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Corrosion Compatibility of Stainless Steels and Nickel in Pyrolysis Biomass-Derived Oil at Elevated Storage Temperatures

Corrosion compatibility of stainless steels and nickel (Ni200) was assessed in fast pyrolysis bio-oil produced from pyrolysis of high ash and high moisture forest residue biomass. Sample mass change, ICP-MS and post-exposure electron microscopy characterization was used to investigate the extent of corrosion. Among the tested samples, type 430F and type 316 stainless steels (SS430F and SS316) and Ni200 (~98.5% Ni) showed minimal mass changes (less than 2 mg∙cm−2) after the bio-oil exposures at 50 and 80 °C for up to 168 h. SS304 was also considered to be compatible in the bio-oil due to its relatively low mass change (1.6 mg∙cm−2 or lower). SS410 samples showed greater mass loss values even after exposures at a relatively low temperature of 35 °C. Fe/Cr values from ICP-MS data implied that Cr enrichment in stainless steels would result in a protective oxide layer associated with corrosion resistance against the bio-oil. Post exposure characterization showed continuous and uniform Cr distribution in the surface oxide layer of SS430F, which showed a minimal mass change, but no oxide layer on a SS430 sample, which exhibited a significant mass loss.

09 BIOMASS FUELS↗

Parameter development and characterization of laser powder directed energy deposition of Nb – Alloy C103 for thin wall geometries

This work focuses on the parameter development and microstructural characterization of Nb-based alloy C103 for thin wall structures produced via laser powder – directed energy deposition (LP – DED). Laser power and scanning speeds were varied as part of a design of experiments to identify adequate print parameters. Combinations were evaluated for relative density, porosity, and geometrical accuracy. A combination of a laser power of 1420 W and scanning speed of 14 mm/s resulted in a relative density >99%, exhibited a consistent weld bead profile and was used for further microstructural evaluation. A mix of optical and scanning electron microscopy (SEM) revealed small, slightly elongated grains along the edges and large epitaxial grains in the central region along the Build – Transverse view. Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) analysis revealed Hf rich columnar cells in the center that transition into an evenly spaced cellular structure towards the edges of the built sample. Electron backscatter diffraction (EBSD) scans show a sharp [001] texture when looking at the cross section of the sample along the build direction. The Build – Scan view revealed a zig – zag pattern that follows the back – and – forth deposition strategy that was used. Finally, microhardness measurements were taken in the as – built (AB) and stress relieved (SR) conditions to baseline preliminary mechanical properties. The AB condition exhibited a large amount of scatter in the data and averages up to 11% larger than the SR condition. The reduction in scatter upon applying the SR cycle are indicative of a large concertation of dislocations present in the AB condition.

36 MATERIALS SCIENCE↗

Cryo-EM model validation recommendations based on outcomes of the 2019 EMDataResource challenge

This paper describes outcomes of the 2019 Cryo-EM Model Challenge. The goals were to (1) assess the quality of models that can be produced from cryogenic electron microscopy (cryo-EM) maps using current modeling software, (2) evaluate reproducibility of modeling results from different software developers and users and (3) compare performance of current metrics used for model evaluation, particularly Fit-to-Map metrics, with focus on near-atomic resolution. Our findings demonstrate the relatively high accuracy and reproducibility of cryo-EM models derived by 13 participating teams from four benchmark maps, including three forming a resolution series (1.8 to 3.1 Å). The results permit specific recommendations to be made about validating near-atomic cryo-EM structures both in the context of individual experiments and structure data archives such as the Protein Data Bank. We recommend the adoption of multiple scoring parameters to provide full and objective annotation and assessment of the model, reflective of the observed cryo-EM map density.

59 BASIC BIOLOGICAL SCIENCES↗

Integrated fluorescence light microscopy-guided cryo-focused ion beam-milling for in situ montage cryo-ET

