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At least 451 records · Page 25

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DOE OSTI2024

A Machine Learning Approach to Quantitative Analysis of Enamel Microstructure from Scanning Electron Microscopy Images

Dental enamel, the outermost tissue of mammalian teeth, must withstand a lifetime of wear and cyclic contact. To meet this demand, enamel possesses a combination of high hardness and resistance to fracture, properties that are typically mutually exclusive. The impressive damage tolerance has been attributed largely to decussation of the enamel rods, the principal unit of its microstructure. As such, enamel is inspiring the design of next‐generation structural materials. However, quantitative descriptions of the decussated enamel rod microstructure remain limited due to challenges encountered in applying computed tomography and in acquiring quality images appropriate for traditional digital processing methods. Here, a machine learning segmentation method is applied to images of the enamel obtained using scanning electron microscopy to support quantitative analysis of the microstructure. A pretrained convolutional neural network is used to expand the input training image dataset to allow the training of a random forest classifier, which ultimately segments the image with a very small training set ( n = 3 images). A validation of this segmentation method is presented, in addition to its application to calculate relevant microstructural parameters for images of tooth enamel from selected mammalian species. The methodology applied here is equally applicable to other hard tissues.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Using X-ray Micro-Computed Tomography to Three-Dimensionally Visualize the Foregut of the Glassy-Winged Sharpshooter ( Homalodisca vitripennis )

Dissecting the heads of small insects belonging to the order Hemiptera for detailed anatomical investigation with light or scanning electron microscopy is difficult, time-consuming, and destructive, often resulting in sample preparation artifacts. Nevertheless, the structural details of these insects often hold critical information regarding their interactions with bacterial pathogens. For example, the glassy-winged sharpshooter (GWSS) is an efficient vector of the bacterium Xylella fastidiosa, the causal agent of Pierce’s disease in grape vines, but the foregut of this species is exceptionally difficult to dissect. Here, we describe a simple, non-destructive method to investigate the structure of the anterior gut of GWSS using high-resolution micro-computed X-ray tomography (microCT). The use of microCT eliminates the need for destructive dissection and reveals the morphology of small insects in three dimensions, allowing the user to virtually dissect the sample. The use of microCT imaging is a promising and powerful tool in the entomological sciences for studying the structures of vector insects, especially for difficult-to-dissect regions such as the foregut.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2021

Effects of niobium and tantalum on the microstructure and strength of ferritic-martensitic steels

Herein, detailed investigations of two ferritic-martensitic steels, i.e., Nb- and Ta-steel, indicate that the higher Nb diffusivity and the lower nucleation driving force of Nb-carbide promote preferential nucleation of Nb-carbides at grain boundaries and thus a higher boundary occupancy than Ta-carbides, which favored greater creep resistance of Nb-steel than that of Ta-steel despite their similar yield strength.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Evolution of micro-pores in Ni–Cr alloys via molten salt dealloying

Porous materials with high specific surface area, high porosity, and high electrical conductivity are promising materials for functional applications, including catalysis, sensing, and energy storage. Molten salt dealloying was recently demonstrated in microwires as an alternative method to fabricate porous structures. The method takes advantage of the selective dissolution process introduced by impurities often observed in molten salt corrosion. This work further investigates molten salt dealloying in bulk Ni–20Cr alloy in both KCl–MgCl 2 and KCl–NaCl salts at 700 °C, using scanning electron microscopy, energy dispersive spectroscopy, and X-ray diffraction (XRD), as well as synchrotron X-ray nano-tomography. Micro-sized pores with irregular shapes and sizes ranging from sub-micron to several microns and ligaments formed during the process, while the molten salt dealloying was found to progress several microns into the bulk materials within 1–16 h, a relatively short reaction time, enhancing the practicality of using the method for synthesis. The ligament size increased from ~ 0.7 μm to ~ 1.3 μm in KCl–MgCl 2 from 1 to 16 h due to coarsening, while remaining ~ 0.4 μm in KCl–NaCl during 16 h of exposure. The XRD analysis shows that the corrosion occurred primarily near the surface of the bulk sample, and Cr 2 O 3 was identified as a corrosion product when the reaction was conducted in an air environment (controlled amount sealed in capillaries); thus surface oxides are likely to slow the morphological coarsening rate by hindering the surface diffusion in the dealloyed structure. 3D-connected pores and grain boundary corrosion were visualized by synchrotron X-ray nano-tomography. This study provides insights into the morphological and chemical evolution of molten salt dealloying in bulk materials, with a connection to molten salt corrosion concerns in the design of next-generation nuclear and solar energy power plants.

