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At least 19 records

EDS-PhaSe: Phase Segmentation and Analysis from EDS Elemental Map Images Using Markers of Elemental Segregation

Scanning electron microscopy (SEM), combined with energy-dispersive spectroscopy (EDS), is an extensively used technique for in-depth microstructural analysis. Here, we present the EDS-Phase Segmentation (EDS-PhaSe) tool that enables phase segmentation and phase analysis using the EDS elemental map images. Importantly, it converts the EDS map images into estimated composition maps for calculating markers of selective elemental redistribution in the scanned area and creates a phase-segmented micrograph while providing approximate fraction and composition of each identified phase. EDS-PhaSe offers two unique advantages. Firstly, it enables the direct processing of EDS elemental map images without requiring any raw or proprietary data/software, thereby allowing the analysis of EDS results available in the published literature as images. Secondly, it enables segmentation and analysis of phases even when the phase contrast is missing in backscattered micrographs, assisting in correlating the XRD and SEM-EDS data as shown in this work for a AlCoCrFeNi high-entropy alloy.

36 MATERIALS SCIENCE↗

Measurement Error in Atomic-Scale Scanning Transmission Electron Microscopy—Energy-Dispersive X-Ray Spectroscopy (STEM-EDS) Mapping of a Model Oxide Interface

Abstract With the development of affordable aberration correctors, analytical scanning transmission electron microscopy (STEM) studies of complex interfaces can now be conducted at high spatial resolution at laboratories worldwide. Energy-dispersive X-ray spectroscopy (EDS) in particular has grown in popularity, as it enables elemental mapping over a wide range of ionization energies. However, the interpretation of atomically resolved data is greatly complicated by beam–sample interactions that are often overlooked by novice users. Here we describe the practical factors—namely, sample thickness and the choice of ionization edge—that affect the quantification of a model perovskite oxide interface. Our measurements of the same sample, in regions of different thickness, indicate that interface profiles can vary by as much as 2–5 unit cells, depending on the spectral feature. This finding is supported by multislice simulations, which reveal that on-axis maps of even perfectly abrupt interfaces exhibit significant delocalization. Quantification of thicker samples is further complicated by channeling to heavier sites across the interface, as well as an increased signal background. We show that extreme care must be taken to prepare samples to minimize channeling effects and argue that it may not be possible to extract atomically resolved information from many chemical maps.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Book Review: Reiner Salzer and Heinz W. Siesler (Eds.): Infrared and Raman spectroscopic imaging, 2nd ed.

This second edition of "Infrared and Raman Spectroscopic Imaging" propels practitioners in that wide-ranging field, as well as other readers, to the current state of the art in a well-produced and full-color, completely revised and updated, volume. This new edition chronicles the expanded application of vibrational spectroscopic imaging from yesterday's time-consuming point-by-point buildup of a hyperspectral image cube, through the improvements afforded by the addition of focal plane arrays and line scan imaging, to methods applicable beyond the diffraction limit, instructs the reader on the improved instrumentation and image and data analysis methods, and expounds on their application to fundamental biomedical knowledge, food and agricultural surveys, materials science, process and quality control, and many others.

74 ATOMIC AND MOLECULAR PHYSICS↗

Enhancement of Optical Efficiency of CSP Mirrors for Reducing O&M Cost via Near-Continuous Operation of Self-Cleaning Electrodynamic Screens (EDS). Final Report

