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At least 73 records · Page 4

Web-based Preprocessing and Visualization of 3D FIB Tomography Data for Nuclear Fuel Characterization

Three-dimensional (3D) focused ion beam (FIB) tomography enables reconstruction of internal nuclear fuel features that can't be fully evaluated through surface imaging alone. This capability supports characterization of fuel constituents and defects under thermal and irradiation conditions relevant to microreactor development. However, large tomography datasets can create data-handling, loading, and visualization challenges, especially when image-stack preparation and file conversion must be completed with separate tools. The Computational Ultraspatial Tomography Toolkit for High-Resolution Object Analysis Tools (CUTTRHOAT) is an open-source web application being developed to display FIB tomography datasets available through the Nuclear Research Data System (NRDS). The current alpha version requires prepared HDF5 datasets and has limited integrated data-preparation capabilities. This project improves CUTTHROAT by adding dataset-folder selection, automatic input detection, dataset scanning, missing-slice identification, blank-slice insertion, and image-stack-to-HDF5 conversion. Two applications will be compared: the baseline CUTTHROAT alpha workflow and the updated application containing the integrated data-handling and preprocessing functions. Evaluation will consider dataset detection accuracy, conversion success, loading time, rendering responsiveness, application stability, and user interaction. Preliminary results demonstrate successful loading of existing HDF5 files and converted image stacks, while testing also identified performance reductions caused by excessive blank-slice generation. The updated workflow reduces reliance on external preparation tools and supports more direct movement from image stacks to color-code 3D visualization. Future work includes refining missing-slice handling, integrating additional preprocessing functions, like a denoising feature, parsing TIFF metadata for automatic voxel scaling, and adding manual X, Y, and Z voxel-spacing inputs for PNG and JPEG.

36 - MATERIALS SCIENCE↗

3013 Inner Container Closure Weld Region (ICCWR) Characterization by Wide Area 3D Measurement System (WAMS) Analysis (FY21 Progress Report)

As part of the 3013 Surveillance Program, through-wall penetration from stress corrosion cracking (SCC) of the 3013 inner containers has been identified as the most credible condition for failure withing the 50- years lifetime. Chlorides contained in Pu-bearing material, together with intra-canister humidity levels, metallurgical conditions, and internal stresses have been found to produce corrosion in the Inner Container Closure Weld Region (ICCWR) of the 3013 canister system. A Laser Confocal Microscope (LCM) is used as part of the 3013 Surveillance Program protocol to identify the prevalence of corrosion and corrosionrelated cracking in the ICCWR2. With the LCM, a close visual examination is made of the ICCWR surface along with measurements of corrosion-related features. LCM inspections produce immense amounts of image data that is time intensive to analyze. There is also a 9-year backlog of images, with approximately 49 canisters that must be evaluated. To expedite data analysis and reduce the amount of generated data, a Wide Area 3D Measurement System (WAMS) microscope has been added to the examination protocol. Although WAMS is a lower resolution microscope, small features of interest can be still identified. The advantage of collecting data for the full circumference using the WAMS is that it can take about 1/16 of the time needed with the LCM. Both systems offer capabilities that combined can be utilized to expedite the examination of the ICCWR. The WAMS is an efficient system for screening and identification of corrosion features while the LCM can be utilized to obtain higher resolution images areas identified by the WAMS. This report explains and justifies the data collection methods used with the WAMS. It includes a summary of the data generated by WAMS in FY21. The goals set for data collection in FY21 were met. A total of twenty-two DE’s were imaged, and analysis was carried out on eleven samples. The analyzed samples showed large numbers of potential cracks and pits distributed throughout the surfaces. Lastly, to explain the advantages of the WAMS, its capabilities were compared to those of a simpler microscope. Micrographs of the samples imaged in FY21 and those analyzed are included in the appendices.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Subsurface Characterization of Hydraulic Fracture Test Site-2 (HFTS-2), Delaware Basin

