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Rapid kVp switching dual-energy CT in the assessment of urolithiasis in patients with large body habitus: preliminary observations on image quality and stone characterization

Purpose: The purpose of this study was to investigate the image quality (IQ) considerations of rapid kVp switching dual-energy CT (rsDECT) in the assessment of urolithiasis in patients with large body habitus and to evaluate whether it allows stone characterization. Materials and methods: In this IRB-approved, HIPAA compliant retrospective study, 93 consecutive patients (M/F = 72/21, mean age 56.9 years, range 23–83 years) with large body habitus (> 90 kg/198 lbs) who underwent dual-energy (DE) stone protocol CT on a rapid kVp switching DECT scanner between January 2013 and December 2016 were included. Scan acquisition protocol included an initial unenhanced single-energy CT (SECT) scan of KUB followed by targeted DECT in the region of stones. Two readers evaluated both CT data sets (axial 5 mm 120 kVp/140 kVp QC/70 keV monoenergetic, material density water/iodine images and coronal/sagittal 3 mm images) for the assessment of image quality (Scores: 1–4) and characterization of stone composition (reference standard: crystallography). Results: One hundred and five CT examinations were performed in 93 patients (mean body weight 105.12 ± 13.53 kg, range 91–154 kg), and a total of 321 urinary tract calculi (mean size-4.8 ± 3.2 mm, range 1.2–22 mm) were detected. Both SECT and targeted monoenergetic images were of acceptable image quality (mean IQ: 3.77 and 3.83, kappa 0.79 and 0.87 respectively). Material density water and iodine images had lower IQ scores (mean IQ: 2.97 and 3.09 respectively) with image quality deterioration due to severe photon starvation/streak artifacts in 20% (21/105) and 17% (18/105) scans, respectively. Characterization of stone composition into uric acid/non-uric acid stones was achieved in 93.14% (299/321) of calculi (mean size: 4.99 ± 3.3 mm, range 1.2–22 mm), while 7% (22/321) stones could not be characterized (mean size 3.03 ± 1.16 mm, range 1.6–6.4 mm) (p < 0.001). Most common reason for non-characterization was image quality deterioration of the material density iodine images due to severe photon starvation artifacts. On multivariate regression, stone size and patient weight were predictors of stone composition determination on DECT (p < 0.05). The transverse diameter had a weak negative correlation with stone composition determination, but it was not statistically significant. Stone characterization into uric acid vs. non-uric acid stones was accurate in 95% (n = 38/40) of stones in comparison with crystallography. Conclusion: In patients with large body habitus, rsDECT allowed characterization of most calculi (93%) despite image quality deterioration due to photon starvation/streak artifacts in up to 20% of material density images. Stone size and patient weight were predictors of stone composition determination on DECT, and small calculi in very large patients may not be characterized.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

Advanced Characterization of Thin Film Solar Cells

Polycrystalline thin-film solar cells have reached a levelized cost of energy that is competitive with all other sources of electricity. The technology has significantly improved in recent years, with laboratory cell efficiencies for cadmium telluride (CdTe), perovskites, and copper indium gallium diselenide (CIGS) each exceeding 22 percent. Both CdTe and CIGS solar panels are now produced at the gigawatt scale. However, there are ongoing challenges, including the continued need to improve performance and stability while reducing cost. Advancing polycrystalline solar cell technology demands an in-depth understanding of efficiency, scaling, and degradation mechanisms, which requires sophisticated characterization methods. These methods will enable reseachers and manufacturers to improve future solar modules and systems. This work provides researchers with a concise overview of the status of thin-film solar cell technology and characterization. Chapters describe material systems and their properties and then provide an in-depth look at relevant characterization methods and the learning facilitated by each of these. Following an introductory chapter, the book provides systematic and thorough coverage of the following topics: trends to improve CdTe solar cell performance; Cu(In,Ga)Se2 and related materials; perovskite solar cells; photovoltaic device modelling; luminescence and thermal imaging of thin-film photovoltaic materials, devices, and modules; application of spatially resolved spectroscopy characterization techniques on Cu2ZnSnSe4 solar cells; time-resolved photoluminescence characterization of polycrystalline thin-film solar cells; fundamentals of electrical material and device spectroscopies applied to thin-film polycrystalline chalcogenide solar cells; nanometer-scale characterization of thin-film solar cells by atomic force microscopy-based electrical probes; scanning transmission electron microscopy characterization of solar cells; photoelectron spectroscopy methods in solar cell research; time-of-flight secondary-ion mass spectrometry and atom probe tomography; and solid-state nuclear magnetic resonance characterization for photovoltaic applications. The final chapter provides an overview and describes future prospects.