Over the past decade, techno-economical advancements in solar energy systems, particularly the improvement in the conversion efficiency of PV modules made with mono-crystalline silicon solar cells from 12% to 20%, as well as the cost reduction in manufacturing by a factor of about 10%, have made it possible to achieve a levelized cost of electricity (LCOE) in PV plants that is comparable to, or less than, the cost of deriving electricity from fossil fuels. Operating PV plants in mid-latitude sun-belt regions, where the solar irradiance level is highest, provides a high annual energy-yield (kWh/kWp) due to two factors: (1) the availability of predictable high solar irradiance throughout the year with the fewest interruptions in solar flux from clouds and rain, and (2) the increased conversion efficiency of crystalline solar cells, as recombination loss has decreased with increased intensity of the sunlight that illuminates the silicon solar cells. Semi-arid and desert regions, however, are plagued by high atmospheric dust concentrations and frequent sand storms. The deposition of a layer of dust on the optical surfaces of solar collectors such as PV modules and concentrating mirrors reduces the transmission efficiency of sunlight that actually reaches the solar cells or receivers, resulting in high energy-yield soiling loss. There are two major cost components to operating a solar plant: (1) installation costs, and (2) operation-and-maintenance (O&M) costs. There is no fuel cost; hence operating a solar plant in a semi-arid or desert region provides high returns on investment if soiling losses are mitigated via efficient cleaning methods and optimized cleaning frequency. If solar collectors are not cleaned, the accumulation of dust layers on solar collectors may cause the operation of such plants in arid regions to become economically unviable. Washing solar collectors with water and detergent, as is most commonly done now, is an efficient method for cleaning. The conventional approach in utility-scale solar plants is to use a large truck with a water tank and pump system for spraying deionized water on the surface of the solar collectors. Robotic cleaning with brushes, used for many solar plants, requires lesser water for cleaning. The water consumed using semi-automated cleaning of PV modules in utility-scale solar plants is approximately 2 liters/m 2 per cleaning cycle. The total optical surface area of the solar collectors in 1 TW-scale solar installation will be more than 3 × 109 m 2 ; hence an enormous amount of water be needed for cleaning. There simply is not enough fresh water in the sun-belt areas of the world for predicted cleaning needs. In solar power plants, the estimated cost of cleaning solar collectors includes expenses related to the equipment used, labor, cost of transportation of water, the energy required for cleaning, plus ancillary costs whereas the cost of water is not considered. The water used is obtained from sources located close to plant sites, unmindful of the environmental and societal impact as the power plants are oftentimes located in regions that face severe drought. This practice is very similar to the cost calculations in deriving the levelized cost of electricity (LCOE) in conventional power plants based on burning fossil fuel such as coal and gas, while disregarding the cost of climate change and health effects. Unless a water-free or low-water cleaning method is established, the expansion of solar plants may lose public support in areas suffering long intervals of drought. The goal of this research project has been the development and application of the Electrodynamic Screen (EDS) as a means for a water-free, scalable cleaning process applicable to solar-power installations, including rooftop applications. We describe here the development of an EDS film-based cleaning process as an emerging method for use on PV modules, parabolic troughs, and heliostats. This report aims to show the feasibility of integrating or retrofitting EDS films onto the optical surfaces of solar collectors (both PV and CSP) while maintaining high transmission or reflection efficiency. The cleaning action provided by the EDS film is an active method to remove dust deposits by electrodynamic force. Current lab-scale prototype EDS films, retrofitted onto solar panels and mirrors, have shown to be capable of maintaining optical transmission or specular-reflection efficiencies higher than 90% of initial values under clean conditions. The optical surfaces of solar collectors laminated with EDS films can remove more than 90% of deposited dust when the EDS is activated for less than two minutes. As an electrodynamic dust removal process, the EDS film-based method is designed primarily for the removal of dust in solar installations located in semi-arid and desert areas, where the atmosphere is often dry and dusty and rainfall is infrequent. While EDS film application minimizes water consumption and facilitates cleaning as frequently as needed, it has limitations in removing contaminants such as soot, organic pollutants deposited as fine films on the surface, and bird droppings. The dust removal efficiency of the EDS is maximum at relative humidity RH is 40 to 50% and decreases at when RH > 65%. Many