Hydraulic Fracturing Test Site-2 (HFTS-2) is a field-based research experiment performed in the Wolfcamp Formation of the Permian (Delaware) Basin. This paper focuses on integration, advanced geological characterization, and 3D subsurface modeling of the comprehensive HFTS-2 dataset. The study showcases a multidisciplinary reservoir characterization approach that incorporates geology, petrophysics, geochemistry, geomechanics, microseismic, and subsurface engineering analysis. Subsurface characterization of organic-rich mudstone formations requires understanding complex hydraulic fracture network growth in relation to inherent lithology, geomechanical properties, and interaction with pre-existing natural fractures. This paper presents a characterization workflow incorporating pre- and post-stimulation subsurface data, unique to the HFTS-2 dataset. The study integrated: (1) rock properties from logs, cores, and thin sections; (2) natural and hydraulic fracture descriptions from cores and image logs; (3) local and regional stresses; (4) geomechanics; (5) microseismic; (6) fiber optic (FO) and bottomhole pressure gauge (BHPG) response; and (7) produced fluids analysis. During a stimulation treatment, creation of the stimulated rock volume (SRV) is influenced by several subsurface factors. Key contributing factors include structural context, stress conditions, lithology, facies architecture, pre-existing natural fractures, and geomechanical properties. The HFTS-2 subsurface data integration indicates that the SRV is comprised of a complex juxtaposition of hydraulic fracture swarms, as evidenced by image logs analysis, core description, and microseismic monitoring. The HFTS-2 microseismic event density was used to generate 3D heat maps that serve as a representative SRV footprint, corroborated by secondary datasets. These maps were further integrated with petrophysical and geomechanical characteristics, as well as responses from FO and BHPG, to estimate the lateral and vertical dimensions of the effective fractures. The geological characterization for the HFTS-2 dataset combined with 3D modeling for petrophysical and geomechanical properties provides a strong foundation for subsurface simulation and optimization studies. Downloaded from http://onepetro.org/URTECONF/proceedings-pdf/21URTC/1-21URTC/D011S005R001/2477501/urtec-2021-5243-ms.pdf/1 by Carol Worster on 28 February 2022 URTeC 5243 The workflow improved our understanding of HFTS-2 hydraulic fracture propagation and characteristics in relation to offset pressure depletion and interaction with pre-existing natural fractures. Analysis showed that fracture geometry varies by stage and by well, and a complex fracture network is generated with varying fracture density. The multidisciplinary workflow presented herein for integration and characterization serves as a foundation to evaluate completion efficiency and estimate areal and vertical stimulation and depletion extent for the project. Furthermore, the workflow and learnings can also be transferred to other unconventional plays.

58 GEOSCIENCES↗

Critical length scales for chemical heterogeneity at Cu/Nb 3D interfaces by atom probe tomography

Cu/Nb nanocomposites containing sharp, two-dimensional (2D) interfaces have outstanding strength but limited deformability. In contrast, Cu/Nb with three dimensional (3D) biphase interfaces exhibiting crystallographic, topological, and chemical variations in all spatial dimensions overcomes this limitation by simultaneously enhancing material strength and deformability. Here, while structural characterization of 3D interfaces has been performed to understand their mechanical behavior, three dimensional chemical characterization of such interfaces is lacking. In this work we quantify the local chemistry of 3D interfaces in Cu/Nb nanocomposites using atom probe tomography (APT). Our analysis demonstrates chemical heterogeneities along all spatial dimensions in 3D interfaces, establishes the length scale of such features, and quantifies the morphology of 3D interfaces. 3D interface heterogeneities form by surface diffusion during physical vapor deposition (PVD), suggesting that deposition parameters can be used to control interface structure and provide unique ways to explore processing-structure-property relationships in interface-dominated nanocomposites.

36 MATERIALS SCIENCE↗

General approaches for shear-correcting coordinate transformations in Bragg coherent diffraction imaging. Part I