36 MATERIALS SCIENCE↗

DOE OSTI2024

The SciDAC QuantOm Framework: A composable Workflow

As part of the Scientific Discovery through Advanced Computing (SciDAC) program, the Quantum Chromodynamics Nuclear Tomography (QuantOM) project aims to analyze data from Deep Inelastic Scattering (DIS) experiments conducted at Jefferson Lab and the upcoming Electron Ion Collider. The DIS data analysis is performed on an event-level by leveraging nuclear theory models and accounting for experimental conditions. In order to efficiently run multiple analyses under varying conditions, a composable workflow was designed where each section (theory, experiment, objective minimization, etc.) has its own dedicated module. The optimization, i.e. the fit of theory to experimental data is carried out by deep learning techniques, such as Generative Adversarial Networks (GANs) or Reinforcement Learning (RL). This presentation gives an overview of the current status of the workflow, highlights present and future challenges, and highlights possible extensions to other projects with similar requirements.

Lersch, Daniel↗

DOE OSTI2024

Scaling the SciDAC QuantOm Workflow

As part of the Scientific Discovery through Advanced Computing (SciDAC) program, the Quantum Chromodynamics Nuclear Tomography (QuantOM) project aims to analyze data from Deep Inelastic Scattering (DIS) experiments conducted at Jefferson Lab and the upcoming Electron Ion Collider. The DIS data analysis is performed on an event-level by combining the input from theoretical and experimental nuclear physics into a single, composable workflow. The optimization itself (I.e. fitting the experimental data with theoretical predictions) is carried out by a machine / deep learning algorithm. The size of the acquired DIS data as well as the complexity of the workflow itself require that the analysis is performed across multiple GPUs on high performance computing systems, such as Polaris at Argonne National Laboratory. This presentation discusses the novelties and challenges that came along with parallelizing this workflow. Recent results are compared to common distributed training techniques.

Lersch, Daniel↗

DOE OSTI2025

Characterization of Build Parameters and Microstructure in Low Heat Input WAAM of Ni-Based Superalloy Haynes 282

Ni-based superalloy Haynes® 282® is being targeted for various applications in advanced power generation systems for its superior fabricability, weldability, and excellent high temperature creep and corrosion performance. This process optimization study aims to use a low heat-input, high deposition rate, controlled Gas Metal Arc Welding (GMAW) process, Cold Metal Transfer (CMT) by Fronius, attempting to achieve fully dense fabrication and possibly avoid the need for HIP. Twenty-one multilayer blocks (~25x100x40 mm3) were deposited to explore a large set of build parameters variations that focused on varying the travel speed from 14 to 42 inches per minute (ipm) and wire feed speed from 150 to 450 ipm. A strong correlation has been observed between arc energy – controlled primarily by travel and wire feed speed. Initial visual inspection, internal microstructural examination, and computed tomography (CT) have been used to determine the effects of built parameters on evolution of internal porosity and defects. Scanning electron microscopy techniques enabled structural and compositional imaging of heterogeneity and changes in microstructural properties.

additive manufacturing↗

DOE OSTI2025

Characterization of Build Parameters and Microstructure in Low Heat Input WAAM of Ni-Based Superalloy Haynes 282

additive manufacturing↗

DOE OSTI2023

Irradiation damage reduces alloy corrosion rate via oxide space charge compensation effects

Radiation effects in materials often compound and accelerate other detrimental phenomena such as embrittlement, oxidation and creep. However, irradiation can also decrease the oxidation rate, for instance with ZrNb alloys nuclear fuel cladding. In this study, we rationalize this observation on Zr-0.5Nb alloy by introducing a mechanism based on oxide space charge modification, resulting from irradiation enhanced Nb clustering. Here, this mechanism is investigated using a multiscale approach: from the macroscale, to determine post-irradiation oxidation kinetics, to the atomic scale, using in-situ atom probe tomography sample oxidation, to observe elemental solute redistribution across the oxide/metal interface. The mechanism is further supported by high resolution transmission electron microscopy characterization and density functional theory calculations. A point defect model is proposed to account for oxide space charge effects and their changes under irradiation. This integrated, multiscale experimental and modeling approach challenges the current paradigm on irradiation effects and how they can potentially improve materials performance in extreme environments.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Scan strategies in EBM-printed IN718 and the physics of bulk 3D microstructure development