solar plant sites undergo diurnal and seasonal cycles of high ambient, early afternoon temperatures and an RH that reaches the dew point early in the morning. These variations in atmospheric conditions do not limit the operation of the EDS film. This report presents a brief review of the progress and the potential of EDS film technology for mitigating the impact of dust on solar collectors via water-free cleaning, as well as current technical challenges regarding efficiency and durability. Our experimental data on the performance of EDS films show that: (1) the dust-removal efficiency (DRE) can reach levels higher than 90%, (2) the specular reflectivity (SR) of EDS film-laminated second-surface mirrors reach levels in excess of 90%, (3) the specular reflectivity restoration (SRR) can exceed 90%, (4) the output-power restoration (OPR) of PV modules can exceed 95%, and (5) the optical transmission efficiency (TE) of the EDS films can be greater than 90%. Working with Sandia National Laboratories (NM), Corning Research and Development Corporation (NY), Eastman Kodak (NY), Tomark-Worthen Industries (NH), and EDS Chile SPA (Chile), we have produced EDS film-laminated PV modules and demonstrated their self-cleaning functions without requiring water. We have demonstrated that the operational range of EDS films will cover the expected ambient temperature of solar fields at RH cycling varying from 20 to 95% as long as the EDS films are activated in the RH range 20 to 50%. (Typical solar-field climates in deserts and semi-arid lands often reach near dew point in coastal areas.) Our experiments on the application of hydrophobic-fluorinated nanoparticle coatings on EDS film surfaces show that the EDS operational range can be extended to higher RH levels that approach the dew point. At Eastman Kodak, as one of our industrial partners, we were able to establish a process for manufacturing EDS films using flexographic printing of the electrodes onto transparent polymer films. This process utilizes an existing manufacturing line at Eastman Kodak that allows fabrication of medium-scale EDS films (26 cm × 30 cm). The manufacturing process has the capacity to produce EDS films at high production speeds. The medium-scale EDS films that have been printed at Kodak were evaluated in the lab at Boston University. The EDS films produced at Kodak were laminated at Tomark-Worthen using an industrial scale vacuum laminator to produce EDS film stacks, which can be affixed onto the optical surfaces of PV modules or concentrating mirrors. The EDS film stack consists of the EDS films that have Willow® Glass (WG) which has a thickness of 100 μm as the front surface. The WG sheets obtained from Corning Research and Development Corporation are customized in size and shape to cover the active area of the EDS films. The back surface of the EDS film stack is integrated onto the optical surface of the solar panel or mirror using optically clear adhesive (OCA) films or silicone adhesives. The OCA films (thickness 25 μm) are produced by 3M. The EDS film stacks have the architecture: WG/OCA/EDS Film/OCA/ over PV module or solar mirror. The power-supply units needed for activating the electrodes of the EDS film were designed and produced at Boston University. These power supply units provide three-phase, 1.2 kV voltage pulses at a very low current (micro-ampere) level and at a low frequency (≈ 5 Hz). The voltage pulses are applied to the electrodes in a sequence such that the train of pulses resembles a unidirectional traveling wave of electrical field on the surface of the EDS film. The dust particles on the surface become charged electrostatically and are levitated by the Coulomb force. The lateral sweeping action of the traveling electric field created by the three-phase voltages pulses then sweeps the dust off the surface. The energy consumed by the EDS electrodes is less than 0.2 Wh/m 2 /cleaning cycle, enabling energy-efficient restoration of output power (OPR) of PV module or specular reflectivity restoration (SRR) for solar mirrors. The EDS system consists of (1) an EDS film stack laminated onto the solar collectors, (2) connection of the EDS film to its power supply unit and (3) Interconnection of the power supply to PV modules or solar mirrors. Design, construction and assessment of field-testing units that have EDS stack laminated PV modules for evaluating the performance of the EDS films in solar fields is being carried out at BU. Our progress under this project, aimed at the advancement of EDS film technology, has reached DOE Technology Readiness Level (TRL) 6. Based on the extensive laboratory evaluations and limited field trials, as well as contacts with potential users, we believe that the technology has reached its commercial stage. We are conducting a cost analysis using the National Renewable Energy Laboratory (NREL) System Advisory Model (SAM) and are preparing for field trials of EDS films in different solar fields in the US, Chile, India and in the Middle East. A brief description of EDS film performance, construction and testing of the field-test unit, autonomous operation of the field-test unit for evaluating EDS performance in increasing energy yield, associated revenue savings, and water conservation is presented.