41 EE - Solar Energy Technologies Office (EE-4S)↗

Characterization Report for the MP-1 Experiment Fabrication Campaign

This report covers the results of MP 1 fuel characterization analysis to provide a detailed understanding of the as-fabricated fuel that would be irradiated in the MP 1 (Mini-Plate 1) experiment. The work was performed at Pacific Northwest National Laboratory (PNNL), Idaho National Laboratory (INL), and Los Alamos National Laboratory (LANL). Characterization of the as-fabricated fuel was performed in accordance with Characterization Plan for the Fabrication of U 10Mo for the MP 1 Experiment, hereinafter the MP 1 Characterization Plan (MAQP 2016). Under the MP 1 Characterization Plan, fuel foils at different points in the foil fabrication process (e.g., hot rolled annealed, cold rolled annealed) were studied to understand the effect of various thermomechanical processes on the fuel microstructure. Samples were sent to each of the three organizations so that testing and analysis could be performed independently using similar equipment and a standardized set of measurement and analysis procedures. The MP 1 experiment will provide an opportunity to understand the effects of processing conditions on the final fuel microstructure, to compare independently obtained results, and achieve a three-way validation. PNNL characterized 28 uranium–10 wt% molybdenum (U 10Mo) samples. Six pieces/specimens from each sample/foil were sectioned, in accordance with the MP 1 Characterization Plan. Similarly, INL and LANL also examined 24 and 17 U 10Mo specimens, respectively. These total 69 samples consist of six types of MP 1 characterization foils fabricated by Babcock and Wilcox Technologies (BWXT) from ingots produced by the Y-12 National Security Complex: • 0.047 in.-thick hot-rolled and annealed samples with and without Zr layers • 0.02 in.-thick cold-rolled and annealed samples with and without Zr layers • 0.01 in.-thick cold-rolled and annealed samples with and without Zr layers. Microstructure, chemical composition, carbide morphology, U 10Mo foil thickness, Zr thickness, mechanical properties (microhardness), and density were evaluated in both longitudinal and transverse directions for foils of the three different thicknesses.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Report on initial development of a database of nuclear graphite characteristics based on microstructural characterization

This report outlines the current and future efforts to produce a comprehensive library of microstructures of nuclear graphite and carbon-based materials that are candidate materials for nuclear applications in the United States. This library must contain extensive characterizations of unirradiated graphite materials, a guide to some of the techniques used to characterize graphite, a compendium of characterization data of neutron-irradiated or oxidized material, and a compendium of microstructural information of carbon-based materials. These characterization efforts are being conducted at various length scales to understand these complex materials’ local structure and property relationships. Achieving this goal requires further developing or adapting advanced characterization techniques that capture graphite’s most relevant characteristics. Some of the general objectives of this project are to aid with the material selection, licensing, management, and core assessments of a graphite core by documenting the unirradiated microstructure of relevant grades or by characterizing the evolution of the microstructure under the reactor environment. Moreover, this project aims to provide additional information, guidelines for characterizing graphite, and a protocol to assess a nuclear graphite grade. This report also summarizes some of the initial results and some of the techniques commonly used to characterize nuclear graphite.