Three-dimensional (3D) characterization provides opportunities for understanding processing-structure relationships in additively manufactured (AM) materials. Bulk samples of Inconel 718 were fabricated via electron beam melting (EBM) in order to study microstructural development as a function of energy input and beam scan strategy. TriBeam tomography of bulk Inconel 718 microstructures built under steady-state growth conditions reveals the sensitivity of microstructure formation and evolution to machine process parameters. Here, samples manufactured using a narrow range of energy input per unit build area result in varied grain morphologies and crystallographic textures. Using TRUCHAS, a thermal simulation software, the thermal history of bulk scan strategies was predicted, and combined with a calibrated microstructure-processing map to accurately predict bulk grain morphologies. The solidification parameters and the 3D measured nucleation density are used to predict the transition between columnar and equiaxed grain morphologies, providing a process map to guide AM parameter choices to locally control as-printed microstructure. A two-dimensional metric for characterizing bulk grain morphology was also found to agree well with predictions from the process map calibrated by 3D data. Combined with 3D tomography and thermal modelling, the physics of structure development were understood at a new level of detail with respect to the competing processes of grain nucleation and epitaxial growth.

36 MATERIALS SCIENCE↗

DOE OSTI2020

In Situ Investigation of Chemomechanical Effects in Thiophosphate Solid Electrolytes

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

25 ENERGY STORAGE↗

DOE OSTI2021

Radiation Enhanced Anion Diffusion in Chromia

Cr 2 O 3 is a ubiquitous passivating film on alloys that is vital to their stability and performance in hostile environments. In this study, we directly observe and measure how anion transport through the oxide is affected by 400 keV Ar 2+ ion irradiation as a function of temperature (30–500 °C) and dose (0.33–2.00 dpa) in single-crystal Cr 2 O 3 films using embedded 18 O isotopic tracers and atom probe tomography. Diffusion coefficients are experimentally determined and compared to a chemical rate theory model. Experimental and theoretical results are broadly in agreement, showing anion diffusion increases by at least 4–5 orders of magnitude upon irradiation with a weak dependence on temperature and a stronger dose-driven sink-strength dependence. These results reveal that radiation could significantly reduce the protectiveness of Cr 2 O 3 films when passivity relies upon limited anion diffusivity, even at relatively modest levels of irradiation and low temperatures.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2021

Persistence of crystal orientations across sub-micron-scale "super-grains" in self-organized Cu-W nanocomposites

We use precession electron diffraction to investigate the crystallographic character of copper (Cu)-tungsten (W) nanocomposites fabricated via physical vapor co-deposition at 400 oC. We observe sub-micron-scale regions, where apparently disconnected Cu and W grains have near identical crystallographic orientations. This persistence of grain orientations suggests Cu and W grains within these regions are interconnected in 3-D when they first form and may be considered as intercalated, sub-micron-scale "super-grains". Indeed, atom probe tomography provides direct evidence of 3-D interconnectivity of W domains. Our findings shed light on the structure and self organization mechanisms of nanocomposites formed by spontaneous phase separation of co-deposited metals.

Yadav, Digvijay↗

DOE OSTI2026

Correlated purification for restoring 𝑁-representability in quantum simulation

Experimentally measured reduced density matrices (RDMs) often violate constraints that ensure they represent N-electron states—known as N-representability conditions—because of statistical and hardware noise. In this work, we present a correlated purification framework based on semidefinite programming to restore the accuracy of a noisy, unphysical two-electron RDM (2-RDM). The method performs a bi-objective optimization that minimizes both the many-electron energy and the nuclear norm of the correction to the measured 2-RDM. The nuclear norm, often employed in matrix completion, promotes low-rank corrections, while the energy term acts as a regularization term that can improve the purity of the ground state. While the method is particularly effective for ground states, it can also be applied to excited and nonstationary states by decreasing the weight of the energy relative to the error norm. In an application to fermionic shadow tomography of large hydrogen chains, correlated purification yields substantial reductions in both energy and 2-RDM error, achieving chemical accuracy across dissociation curves. This framework provides a robust strategy for tomography in many-body quantum simulations.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2023

The solenoidal large intensity device (SoLID) for JLab 12 GeV

The solenoidal large intensity device (SoLID) is a new experimental apparatus planned for Hall A at the Thomas Jefferson National Accelerator Facility (JLab). SoLID will combine large angular and momentum acceptance with the capability to handle very high data rates at high luminosity. With a slate of approved high-impact physics experiments, SoLID will push JLab to a new limit at the QCD intensity frontier that will exploit the full potential of its 12 GeV electron beam. In this paper, we present an overview of the rich physics program that can be realized with SoLID, which encompasses the tomography of the nucleon in 3D momentum space from semi-inclusive deep inelastic scattering, expanding the phase space in the search for new physics and novel hadronic effects in parity-violating DIS, a precision measurement of J/ψ production at threshold that probes the gluon field and its contribution to the proton mass, tomography of the nucleon in combined coordinate and momentum space with deep exclusive reactions, and more. To meet the challenging requirements, the design of SoLID described here takes full advantage of recent progress in detector, data acquisition and computing technologies. In addition, we outline potential experiments beyond the currently approved program and discuss the physics that could be explored should upgrades of CEBAF become a reality in the future.

