosity, high-permeability limestone, whereas both the porosity and permeability of the Carthage Marble (Burlington Limestone) are relatively low. Altered limestones were imaged using scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDX), Time-of-Flight Secondary Ion Mass Spectrometry (ToF–SIMS) and electron microprobe analysis (EMPA). A representative grain boundary of the low-porosity limestone was targeted for a focused ion beam (FIB) lift-out and characterized using transmission electron microscopy (TEM). These results were coupled with analyses of radial changes in the porosity distribution of the core derived from X-ray and neutron small- and ultra-small angle scattering ((U)SANS/(U)SAXS).The high-porosity/permeability limestone showed a four times faster bulk replacement rate than the lower-porosity/permeability material, and a different mechanism of porosity development. For the low-porosity limestone, a two-stage replacement occurred, with the reacted region of the core consisting of an inner rim in which the limestone was replaced by two calcite-dolomite solid solutions, and an outer rim in which the dolomite was replaced by magnesite. Elongated pores formed along grain boundaries at the initial limestone/dolomite reaction interface, and additional nanometer-scale porosity was formed at the secondary magnesite replacement rim. Grain boundaries were identified as preferential pathways for transport leading to dolomitization and a grain boundary diffusion rate was calculated based on microstructural characterization. In contrast, replacement in the high-porosity limestone was accompanied by porosity generation through replacement of individual grains by dolomite throughout the sample and, in longer runs, magnesite in outer parts of the core. These observations emphasize that both the mechanisms of the replacement reaction and the microstructure and chemistry of the replaced product are contingent on the initial structure of the starting material.

36 MATERIALS SCIENCE↗
NASA NTRS2003

High-Performance Acousto-Ultrasonic Scan System Being Developed

Acousto-ultrasonic (AU) interrogation is a single-sided nondestructive evaluation (NDE) technique employing separated sending and receiving transducers. It is used for assessing the microstructural condition and distributed damage state of the material between the transducers. AU is complementary to more traditional NDE methods, such as ultrasonic cscan, x-ray radiography, and thermographic inspection, which tend to be used primarily for discrete flaw detection. Throughout its history, AU has been used to inspect polymer matrix composites, metal matrix composites, ceramic matrix composites, and even monolithic metallic materials. The development of a high-performance automated AU scan system for characterizing within-sample microstructural and property homogeneity is currently in a prototype stage at NASA. This year, essential AU technology was reviewed. In addition, the basic hardware and software configuration for the scanner was developed, and preliminary results with the system were described. Mechanical and environmental loads applied to composite materials can cause distributed damage (as well as discrete defects) that plays a significant role in the degradation of physical properties. Such damage includes fiber/matrix debonding (interface failure), matrix microcracking, and fiber fracture and buckling. Investigations at the NASA Glenn Research Center have shown that traditional NDE scan inspection methods such as ultrasonic c-scan, x-ray imaging, and thermographic imaging tend to be more suited to discrete defect detection rather than the characterization of accumulated distributed microdamage in composites. Since AU is focused on assessing the distributed microdamage state of the material in between the sending and receiving transducers, it has proven to be quite suitable for assessing the relative composite material state. One major success story at Glenn with AU measurements has been the correlation between the ultrasonic decay rate obtained during AU inspection and the mechanical modulus (stiffness) seen during fatigue experiments with silicon carbide/silicon carbide (SiC/SiC) ceramic matrix composite samples. As shown in the figure, ultrasonic decay increased as the modulus decreased for the ceramic matrix composite tensile fatigue samples. The likely microstructural reason for the decrease in modulus (and increase in ultrasonic decay) is the matrix microcracking that commonly occurs during fatigue testing of these materials. Ultrasonic decay has shown the capability to track the pattern of transverse cracking and fiber breakage in these composites.