36 MATERIALS SCIENCE↗

Characterization Report for the MP-1 Experiment Fabrication Campaign (Rev.1)

This report covers the results of MP 1 fuel characterization analysis to provide a detailed understanding of the as-fabricated fuel that would be irradiated in the MP 1 (Mini-Plate 1) experiment. The work was performed at Pacific Northwest National Laboratory (PNNL), Idaho National Laboratory (INL), and Los Alamos National Laboratory (LANL). Characterization of the as-fabricated fuel was performed in accordance with Characterization Plan for the Fabrication of U 10Mo for the MP 1 Experiment, hereinafter the MP 1 Characterization Plan (MAQP 2016). Under the MP 1 Characterization Plan, fuel foils at different points in the foil fabrication process (e.g., hot rolled annealed, cold rolled annealed) were studied to understand the effect of various thermomechanical processes on the fuel microstructure. Samples were sent to each of the three organizations so that testing and analysis could be performed independently using similar equipment and a standardized set of measurement and analysis procedures. The MP 1 experiment will provide an opportunity to understand the effects of processing conditions on the final fuel microstructure, to compare independently obtained results, and achieve a three-way validation. PNNL characterized 28 uranium–10 wt% molybdenum (U 10Mo) samples. Six pieces/specimens from each sample/foil were sectioned, in accordance with the MP 1 Characterization Plan. Similarly, INL and LANL also examined 24 and 17 U 10Mo specimens, respectively. These total 69 samples consist of six types of MP 1 characterization foils fabricated by Babcock and Wilcox Technologies (BWXT) from ingots produced by the Y-12 National Security Complex: (a.) 0.047 in.-thick hot-rolled and annealed samples with and without Zr layers; (b.) 0.02 in.-thick cold-rolled and annealed samples with and without Zr layers; and (c.) 0.01 in.-thick cold-rolled and annealed samples with and without Zr layers. Microstructure, chemical composition, carbide morphology, U 10Mo foil thickness, Zr thickness, mechanical properties (microhardness), and density were evaluated in both longitudinal and transverse directions for foils of the three different thicknesses.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Interface Characterization within a Nuclear Fuel Plate

To predict the performance of nuclear fuels and materials, irradiated fuel plates must be characterized efficiently and accurately in highly radioactive environments. The characterization must take place remotely and work in settings largely inhospitable to modern digital instrumentation. Characterization techniques based on non-contacting laser sensing methods enable remote operation in a robust manner within a hot-cell environment. Laser characterization instrumentation can offer high spatial resolution and remain effective for scanning large areas. A laser shock (LS) system is currently being developed as a post-irradiation examination (PIE) technique in the hot fuel examination facility (HFEF) at the Idaho National Laboratory (INL). The laser shock technique will characterize material properties and failure loads/mechanisms in various composite components and materials such as plate fuel and next-generation fuel forms in high radiation areas. The laser shock-technique induces large amplitude shock waves to mechanically characterize interfaces such as the fuel–clad bond. As part of the laser shock system, a laser-based ultrasonic C-scan system will be used to detect and characterize debonding caused by the application of the laser shock. The laser shock system has been used to characterize the resulting bond strength within plate fuels which have been fabricated using different fabrication processes. The results of this study will be to select the fabrication process that provides the strongest interface.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

International Network for Nuclear Waste Characterization (IAEA-Labonet) - Facts and Future - 18566

LABONET was launched early 2011 by the International Atomic Energy Agency (IAEA) as an international network on nuclear waste characterization. Its objective is to improve the quality of, and harmonize, activities related to the radioactive waste characterization in IAEA Member States. It is widely accepted that proper characterization of radioactive waste through its entire flow-sheet is a key activity. In particular the needs and problems in radioactive waste characterization in the participating countries are a main concern within LABONET, as the programs are not elaborated to the same level in the various countries. LABONET wants to facilitate the exchange of international experience in the application of proven, quality assured practices for the characterization of waste and waste packages. This will be beneficial for the less developed countries. The objectives of LABONET are achieved via different actions: a) exchanging information and expertise via presentations and discussions at technical meetings; b) expert meetings on particular topics of interest, for instance e-learning and e-platforms; c) training sessions in less developed countries, for instance, on non-destructive assay of waste packages; d) facilitate the exchange of information amongst its members; and e) assist member states in establishing characterization plans that are cost effective and of good quality. LABONET is continuously encouraging institutions or professionals who need some assistance or can help in solving questions about characterization to be a member. Currently, LABONET is preparing for its future, including projects addressing common problems of its members. Aiming at the dissemination of this important network for the professionals involved in radioactive waste characterization, this paper will discuss the following issues: (1) the objectives of LABONET, (2) its structure, membership and organization of meetings, (3) some achievements, and (4) plans for the future. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Development of a Technical Standard for Radiological Characterization of DAW - 19552

