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At least 73 records · Page 4

Analysis of neptunium oxides produced through modified direct denitration

Production of neptunium-237 ( 237 Np) target materials for plutonium-238 ( 238 Pu) radioisotope thermoelectric generators (RTGs) for deep space exploration requires advanced chemistry and engineering development. Currently, the domestic Pu-238 Supply Program at Oak Ridge National Laboratory produces neptunium dioxide (NpO 2 ) for target material using a modified direct denitration (MDD) flowsheet. Although the chemistry, reaction mechanisms, and product characteristics of MDD are well understood for uranium, corresponding studies of the neptunium system are still needed to continue optimization of target material properties, production equipment design, and production flowsheets. Here, the objective of this work is to characterize crystalline phases, morphology, surface texture, and particle size of NpO 2 produced via MDD reactions. Solid-phase characterization techniques, including powder X-ray diffraction (pXRD) and scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS), were employed to achieve this objective. Subsequent data processing using the Morphological Analysis for Material Attribution (MAMA) software was performed to analyze particle morphology and size. Broadly, the powders were found to contain a mixture of NpO 2 and Np 2 O 5 after denitration with a variety of morphologies. After high-firing, the product was found to be NpO 2 with a typical polycrystalline oxide morphology and a grain size ranging from 0.72 to 0.94 µm. These analyses provide knowledge on the reaction pathway for a non-traditional NpO 2 synthesis method and offer additional unique insight into production-scale environments for transuranic materials.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Crystal Size Distributions from Porphyritic Olivine Chondrules: Insights into Formation Conditions

Most chondrules preserve, in their texture, a record of their precursor material and the nature and intensity of the nebular events in which they were formed. We have used crystal size distributions (CSDs) together with crystallization experiments to explore the textures of natural chondrules and their relationships to natural formation conditions. Many careful experimental studies have demonstrated fundamental relationships between the texture of a chondrule and its precursor material, melting intensity, and cooling rate. However, until recently most studies have focused on distinctions between textural types (e.g., barred, radial, porphyritic). Previous work has shown that CSDs provide precise, reproducible characterizations of chondrule-scale textures, and can be used together with crystallization experiments to estimate chondrule formation conditions. Here, we expand this study to investigate the link between texture and formation conditions for a range of natural porphyritic olivine (PO) chondrules.

Zieg, M. J.↗

Grain structure and texture selection regimes in metal powder bed fusion

Additive manufacturing (AM) offers opportunities to produce complex part geometries not possible with conventional processing and in some cases even improve part performance. However, adoption has been slowed by difficulties assessing microstructure variability and there is no straightforward approach to relate processing to grain structure characteristics. In this study, datasets from AdditiveFOAM heat transport simulations of laser powder bed fusion (LPBF) are used to drive ExaCA simulations of grain structure. The GPU utilization of ExaCA and an algorithmic update for modeling melt pool overlap region solidification enabled rapid and parallel simulation across a wider range of process conditions than previously explored with cellular automata-based solidification models. A texture selection angle $θ_s$ is defined based on melt pool overlap geometry, and the range of $θ_s$ over which a commonly observed texture transition occurs in characterized AM builds was well-reproduced by ExaCA simulations over a wide range of melt pool shape, hatch spacing, and layer height. ExaCA simulations with 90 degree rotation of the scan direction on every other layer reproduced a number of trends from the AM literature including grain refinement, the dominance of layers with larger melt pools on the final grain structure, and the weakening or strengthening of texture depending on odd and even layer melt pool overlap geometry. EBSD data from a benchmark AM part is used to validate the simulated mechanism of a layer rotation-induced texture strengthening effect. Importantly, these results expand the understanding of the mechanisms for texture selection in alloys with cubic crystal symmetry and offer an approach to easily evaluate processing conditions. With this new understanding, these modeling tools will enable anticipation of previously unexpected variations in grain structure and target specific microstructures and properties.

36 MATERIALS SCIENCE↗

Automated site characterization for robotic sample acquisition systems

A mobile, semi-autonomous vehicle with multiple sensors and on-board intelligence is proposed for performing preliminary scientific investigations on extraterrestrial bodies prior to human exploration. Two technologies, a hybrid optical-digital computer system based on optical correlator technology and an image and instrument data analysis system, provide complementary capabilities which might be part of an instrument package for an intelligent robotic vehicle. The hybrid digital-optical vision system could perform real-time image classification tasks using an optical correlator with programmable matched filters under control of a digital microcomputer. The data analysis system would analyze visible and multiband imagery to extract mineral composition and textural information for geologic characterization. Together these technologies would support the site characterization needs of a robotic vehicle for both navigational and scientific purposes.