Cryogenic-electron tomography (cryo-ET) permits the in situ visualization of biological macromolecules at the molecular level. Owing to the variable thickness of cells, tissues and organisms, frozen specimens may need to be thinned by cryo-focused ion beam (FIB) milling to produce thin (<500 nm) cryo-lamellae suitable for cryo-ET. Locating regions of interest remains a challenge because untargeted milling can lead to inadvertent ablation and removal of regions of interest. Correlative light and electron microscopy, combined with cryo-FIB milling, can guide the identification of labeled targets in the cellular milieu. Multiple transfers between cryo-imaging instruments, cumbersome correlation algorithms, limited accuracy and low throughput have hindered the routine adoption of cryo-FIB milling within a multimodal correlative workflow for in situ structural biology. Here, in this study, we present a workflow for 3D correlative cryo-fluorescence light microscopy-FIB-ET that streamlines fluorescence light microscopy-guided FIB milling, improving throughput while preserving both structural and contextual information. The complete integration of hardware and software described here minimizes sample contamination from cross-platform exchanges and greatly enhances the efficiency of 3D targeting in cryo-milling. We then describe procedures for implementing montage parallel array cryo-ET (MPACT), which can be easily adapted to any modern life-science transmission electron microscope. MPACT supports high-throughput cryo-ET acquisitions (10 tilt series in 1.5 h) for structure determination and comprehensive contextual understanding of macromolecules within their native surroundings. A complete session from sample preparation to MPACT data processing takes 5−7 d for an individual experienced in both cryo-EM and cryo-FIB milling.

Yang, Jie E. [Univ. of Wisconsin, Madison, WI (Uni↗

Quantum decoherence by Coulomb interaction

The performance of modern quantum devices in communication, metrology or microscopy relies on the quantum-classical interaction which is generally described by the theory of decoherence. Despite the high relevance for long coherence times in quantum electronics, decoherence mechanisms mediated by the Coulomb force are not well understood yet and several competing theoretical models exist. Here, we present an experimental study of the Coulomb-induced decoherence of free electrons in a superposition state in a biprism electron interferometer close to a semiconducting and metallic surface. The decoherence was determined through a contrast loss at different beam path separations, surface distances and conductibilities. To clarify the current literature discussion, four theoretical models were compared to our data. We could rule out three of them and got good agreement with a theory based on macroscopic quantum electrodynamics. The results will enable the determination and minimization of specific decoherence channels in the design of novel quantum instruments.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Purification of recombinant budgerigar fledgling disease virus VP1 capsid protein and its ability for in vitro capsid assembly

A recombinant system for the major capsid VP1 protein of budgerigar fledgling disease virus has been established. The VP1 gene was inserted into a truncated form of the pFlag-1 vector and expressed in Escherichia coli. The budgerigar fledgling disease virus VP1 protein was purified to near homogeneity by immunoaffinity chromatography. Fractions containing highly purified VP1 were pooled and found to constitute 3.3% of the original E. coli-expressed VP1 protein. Electron microscopy revealed that the VP1 protein was isolated as pentameric capsomeres. Electron microscopy also revealed that capsid-like particles were formed in vitro from purified VP1 capsomeres with the addition of Ca2+ ions and the removal of chelating and reducing agents.

NASA Discipline Developmental Biology↗

Observation of Topological Chirality Switching Induced Freezing of a Skyrmion Crystal

Magnetic skyrmions are topologically protected quasi-particles with a well-defined chirality. Control over their chirality is proposed as an additional feature for encoding data bits or as qubits in quantum computing due to their high efficiency and stability against achiral magnetic textures. Here it is shown that an in-plane magnetic field can be utilized to reshape the energy barriers between different skyrmionic bubbles (e.g., Bloch type, type-II) enabling spontaneous chirality fluctuations with a frequency that increases with the strength of the in-plane field. The insulating van der Waals ferromagnet CrBr3 is used as an archetypal system for low damping, reduced energy dissipation and a high number of magnetic phases to capture the chirality dynamics in real time through cryo-Lorentz transmission electron microscopy. It is observed that the interplay between the intrinsic Dzyaloshinskii–Moriya interaction and out-of-plane field biased the chirality dynamics, favoring one handedness over the other. A remarkable consequence of the spontaneous chirality switching mechanism is that it induces a freezing (or crystallization) process in the skyrmion lattice. As the bubbles fluctuate between Bloch and type-II they elongate and shrink parallel to the in-plane field. Subsequently, the overall lattice crystallizes along the in-plane field direction, inducing a phase transition from a disordered liquid state to a hexatic phase where skyrmions are highly ordered resembling that of a solid. The results indicate chirality as an active element in the creation of topologically protected skyrmion crystals unveiling pathways toward chiral spintronic device platforms with tunable embedded configuration.