This two-part article series provides a generalized description of the scattering geometry of Bragg coherent diffraction imaging (BCDI) experiments, the shear distortion effects inherent in the 3D image obtained from presently used methods and strategies to mitigate this distortion. Part I starts from fundamental considerations to present the general real-space coordinate transformation required to correct this shear, in a compact operator formulation that easily lends itself to implementation with available software packages. Such a transformation, applied as a final post-processing step following phase retrieval, is crucial for arriving at an undistorted, correctly oriented and physically meaningful image of the 3D crystalline scatterer. As the relevance of BCDI grows in the field of materials characterization, the available sparse literature that addresses the geometric theory of BCDI and the subsequent analysis methods are generalized here. This geometrical aspect, specific to coherent Bragg diffraction and absent in 2D transmission CDI experiments, gains particular importance when it comes to spatially resolved characterization of 3D crystalline materials in a reliable nondestructive manner. This series of articles describes this theory, from the diffraction in Bragg geometry to the corrections needed to obtain a properly rendered digital image of the 3D scatterer. Part I of this series provides the experimental BCDI community with the general form of the 3D real-space distortions in the phase-retrieved object, along with the necessary post-retrieval correction method. Part II builds upon the geometric theory developed in Part I with the formalism to correct the shear distortions directly on an orthogonal grid within the phase-retrieval algorithm itself, allowing more physically realistic constraints to be applied. Taken together, Parts I and II provide the X-ray science community with a set of generalized BCDI shear-correction techniques crucial to the final rendering of a 3D crystalline scatterer and for the development of new BCDI methods and experiments.

36 MATERIALS SCIENCE↗

Machine Learning to Identify Geologic Factors Associated with Production in Geothermal Fields: A Case-Study Using 3D Geologic Data from Brady Geothermal Field and NMFk

In this paper, we present an analysis using unsupervised machine learning (ML) to identify the key geologic factors that contribute to the geothermal production in Brady geothermal field. Brady is a hydrothermal system in northwestern Nevada that supports both electricity production and direct use of hydrothermal fluids. Transmissive fuid-fow pathways are relatively rare in the subsurface, but are critical components of hydrothermal systems like Brady and many other types of fuid-fow systems in fractured rock. Here, we analyze geologic data with ML methods to unravel the local geologic controls on these pathways. The ML method, non-negative matrix factorization with k-means clustering (NMFk), is applied to a library of 14 3D geologic characteristics hypothesized to control hydrothermal circulation in the Brady geothermal field. Our results indicate that macro-scale faults and a local step-over in the fault system preferentially occur along production wells when compared to injection wells and non-productive wells. We infer that these are the key geologic characteristics that control the through-going hydrothermal transmission pathways at Brady. Our results demonstrate: (1) the specific geologic controls on the Brady hydrothermal system and (2) the efficacy of pairing ML techniques with 3D geologic characterization to enhance the understanding of subsurface processes. This submission includes the published journal article detailing this work, the published 3D geologic map of the Brady Geothermal Area used as a basis to develop structural and geological variables that are hypothesized to control or effect permeability or connectivity, 3D well data, along which geologic data were sampled for PCA analyses, and associated metadata file. This work was done using the GeoThermalCloud framework, which is part of SmartTensors (both are linked below).

15 GEOTHERMAL ENERGY↗

Time-lapse VSP integration and calibration of subsurface stress field utilizing machine learning approaches: A case study of the morrow B formation, FWU

This study aims to develop a methodology for calibrating subsurface stress changes through time-lapse vertical seismic profiling (VSP) integration. The selected study site is a region around the injector well located within Farnsworth field unit (FWU), where there is an ongoing CO 2 -enhanced oil recovery (EOR) operation. In our study, a site-specific rock physics model was created from extensive geological, geophysical, and geomechanical characterization through 3D seismic data, well logs, and core assessed as part of the 1D MEM conducted on the characterization well within the study area. Here, the Biot-Gassmann workflow was utilized to combine the rock physics and reservoir simulation outputs to determine the seismic velocity change due to fluid substitution. Modeled seismic velocities attributed to mean effective stress were determined from the geomechanical simulation outputs, and the stress-velocity relationship developed from ultrasonic seismic velocity measurements. A machine learning-assisted workflow comprised of an artificial neural network and a particle swarm optimizer (PSO) was utilized to minimize a penalty function created between the modeled seismic velocities and the observed time-lapse VSP dataset. The successful execution of this workflow has affirmed the suitability of acoustic time-lapse measurements for 4D-VSP geomechanical stress calibration pending measurable stress sensitivities within the anticipated effective stress changes and the availability of suitable and reliable datasets for petroelastic modeling. © 2023 Society of Chemical Industry and John Wiley & Sons, Ltd.