Scholl, Marija S.↗

Computational Characterization and Model Verification for 3D Microstructure Reconstruction of Additively-Manufactured Materials

The goal of this study is to characterize and validate the texture and grain topology of additively-manufactured anisotropic three-dimensional (3D) polycrystalline microstructures. The special focus is on developing methodologies to compare the grain shapes and orientations of two-dimensional (2D) and 3D microstructure representations using the same metric. To generate statistical data, synthetic microstructures are reconstructed from experimental data using Markov random field (MRF). The statistical similarity between the experimental and synthetic microstructures is verified by comparing their grain topologies. A universal measure to compare 2D and 3D grains is portrayed through the concept of image moments that are invariant to shape transformations. The graphical plots developed based on moment invariants to compare the 2D and 3D grains are used to verify the synthetic model

Materials Characterization↗

Microstructural Evolution of the Civet Cat Norite (72255)

The ‘Civet Cat Norite’ is a ~ 2.5 cm clast within the Apollo impact melt breccia sample 72255 collected during Apollo 17 EVA 2 at Boulder 1. The norite is primarily composed of plagioclase and orthopyroxene with fine-scale exsolution lamellae of augite. The plagioclase and orthopyroxene (OPX) coexist with minor quartz and augitic clinopyroxene (CPX), and accessory apatite, baddeleyite, chromite, ilmenite, loveringite, merrillite, rutile and zircon. The major minerals range from 1 to 4 mm in size and show a cataclastic texture indicated by banding of the light and dark phases]. The chemical composition of the orthopyroxene, augitic exsolution lamellae, and exsolved oxides suggest the norite crystallized in the lower crust of the Moon (10 – 70 km depth) and was subsequently excavated by impact(s). Shock pressure estimates for the norite range from 15 – 35 GPa based on maskeleynite formation within the plagioclase, kink banding in pyroxenes, and granular recrystallization in the accessory phosphates. Previous Rb-Sr and 40 Ar/ 39 Ar analyses recalculated with modern decay constants yield relatively young ages of 4.16 ± 0.05 Ga and 3.99 ± 0.03 Ga, respectively. However, recent U-Pb analyses of some zircon grains from within the Civet Cat yield an age of 4.45 ± 0.03 Ga. While this is the oldest age for any rock recovered from the Moon, the full age spread of zircon from the Civet Cat range from ca. 4.46 to 4.02 Ga, indicating variable Pb-loss and complicating interpretation of the primary age. Recent atom probe analyses indicate minimal Pb mobilization within the oldest zircon grain from Civet Cat, supporting the interpretation that these ancient zircon ages reflect the age of the norite, rather than an apparent antiquity caused by reverse discordance. To investigate the potential antiquity and deep crustal origin of the Civet Cat norite, we have undertaken high resolution microstructural analyses of the major, minor, and accessory minerals to characterize the primary igneous textures and secondary overprinting by impact and metamorphism. The employed analytical techniques include scanning electron microscope-based electron backscatter diffraction (EBSD) analyses, electron probe microanalyzer (EPMA) chemical analyses, and transmission electron microscopy (TEM) of pyroxene, plagioclase, quartz, zircon, and phosphates.

T M Erickson↗

Characterizing microscale signatures in uranium ore concentrates using electron probe microanalyzer

Impurities in uranium ore concentrates (UOCs) serve as forensic signatures of processing history and origin. Here, this study utilizes Electron Probe Microanalyzer (EPMA) to characterize microscale compositional and textural features in individual UOC particles from both commercial and bench-scale production. At the particle scale, multiple internal phases with distinct morphologies, chemical signatures, and stoichiometries are documented. Our data shows that chemical impurities are heterogeneously distributed within single particles and among particles within a sample. These microscale heterogeneities correlate with known processing histories, indicating that microscale signatures of early fuel cycle materials can provide valuable information for nuclear forensic material analysis.

organic↗

Evolution of microstructure and strength of a high entropy alloy undergoing the strain-induced martensitic transformation