Since the Manhattan Project, the U.S. Department of Energy (DOE) and its predecessor agencies have performed a wide mission involving nuclear materials and weapons development, production, testing, and modernization. While the initial mission components relied heavily upon reactor physics and chemistry, the environmental programs have increasingly relied upon development of more accurate and effective measurement methodologies to determine the radiological and chemical properties of the unique waste streams that were generated during the weapons production and testing mission. During the ongoing site cleanup program, the DOE laboratories and former production sites have developed a wide range of site-specific processes and procedures for conducting radiological characterization of dry active waste (DAW) that is managed as low-level radioactive waste. This has resulted in a Complex-wide variability among sites with respect to the methodologies and instrumentation used to characterize individual waste streams. The DAW-type waste was selected for development of a characterization standard since it is a simple, voluminous, and repetitive waste stream with a substantial knowledge base, established experience history at multiple site locations, and the potential for realization of programmatic benefits though standardization. Implementation of a consistent, standardized approach to DAW characterization will take advantage of multiple applications for a technology that is both mature and stable. The DAW characterization process is repetitive and lends itself to implementation at a wide range of operating locations - resulting in economies of scale, compliance with regulatory requirements, and consistent implementation of procedures which support design, operations, maintenance, and management of facilities, activities and environmental restoration programs. In response to a request from DOE, the Energy Facility Contractors Group (EFCOG) Waste Management Working Group (WMWG) is supporting the development of a new DOE Technical Standard for Radiological Characterization of DAW. The purpose of the proposed new standard is to provide a technical resource that integrates and enhances the utilization of current site-specific methodologies and processes. An EFCOG/WMWG technical team has prepared a Technical Basis Document (TBD) to support the development and utilization of the new standard. The TBD provides detailed reference information for use by site personnel when implementing the guidance to be provided in the standard. It also provides the rationale for and details concerning the recommended technical approaches for radiological characterization of representative DAW-type waste streams. The TBD is an essential resource and will be included as an appendix to the proposed standard. Formulation of the new standard will draw upon the information contained in the TBD in order to integrate and improve the utilization of current site-specific methodologies and processes. It will also include a comparison of current radiological characterization methodologies to determine which ones are most reliable and effective in producing relevant and valid data. In view of the long history and participation by several agencies in the regulation of nuclear programs, existing Voluntary Consensus Standards have also been identified in the TBD and will be referenced for relevancy and applicability to the new proposed standard. A Project Justification Statement (PJS) was also developed by the EFCOG/WMWG Team. Following internal Team review and approval by EFCOG, the draft PJS was submitted through Argonne National Laboratory (ANL) and the DOE Argonne Site Office Technical Standards Managers for review and approval by the DOE Argonne Site Office Manager. After resolution of comments and approval by the Manager, the PJS will be submitted to the DOE/HQ Technical Standards Program Manager (TSPM) for formal coordination. Following resolution of technical comments received during the PJS coordination process and receipt of a technical standards project number assigned by the TSPM, the Team will confirm the overall preparation schedule and develop an Internal Draft Technical Standard for coordination with the DOE Argonne Site Office. Following comment resolution, the Team will then prepare a Coordination Draft for submittal to the DOE Technical Standards RevCom review process and will respond to comments generated during this Complex-wide review. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Examples of X-Ray Characterization Techniques in Energy Storage Research