58 GEOSCIENCES↗

Three-dimensional seismic characterization and imaging of the Soda Lake geothermal field

Accurate characterization of subsurface geophysical properties and detection of the fault system are essential for geothermal energy exploration and production. The Soda Lake geothermal field is in western Nevada with a complex fault system. Previous seismic characterization only produced a low-resolution, smooth velocity model along with a simple, conceptual fault model. Using optimized correlation-based full-waveform inversion, wavefield-separation-based reverse-time migration, and automatic fault detection techniques, we present 3D seismic characterization for the Soda Lake geothermal field using 3D surface seismic data acquired with Vibroseis sources. Here, we obtain 3D high-resolution velocity, density, and acoustic impedance models, 3D seismic images with different grid spacings, and a high-resolution fault system. Consistency check between the constructed faults and currently active injection and production geothermal wells verifies that our seismic inversion and imaging results and detected faults are reliable. These results can provide valuable information for optimizing well placement and geothermal energy production at the Soda Lake geothermal field.

15 GEOTHERMAL ENERGY↗

Five-second STEM dislocation tomography for 300 nm thick specimen assisted by deep-learning-based noise filtering

Scanning transmission electron microscopy (STEM) is suitable for visualizing the inside of a relatively thick specimen than the conventional transmission electron microscopy, whose resolution is limited by the chromatic aberration of image forming lenses, and thus, the STEM mode has been employed frequently for computed electron tomography based three-dimensional (3D) structural characterization and combined with analytical methods such as annular dark field imaging or spectroscopies. However, the image quality of STEM is severely suffered by noise or artifacts especially when rapid imaging, in the order of millisecond per frame or faster, is pursued. Here we demonstrate a deep-learning-assisted rapid STEM tomography, which visualizes 3D dislocation arrangement only within five-second acquisition of all the tilt-series images even in a 300 nm thick steel specimen. The developed method offers a new platform for various in situ or operando 3D microanalyses in which dealing with relatively thick specimens or covering media like liquid cells are required.

47 OTHER INSTRUMENTATION↗

X-ray ptychographic tomography reveals buried 3D structural defects in metal halide perovskites

For the first of its kind, X-ray ptychographic imaging is utilized for probing metal halide perovskite crystals, revealing various 3D structural defects fully or partially buried underneath the perovskite surface. Here, this work demonstrates a powerful, non-intrusive 3D tomographic characterization method to illuminate the complete microstructure of perovskites for advanced energy applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Neutrino heating in 1D, 2D, and 3D core-collapse supernovae: characterizing the explosion of high-compactness stars

Massive stars can end their lives with a successful supernova explosion (leaving behind a neutron star or, more rarely, a black hole), or a failed explosion that leaves behind a black hole. The density structure of the pre-collapse progenitor star already encodes much of the information regarding the outcome and properties of the explosion. However, the complexity of the collapse and subsequent shock expansion phases prevents drawing a straightforward connection between the pre-collapse and post-explosion properties. In order to derive such a connection several explodability studies have been performed in recent years. However, different studies can predict different explosion outcomes. In this article, we show how compactness, which is related to the average density of the star’s core, has an important role in determining the efficiency of neutrino heating, and therefore the outcome of the explosion. Commonly, high-compactness progenitors are assumed to yield failed explosions, due to their large mass accretion rates, preventing the shock from expanding. We show by analysing ~150 2D flash and F ornax simulations and 20 3D F ornax simulations that this is not the case. Instead, due to the rapid increase of neutrino heating with compactness, high-compactness progenitors lead to successful shock revival. We also show that 1D+ simulations that include v-driven convection using a mixing-length theory approach correctly reproduce this trend. Finally, we compare 1D+ models, which we show can reproduce some aspects of multi-D simulations with reasonable accuracy, with other widely used 1D models in the literature.

neutrinos↗

Non-Solvent Induced Phase Separation Enables Designer Redox Flow Battery Electrodes