2D Phase Transition↗

Solute effects upon dislocation motion and recovery in Mg alloys (Final Report)

The objective the research was to develop a firmer understanding of the interactions between substitutional solute atoms and dislocations within Mg alloys. These interactions govern the absolute and relative mobilities of various types of dislocations in Mg (e.g., basal < a>, non-basal < a>, and pyramidal < c+a>). Furthermore, they have an impact on dislocation recovery processes (e.g., cross-glide, climb, rearrangement, and annihilation). Ultimately, solute-dislocation interactions strongly impact a) strain hardening, b) strain rate sensitivity, c) plastic anisotropy of textured polycrystals, d) texture evolution, e) dislocation substructures evolution, and even f) recrystallization behavior. It is broadly known that Mg alloys exhibit poor low temperature formability. Since formability is largely governed by properties (a) – (c) in this list, it is critical to develop a better understanding of solute-dislocation interactions, if one hopes to improve the situation. While the theory of static solute strengthening is well developed, especially for alloys with face centered cubic (FCC) crystal structures, there are outstanding questions related to applications to hexagonal close packed (HCP) crystal structures and dynamic strain aging (DSA) in materials of various structures. DSA has far-reaching implications for metal formability and, in the case of Mg alloys, appears to correlate with the so-called rare-earth (RE) texture which has been shown to benefit formability. The Portevin-Le Chatelier (PLC) effect, and associated negative strain rate sensitivity, occur at higher temperatures (>100℃) in Mg alloys as compared with similar Al alloys, even though they have similar melting points and solute diffusivities. Our preliminary research has shown that modern, physics-based models of DSA can be tuned to describe the behavior of Mg alloys if a rather higher activation enthalpy is assumed for cross-core diffusivity. While this partially explains the delay in DSA to higher temperatures, it is also hypothesized that this delay is due in part to the intrinsically more thermally activated (rate sensitive) nature of non-basal < a> dislocation motion which is required for macroscopic flow of Mg alloys, whereas octahedral slip in many FCC metals like aluminum is essentially athermal at room temperature. It was originally proposed to employ a combination of in-situ diffraction-based experimental characterization to validate existing theory. It was envisioned to perform in-situ transmission electron microscopy (TEM) to assess individual dislocation behavior and in-situ high-energy X-ray diffraction (HEXRD) techniques which were showing great promise for elucidating collective dislocation behavior, 2 including recovery, especially if the contributions to various forms of diffraction peak broadening (𝜂𝜂,𝜔𝜔,and 2𝜃𝜃) can be effectively integrated. Finally, it was envisioned to perform discrete dislocation dynamics (DDD) modeling approaches to aide in the interpretation of both TEM and HEXRD experiments. In the end, mechanical tests were performed on more complex Mg alloys which exhibited evidence of dynamic strain aging, and this led to the establishment of another project. Mechanical test data obtained at McMaster University served as the basis of an assessment of the applicability of Bazinski’s “stress equivalence” theory of solute strengthening to polycrystalline alloys of Mg. Although we did not succeed in applying the approach to Mg alloys, we did develop expertise with the HEXRD approach using a BCC, β-Ti alloy and demonstrated numerous new capabilities that may be applied to any polycrystalline material in collaboration with researchers at CHESS and around the world: (1) assessment of details of the elastoplastic transition (yielding) using a combination of HEXRD and full-field polycrystal plasticity modeling, (2) the first-ever experimental observation of strong stress rotation within the individual grains of a polycrystalline material, and (3) a comprehensive analysis of the grain-level dislocation density evolution based upon diffraction peak broadening along 𝜂𝜂,𝜔𝜔,and 2𝜃𝜃 directions. This final aspect allowed us to confirm that dislocations were gliding on multiple plane types and not restricted to {110} type planes, and it also provided clues as to why some grains were unloading during straining, with surprising implications for our understanding of the effects of geometrically necessary dislocations (GNDs). Finally, graduate student, Mohammed Shabana, developed a MATLAB code which confirmed the conclusions of Prof. Catalin Picu (Rensallear Polytechnic Institute, RPI) regarding the effect of solute-trapped, forest dislocations on the breaking stress of Lomer lock junctions in FCC metal alloys. He applied the same anisotropic line-tension model to a variety of dislocation junction configurations and found an inconsistency in the widely cited results of Dupuy and Fivel regarding the Hirth Lock, and he outlined an approach to extend these finding to HCP Mg alloys that we are still pursuing with discretionary fundings at UVA.

