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At least 325 records · Page 18

Composition Quantification of SiGeSn Alloys Through Time-of-Flight Secondary Ion Mass Spectrometry: Calibration Methodologies and Validation With Atom Probe Tomography

Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) is a powerful technique for elemental compositional analysis and depth profiling of materials. However, it encounters the problem of matrix effects that hinder its application. In this work, we introduce a pioneering ToF-SIMS calibration method tailored for SixGeySnz ternary alloys. SixGe1-x and Ge1-zSnz binary alloys with known compositions are used as calibration reference samples. Through a systematic SIMS quantification study of SiGe and GeSn binary alloys, we unveil a linear correlation between secondary ion intensity ratio and composition ratio for both SiGe and GeSn binary alloys, effectively mitigating the matrix effects. Extracted relative sensitivity factor (RSF) value from SixGe1-x (0.07 < x < 0.83) and Ge1-zSnz (0.066 < z < 0.183) binary alloys are subsequently applied to those of SixGeySnz (0.011 < x < 0.113, 0.863 < y < 0.935 and 0.023 < z < 0.103) ternary alloys for elemental compositions quantification. These values are cross-checked by Atom Probe Tomography (APT) analysis, an indication of the great accuracy and reliability of as-developed ToF-SIMS calibration process. Furthermore, the proposed method and its reference sample selection strategy in this work provide a low-cost as well as simple-to-follow calibration route for SiGeSn composition analysis, thus driving the development of next-generation multifunctional SiGeSn-related semiconductor devices.

36 MATERIALS SCIENCE↗

On the formation of swelling and related flaws in laser powder bed fusion

Process monitoring in laser powder bed fusion additive manufacturing can provide insights into stochastic anomalies, melt pool and plume dynamics, and part quality. Swelling, a build anomaly where overbuilt material protrudes through the powder layer after recoating, is readily detectable in post-recoat visible light images of the powder bed. Here, this work identifies several of the underlying mechanisms driving swelling formation by analyzing the influence of processing parameters, laser scan paths, and build plate locations on the presence of swelling detected in situ. Swelling near the edge of the part and swelling in the internal region of the part are shown to correlate with different process conditions. Edge and internal swelling may be driven by different phenomena, with edge swelling predominately occurring on the edge of a part facing the laser module and correlated to clusters of near-surface voids (detected with X-ray computed tomography). A larger spot size, higher laser power, and lower scan velocity also increased the presence of edge swelling. Laser spot size and scan path influenced internal swelling, which occurred preferentially with a larger spot size and in regions with large melt pools, caused by localized heat accumulation due to non-optimal processing parameters or scan path strategies. For coupons processed with a slicer-defined maximum scan vector length, swelling seldom occurred at internal vector-stripe boundaries. These results provide a mechanistic understanding of how swelling can be linked to material flaws, insight into how some instances of swelling can be avoided, and evidence supporting the use of swelling as an in situ indicator for quality assurance and part qualification.

Anomaly↗

An intensity-based post-processing tool for 3D instance segmentation of organelles in soft X-ray tomograms

Investigating the 3D structures and rearrangements of organelles within a single cell is critical for better characterizing cellular function. Imaging approaches such as soft X-ray tomography have been widely applied to reveal a complex subcellular organization involving multiple inter-organelle interactions. However, 3D segmentation of organelle instances has been challenging despite its importance in organelle characterization. Here we propose an intensity-based post-processing tool to identify and separate organelle instances. Our tool separates sphere-like (insulin vesicle) and columnar-shaped organelle instances (mitochondrion) based on the intensity of raw tomograms, semantic segmentation masks, and organelle morphology. We validate our tool using synthetic tomograms of organelles and experimental tomograms of pancreatic β -cells to separate insulin vesicle and mitochondria instances. As compared to the commonly used connected regions labeling, watershed, and watershed + Gaussian filter methods, our tool results in improved accuracy in identifying organelles in the synthetic tomograms and an improved description of organelle structures in β -cell tomograms. In addition, under different experimental treatment conditions, significant changes in volumes and intensities of both insulin vesicle and mitochondrion are observed in our instance results, revealing their potential roles in maintaining normal β -cell function. Our tool is expected to be applicable for improving the instance segmentation of other images obtained from different cell types using multiple imaging modalities.

