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At least 1,783 records · Page 99

Calibration and Data Analysis of a Frequency Selectable Laser Source for CMB Detector Characterization

Cosmic Microwave Background (CMB) experiments study faint radiation left over from the early universe. The CMB was created when the universe became cool enough for light to travel freely through space, and today it gives scientists one of the earliest images of the universe. One important goal of modern CMB experiments is to measure this radiation with higher precision in order to search for evidence that supports the theory of cosmic inflation. To do this, scientists use extremely sensitive detectors that must be calibrated accurately. The Frequency Selectable Laser Source, or FLS, is a new calibration tool that can send selected frequencies to detectors and help measure their response. During my internship, I worked on the FLS after it returned to Fermilab from Chile, where it had been used to characterize detectors at the Simons Observatory. The system came back in parts, so the first part of my project was helping rebuild the optical and mechanical setup. After the system was rebuilt, we performed alignments to maximize the receiver photocurrent. We then collected calibration measurements over different frequency ranges, including 543 GHz to 568 GHz, 740 GHz to 766 GHz, and 60 GHz to 500 GHz. These measurements were used to check waterline calibration and reflectivity features and compare new data with previous data. Another major part of my project was learning Python so I could understand previous analysis code, modify it for new files, and write my own code to compare the mean response between datasets. The results showed that the new data was close to previous measurements and that waterline features near 556 GHz and 752 GHz were found within less than 1.5 GHz of the expected values. I also completed the reflectivity analysis for five prisms in two polarization orientations. In the original orientation, the results were consistent between the five prisms and close to values measured on a different system at the University of Chicago. I then collected a second set of measurements on my own with the polarization of the laser rotated by 90 degrees and compared them with the original data using the same Python workflow. The measured reflectivity increased for all five prisms in the new orientation, showing that the prism reflectivity depends on polarization. Future work will focus on using the FLS to characterize real CMB detectors.

Pumarino Meza, Rafael [Unlisted, US; Fermilab]↗

Calibration and Data Analysis of a Frequency Selectable Laser Source for CMB Detector Characterization

Cosmic Microwave Background (CMB) experiments study faint radiation left over from the early universe. The CMB was created when the universe became cool enough for light to travel freely through space, and today it gives scientists one of the earliest images of the universe. One important goal of modern CMB experiments is to measure this radiation with higher precision in order to search for evidence that supports the theory of cosmic inflation. To do this, scientists use extremely sensitive detectors that must be calibrated accurately. The Frequency Selectable Laser Source, or FLS, is a new calibration tool that can send selected frequencies to detectors and help measure their response. During my internship, I worked on the FLS after it returned to Fermilab from Chile, where it had been used to characterize detectors at the Simons Observatory. The system came back in parts, so the first part of my project was helping rebuild the optical and mechanical setup. After the system was rebuilt, we performed alignments to maximize the receiver photocurrent. We then collected calibration measurements over different frequency ranges, including 543 GHz to 568 GHz, 740 GHz to 766 GHz, and 60 GHz to 500 GHz. These measurements were used to check waterline calibration and reflectivity features and compare new data with previous data. Another major part of my project was learning Python so I could understand previous analysis code, modify it for new files, and write my own code to compare the mean response between datasets. The results showed that the new data was close to previous measurements and that waterline features near 556 GHz and 752 GHz were found within less than 1.5 GHz of the expected values. I also completed the reflectivity analysis for five prisms in two polarization orientations. In the original orientation, the results were consistent between the five prisms and close to values measured on a different system at the University of Chicago. I then collected a second set of measurements on my own with the polarization of the laser rotated by 90 degrees and compared them with the original data using the same Python workflow. The measured reflectivity increased for all five prisms in the new orientation, showing that the prism reflectivity depends on polarization. Future work will focus on using the FLS to characterize real CMB detectors.