14 SOLAR ENERGY↗

Benefits of using Electronic Data Sheets (EDS) with coreFlight Systems (cFS) - A Project Example

Recently there has been interest in the incorporation of core Flight Systems (cFS) with Spacecraft Onboard Interface Services (SOIS) Electronic Data Sheets (EDS) in the spaceflight software community. The Regenerative Fuel Cell project at the Glenn Research Center is using cFS architecture with EDS support for its monitoring and control software. The presentation will outline the benefits to using cFS with EDS support: First, EDS establishes a single source of truth for the definitions of data structures used throughout an entire mission that may otherwise be programmed in different languages and designed with different processor architectures. Not only does this help with inter-application communication via the software bus, but it also greatly simplifies communication between systems. An EDS Application Programming Interface (API) library allows the conversion of EDS data structures to and from native data structures. Second, bindings for other programming languages (e.g. Lua, Python, JSON) have been written to allow the creation and manipulation of EDS data objects within those languages. The RFC project uses Lua scripts to automatically generate binary configuration files at build time to be loaded into our cFS programs. We also use Python bindings in a graphical user interface (GUI) to allow an operator to send commands and view telemetry messages sent from cFS instances. Finally, using Lua scripts we can set up specific simulation scenarios to perform automatic functional testing. During the development of the RFC software, the software team put together a generic python GUI called “cFS-EDS-GroundStation” that provides a basic interface to an instance of cFS with EDS support. The GUI includes a basic telecommand and telemetry system that reads directly from the generated EDS databases. In the telecommand system, dropdown menus are populated with all user commands that are defined in EDS. In the telemetry system, telemetry messages are automatically decoded, written to the screen, and saved to a binary file. Additional Python scripts have been written to convert the binary data files into a comma separated value (CSV) format for further processing. We will demonstrate the basic use of the cFS-EDS-GroundStation software including adding additional commands and telemetry payload values in EDS and see them appear automatically in the cFS-EDS-Groundstation software. About the RFC project: The Regenerative Fuel Cell project is tasked with developing and demonstrating a power system consisting of a fuel cell and electrolyzer to provide power during a lunar day/night cycle. During the night, the fuel cell takes Hydrogen and Oxygen gasses and converts them into electricity, water, and heat. During the day, the electrolyzer takes input power (e.g. from a photovoltaic array) and converts water back into Hydrogen and Oxygen gasses.

Mathew Mccaskey↗

EDS to the Moon!

The Electrostatics and Surface Physics Laboratory at NASA Kennedy Space Center is slated to send multiple Electrodynamic Dust Shields (EDS) to the surface of the moon. This paper discusses the EDS onboard a Commercial Lunar Payload System or CLPS mission slated to launch to the moon on July 27, 2023 on Firefly Aerospace’s Blue Ghost Lander to Mare Crisium. The EDS payload consists of a camera EDS, a separate glass EDS, a thermal radiator EDS as well as a Re-Duster system based on EDS technology. The EDS will be deposited on the ground by a deployable structure on the lunar lander shortly after touchdown and its operations will take precedence over the other 10 payloads on the lander. The camera will record images and videos of dust deposition and removal on both the Thermal Radiator EDS and the Glass EDS. Data handling will be done using a Data Storage Unit (DSU) developed by NASA Langley Research Center and downlinked to Earth in real time.

Charles R Buhler↗

Electrodynamic Dust Shield (EDS) Preparation for MISSE-11 Launch

The dusty surfaces of the Moon, Mars, and various asteroids present a significant challenge to NASA’s manned and unmanned space exploration efforts. The fine, electrostatically charged dust is difficult to remove and has resulted in vision obscuration, false instrument readings, contamination, elevated temperatures, performance reduction, and equipment failure. To alleviate these problems, NASA KSC’s Electrostatics and Surface Physics Laboratory (ESPL) is developing active dust mitigation systems for solar system exploration and in situ resource utilization (ISRU). Part of KSC’s Swamp Works system, the lab emphasizes fast-paced, hands-on, cost-effective, and collaborative innovation. The Electrodynamic Dust Shield (EDS) is an ESPL technology being developed to prevent dust accumulation on space components. It consists of a dielectric substrate embedded with parallel electrodes which, when applied with high voltage out-of-phase waveforms, produce a traveling electric field wave that scatters dust particles from its surface via dielectrophoretic and electrostatic forces. The EDS is currently fully functional and has been tested for scalability and endurance in reduced gravity/pressure flight. Next, it will be part of the May 2019 Materials International Space Station Experiment-11 (MISSE-11) payload, which will test small shield samples for performance durability with exposure to the harsh space environment. The summer objective was to test EDS functionality before active and passive dust shield samples launch on MISSE-11, in order to screen for good flight/control samples as well as to compare pre-flight and post-flight clearing efficiencies. I imaged glass and Kapton shields of 2-phase and 3-phase electrode configurations with the Keyence VHX-5000 digital microscope to check for damage before and after all testing for a qualitative pre-flight baseline; helped with vacuum testing of high-voltage shield breakdown; assembled shields and wires using Electrobond 004 silver epoxy; and helped with vacuum and cryogenic dust clearance testing of assembled EDS systems. I learned CAD (computer-aided design) and 3D printing skills to create parts for a shaker table/motor assembly, which will allow for repeatable experiments by evening out EDS dust distribution in a consistent manner prior to dust scattering testing. I will also be improving the interfacing with Alpha Space’s prototype Data Communications Unit (DCU), a payload component to control power to the EDS and store data, by mapping the DCU structure upon power-up and writing shell scripts to improve various processes. Finally, I also CADed and 3D-printed plastic supports for three different geometries of the Electrostatic Precipitator (ESP), a project that aims to use high voltage electrodes to charge and filter out dust from the Martian atmosphere drawn for ISRU devices. This work on dust mitigation technologies will help to support future robotic and human space exploration missions, including NASA’s Journey to Mars; the EDS has especially significant applications to spacecraft solar panels, thermal radiators, viewports, and astronaut visors. This opportunity has also allowed me to become more familiar with various lab equipment and hardware testing, develop key modeling skills in SolidWorks, explore past and present components critical to America’s space program, work with inspiring peers and mentors, and ascertain my dream of working permanently for NASA.