59 BASIC BIOLOGICAL SCIENCES↗

Permeability Hysteresis From Microchannels Opening During Dissolution/Reprecipitation Cycle

Abstract Permeability is a critical parameter for geological resources characterization. Its evolution with respect to porosity is particularly interesting and many research initiatives focus on deriving such relationships, to understand some hydraulic impacts of microstructure alteration. Permeability evolution from chemical reactions, for instance, can become complex as flow channels may open during rock dissolution. In this contribution, we show that this phenomenon can lead to irregular porosity‐permeability curves and permeability hysteresis after reprecipitation. Current approaches describing permeability as a simple function of porosity can therefore not capture this behavior, and we advocate instead the use of dynamic modeling for such scenarios. We demonstrate our approach by modeling a dissolution/precipitation cycle for a unit cell pore channel and quantify the process at larger scale on three different rock samples, whose microstructures are reconstructed from segmented micro‐Computerised Tomography scans.

Lesueur, Martin↗

Skeletal Responses to Long-Duration Simulated Weightlessness in Rats

Damaging effects due to spaceflight and long-duration weightlessness are seen in the musculoskeletal system, specifically with regards to bone loss, bone resorption, and changes in overall bone structure. These adverse effects are all seen with indicators of oxidative stress and a variation in the levels of oxidative gene expression. Once gravity is restored, however, the recovery is slow and incomplete. Despite this, few reports have investigated the correlation between oxidative damage and general modifications within the bone. In this project, we will make use of a ground-based model of simulated weightlessness (hindlimb unloading, HU) in order to observe skeletal changes in response to induced microgravity due to changes in oxidative pressures. With this model we will analyze samples at 14-day and 90-day time points following HU for the determination of acute and chronic effects, each with corresponding controls. We hypothesize that simulated microgravity will lead to skeletal adaptations including time-dependent activation of pro-oxidative processes and pro-osteoclastogenic signals related to the progression, plateau, and recovery of the bone. Microcomputed tomography techniques will be utilized to measure skeletal changes in response to HU. With the results of this study, we hope to further the understanding of skeletal affects as a result of long-duration weightlessness and develop countermeasures to combat bone loss in spaceflight and osteoporosis on Earth.

hindlimb unloading↗

Formation and Consolidation of UN Nanostructures in U-Mo Fuel via Mechanical Alloying and Spark Plasma Sintering

Uranium-molybdenum (U-Mo) alloys show promise as a nuclear fuel system due to their high thermal conductivity and high fuel loading capability. However, U-Mo systems suffer from irradiation induced swelling ultimately affecting the cladding via mechanical and chemical interaction. To address these shortcomings, this thesis investigated the formation of uranium mononitride (UN) nanoparticles within a U-10Mo matrix. To promote the formation of UN, U-10Mo powders were mechanically alloyed under a high purity nitrogen cover gas (99.9995%) atmosphere. Variations were made in stainless steel milling media size, duration of milling, and number of times the milling jar was re-aerated with nitrogen gas. UN nanoparticulates were successfully formed within the U-Mo matrix and was characterized utilizing light element analysis, X-ray diffractometry, scanning and transmission-electron microscopy, electron energy loss spectroscopy, and atom probe tomography. Presence of the UN nanoparticles was found as early as 1-hour into the mechanical alloying process, and significant iron contamination found after 10-hours of milling. The U-Mo/UN powders were compacted using spark plasma sintering techniques in order to stabilize the nanostructure. U-Mo/UN compacts containing small amounts of neodymium and helium were analyzed to observe the defect migration tendencies of fission products within the fuel.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Formation of uranium nitride nanoparticles via mechanical alloying of uranium-molybdenum alloy fuels in gaseous nitrogen