Pumarino Meza, Rafael [Unlisted, US; Fermilab]↗

Characterization of Advanced Imaging Systems for High-Resolution and Event-Mode Detection

Post-irradiation examination (PIE) is a continually growing field critical to the development of improved nuclear fuels. To characterize these materials, neutron imaging systems are employed and outfitted with, typically, CMOS or CCD cameras - complementary metal oxide semiconductor sensors and charge-couple devices. Imaging systems are a team-effort between the camera, scintillating materials, and object of interest, as a result of neutrons' inherent need to be converted to a detectable signal. High resolution imaging, flash radiography imaging, and event-mode detection systems are three systems undergoing development, construction, and characterization for improved spatial resolution and time-of-flight detection for PIE efforts.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Standardization Gaps in Powder Feedstock Characterization and Establishing Acceptability for Reuse in Additive Manufacturing

Characterization techniques for powder feedstocks used in additive manufacturing (AM) have long been relied upon to describe the inputs to an AM workflow. However, functional gaps remain between tests to measure intrinsic and extrinsic properties with the direct performance within AM equipment. Furthermore, the common practice of reusing powder through multiple build cycles introduces effects and changes to feedstock performance that are otherwise difficult to measure quantitatively. Here, standardization and the development of new test methods have not kept pace with the rapid evolution of the AM industry and its reliance on highly coupled process-structure–property-performance relationships.

Characterization and Analytical Technique↗

High-Throughput Microstructural Characterization and Process Correlation Using Automated Electron Backscatter Diffraction

The need to optimize the processing conditions of additively manufactured (AM) metals and alloys has driven advances in throughput capabilities for material property measurements such as tensile strength or hardness. High-throughput (HT) characterization of AM metal microstructure has fallen significantly behind the pace of property measurements due to intrinsic bottlenecks associated with the artisan and labor-intensive preparation methods required to produce highly polished surfaces. This inequality in data throughput has led to a reliance on heuristics to connect process to structure or structure to properties for AM structural materials. In this study, we show a transformative approach to achieve laser powder bed fusion (LPBF) printing, HT preparation using dry electropolishing and HT electron backscatter diffraction (EBSD). This approach was used to construct a library of > 600 experimental EBSD sample sets spanning a diverse range of LPBF process conditions for AM Kovar. This vast library is far more expansive in parameter space than most state-of-the-art studies, yet it required only approximately 10 labor hours to acquire. Build geometries, surface preparation methods, and microscopy details, as well as the entire library of >600 EBSD data sets over the two sample design versions, have been shared with intent for the materials community to leverage the data and further advance the approach. Using this library, we investigated process–structure relationships and uncovered an unexpected, strong dependence of microstructure on location within the build, when varied, using otherwise identical laser parameters.

Characterization and Analytical Technique↗

Multi-modal tomographic imaging system for poolside characterization of nuclear test fuels: Design considerations and studies

Testing and qualification of advanced nuclear fuels involves an iterative process of prototyping, in-pile irradiation testing, and in-situ or ex-situ examination. Fuel restructuring and fission product migration during burnup are among the most important aspects of fuel evolution that affect several important performance characteristics such as heat removal, accident tolerance, and fission product retention. Pool-side non-destructive characterization techniques provide fuel developers with tools to understand fuel evolution at different points of burnup. A design for a compact, submersible, and multi-modal gamma-ray tomography system for imaging irradiated nuclear fuel is presented here. Detector selection, collimator geometry and fabrication, mechanical design, imaging protocol and acquisition speed are discussed. Modeling calculations show that sub-millimeter resolution can be achieved in both transmission computed tomography images as well as in emission computed tomography images in a matter of hours. Several design compromises and fabrication challenges are discussed which should be taken into consideration for future submersible gamma-ray tomography instruments.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Characterizing Variability in Lignocellulosic Biomass: A Review

Feedstock variability is a significant barrier to the scale-up and commercialization of lignocellulosic biofuel technologies. Variability in feedstock characteristics and behavior creates numerous challenges to the biorefining industry by affecting continuous operation and biofuels yields. Recently, feedstock variability is understood and explained largely on the basis of chemical composition. Physical and mechanical properties and behavior of lignocellulosic feedstock in various unit operations, studied through advanced analytical methods, can further explain variability. Such studies will enable us in developing processes and designing equipment to improve operation and conversion performance. In this perspective, we review several advanced analytical methods that measure density, moisture content, thermal properties, flowability, grindability, rheology properties, and micromorphological characteristics. We also discuss the correlations and interactions among these properties that reflect the complexity of lignocellulosic biomass as a feedstock and the associated quality metrics and logistics of supplying consistent quality feedstock to a biorefinery. We further examine methods that have not traditionally been used to characterize lignocellulosic feedstocks but have the potential to bridge the gap in our explanation of feedstock variability.