3D imaging↗

DOE OSTI2024

Scintillation and cherenkov photon counting detectors with analog silicon photomultipliers for TOF-PET

Objective. Standard signal processing approaches for scintillation detectors in positron emission tomography (PET) derive accurate estimates for 511 keV photon time of interaction and energy imparted to the detection media from aggregate characteristics of electronic pulse shapes. The ultimate realization of a scintillation detector for PET is one that provides a unique timestamp and position for each detected scintillation photon. Detectors with these capabilities enable advanced concepts for three-dimensional (3D) position and time of interaction estimation with methods that exploit the spatiotemporal arrival time kinetics of individual scintillation photons. Approach. In this work, we show that taking into consideration the temporal photon emission density of a scintillator, the channel density of an analog silicon photomultiplier (SiPM) array, and employing fast electronic readout with digital signal processing, a detector that counts and timestamps scintillation photons can be realized. To demonstrate this approach, a prototype detector was constructed, comprising multichannel electronic readout for a bismuth germanate (BGO) scintillator coupled to an SiPM array. Main Results. In proof-of-concept measurements with this detector, we were able to count and provide unique timestamps for 66% of all optical photons, where the remaining 34% (two-or-more-photon pulses) are also independently counted, but each photon bunch shares a common timestamp. We show this detector concept can implement 3D positioning of 511 keV photon interactions and thereby enable corrections for time of interaction estimators. The detector achieved 17.6% energy resolution at 511 keV and 237 ± 10 ps full-width-at-half-maximum coincidence time resolution (CTR) (fast spectral component) versus a reference detector. We outline the methodology, readout, and approach for achieving this detector capability in first-ever, proof-of-concept measurements for scintillation photon counting detector with analog silicon photomultipliers. Significance. The presented detector concept is a promising design for large area, high sensitivity TOF-PET detector modules that can implement advanced event positioning and time of interaction estimators, which could push state-of-the-art performance.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

DOE OSTI2025

SAGIPS: A scalable Framework for scidac quantom

As part of the Scientific Discovery through Advanced Computing (SciDAC) program, the Quantum Chromodynamics Nuclear Tomography (QuantOM) project aims to analyze data from Deep Inelastic Scattering (DIS) experiments conducted at Thomas Jefferson National Accelerator Facility and the upcoming Electron Ion Collider. The DIS data analysis is performed on an event level by taking into leveraging nuclear theory models and accounting for experimental conditions. In order to efficiently run multiple analyses under varying conditions, a composable workflow was designed where each section (theory, experiment, objective minimization, etc.) has its own dedicated module. This presentation gives an overview over of the current status of this workflow, highlights present and future challenges, and highlights possible extensions to other projects with similar requirements.

Lersch, Daniel [Thomas Jefferson National Accelera↗

DOE OSTI2024

Fluoro‐Ethylene‐Carbonate Plays a Double‐Edged Role on the Stability of Si Anode‐Based Rechargeable Batteries During Cycling and Calendar Aging

Abstract The energy storage density of Li‐ion batteries can be improved by replacing graphite anodes with high‐capacity Si‐based materials, though instabilities have limited their implementation. Performance degradation mechanisms that occur in Si anodes can be divided into cycling stability (capacity retention after repeated battery cycles) and calendar aging (shelf life). While cycling instabilities and improvement strategies have been researched intensively, there is little known about the underlying mechanisms that cause calendar aging. In this work, multiple electron microscope techniques are used to explore the mechanism that governs calendar aging from the sub‐nanometer‐to‐electrode scale. Plasma focused ion beam tomography is used to create 3D reconstructions of calendar aged electrodes and revealed the growth of a LiF‐rich layer at the interface between the copper current collector and the silicon material, which can lead to delamination and increased interfacial impendence. The LiF layer appeared to derive from the fluoro‐ethylene‐carbonate electrolyte additive, which is commonly used to improve cycling stability in Si‐based systems. The results reveal that additives necessary to improve cycling stability can cause performance degradation over the long‐term during calendar aging. The results show that high performing, stable systems require careful design to simultaneously mitigate both cycling and calendar aging instabilities.

25 ENERGY STORAGE↗