Porous carbonaceous electrodes are performance-defining components in redox flow batteries (RFBs), where their properties impact the efficiency, cost, and durability of the system. The overarching challenge is to simultaneously fulfill multiple seemingly contradictory requirements—i.e., high surface area, low pressure drop, and facile mass transport—without sacrificing scalability or manufacturability. Here, non-solvent induced phase separation (NIPS) is proposed as a versatile method to synthesize tunable porous structures suitable for use as RFB electrodes. The variation of the relative concentration of scaffold-forming polyacrylonitrile to pore-forming poly(vinylpyrrolidone) is demonstrated to result in electrodes with distinct microstructure and porosity. Tomographic microscopy, porosimetry, and spectroscopy are used to characterize the 3D structure and surface chemistry. Flow cell studies with two common redox species (i.e., all-vanadium and Fe2+/3+) reveal that the novel electrodes can outperform traditional carbon fiber electrodes. It is posited that the bimodal porous structure, with interconnected large (>50 µm) macrovoids in the through-plane direction and smaller (<5 µm) pores throughout, provides a favorable balance between offsetting traits. Although nascent, the NIPS synthesis approach has the potential to serve as a technology platform for the development of porous electrodes specifically designed to enable electrochemical flow technologies.

36 MATERIALS SCIENCE↗

Understanding coarsening of a post-corrosion microstructure in a molten salt by combining phase-field modeling and in situ tomography

Alloys corroding in molten salt have been observed to form bicontinuous, nanoporous microstructures via dealloying, which subsequently undergo coarsening due to facile transport in high-temperature conditions. In this work, we describe a methodology to elucidate the underlying transport mechanisms during coarsening of a bicontinuous microstructure via quantitative comparisons between phase-field simulations and four-dimensional in situ experiments, in this case X-ray nanotomography of the coarsening of a dealloyed 80 wt% Ni-20 wt% Cr microwire in molten KCl-MgCl 2 at 800°C. We conduct phase-field simulations initialized from experimental data to model coarsening via three different transport mechanisms: surface diffusion, solid bulk diffusion, and liquid bulk diffusion. These simulations reproduce key features of the experiment, such as the densification of the outer layer of the dealloyed wire and the reduction in radius over time. We quantitatively compare different microstructural characteristics between the simulations and experiment and extract temporal scaling factors that optimally match the time scales of the simulations to that of the experiment. This allows us to evaluate morphological similarity between the simulations and experiment and relate the experimental coarsening kinetics to fundamental material properties. We find that surface diffusion is most likely to be the dominant coarsening mechanism, and its kinetics imply a surface diffusivity of D S = 8.9 x 10 -20 m 3 /s, which is within the range of reported values for Ni-vacuum interfaces at 800°C. However, the difference between the experiment and the surface diffusion simulation increases substantially at late times, suggesting that other mechanisms, such as the dissolution of residual Cr, may be at play.

36 MATERIALS SCIENCE↗

Estimation of hydraulic conductivity in a watershed using sparse multi-source data via Gaussian process regression and Bayesian experimental design

Enhanced water management systems depend on accurate estimation of subsurface hydraulic properties. However, geologic formations can vary significantly, so information from a single source (e.g., widely spaced boreholes) is insufficient in characterizing subsurface aquifer properties. Therefore, multiple sources of information are needed to complement the hydrogeology understanding of a region. Here, this study presents a numerical framework in which information from different measurement sources is combined to characterize the 3D random field in a multi-fidelity prediction model. Coupled with the model, a Bayesian experimental design was used to determine the best future sampling locations. The Upper Sangamon watershed in east-central Illinois was selected as the case study site, where the multi-fidelity Gaussian process model was used to estimate the hydraulic conductivity in the region of interest. Multi-source observation data were obtained from electrical resistivity and borehole pumping tests. The accuracy of the model prediction is dependent on the locations and the distribution of both high- and low-fidelity data. Furthermore, the multi-fidelity model was compared with the single-fidelity model. The uncertainties and confidence in the measurements and parameter estimates were quantified and used to design future cycles of data collection to further improve the confidence intervals.