09 BIOMASS FUELS↗

Process design for calcination of nickel-based cathode materials by in situ characterization and multiscale modeling

Developing battery materials towards commercial use, from the early discovery through synthesis, processing, scaling up, and eventually to industrial production, may take decades. A notable example is Ni-based layered oxides, which were discovered as early as 1950s and intensively pursued as cathode active materials (CAMs) since the early 90s but have yet to realize their full commercial potential. Significant efforts have been devoted to materials development aiming at improving performance, far less to process development for large-scale synthesis and processing of CAMs. In this paper, we present a rational design of calcination for scalable production of Ni-based CAMs. We start with an overview of the current understanding and knowledge gaps hindering rational process design and scaling-up of the calcination process. Then with specific examples, we demonstrate how to tackle those fundamental challenges through in situ characterization and multiscale modeling. Finally, we conclude by providing perspectives on the remaining challenges and emerging opportunities in commercial development of Ni-based cathodes, calling for more endeavors in this field.

25 ENERGY STORAGE↗

Geologic Characterization for CO 2 Storage with Enhanced Oil Recovery in Northern Michigan

The Midwest Regional Carbon Sequestration Partnership (MRCSP) was founded in 2003 as part of the U.S. Department of Energy’s (DOE’s) Regional Carbon Sequestration Partnership initiative. Since its founding, MRCSP has made significant strides toward making CCUS a viable option for states in the region. The public/private consortium, funded through the DOE Regional Carbon Sequestration Initiative, brings together nearly 40 industry partners and 10 states. Battelle, as the project lead, oversees research, development and operations and coordinates activities among the partners. The incremental, phased approach has built a valuable knowledge base for the industry and paved the way for commercial-scale adoption of CCUS technologies. From 2008 to 2020, MRCSP Phase III focused on the development of large-scale injection projects. This report is part of a series of reports prepared under the Midwestern Regional Carbon Sequestration Partnership (MRCSP) Phase III (Development Phase). These reports summarize and detail the findings of the work conducted under the Phase III project. This report compiles the results of geologic characterization of late-stage reefs, active EOR reefs, and new EOR reefs in the Northern Niagaran Pinnacle Reef Trend (NNPRT) in Michigan to demonstrate developed methodologies, geologic variability, and reservoir potential for CO 2 storage. Conducting CO 2 injection and monitoring in these settings provide significant insights for addressing the project objectives: assessment of injectivity in complex carbonate reef deposits; assessing CO 2 trapping mechanisms in a closed reservoir system; assessing any final oil recovery from transitional or residual oil zones in a field where CO 2 flooding is nearing completion; evaluating the transition from EOR to storage of CO 2 ; assessing regional commercialization; assessing new technologies for tracking CO 2 , brine, and oil movements underground; and monitoring options in a closed reservoir with oil, residual oil, and water zones.

01 COAL, LIGNITE, AND PEAT↗

In Situ Microstructure Characterization of Potassium Di-Phosphate (KDP) Densification during Cold Sintering

In order for ceramic additive manufacturing (AM) to achieve its full potential, it is increasingly important to develop a more rigorous understanding of fundamental phenomena that govern the kinetics and thermodynamics of ceramic AM processes. In the case of additive build processes, such as direct ink write and ceramic extrusion, methods for densifying the resulting green-body product need to be considered to complement the efficiencies of ceramics AM, itself. One densification route, at least for monolithic components, built layer-by-layer, is offered by the recently developed cold sintering process, whereby high-density final product is achieved through addition of a small amount of liquid solvent and application of modest uniaxial compressive stress at relatively low temperature. In situ small-angle X-ray scattering methods and X-ray diffraction have been applied to characterize and quantify the pore morphology evolution during cold sintering for a model system: potassium di-phosphate, KH 2 PO 4 (KDP). It is shown that both temperature and applied stress affect the densification rate, but stress has a stronger effect on the evolving morphology. A regime with an approximate linear densification rate can be identified, yielding an effective densification activation energy of ≈90 kJ/mol.