Uranium-molybdenum (U-Mo) alloys show promise as a nuclear fuel system due to their high thermal conductivity and fuel loading capability. However, U-Mo systems are susceptible to irradiation induced swelling ultimately affecting the cladding via mechanical and chemical interactions. To address these shortcomings, this research investigated the formation of uranium mononitride (UN) nanoparticles within a 90 wt% U/10 wt% Mo (U-10Mo) matrix to act as a prospective defect sink for fission products at nanometric hetero-interfaces. To promote the formation of UN, U-10Mo powders were mechanically alloyed under a high purity nitrogen atmosphere. Variations of the milling process investigated included media size, duration of milling, and number of times the milling jar was re-aerated with nitrogen gas. Characterization of the fuel microstructure was completed using light element analysis, X-ray diffraction, scanning and transmission-electron microscopy, electron energy loss spectroscopy, and atom probe tomography. UN nanoparticles measuring 1–5 nm in radius were observed in the U-Mo matrix as early as 1 h into the mechanical alloying process. Milling time in excess of 10 h was found to lead to deleterious effects induced by the stainless-steel milling media.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Proteomic Assessment of Fluid Shifts and Association with Visual Impairment and Intracranial Pressure in Twin Astronauts

BACKGROUND: Astronauts participating in long duration space missions are at an increased risk of physiological disruptions. The development of visual impairment and intracranial pressure (VIIP) syndrome is one of the leading health concerns for crew members on long-duration space missions; microgravity-induced fluid shifts and chronic elevated cabin CO2 may be contributing factors. By studying physiological and molecular changes in one identical twin during his 1-year ISS mission and his ground-based co-twin, this work extends a current NASA-funded investigation to assess space flight induced "Fluid Shifts" in association with the development of VIIP. This twin study uniquely integrates physiological and -omic signatures to further our understanding of the molecular mechanisms underlying space flight-induced VIIP. We are: (i) conducting longitudinal proteomic assessments of plasma to identify fluid regulation-related molecular pathways altered by long-term space flight; and (ii) integrating physiological and proteomic data with genomic data to understand the genomic mechanism by which these proteomic signatures are regulated. PURPOSE: We are exploring proteomic signatures and genomic mechanisms underlying space flight-induced VIIP symptoms with the future goal of developing early biomarkers to detect and monitor the progression of VIIP. This study is first to employ a male monozygous twin pair to systematically determine the impact of fluid distribution in microgravity, integrating a comprehensive set of structural and functional measures with proteomic, metabolomic and genomic data. This project has a broader impact on Earth-based clinical areas, such as traumatic brain injury-induced elevations of intracranial pressure, hydrocephalus, and glaucoma. HYPOTHESIS: We predict that the space-flown twin will experience a space flight-induced alteration in proteins and peptides related to fluid balance, fluid control and brain injury as compared to his pre-flight protein/peptide signatures. Conversely, the trajectory of these protein signatures will remain relatively constant in his ground based co-twin. METHODS: We are using proteomic and standard immunoelectrophoresis techniques to delineate the change in protein signatures throughout the course of a long duration space flight in relation to the development of VIIP. We are also applying a novel cell-based metaboloic organ system assay ("Organs on a Plate") to address how these circulating biomarkers affect physiological processes at the cellular and organ level which could result in VIIP symptoms. These molecular data will be correlated with physiological measures (eg. extra and intracellular fluid volume, vascular filling/flow patterns, MRI, and Optic Coherence Tomography. DISCUSSION: Pre- and in-flight data collection is in progress for the space-flown twin, and similar data have been obtained from the ground-based twin. Biosamples will be batch processed when received from ISS after the conclusion of the 1-year mission. Omic and Physiological measures from the twin astronauts will be compared to similar data being collected on twin subjects who participated in simulated microgravity study. bed rest study.

Rana, Brinda K.↗

Development of Thermal Tomography Imaging System for In-Service Nondestructive Evaluation of Additively Manufactured Components

Additive manufacturing (AM) is an emerging method for cost-efficient fabrication of nuclear reactor parts. AM of metallic structures for nuclear energy applications is currently based on laser powder bed fusion (LPBF) process, which can introduce internal material flaws, such as pores and anisotropy. Integrity of AM structures needs to be evaluated nondestructively because material flaws could lead to premature failures due to exposure to high temperature, radiation and corrosive environment in a nuclear reactor. Thermal tomography (TT) provides a capability for non-destructive evaluation of sub-surface defects in arbitrary size structures. We investigate TT of AM stainless steel 316L specimen with imprinted internal porosity defects using relatively low-cost, small form factor infrared (IR) camera based on uncooled micro bolometer detector. Sparse coding related K-means singular value decomposition (SVD) machine learning, image processing algorithms are developed to improve quality of TT images through removal of Additive white Gaussian noise without blurring the images. Following initial qualification of an AM component for deployment in a nuclear reactor, a compact TT can also be used for in-service nondestructive evaluation (NDE). With capability to perform in-service NDE of the AM component lifecycle, TT data can be used for development of a component digital twin. MIT research reactor (MITR) has been identified as a representative environment to perform investigation of feasibility of in-service NDE during shutdown. Preliminary study of radiation level in the MITR viewport, with geometric parameters potentially compatible with compact TT system, has been conducted.