36 MATERIALS SCIENCE↗

Cave Thiovulum ( Candidatus Thiovulum stygium) differs metabolically and genomically from marine species

Thiovulum spp. (Campylobacterota) are large sulfur bacteria that form veil-like structures in aquatic environments. The sulfidic Movile Cave (Romania), sealed from the atmosphere for ~5 million years, has several aqueous chambers, some with low atmospheric O 2 (~7%). The cave’s surface-water microbial community is dominated by bacteria we identified as Thiovulum. We show that this strain, and others from subsurface environments, are phylogenetically distinct from marine Thiovulum. We assembled a closed genome of the Movile strain and confirmed its metabolism using RNAseq. We compared the genome of this strain and one we assembled from public data from the sulfidic Frasassi caves to four marine genomes, including Candidatus Thiovulum karukerense and Ca. T. imperiosus, whose genomes we sequenced. Despite great spatial and temporal separation, the genomes of the Movile and Frasassi Thiovulum were highly similar, differing greatly from the very diverse marine strains. We concluded that cave Thiovulum represent a new species, named here Candidatus Thiovulum stygium. Based on their genomes, cave Thiovulum can switch between aerobic and anaerobic sulfide oxidation using O 2 and NO 3 - as electron acceptors, the latter likely via dissimilatory nitrate reduction to ammonia. Thus, Thiovulum is likely important to both S and N cycles in sulfidic caves. Electron microscopy analysis suggests that at least some of the short peritrichous structures typical of Thiovulum are type IV pili, for which genes were found in all strains. These pili may play a role in veil formation, by connecting adjacent cells, and in the motility of these exceptionally fast swimmers.

59 BASIC BIOLOGICAL SCIENCES↗

Active Learning Surrogates for Integrating Electron Microscopy and Computational Insights from Simulations in Autonomous Experiments

Artificial Intelligence (AI) combined with simulations and experiments has great potential to accelerate scientific discovery across technology and pharmaceuticals. However, the gap between simulations and experiments is challenging due to disparities in time and scale, making it difficult to estimate properties like energy and electronic states from experiments, and to provide feedback based on theoretical insights.Our research addresses the challenge by developing unique deep kernel based surrogate models that learns from microscopic images, mapping structural features to energy differences from defect formation. We start with full-training using simulated images to determine optimal settings, establishing a baseline for active learning. Using these settings from the baseline, active learning is trained, and predicts structures along simulation trajectories based on uncertainty and energetic stability, thus reducing data requirements, simulation time and computational costs. The results demonstrate that the model achieves a low average error margin of approximately 0.03 meV, indicating good performance. To enhance feature extraction and reconstruction capabilities, we developed an autoencoder-decoder as additional surrogate to create latent space to capture essential features, enabling precise comparisons between simulations and experiments. The results from this model achieved a reconstruction loss of around 0.2 and accurately reconstructed molecular structures.Overall, this work advances the steering of experiments through computational simulations by employing a surrogate models that actively predicts the trajectories of structural evolution, achieving time-to-solution comparable to experimental measurements.

Saranathan, Gayathri [Hewlett-Packard]↗

High signal-to-noise ratio differential conductance spectroscopy

The scanning tunneling microscope (STM) has enabled manipulation and interrogation of surfaces with atomic-scale resolution. Electronic information about a surface is obtained by combining the imaging capability of the STM with scanning tunneling spectroscopy, i.e., measurement of current-voltage (I/V) characteristics of the surface. We propose a change in the STM feedback loop that enables capturing a higher quality dI/dV image. A high frequency dither voltage is added to the bias voltage of the sample, and the fundamental frequency component of the resulting current is demodulated. The in-phase component of this signal is then plotted along with the X and Y position data, constructing the dI/dV image. Here, we show that by incorporating notch filters in the STM feedback loop, we may utilize a high-amplitude dither voltage to significantly improve the quality of the obtained dI/dV image.