Roth, Don J.↗
DOE OSTI2020

Microstructure reconstruction of battery polymer separators by fusing 2D and 3D image data for transport property analysis

A new approach to generate high-fidelity 3D microstructure reconstructions by leveraging resolution and sample volume characteristics from 2D and 3D microscopy methods is presented here. This approach is employed to model the microstructure of a highly orthotropic polypropylene separator used in lithium-ion batteries, which have challenging multi-scale features of fibrils (<100 nm) and lamellae (>100 nm) to resolve in 3D. Phase contrast nano X-ray computed tomographic data are used to reconstruct the lamellae phase, while 2D scanning electron microscopy data are used to characterize sub-100 nm microstructure features such as the thin fibrils that are beyond the effective resolution of X-ray computed tomography. Fibril geometries are reconstructed stochastically based on the 2D higher resolution data, and integrated with the lamellae geometries in 3D space. Transport property analyses are performed to investigate the bias of microstructure models without considering the fibrils. A sensitivity study is also conducted to facilitate understanding of the relationship between microstructure characteristics and transport properties.

25 ENERGY STORAGE↗
NASA NTRS2003

High-Performance Acousto-Ultrasonic Scan System Being Developed

Acousto-ultrasonic (AU) interrogation is a single-sided nondestructive evaluation (NDE) technique employing separated sending and receiving transducers. It is used for assessing the microstructural condition and distributed damage state of the material between the transducers. AU is complementary to more traditional NDE methods, such as ultrasonic cscan, x-ray radiography, and thermographic inspection, which tend to be used primarily for discrete flaw detection. Throughout its history, AU has been used to inspect polymer matrix composites, metal matrix composites, ceramic matrix composites, and even monolithic metallic materials. The development of a high-performance automated AU scan system for characterizing within-sample microstructural and property homogeneity is currently in a prototype stage at NASA. This year, essential AU technology was reviewed. In addition, the basic hardware and software configuration for the scanner was developed, and preliminary results with the system were described. Mechanical and environmental loads applied to composite materials can cause distributed damage (as well as discrete defects) that plays a significant role in the degradation of physical properties. Such damage includes fiber/matrix debonding (interface failure), matrix microcracking, and fiber fracture and buckling. Investigations at the NASA Glenn Research Center have shown that traditional NDE scan inspection methods such as ultrasonic c-scan, x-ray imaging, and thermographic imaging tend to be more suited to discrete defect detection rather than the characterization of accumulated distributed micro-damage in composites. Since AU is focused on assessing the distributed micro-damage state of the material in between the sending and receiving transducers, it has proven to be quite suitable for assessing the relative composite material state. One major success story at Glenn with AU measurements has been the correlation between the ultrasonic decay rate obtained during AU inspection and the mechanical modulus (stiffness) seen during fatigue experiments with silicon carbide/silicon carbide (SiC/SiC) ceramic matrix composite samples. As shown in the figure, ultrasonic decay increased as the modulus decreased for the ceramic matrix composite tensile fatigue samples. The likely microstructural reason for the decrease in modulus (and increase in ultrasonic decay) is the matrix microcracking that commonly occurs during fatigue testing of these materials. Ultrasonic decay has shown the capability to track the pattern of transverse cracking and fiber breakage in these composites.

Roth, Don J.↗
NASA NTRS2022

Effects of Debulking on the Fiber Microstructure and Void Distribution in Carbon Fiber Reinforced Plastics

Carbon Fiber Reinforced Plastics (CFRPs) are widely used due to their high stiffness to weight ratios. A common process manufacturers use to increase the strength to weight ratio is debulking. Debulking is the process of compacting a dry fibrous reinforcement prior to resin infusion. This process is meant to decrease the average inter-fiber distance, effectively increasing the fiber volume fraction of the sample. While this process is widely understood macroscopically its effects on fibrous microstructures have not yet been well characterized. The aim of this work is to compare the microstructures of three CFRP laminates, varying only the debulking step in the manufacturing process. High resolution serial sections of all three laminates were taken for analysis. Using these scans, the fiber positions were reconstructed. Statistical descriptors such as local fiber and void volume fractions, fiber orientation, and void distribution and morphology were then generated for each sample. Fiber clusters present within the material were identified and analyzed for each level of debulking applied. Using these descriptors, the effects of debulking on the morphology and organization of the composite microstructure was evaluated.