36 MATERIALS SCIENCE↗

Joint Geophysical and Numerical Insights of the Coupled Thermal‐Hydro‐Mechanical Processes During Heating in Salt

Abstract Salt offers an optimal medium for the permanent isolation of heat‐producing radioactive waste due to its impermeability, high thermal conductivity, and ability to close fractures through creep. A thorough understanding of the thermal‐hydrological‐mechanical (THM) processes, encompassing brine migration, is fundamental for secure radioactive waste disposal within salt formations. At the Waste Isolation Pilot Plant (WIPP), we conducted joint in situ geophysical monitoring experiments during active heating to investigate brine migration near excavations. This experiment incorporated electrical resistivity tomography (ERT) alongside high‐resolution fiber‐optic‐based distributed temperature sensing within a controlled heating experiment. Additionally, discrete element model (DEM) based numerical simulations were conducted to simulate THM processes during heating, providing a more mechanistic understanding of the coupled processes leading to the observed changes in geophysical measurements. During heating, resistivity shifts near the heater were reasonably explained by temperature effects. However, in more distant, cooler regions, the resistivity decrease exceeded predictions based solely on temperature. DEM simulations highlighted brine migration, propelled by pore pressure gradients, as the likely primary factor contributing to the additional resistivity decline beyond temperature effects. The comparison between the predicted ERT responses and observations was much improved when considering the effects of brine migration based on the DEM simulations. These geophysical and simulation findings shed light on brine migration in response to salt heating, enhancing our understanding of the coupled THM processes in salt for safe radioactive waste disposal.

58 GEOSCIENCES↗

Microgravity effects on nonequilibrium melt processing of neodymium titanate: thermophysical properties, atomic structure, glass formation and crystallization

The relationships between materials processing and structure can vary between terrestrial and reduced gravity environments. As one case study, we compare the nonequilibrium melt processing of a rare-earth titanate, nominally 83TiO 2 -17Nd 2 O 3 , and the structure of its glassy and crystalline products. Density and thermal expansion for the liquid, supercooled liquid, and glass are measured over 300–1850 °C using the Electrostatic Levitation Furnace (ELF) in microgravity, and two replicate density measurements were reproducible to within 0.4%. Cooling rates in ELF are 40–110 °C s -1 lower than those in a terrestrial aerodynamic levitator due to the absence of forced convection. X-ray/neutron total scattering and Raman spectroscopy indicate that glasses processed on Earth and in microgravity exhibit similar atomic structures, with only subtle differences that are consistent with compositional variations of ~2 mol. % Nd 2 O 3 . The glass atomic network contains a mixture of corner- and edge-sharing Ti-O polyhedra, and the fraction of edge-sharing arrangements decreases with increasing Nd 2 O 3 content. X-ray tomography and electron microscopy of crystalline products reveal substantial differences in microstructure, grain size, and crystalline phases, which arise from differences in the melt processes.

36 MATERIALS SCIENCE↗

Microgravity Effects on Nonequilibrium Melt Processing of Neodymium Titanate: Thermophysical Properties, Atomic Structure, Glass Formation and Crystallization