36 MATERIALS SCIENCE↗

Comparison of Microbial Profiling and Tracer Testing for the Characterization of Injector-Producer Interwell Connectivities

Insufficient understanding of the microbial communities and associated microbial processes in geological reservoirs hinders the utilization of this rich data source for improved resource management. In this study, along with four interwell tracer tests at a 1478-m deep fractured crystalline-rock aquifer, we analyzed the microbial communities in the injected and produced water by high-throughput sequencing. The microbial community similarities across boreholes during an interwell flow scenario frequently encountered in reservoir development was explored. Despite the significant tracer recoveries (~30%) in all tracer tests and the cumulatively >100,000 L of exogenous water (carrying exogenous microbes) injected into the 10-m-scale reservoir, the overall structure of produced-fluid microbiome did not increasingly resemble that of the injectate. However, producers with better connectivity with the injector (based on tracer test results) did have more amplicon sequence variants (ASVs) that overlapped with those in the injectate. We identified possible drivers behind our observations and verified the practicality of repeated microbial sampling in the context of reservoir characterization and long-term monitoring. We highlight that injector-producer microbial profiling could provide insights on the relative connectivities across different producers with a given injector, and that the associated logistical needs may be comparable or even less than that of classic tracer tests.

59 BASIC BIOLOGICAL SCIENCES↗

Multiscale Materials Characterization

The National Renewable Energy Laboratory (NREL) is advancing the state of the art in multiscale characterization to solve critical issues in materials science. We enthusiastically welcome industry, manufacturing, and government enterprises to partner with us on design integration that ranges from materials selection to manufacturing to reliability.

characterization↗

Characterization of ambient polychlorinated biphenyl background conditions in surface waters of the Pajarito Plateau, New Mexico

Abstract This study presents the development of polychlorinated biphenyl (PCB) background threshold values (BTVs) that statistically characterize ambient background conditions for surface waters in undeveloped and developed landscapes of the Pajarito Plateau in the Rio Grande Basin of New Mexico. Between 2009 and 2018, surface water data were collected at 45 locations under a variety of flow conditions and regimes. A total of 163 samples were collected, with roughly 1/3 of samples and locations being in undeveloped areas (n = 53 from 17 locations), and the remainder being in developed areas (n = 110 from 28 locations). While there are areas on the Pajarito Plateau where PCB point sources are known or likely to have contributed to PCBs in soils, PCB BTVs calculated for undeveloped portions of watersheds (upstream of areas where PCB point sources are known or likely to have contributed to PCBs in soils, and therefore not affected by PCB sources within the watershed) are well above New Mexico's human health organism-only (HH-OO) water quality criterion (0.64 ng/L). Background threshold values are even higher in developed areas upstream of managed soil sites, suggesting that in developed areas, both diffuse ambient PCB sources (e.g., atmospheric deposition) and localized urban sources (e.g., building materials, paints, and electrical equipment) contribute to PCBs in those watersheds. These findings indicate that New Mexico's current HH-OO water quality criterion for PCBs cannot practicably be met due to ambient conditions. It is also impracticable to meet the US Environmental Protection Agency (EPA) criterion continuous concentration (CCC) of 14 ng/L in developed background areas, where the BTV is approximately 1.5 times the CCC. Integr Environ Assess Manag 2023;19:1307–1319. © 2022 SETAC

54 ENVIRONMENTAL SCIENCES↗

Characterization of PuO 2 With Visible and UV Raman Spectroscopy: Discrimination Between the Bulk, Surface, and an Intermediate Disordered Layer

Raman spectroscopy is an ideal tool in the characterization of materials including PuO 2 . The wavelength-dependent absorptivity of the material defines the light penetration depth and the relative Raman scattering contribution from the bulk and the surface. Here, the surface contribution to the total Raman scattering was investigated for PuO 2 calcined at various temperatures and recorded with laser wavelengths of 355, 325, and 244 nm. These experiments provided the first glimpse of the wavelength-dependent disappearance and emergence of new phonons and electronic bands from the PuO 2 surface layers. The first indication of the wavelength transition in the Raman spectra was the loss of the 2LO2 (overtone, ~1155 cm -1 ) band and the weakening intensity of the Г 1 → Γ 5 electronic band (~2135 cm -1 ) with the 355-nm excitation laser. The Γ 5 electronic band was barely visible with the 244-nm excitation. The electronic band located at ~1050 cm -1 , corresponding to the Г 1 → Γ 4 electronic transition was observed to dramatically increase in intensity while the Г 1 → Γ 3 electronic band (2640 cm -1 ) sharpened as the UV wavelength was increased in energy from the near- to deep-UV (355–325–244 nm). The FWHM of the T 2g band was found to vary with calcination temperature (450°C and 900°C) with the 325-nm laser and the 244-nm laser. The T 2g band attributes, the strong emergence of the Г 1 → Γ 4 electronic band, and the disappearance of the 2LO2 overtone acquired with the 244-nm excitation for the different calcination temperatures suggest a shallow penetration depth.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Characterizing mechanical and microstructural properties of novel montmorillonite-rich polyethylene composites