carbon fiber↗
NASA NTRS2012

Comparative Mineralogy, Microstructure and Compositional Trends in the Sub-Micron Size Fractions of Mare and Highland Lunar Soils

The morphology, mineralogy, chemical composition and optical properties of lunar soils show distinct correlations as a function of grain size and origin [1,2,3]. In the <20 m size fraction, there is an increased correlation between lunar surface properties observed through remote sensing techniques and those attributed to space weathering phenomenae [1,2]. Despite the establishment of recognizable trends in lunar grains <20 in size [1,2,3], the size fraction < 10 m is characterized as a collective population of grains without subdivision. This investigation focuses specifically on grains in the <1 m diameter size fraction for both highland and mare derived soils. The properties of these materials provide the focus for many aspects of lunar research including the nature of space weathering on surface properties, electrostatic grain transport [4,5] and dusty plasmas [5]. In this study, we have used analytical transmission and scanning transmission electron microscopy (S/TEM) to characterize the mineralogy type, microstructure and major element compositions of grains in this important size range in lunar soils.

Thompson, M. S.↗
DOE OSTI2020

In Situ Investigation of Chemomechanical Effects in Thiophosphate Solid Electrolytes

Solid-state batteries can suffer from catastrophic failure at high current densities due to solid electrolyte fracture, interface decomposition, or lithium filament growth. Failure is linked to chemomechanical material transformations that can manifest during electrochemical cycling. We systematically investigate how solid electrolyte microstructure and interfacial decomposition (e.g., interphase) affect failure mechanisms in lithium thiophosphates (Li3PS4, LPS) electrolytes. Kinetically metastable interphases are engineered with iodine doping, and microstructural control is achieved using milling and annealing processing techniques. In situ transmission electron microscopy reveals iodine diffusion to the interphase, and upon electrochemical cycling, pores are formed in the interphase region. In situ synchrotron tomography reveals that interphase pore formation drives edge fracture events, which are the origin of through-plane fracture failure. Fractures in thiophosphate electrolytes actively grow toward regions of higher porosity and are affected by heterogeneity in microstructure (e.g., porosity factor). This report provides fundamental design guidelines for high-performance solid-state batteries.

25 ENERGY STORAGE↗
DOE OSTI2020

α-U and ω-UZr 2 in neutron irradiated U-10Zr annular metallic fuel

Here, to develop metallic fuel with ultra-high burnup of 30%-40%, an annular U-10Zr fuel with 55% smear density was fabricated through a casting route and irradiated at the Advanced Test Reactor at Idaho National Laboratory. The annular fuel design also serves as a demonstration of the feasibility to replace sodium bond with a helium bond to benefit the geological disposal of irradiated fuel, cut the cost of fuel fabrication, and boost the overall metallic fuel economy. This paper reports the results from transmission electron microscopy (TEM) based post-irradiation examination of this fuel type irradiated to a burnup of 3.3% fissions per initial heave metal atoms for initial screening purpose. After irradiation, the initial U-10Zr separated into an a-U annular region and an UZr 2+x center region with nanoscale spinodal decomposed microstructure. Because of the provided large amount of coherent interface areas, the fission gas atoms and vacancies generated in UZr 2+x phase are possibly pinned at the interface areas, leading to 20 times smaller fission gas bubbles than those in the neighboring a-U. The large bubbles in a-U become connected and merged into large pores that provide fast release paths for fission gas which prevents further fuel swelling. The fuel center still has open space to accommodate further fuel swelling from solid fission products at higher burnup. Other neutron irradiation induced phase and microstructure change are also characterized and compared with traditional solid fuel designs.

36 MATERIALS SCIENCE↗