The relationships between materials processing and structure can vary between terrestrial and reduced gravity environments. As one case study, we compare the nonequilibrium melt processing of a rare-earth titanate, nominally 83TiO 2 -17Nd 2 O 3 , and the structure of its glassy and crystalline products. Density and thermal expansion for the liquid, supercooled liquid, and glass are measured over 300–1850 °C using the Electrostatic Levitation Furnace (ELF) in microgravity, and two replicate density measurements were reproducible to within 0.4%. Cooling rates in ELF are 40–110 °C s −1 lower than those in a terrestrial aerodynamic levitator due to the absence of forced convection. X-ray/neutron total scattering and Raman spectroscopy indicate that glasses processed on Earth and in microgravity exhibit similar atomic structures, with only subtle differences that are consistent with compositional variations of ~2 mol. % Nd 2 O 3 . The glass atomic network contains a mixture of corner- and edge-sharing Ti-O polyhedra, and the fraction of edge-sharing arrangements decreases with increasing Nd 2 O 3 content. X-ray tomography and electron microscopy of crystalline products reveal substantial differences in microstructure, grain size, and crystalline phases, which arise from differences in the melt processes.

thermophysical properties↗

Micro X-ray computed tomography examination of mini plate fuel with hot isostatic pressed aluminum cladding

In order to minimize proliferation risks and improve security of nuclear material, the United States high performance research and test reactors (USHPRR) program is tasked with converting nuclear reactors that are fueled with highly enriched uranium (HEU) fuels to operate with low-enriched uranium (LEU) nuclear fuels. One favorable LEU fuel configuration is plate fuel with a metallic uranium-molybdenum foil clad within an aluminum alloy (AA 6061). In this fuel, the aluminum cladding is bonded with a hot isostatic pressing (HIP) method to seal the cladding around the fuel meat. However, the HIP process parameters influence the cladding performance, as a defective or incomplete bond can cause a pathway for corrosion. Micro X-ray computed tomography (XCT), a nondestructive technique that provides volumetric imaging, can be applied to inspect fuel plate cladding at the engineering scale. In this work, XCT methodology was developed and successfully utilized to not only observe the bond line of unirradiated mini fuel plates, but to also identify subsurface abnormalities in the plates’ cladding. Importantly, in future work, this technique could be applied to fuel plates, pre- and post-irradiation, to quantify irradiation effects on cladding defects and bond line integrity.

36 MATERIALS SCIENCE↗

Computed Tomography 3-D Imaging of the Metal Deformation Flow Path in Friction Stir Welding

In friction stir welding (FSW), a rotating threaded pin tool is inserted into a weld seam and literally stirs the edges of the seam together. To determine optimal processing parameters for producing a defect free weld, a better understanding of the resulting metal deformation flow path is required. Marker studies are the principal method of studying the metal deformation flow path around the FSW pin tool. In our study, we have used computed tomography (CT) scans to reveal the flow pattern of a lead wire embedded in a FSW weld seam. At the welding temperature of aluminum, the lead becomes molten and is carried with the macro-flow of the weld metal. By using CT images, a 3-dimensional (3D) image of the lead flow pattern can be reconstructed. CT imaging was found to be a convenient and comprehensive way of collecting and displaying tracer data. It marks an advance over previous more tedious and ambiguous radiographic/metallographic data collection methods.

Schneider, Judy↗

Acoustic Travel-Time Tomography for Wind Energy

New remote sensing technologies for direct observation of the atmospheric flow in the proximity of operating wind turbines are necessary for the advancement of wind turbine design, wind plant control, and the validation of high-fidelity numerical models; fundamental goals of the DOE Wind Energy Technology Office's (WETO's) A2e program. Modern remote sensing technologies for commercial and research applications rely on the backscatter of light or sound waves, which limits spatial and temporal resolution and cannot produce reliable flow estimates near solid bodies or reflective surfaces. Acoustic tomography (AT) is an innovative sensing technology based on fundamental thermodynamic properties of the atmosphere and an inverse algorithm that can reconstruct both velocity and temperature fields within a network of acoustic transducers. AT relies on the direct travel path of acoustic signals between speakers and microphones in the network and can achieve much higher resolutions than conventional backscatter technologies. For wind energy R&D applications, AT represents an extremely economical option over other remote sensing technologies, integrating mature and commonly available acoustic and signal processing hardware. This report is intended as an update on the development of the AT array on the NREL Flatirons Campus (FC) and includes a brief review of the instrumentation, the calibration of equipment, signal processing, and resulting flow field estimates. Designs for future AT systems and applications are detailed in this report, including summaries of new capabilities, engineering and theoretical challenges, and anticipated costs help to outline future directions for AT technology R\&D. The potential for application of AT to utility-scale turbines is also discussed. Investing in the development of the proposed instrument will establish AT as a transformational RS technique that represents a significant advance in measurement instrumentation, enabling new fundamental insights into the structure of the atmospheric boundary layer and supporting applications for wind energy, pollution transport, and resource characterization. AT is also an extremely economical option over other RS instruments, integrating mature and commonly available acoustic and signal processing hardware.