In a recent work, we have reported outstanding strength and work hardening exhibited by a metastable high entropy alloy (HEA), Fe 42 Mn 28 Co 10 Cr 15 Si 5 (in at. %), undergoing the strain-induced martensitic transformation from metastable gamma austenite (γ) to stable epsilon martensite (ε). However, the alloy exhibited poor ductility, which was attributed to the presence of the brittle sigma (σ) phase in its microstructure. The present work reports the evolution of microstructure, strength, and ductility of a similar HEA, Fe 38.5 Mn 20 Co 20 Cr 15 Si 5 Cu 1.5 (in at. %), designed to suppress the formation of σ phase. A cast and then rolled plate of the alloy was processed into four conditions by annealing for 10 and 30 min at 1100 °C and by friction stir processing (FSP) at tool rotation rates of 150 and 400 revolutions per minute (RPM) to facilitate detailed examinations of variable initial grain structures. Neutron diffraction and electron microscopy were employed to characterize the microstructure and texture evolution. The initial materials had variable grain size but nearly 100% γ structure. Diffusionless strain induced γ→ε phase transformation took place under compression with higher rate initially and slower rate at the later stages of deformation, independent on the initial grain size. The transformation facilitated part of plastic strain accommodation and rapid strain hardening owing to a transformation-induced dynamic Hall-Petch-type barrier effect, increase in dislocation density, and texture. Here, the peak strength of nearly 2 GPa was achieved under compression using the structure created by double pass FSP (150 RPM followed by 150 RPM). Remarkably, the tensile elongation exhibited by the alloy was nearly 20% with fracture surfaces featuring a combination of ductile dimples and cleavage.

36 MATERIALS SCIENCE↗

Why does a phosphonium-phosphinate ionic liquid protect the contact surfaces from wear and micropitting but increase vibration when used as an additive in rolling-sliding lubrication?

A phosphonium-phosphinate ionic liquid (IL) was studied as a lubricant additive for rolling-sliding contacts. The bench-scale test was designed to simulate automotive rear axle operation during cold start, highway towing, and overload conditions. Adding such an IL (2%) into a base oil significantly reduced wear loss and rolling contact fatigue, e.g., microcracking and micropitting, but made the vibrational noise notably higher under a low (-1.5%) sliding roll ratio (SRR). Additionally, worn surface characterization revealed an interesting texture pattern with alternating smoother plateaus and rougher valleys, which is believed to cause the high vibration. No increased vibration was observed at a high (-30%) SRR, possibly because the more aggressive sliding abrasion prevented such a surface texture from forming.

36 MATERIALS SCIENCE↗

Magnetic skyrmionic structures with variable topological charges in engineered Dzyaloshinskii-Moriya interaction systems

Magnetic skyrmionic structures, including magnetic skyrmions and antiskyrmions, are characterized by swirling spin textures with non-trivial topologies. They are featured with specific topological charges, Q , which are of crucial importance in determining their topological properties. Owing to the invariance of the chiral nature, it is generally believed that Q is conserved in a given magnetic skyrmionic structure and is hard to alter. Here, we experimentally realize the control of Q of magnetic skyrmionic structures at room temperature in a Dzyaloshinskii-Moriya interaction (DMI) platform with spatially alternating signs. Depending on how many times it crosses the interfaces between DMI regions with opposite signs, the magnetic skyrmionic structures possess different Q . Modifying the DMI energy landscape through chemisorbed oxygen, a magnetic topological transition is realized. This creation and manipulation of magnetic skyrmionic structures with controllable Q , in particular the DMI-stabilized thin-film antiskyrmions and high- Q skyrmionic structures, enables a new degree of freedom to control their dynamics via a novel DMI confinement effect. Our findings open up an unexplored avenue on various topological magnetic skyrmionic structures and their potential applications.

magnetic properties and materials↗

Frieze charge-stripes in a correlated kagome superconductor

In kagome metals, geometric frustration, electronic correlations and band topology combine to produce a wide range of intriguing phenomena. Among them, CsCr$_3$Sb$_5$ offers an opportunity to investigate unconventional superconductivity in a strongly correlated kagome system, with indications of frustrated magnetism and quantum criticality. Here, we demonstrate a cascade of density-wave transitions with distinct symmetries in bulk single crystals of CsCr$_3$Sb$_5$. Using spectroscopic imaging scanning tunneling microscopy, we uncover a unidirectional density wave that breaks all mirror symmetries -- resembling a chiral density wave -- but that also retains a mirror glide symmetry. We refer to this as a frieze charge stripe order phase, as its symmetry properties correspond to one of the fundamental frieze symmetry groups. A combination of high-resolution imaging, Fourier analysis and theoretical simulations reveal the key role of sublattice degrees of freedom in stabilizing this phase, characterized by internal chiral textures of opposite handedness. These findings suggest that superconductivity in CsCr$_3$Sb$_5$ emerges from this distinct density wave state and provide fresh insight into realizing electronic phases governed by frieze symmetry groups in quantum materials.