42 ENGINEERING↗

Long term effects of low doses of 56Fe ions on the brain and retina of the mouse: ultrastructural and behavioral studies

Eight month old male C57BL6 mice were exposed without anesthesia to whole-body irradiation in circular holders. The mice were tested for behavioral decrements after 0.5 and 50 rads of Fe particle irradiation at 6 and 12 months post irradiation to obtain long term results. A standard maze was used and the animals were timed for completion thereof. A string test also was administered to the mice, testing their ability to grasp and move along a string to safety. The results from animals exposed to 50 rads were significantly different from [correction of fron] control results to p = < .001 in both systems of testing. The hippocampus (believed to be the location of environmental interaction in the brain) and the retina were examined for ultrastructural changes. The ultrastructural changes were similar to those we found in our Cosmos 782, 936 and in our Argon experiments. The mouse data indicate that iron particles were able to induce long term changes in the central nervous system which lead to behavioral impairment.

NASA Program Space Medicine↗

Impact of Controlled Storage Conditions on the Hydrolysis and Surface Morphology of Amorphous-UO 3

The hydration and morphological effects of amorphous (A)-UO 3 following storage under varying temperature and relative humidity have been investigated. This study provides valuable insight into U-oxide speciation following aging, the U-oxide quantitative morphological data set, and, overall, the characterization of nuclear material provenance. A-UO 3 was synthesized via the washed uranyl peroxide synthetic route and aged based on a 3-factor circumscribed central composite design of experiment. Target aging times include 2.57, 7.00, 14.0, 21.0, and 25.4 days, temperatures of 5.51, 15.0, 30.0, 45.0, and 54.5 °C, and relative humidities of 14.2, 30.0, 55.0, 80.0, and 95.8% were examined. Following aging, crystallographic changes were quantified via powder X-ray diffraction and an internal standard Rietveld refinement method was used to confirm the hydration of A-UO 3 to crystalline schoepite phases. The particle morphology from scanning electron microscopy images was quantified using both the Morphological Analysis of MAterials software and machine learning. Results from the machine learning were processed via agglomerative hierarchical clustering analysis to distinguish trends in morphological attributes from the aging study. Significantly hydrated samples were found to have a much larger, plate-like morphology in comparison to the unaged controls. Predictive modeling via a response surface methodology determined that while aging time, temperature, and relative humidity all have a quantifiable effect on A-UO 3 crystallographic and morphological changes, relative humidity has the most significant impact.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Characterization and Quantification of Radiation-Induced Clusters/Precipitates in RPV Steels Using STEM-EDS and Machine Learning

Over the operational lifespan of a nuclear reactor, reactor pressure vessel (RPV) steels are subjected to significant neutron irradiation, resulting in complex microstructural changes and the consequent degradation of mechanical properties. Various physically motivated correlation models have been developed to predict neutron irradiation-induced embrittlement of RPVs under different irradiation conditions. However, the efficient and accurate characterizations and quantification of radiation-induced clusters in RPVs are still challenging, which will affect the precision of the predictive models for embrittlement of RPV components. In the DOE Visiting Faculty Program (VFP) research work at Oak Ridge National Lab (ORNL), I integrate machine learning to aid Scanning Transmission Electron Microscopy – Energy Dispersive X-ray Spectroscopy (STEM-EDS) analyses, which improve the characterization and quantification of radiation-induced clusters in RPV steels, thereby enabling more accurate predictions of material behavior under irradiation. The surveillance base- and welded- RPV steels were annealed at various temperatures of 340 °C, 450 °C and 500 °C for up to 168 hours, respectively. Afterwards, I have characterized radiation-induced clusters using advanced STEM-EDS techniques and subsequently applying machine learning algorithms to analyze and refine STEM-EDS datasets, enhancing the quantification of clusters compositions and distributions. In the end, an efficient workflow for integrating STEM-EDS data analysis with machine learning to address challenges including noise reduction has been developed. The completion of this VFP work will support bridge critical gaps in the accurate quantification of radiation-induced clusters in RPV steels using STEM-EDS and support the development of more precise models for predicting RPV embrittlement in the Light Water Reactor Sustainability program supported by Department of Energy and enhancing the collaboration between ORNL and Alred University. The outcome of the VFP project will leverage a few research papers submission to peer-reviewed journals in the relevant scientific field and a few oral presentations at national and international conferences.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Uniaxial compressive creep tests by spark plasma sintering of 70% theoretical density α -uranium and U-10Zr