Montmorillonite (MMT) clays are important industrial materials used as catalysts, chemical sorbents and fillers in polymer–clay nanocomposites. The layered structure of these clays has motivated research into further applications of these low-cost materials, including use as ion exchange media and solid-state ionic conductors. In these applications, the mechanical properties of MMT are key when considering long-term, reliable performance. Previous studies have focused on the mechanical properties of nanocomposites with MMT as the minority component or pure MMT thin films. In this work, the microstructure and mechanical properties of pure MMT and majority MMT/polyethylene composites pressed into dense pellets are examined. Characterization methods such as X-ray diffraction, atomic force microscopy and scanning electron microscopy together with nanoindentation reveal important structure–property relationships in the clay-based materials. Here, utilizing these techniques, we have discovered that MMT processing impacts the layered microstructure, chemical stability and, critically, the elastic modulus and hardness of bulk MMT samples. Particularly, the density of the pellets and the ordering of the clay platelets within them strongly influence the elastic modulus and hardness of the pellets. By increasing pressing force or by incorporating secondary components, the density, and therefore mechanical properties, can be increased. If the layered structure of the clay is destroyed by exfoliation, the mechanical properties will be compromised. Understanding these relationships will help guide new studies to engineer mechanically stable MMT-based materials for industrial applications.

36 MATERIALS SCIENCE↗

Peptoid-based hierarchically-structured biomimetic nanomaterials: Synthesis, characterization and applications

Peptoids (or poly-N-substituted glycines) is a promising class of bioinspired sequence-defined polymers due to their highly efficient synthesis, high chemical stability, enzyme hydrolysis resistance, and biocompatibility. By tuning the side chain chemistry of peptoids, it allows for a precise control over sequences and achieving a large side-chain diversity. Due to these unique features, in the last several years, many amphiphilic peptoids were designed as highly tunable building blocks for the preparation of biomimetic nanomaterials with well-defined hierarchical structures and desired functionalities. In this paper, we provide an overview of the recent achievements in this area by dividing them into the following three aspects. First, mica- and silica-templated peptoid self-assembly was summarized. Here, the presence of inorganic substrates provides the guarantee of investigating their self-assembly mechanisms and interactions between peptoids and substrates using nanoscale characterization techniques, particularly in situ atomic force spectroscopy (AFM) and AFM-based dynamic force spectroscopy (AFM-DFS). Second, solution-phase self-assembly of peptoids into nanotubes and nanosheets was presented, as well as their self-repair properties. Third, the applications of peptoid based nanomaterials were outlined, including the construction of catalytic nanomaterials as a template and cytosolic delivery as cargoes.

36 MATERIALS SCIENCE↗

Multimodal 3D characterization of voids in shock-loaded tantalum: Implications for ductile spallation mechanisms

Predicting the failure of crystalline materials at high strain rates requires knowledge of the underlying failure mechanisms and their dependence on microstructure. However, little experimental consensus exists on the underlying micromechanics of spallation. In this study, a 3D-EBSD characterization experiment is performed on tantalum prior to and after partial spallation by plate impact, which allowed for the statistical assessment of the microstructural neighborhoods surrounding incipient voids. In analyzing the resulting dataset containing 5884 grains and 467 voids, it is observed that the voids were roughly spherical and consistent in size throughout the spalled material. The voids mostly resided at quadruple points, at triple junctions, at grain boundaries, and within grains, in decreasing order of prevalence. Moreover, voids tended to form at grain boundaries with high degrees of plastic incompatibility, growing into the plastically soft grain but orienting primarily with or perpendicular to the loading direction. Here, the statistics from these analyses of 3D microstructural data support dynamic cavitation models for ductile spallation.

36 MATERIALS SCIENCE↗