Cheng, Siyu [Boston College, Chestnut Hill, MA (Un↗

Current-induced switching of thin film α - Fe 2 O 3 devices imaged using a scanning single-spin microscope

Electrical switching of Néel order in an antiferromagnetic insulator is desirable as a basis for memory applications. Unlike electrically driven switching of ferromagnetic order via spin-orbit torques, electrical switching of antiferromagnetic order remains poorly understood. Here we investigate the low-field magnetic properties of 30-nm-thick, c-axis-oriented α-Fe 2 ⁢O 3 Hall devices using a diamond nitrogen-vacancy center scanning microscope. Using the canted moment of α-Fe 2⁢ O 3 as a magnetic handle on its Néel vector, we apply a saturating in-plane magnetic field to create a known initial state before letting the state relax in low field for magnetic imaging. Here, we repeat this procedure for different in-plane orientations of the initialization field. We find that the magnetic field images are characterized by stronger magnetic textures for fields along [$\overline{11}$20] and 11$\overline{2}$0, suggesting that despite the expected 3-fold magnetocrystalline anisotropy, our α-Fe 2 ⁢O 3 thin films have an overall in-plane uniaxial anisotropy. We also study current-induced switching of the magnetic order in α-Fe 2 ⁢O 3 . We find that the fraction of the device that switches depends on the current pulse duration, amplitude, and direction relative to the initialization field.

36 MATERIALS SCIENCE↗

Postweld Heat Treatment on Toughness of Electric- Resistance Welded X70 Steel

In this report the effect of postweld heat treatment (PWHT) on Charpy V-notch impact toughness of a highfrequency electric-resistance welded (HF-ERW) grade X70 pipeline steel is investigated. PWHT thermal cycles are simulated using the Gleeble on the as-welded specimens. Microstructure, along with crystallographic texture and microhardness, is characterized in specimens that are impact tested at –5°C (23°F), –30°C (–22°F), and –45°C (–49°F). The impact toughness values show a wide scatter band and decrease with the increasing peak temperature of the PWHT. For higher peak temperatures, the microstructure of the heat-affected zone (HAZ) gradually changed from equiaxed ferrite to bainitic ferrite. Furthermore, the prior austenite grain size (PAGS) increases with the increasing peak temperature. The density of high-angle grain boundaries decreases, and the fraction of cleavage planes {100} parallel to the impact fracture plane increases for higher peak temperatures of the PWHT

36 MATERIALS SCIENCE↗

Sm-Nd, Rb-Sr, and Mn-Cr Ages of Yamato 74013

Yamato 74013 is one of 29 paired diogenites having granoblastic textures. The Ar-39 - Ar-40 age of Y-74097 is approximately 1100 Ma. Rb-Sr and Sm-Nd analyses of Y-74013, -74037, -74097, and -74136 suggested that multiple young metamorphic events disturbed their isotopic systems. Masuda et al. reported that REE abundances were heterogeneous even within the same sample (Y-74010) for sample sizes less than approximately 2 g. Both they and Nyquist et al. reported data for some samples showing significant LREE enrichment. In addition to its granoblastic texture, Y-74013 is characterized by large, isolated clots of chromite up to 5 mm in diameter. Takeda et al. suggested that these diogenites originally represented a single or very small number of coarse orthopyroxene crystals that were recrystallized by shock processes. They further suggested that initial crystallization may have occurred very early within the deep crust of the HED parent body. Here we report the chronology of Y-74013 as recorded in chronometers based on long-lived Rb-87 and Sm-147, intermediate- lived Sm-146, and short-lived Mn-53.

Nyquist, L. E.↗

Mars Sample Return: The Next Step Required to Revolutionize Knowledge of Martian Geological and Climatological History