space↗

Southeast Regional CO 2 Sequestration Technology Training Program (SECARB-Ed)

Carbon capture and storage (CCS) technologies have tremendous potential for reducing carbon dioxide (CO 2 ) emissions and mitigating global climate change. These technologies encourage economic growth and have manageable influence on energy use. Deploying these technologies on a commercial scale will require expanding the workforce, including geologists, engineers, scientists and technicians, trained in CCS specialties. In 2009, the U.S. Department of Energy’s (DOE) National Energy Technology Laboratory (NETL) selected seven projects to help develop regional sequestration technology training centers in the United States. The “Southeast Regional CO 2 Sequestration Technology Training Program” (SECARB-Ed) was managed and administered by the Southern States Energy Board (SSEB) from November 16, 2009, to November 15, 2012. During this performance period, the SECARB-Ed partners were successful in achieving their primary objective of developing a self-sustaining regional CO 2 sequestration training program to facilitate the transfer of knowledge and technologies required for site development, operations and monitoring of commercial CCS projects. An experienced team of professionals participated in the SECARB-Ed program, with skills and competencies in geosciences, reservoir engineering and CCS related capture/separation, transportation, legal and regulatory disciplines. The SECARB-Ed Advisory Board included representatives from SSEB, Clemson University, GERALD R HILL PHD, Inc. (HILL), EnTech Strategies, LLC- Research Experience in Carbon Sequestration (RECS), Virginia Tech (VAT), Geological Survey of Alabama (GSA) at The University of Alabama and the Bureau of Economic Geology (BEG) at The University of Texas at Austin. The program encompasses fifteen of SSEB’s member states, including: Alabama, Arkansas, Florida, Georgia, Kentucky, Louisiana, Mississippi, Missouri, North Carolina, Oklahoma, South Carolina, Tennessee, Texas, Virginia and West Virginia. The SECARB-Ed partners implemented an organized sponsorship development program, developed short courses on CCS technologies, participated in regional training and other activities through outreach and networking and performed internet-based and electronic regional/basin technology transfer services. The partners addressed the most promising sequestration options in the region; the mix of industry and power plant sources of CO 2 ; regional transportation infrastructure; and the legal, regulatory, and institutional frameworks that exist in the southeast. As a result, SECARB-Ed fostered the development of a future workforce with disciplines specific to applied engineering and CCS science and technologies and advance the United States in its position as the leader in addressing climate change, near-zero emissions technologies and geologic sequestration technologies. The educational and training opportunities detailed in this Final Report demonstrate an effective means of disseminating a broad base of such knowledge and skills to a variety of students and professionals who are interested in the area of CCS technologies. The efforts of the SECARB-Ed Advisory Board and partners have resulted in a total of 1,951 professional development hours (PDHs) awarded to 1,131 participants.

Baskin, Kathryn A.↗

Affine Transformations to Enable Machine Learning for Semi-Quantitative EDS Analysis

Energy Dispersive X-ray Spectroscopy (EDS) is an essential technique for determining elemental concentrations and distributions within microstructures, critical for materials discovery, optimization, and qualification. However, most published EDS data is qualitative because current quantitative EDS analysis methods require extensive calibration and post-processing, limiting their practicality and widespread adoption. This work seeks to establish a framework for accelerated EDS characterization and spectrum analysis that can leverage ML to analyze correlations between various elemental compositions and resulting EDS spectra. The complex physics and data result in a high-dimensional problem that grows exponentially with the number of elements in the system and the complexity of the spectrum analysis. ML provides a way to compute and optimize the results of this highly dimensional problem in a flexible way to tailor it to the user’s specific needs and material system. However, the framework emphasizes transparency through a strictly mathematical affine transformation, so the analysis remains understandable and reviewable to facilitate adoption by the scientific community. While currently implemented methods are simplistic and unvalidated, further development and demonstration of this framework could enable high-throughput, accurate, and accessible EDS characterization.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Affine Transformations to Correlate Experimental and Simulated EDS Spectra for Multi-Element Systems