Metallic fuels hold numerous advantages over conventional uranium dioxide fuels and are a key component of several liquid metal-cooled advanced reactor concepts including sodium fast reactors. These fuels undergo rapid swelling during early burnup; consequently, they spend most of their reactor lifetime in a porous state. The presence of this porosity alters many of the mechanical properties of the fuel including creep impacting fuel deformation during axial swelling. This work investigates the creep behavior of the porous fuel using a spark plasma sintering technique. Creep tests were performed for the first time on porous α-phase uranium and uranium with 10 wt. % zirconium (U-10Zr) samples. The samples of α-phase uranium and U-10Zr were fabricated from depleted uranium by spark plasma sintering and subjected to uniaxial compressive creep testing. Calculated stress exponents were found to be 2.6±1.6 and 5.7±1.4 for α-U and U-10Zr, respectively, and calculated activation energies were found to be 61.6±1.1kJ/mol for α-U. The creep data were also used to evaluate existing porosity inclusive in creep models.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Chicken (Gallus domesticus) inner ear afferents

Neurons from the vestibular (VG) and the statoacoustic (SAG) ganglion of the chick (Gallus domesticus) were evaluated histologically and morphometrically. Embryos at stages 34 (E8 days), 39 (E13 days) and 44 (E18 days) were sacrificed and temporal bones microdissected. Specimens were embedded in JB-4 methacrylate plastic, and stained with a mixture of 0.2% toluidine blue (TB) and 0.1% basic Fuschin in 25% ethanol or with a mixture of 2% TB and 1% paraphenylenediamine (PDA) for axon and myelin measurement study. Images of the VIIIth nerve were produced by a V150 (R) color imaging system and the contour of 200-300 neuronal bodies (perikarya) was traced directly on a video screen with a mouse in real time. The cross-sectional area of VG perikarya was 67.29 micrometers2 at stage 34 (E8), 128.46 micrometers2 at stage 39 (E13) and 275.85 micrometers2 at stage 44 (E18). The cross-sectional area of SAG perikarya was 62.44 micrometers2 at stage 34 (E8), 102.05 micrometers2 at stage 39 (E13) and 165.02 micrometers2 at stage 44 (E18). A significant cross-sectional area increase of the VG perikarya between stage 39 (E13) and stage 44 (E18) was determined. We randomly measured the cross-sectional area of myelin and axoplasm of hatchling afferent nerves, and found a correspondence between axoplasmic and myelin cross-sectional area in the utricular, saccular and semicircular canal nerve branches of the nerve. The results suggest that the period between stage 34 (E8) and 39 (E13) is a critical period for afferent neuronal development. Physiological and behavioral vestibular properties of developing and maturing hatchlings may change accordingly. The results compliment previous work by other investigators and provide valuable anatomical measures useful to correlate physiological data obtained from stimulation of the whole nerve or its parts.