The capability of scientific instrumentation flown on planetary orbiters and landers has made great advances since the signature Viking mission of the seventies. At some point, however, the science return from orbital remote sensing, and even in situ measurements, becomes incremental, rather than revolutionary. This is primarily caused by the low spatial resolution of such measurements, even for landed instrumentation, the incomplete mineralogical record derived from such measurements, the inability to do the detailed textural, mineralogical and compositional characterization needed to demonstrate equilibrium or reaction paths, and the lack of chronological characterization. For the foreseeable future, flight instruments will suffer from this limitation. In order to make the next revolutionary breakthrough in understanding the early geological and climatological history of Mars, samples must be available for interrogation using the full panoply of laboratory-housed analytical instrumentation. Laboratory studies of samples allow for determination of parageneses of rocks through microscopic identification of mineral assemblages, evaluation of equilibrium through electron microbeam analyses of mineral compositions and structures, determination of formation temperatures through secondary ion or thermal ionization mass spectrometry (SIMS or TIMS) analyses of stable isotope compositions. Such details are poorly constrained by orbital data (e.g. phyllosilicate formation at Mawrth Vallis), and incompletely described by in situ measurements (e.g. genesis of Burns formation sediments at Meridiani Planum). Laboratory studies can determine formation, metamorphism and/or alteration ages of samples through SIMS or TIMS of radiogenic isotope systems; a capability well-beyond flight instrumentation. Ideally, sample return should be from a location first scouted by landers such that fairly mature hypotheses have been formulated that can be tested. However, samples from clastic sediments derived from an extensive region of Mars can provide important, detailed understanding of early martian geological and climatological history. Interrogating clastic "sediments" from the Earth, Moon and asteroids has allowed discovery of new crustal units, identification of now-vanished crust, and determination of the geological history of extensive, remote regions. Returned sample of martian fluvial and/or aeolian sediments, for example from Gale crater, could be "read like a book" in terrestrial laboratories to provide truly revolutionary new insights into early martian geological and climatological evolution.

Mittlefehldt, D. W.↗

Are you using the right probe molecules for assessing the textural properties of metal–organic frameworks?

Textural properties—such as the surface area, pore size distribution, and pore volume—are at the forefront of characterization for porous materials. Therefore, it is essential to accurately and reproducibly report a material's textural properties as they could ultimately dictate its applicability. This work aims to provide insightful and comprehensive studies of textural properties for a set of metal–organic frameworks (MOFs), a class of porous materials, using various gases to equip researchers in the field with a helpful guide and reference. Here, we selected a series of nine MOFs with different surface areas, pore sizes, shapes, and chemical environments to represent a wide range of materials. We probed the textural properties of these MOFs using traditional and distinctive gases: N 2 , Kr and O 2 at 77 K, Ar at 87 K, and CO 2 at 195 and 273 K. With regard to surface area, we discuss the validity and challenges associated with the current BET method, the importance of utilizing the Rouquerol et al. consistency criteria to ensure accuracy and reproducibility, and the recommended gas probes for certain materials. For pore size distribution, we discuss the efficacy of each probe for determining the pore sizes within a porous material relative to the calculated distribution from its crystal structure, the limitations of current computational kernels used to calculate pore size distributions, and the need for advanced kernels to envelope the diversity of porous materials. Finally, for pore volume, we discuss the use of the Gurvich rule to obtain the total pore volume in comparison with calculated values from crystal structures and its consistency as a metric for porous materials. Ultimately, we hope that this article will aid researchers in characterizing the textural properties of porous materials and encourage the development of new kernels capable of encompassing the complexity of MOFs and other porous materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Ion beam texturing

A microscopic surface texture is created by sputter etching a surface while simultaneously sputter depositing a lower sputter yield material onto the surface. A xenon ion beam source has been used to perform this texturing process on samples as large as three centimeters in diameter. Ion beam textured surface structures have been characterized with SEM photomicrographs for a large number of materials including Cu, Al, Si, Ti, Ni, Fe, Stainless steel, Au, and Ag. Surfaces have been textured using a variety of low sputter yield materials - Ta, Mo, Nb, and Ti. The initial stages of the texture creation have been documented, and the technique of ion beam sputter removal of any remaining deposited material has been studied. A number of other texturing parameters have been studied such as the variation of the texture with ion beam power, surface temperature, and the rate of texture growth with sputter etching time.

Hudson, W. R.↗

Microstructural Record of Evolving Condensation Processes in Fine-Grained Ca-Al-Rich Inclusions from the Reduced CV3 Chondrites

Fine-grained, spinel-rich Ca-Al-rich inclusions (FGIs) in carbonaceous chondrites consist of numerous layered nodules having cores of spinel, hibonite, and/or perovskite surrounded by multiple thin layers of melilite, anorthite, diopside, and/or olivine. They are interpreted as aggregates of direct high-temperature condensates from an 16O-rich nebular gas that escaped significant melting. However, FGIs are very complex objects composed of intimate intergrowths of fine-grained refractory phases and show extremely large variations in mineralogy, modal abundance, and textures. Thus, detailed FIB/TEM analyses of FGIs are required to fully characterize their micro-to-nanometer scale textures, mineralogy, and chemical compositions and hence elucidate their formation processes and conditions in the early solar nebula. Here, we present our on-going study of pristine FGIs from the reduced CV3 chondrites Efremovka and Thiel Mountains (TIL) 07003 and 07007 that have minimal evidence for secondary parent body alteration.

Han, J.↗