17 WIND ENERGY↗

Seeing the whole picture: Methods for getting the most from micro X-ray computed tomography of TRISO nuclear fuel particles

Tristructural isotropic (TRISO) coated fuel particles are a nuclear fuel form under extensive study for use in advanced nuclear reactor concepts. TRISO fuels are subjected to high temperature neutron irradiations and then examined to assess their performance by determining fission product retention and studying morphological changes. Micro X-ray computed tomography is one method of nondestructively studying the effects of TRISO performance. This work addresses the need for image processing to remove X-ray tomographic reconstruction artifacts that prevent the study of TRISO features, as the TRISO particles’ high Z kernel can introduce metal artifacts that degrade the image quality in the surrounding low Z coating layers. These metal artifacts were reduced by imaging the TRISO particles with both high- and low-energy X-rays and applying a mask to the radiographs obtained with low-energy X-rays to digitally remove the dense fuel kernel region. These masked radiographs were then used to produce a tomographic reconstruction which was combined with the tomographic reconstruction of the high-energy data. This enabled the relatively-low-density TRISO buffer layer to be examined in more detail, providing information on irradiation induced dimensional changes of the coatings. This methodology, which helps see the full picture of a TRISO particle, is not limited to nuclear fuels but can be applied to systems that contain highly attenuating material surrounded by less dense materials.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

High Density of Strong yet Deformable Intermetallic Nanorods Leads to an Excellent Room Temperature Strength-Ductility Combination in a High Entropy Alloy

This paper introduces a new microstructural template for high entropy alloys (HEAs), where the face centered cubic (FCC) complex concentrated solid solution is reinforced with a high density of strong, yet deformable, nanorods of an ordered multi-component intermetallic L12 compound. Thermodynamic modeling has been employed to design this HEA with a large L12 volume fraction. Thermo-mechanical processing by isothermal annealing of the conventionally processed bulk cold-rolled alloy directly at precipitation temperatures, has been applied to produce a high density of uniformly distributed L12 nanorods within refined FCC grains, resulting from concomitant recrystallization and discontinuous precipitation processes. The nanorod morphology of the discontinuous L12 product has been established from three-dimensional atom probe tomography. The refined grains result in a complete coverage of the microstructure with discontinuously precipitated intermetallic nanorods. This nanorod strengthened HEA exhibits an exceptionally high room temperature yield strength of ~1630 MPa, good tensile ductility of ~15%, and an ultimate tensile strength of ~1720 MPa. Furthermore, a single L12 phase alloy, melted based on the precipitate composition in the two-phase FCC + L12 HEA, exhibits very high compressive deformability and strain hardenability, unusual for ordered intermetallic compounds. These results open a new strategy for design of fine-grained microstructures strengthened via ordered intermetallic phases, exploiting the beneficial effects of discontinuous precipitation, for achieving very high room temperature tensile strengths while maintaining good ductility.

Gwalani, Bharat↗

Mechanistic understanding of speciated oxide growth in high entropy alloys

Abstract Complex multi-element alloys are gaining prominence for structural applications, supplementing steels, and superalloys. Understanding the impact of each element on alloy surfaces due to oxidation is vital in maintaining material integrity. This study investigates oxidation mechanisms in these alloys using a model five-element equiatomic CoCrFeNiMn alloy, in a controlled oxygen environment. The oxidation-induced surface changes correlate with each element’s interactive tendencies with the environment, guided by thermodynamics. Initial oxidation stages follow atomic size and redox potential, with the latter becoming dominant over time, causing composition inversion. The study employs in-situ atom probe tomography, transmission electron microscopy, and X-ray absorption near-edge structure techniques to elucidate the oxidation process and surface oxide structure evolution. Our findings deconvolute the mechanism for compositional and structural changes in the oxide film and will pave the way for a predictive design of complex alloys with improved resistance to oxidation under extreme conditions.

36 MATERIALS SCIENCE↗