Energy Dispersive X-ray Spectroscopy (EDS) is an essential technique for determining elemental concentrations and distributions within microstructures, critical for materials discovery, optimization, and qualification. However, most published EDS data is qualitative because current quantitative EDS analysis methods require extensive calibration and post-processing, limiting their practicality and widespread adoption. This work seeks to establish a framework for accelerated EDS characterization and spectrum analysis that can leverage ML to analyze correlations between various elemental compositions and resulting EDS spectra. The complex physics and data result in a high-dimensional problem that grows exponentially with the number of elements in the system and the complexity of the spectrum analysis. ML provides a way to compute and optimize the results of this highly dimensional problem in a flexible way to tailor it to the user’s specific needs and material system. However, the framework emphasizes transparency through a strictly mathematical affine transformation, so the analysis remains understandable and reviewable to facilitate adoption by the scientific community. While currently implemented methods are simplistic and unvalidated, further development and demonstration of this framework could enable high-throughput, accurate, and accessible EDS characterization.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Characterization of Oxide + TiN Inclusions in Fe-16 Mass Pct Cr Ferritic Alloy Using Automatic SEM-EDS Analysis

The assessment of automatic SEM-EDS results is significant to reveal the possible inaccuracy of the results and the limitation of this characterization technique in analyzing inclusions. In current research, the oxide + TiN inclusion in Fe-16 mass pct Cr ferritic alloy is characterized by emphasizing the effects of Mg addition and N content on the composition, morphology, homogeneity of dispersion, and size distribution of inclusions; the assessment of automatic SEM-EDS results in rapid analysis concerning its limitation and the utilization of its advantage to clarify the formation mechanism of inclusions are conducted. The nature of inclusions is revealed. Mg addition makes the number density of inclusions larger and the size of inclusions finer. The effect of N content on the size of oxde + TiN was not obvious. Automatic SEM-EDS analysis is deficient in detecting light elements and low content elements in the inclusions and distinguishing between TiN and oxide + TiN. Optimizing the experimental design and combining automatic SEM-EDS results with manual SEM-EDS and optical microscopy results can contribute to delivering accurate and speedy results.

36 MATERIALS SCIENCE↗

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

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

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Chemical Quantification of Atomic-Scale EDS Maps under Thin Specimen Conditions

We report our effort to quantify atomic-scale chemical maps obtained by collecting energy-dispersive X-ray spectra (EDS) using scanning transmission electron microscopy (STEM) (STEM-EDS). Under a thin specimen condition and when the EDS scattering potential is localized, the X-ray counts from atomic columns can be properly counted by fitting Gaussian peaks at the atomic columns, and can then be used for site-by-site chemical quantification. The effects of specimen thickness and X-ray energy on the Gaussian peak-width are investigated by using SrTiO 3 (STO) as a model specimen. The relationship between the peak-width and spatial-resolution of an EDS map is also studied. Furthermore, the method developed by this work is applied to study a Sm-doped STO thin film and antiphase boundaries present within the STO film. We find that Sm atoms occupy both Sr and Ti sites but preferably the Sr sites, and Sm atoms are relatively depleted at the antiphase boundaries likely due to the effect of strain.

36 MATERIALS SCIENCE↗

Optimization of SEM-EDS to determine the C–A–S–H composition in matured cement paste samples

Microanalysis of characteristic X-rays in the SEM is a powerful method to assess the chemical composition of phases in cement pastes, in particular the calcium silicate hydrate containing aluminium (C–A–S–H). Nevertheless, many variables may influence the results obtained, due mainly to the intimate mixing of C–A–S–H with other hydrate phases and the susceptibility of this phase to damage by the electron beam. In this study the effect of various acquisition parameters was examined, along with methods to determine an “average” C–A–S–H composition. The results acquired in the SEM were compared with the analysis of the same samples in the TEM, where phases can be analyzed without intermixing. A simple method was used to obtain compositions from SEM based analysis that are very close to those which can be obtained in the TEM. - Highlights: •The intermixing of phases is the limiting factor in the analysis of C–A–S–H composition by SEM-EDS •Guidelines to limit beam damage and properly analyze C–A–S–H composition by SEM-EDS are given •SEM-EDS and TEM-EDS give similar results when proper data treatment is made.

36 MATERIALS SCIENCE↗