54 ENVIRONMENTAL SCIENCES↗

Dirigent isoflavene-forming PsPTS2: 3D structure, stereochemical, and kinetic characterization comparison with pterocarpan-forming PsPTS1 homolog in pea

Pea (legume plant defense) phytoalexin pterocarpans (–)-maackiain and (+)-pisatin have opposite C6a and C11a configurations, but how this occurs biosynthetically is unknown. Herein, pea dirigent-protein (DP) PsPTS2, which generates 7,2'-dihydroxy-4',5'-methylenedioxyisoflav-3-ene (DMDIF), was investigated as regards stereoselectivity towards four possible 7,2'-dihydroxy-4',5'-methylenedioxyisoflavan-4-ol (DMDI) stereoisomers. Each DMDI stereoisomer configuration was determined using NMR spectroscopy, electronic circular dichroism, and molecular orbital analyses. PsPTS2 efficiently converted cis-(3R,4R)-DMDI into DMDIF, this being 20-fold faster than with the trans-(3R,4S)-isomer. The 4R-configured substrate’s near ß-axial OH orientation significantly enhanced its leaving group abilities in creating intermediate A-ring mono-quinone methide (QM), whereas the 4S-isomer’s 4-OH group α-equatorial orientation was a poorer leaving group. Substrate docking simulations also indicated that the 4R-configured ß-axial OH was closest to the Asp catalytic center, whereas the 4S-isomer’s α-equatorial OH was further away. Neither cis-(3S,4S)- nor trans-(3S, 4R)-DMDIs were substrates, even with the former having the same C3/C4 stereochemistry as (+)-pisatin. PsPTS2, assayed with cis-(3R,4R)-7,2'-dihydroxy-4'-methoxyisoflavan-4-ol [cis-(3R,4R)-DMI] and its C3/C4 stereoisomers, gave 2',7-dihydroxy-4'-methoxyisoflav-3-ene (DMIF), with the same substrate stereoselectivity. DP homologs may exist in licorice (Glycyrrhiza pallidiflora) and the tree legume Bolusanthus speciosus, as DMIF is found in both. PsPTS1 preferentially utilized cis-(3R,4R)-DMDI to give (–)-maackiain, this being 2200-fold more efficient than with cis-(3R,4R)-DMI. PsPTS1 also slowly converted trans-(3S,4R)-DMDI into (+)-maackiain, again reflecting the better 4R configured OH leaving group. Pea PsPTS2 and PsPTS1 provisionally provide a facile DP-engendered means to enable differing C6a and C11a configurations in (+)-pisatin and (–)-maackiain. Both DP transformations are considered to occur via DP-engendered generation of an identical mono-QM bound intermediate, which with PsPTS2 either re-aromatizes to give DMDIF or with PsPTS1 undergoes intramolecular cyclization to afford (–)-maackiain. Substrate docking simulations using PsPTS2 (2.5 Å resolution) and PsPTS1 (1.5 Å resolution) plausibly indicate that cis-(3R,4R)-DMDI binds in the anti-configuration in the PsPTS2 active site to afford DMDIF, and the syn-configuration in PsPTS1 to give maackiain.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

On the role of geometrically necessary dislocations in void formation and growth in response to shock loading conditions in wrought and additively manufactured Ta

This study investigates the role of geometrically necessary dislocations (GNDs) and microstructure on void nucleation and growth in wrought and additively manufactured (AM) tantalum subjected to high-strain rate loading. Multi-modal 3D data was collected using TriBeam tomography to calculate GND densities and their spatial relationship to voids. A microstructural comparison between the wrought and AM samples identified distinct void shapes and locations, with intragranular voids and more spherical voids frequently observed in the AM dataset. Results indicate that voids preferentially form at both high-angle grain boundaries and low-angle subgrain boundaries, the latter of which are frequently observed in the AM material. Through a radial distribution analysis of all voids in the datasets, significant GND localization to near-void-surface regions was observed in both samples. 3D crystal plasticity simulations were employed to extend the experimental observations, revealing higher void growth rates in [111] oriented grains when compared to [001] grains. The simulations also suggest that GNDs can be generated as part of the void growth process, with more GND accumulation for growth in a [111] grain than a [001] grain. These findings provide valuable insights into the links between nanoscale void nucleation, mesoscale void growth, and microstructural effects in dynamically loaded tantalum.

36 MATERIALS SCIENCE↗