NASA Discipline Neuroscience↗

Creep Properties of NiAl-1Hf Single Crystals Re-Investigated

NiAl-1Hf single crystals have been shown to be quite strong at 1027 C, with strength levels approaching those of advanced Ni-based superalloys. Initial testing, however, indicated that the properties might not be reproducible. Study of the 1027 C creep behavior of four different NiAl-1Hf single-crystal ingots subjected to several different heat treatments indicated that strength lies in a narrow band. Thus, we concluded that the mechanical properties are reproducible. Recent investigations of the intermetallic NiAl have confirmed that minor alloying additions combined with single-crystal growth technology can produce elevated temperature strength levels approaching those of Ni-based superalloys. For example, General Electric alloy AFN 12 {Ni-48.5(at.%) Al-0.5Hf-1Ti-0.05Ga} has a creep rupture strength equivalent to Rene 80 combined with a approximately 30-percent lower density, a fourfold improvement in thermal conductivity, and the ability to form a self-protective alumina scale in aggressive environments. Although the compositions of strong NiAl single crystals are relatively simple, the microstructures are complex and vary with the heat treatment and with small ingot-toingot variations in the alloy chemistry. In addition, initial testing suggested a strong dependence between microstructure and creep strength. If these observations were true, the ability to utilize NiAl single-crystal rotating components in turbine machinery could be severely limited. To investigate the possible limitations in the creep response of high-strength NiAl single crystals, the NASA Glenn Research Center at Lewis Field initiated an in depth investigation of the effect of heat treatment on the microstructure and subsequent 1027 C creep behavior of [001]-oriented NiAl-1Hf with a nominal chemistry of Ni-47.5Al-1Hf-0.5Si. This alloy was selected since four ingots, grown over a number of years and possessing slightly different compositions, were available for study. Specimens taken from the ingots were subjected to several heat treatment schedules, examined by transmission electron microscopy, and tested in both compression and tension. An example of the microstructure found in a [001]-oriented NiAl-1Hf specimen after a solution treatment at 1317 C for 50 hr followed by air cooling is illustrated in the image on the left, where the NiAl matrix contains a uniform distribution of nanometer-scale Gphase (Ni16Hf6Si7) precipitates. Other heat treating schedules produced microstructures with nanometer-sized G-phase cubes and plates or, in an extreme case, produced a microstructure with all the G-phase converted to Heusler (Ni2AlHf) particles. The results of 1027 C creep strength and strain rate testing are illustrated which summarizes data from tensile and compressive testing of samples cut from all four NiAl-1Hf ingots and subjected to a variety of heat treatment schedules. With one exception, all the strength values lie in a narrow band that spans six orders of magnitude in strain rate. The only factor that produced results outside of this band was the heat treatment schedule that dissolved all the G-phase and replaced it with Heusler precipitates. The results portrayed in this figure lead to the important practical conclusion that the elevated-temperature creep properties of NiAl-1Hf single crystals are reproducible and are not affected by small variations in alloy chemistry from ingot to ingot or by different initial distributions of G-phase in the heat-treated alloy. The only variable in this study that produced a significant and delerious effect on mechanical strength was a post-solution heat treatment that lead to the complete disappearance of the G-phase in favor of Heusler precipitates.

Whittenberger, J. Daniel↗

Transmission Electron Microscopy of Itokawa Regolith Grains

Introduction: In a remarkable engineering achievement, the JAXA space agency successfully recovered the Hayabusa space-craft in June 2010, following a non-optimal encounter and sur-face sampling mission to asteroid 25143 Itokawa. These are the first direct samples ever obtained and returned from the surface of an asteroid. The Hayabusa samples thus present a special op-portunity to directly investigate the evolution of asteroidal sur-faces, from the development of the regolith to the study of the effects of space weathering. Here we report on our preliminary TEM measurements on two Itokawa samples. Methods: We were allocated particles RA-QD02-0125 and RA-QD02-0211. Both particles were embedded in low viscosity epoxy and thin sections were prepared using ultramicrotomy. High resolution images and electron diffraction data were ob-tained using a JEOL 2500SE 200 kV field-emission scanning-transmission electron microscope. Quantitative maps and anal-yses were obtained using a Thermo thin-window energy-dispersive x-ray (EDX) spectrometer. Results: Both particles are olivine-rich (Fo70) with μm-sized inclusions of FeS and have microstructurally complex rims. Par-ticle RA-QD02-0125 is rounded and has numerous sub-μm grains attached to its surface including FeS, albite, olivine, and rare melt droplets. Solar flare tracks have not been observed, but the particle is surrounded by a continuous ~50 nm thick, stuctur-ally disordered rim that is compositionally similar to the core of the grain. One of the surface adhering grains is pyrrhotite show-ing a S-depleted rim (~8-10 nm thick) with nanophase Fe metal grains (<5 nm) decorating the outermost surface. The pyrrhotite displays a complex superstructure in its core that is absent in the S-depleted rim. Particle RA-QD02-0211 contains solar flare particle tracks (~2x109 cm-2) and shows a structurally disordered rim ~100 nm thick. The track density corresponds to a surface exposure of ~103-104 years based on the track production rate of [1]. The dis-ordered rim is nanocrystalline with minor amorphous material between crystalline domains. Quantitative element maps show the outermost ~10 nm of the disordered rim is Si-rich. Discussion and Conclusions: Both particles record the ef-fects of space weathering processes on Itokawa. Noguchi et al. [2] proposed that the disordered rims they observed on Itokawa particles largely result from solar wind radiation damage and we arrive at a similar conclusion for the two particles we analyzed. The microstructure of the S-depleted layer on the pyrrhotite grain in RA-QD02-0125 is similar to that observed in troilite irradiated with ~1018 4 kV He+ [3, 4]. Prolonged irradiation has also been shown to disorder pyrrhotite such that the superstructure reflec-tions are lost [5].

Keller, Lindsay P.↗