Lithium-ion batteries have revolutionized the portable electronics and transportation sectors. Their performance is often critically dependent on the crystal structures of the anode and cathode electrode materials, which must enable the transport and reversible storage of lithium ions into and out of the lattice. Because lithium is a low-Z element, characterization of materials for lithium-ion batteries can be particularly challenging. Regardless, X-ray techniques enable analysis of material structures to better understand how battery materials perform and degrade, particularly when combined with other materials characterization and electrochemical characterization techniques. While X-ray techniques are most often used in battery research for phase identification of crystal structures, X-ray characterization techniques are also used for a wide variety of other purposes. I will discuss several examples from my research with various collaborators on several projects that highlight the impact that X-ray characterization techniques can have on battery research. The first example will focus on low-temperature microwave-assisted solvothermal synthesis of vanadium-doped LiFePO4 cathode materials for lithium-ion batteries. (1,2) Through a combination of electrochemical and materials characterization, we determined that low temperature synthesis resulted in metastable phases that enabled incorporation of higher dopant levels than resulting from high-temperature synthesis of thermodynamically stable phases. Rietveld refinement of X-ray diffraction data enabled understanding of how lattice parameters changed with doping levels and synthesis temperature. X-ray absorption near edge spectroscopy enabled understanding of the vanadium and iron oxidation states to confirm how vacancies in the structure caused by doping were charge compensated. This was important to understand because the literature suggests doping can improve LiFePO4 electrical conductivity, which improves battery charge and discharge rates. The second example will focus on understanding residual strain in lithium metal anodes. Lithium-ion batteries typically use graphite anodes, but the charge-storage capacity can be theoretically improved ~10x by using lithium metal as the anode material instead. However, lithium anodes suffer from growth of high-aspect-ratio features, such as dendrites, that can pierce nanoporous polymer separators and lead to short circuits and fires. External pressure is commonly applied to cells to enable better morphological control. We hypothesized that applied pressure may promote strain and possibly work hardening during electrochemical cycling, which motivated us to look for evidence of residual strain in lithium metal cycled under applied pressure using X-ray diffraction and sin2(..psi..) analysis. We found that lithium electrodeposited under high pressure exhibited in-plane compressive strain and that that lithium electrodeposited under low pressure did not. (3) The residual strain that accompanies electrodeposition under high pressure may lead to work hardening, which may explain how a soft metal like lithium can puncture separators and why higher pressure does not always decrease short circuits. (4-6) References: 1) Harrison, K. L.; Manthiram, A. Microwave-Assisted Solvothermal Synthesis and Characterization of Metastable LiFe1- x (VO) x PO4 Cathodes. Inorganic chemistry 2011, 50(8), 3613-3620. 2) Harrison, K. L.; Bridges, C. A.; Paranthaman, M. P.; Segre, C. U.; Katsoudas, J.; Maroni, V. A.; Idrobo, J. C.; Goodenough, J. B.; Manthiram, A. Temperature Dependence of Aliovalent-Vanadium Doping in LiFePO4 Cathodes. Chemistry of Materials 2013, 25(5), 768-781. 3) Rodriguez, M. A.; Harrison, K. L.; Goriparti, S.; Griego, J. J.; Boyce, B. L.; Perdue, B. R. Use of a Be-Dome Holder for Texture and Strain Characterization of Li Metal Thin Films via Sin2 (..psi..) Methodology. Powder Diffraction 2020, 35(2), 89-97. 4) Jungjohann, K. L.; Gannon, R. N.; Goriparti, S.; Randolph, S. J.; Merrill, L. C.; Johnson, D. C.; Zavadil, K. R.; Harris, S. J.; Harrison, K. L. Cryogenic Laser Ablation Reveals Short-Circuit Mechanism in Lithium Metal Batteries. ACS Energy Letters 2021, 6(6), 2138-2144. 5) Harrison, K. L.; Merrill, L. C.; Long, D. M.; Randolph, S. J.; Goriparti, S.; Christian, J.; Warren, B.; Roberts, S. A.; Harris, S. J.; Perry, D. L. Cryogenic Electron Microscopy Reveals That Applied Pressure Promotes Short Circuits in Li Batteries. Iscience 2021, 24(12). 6) Harrison, K. L.; Goriparti, S.; Merrill, L. C.; Long, D. M.; Warren, B.; Roberts, S. A.; Perdue, B. R.; Casias, Z.; Cuillier, P.; Boyce, B. L. Effects of Applied Interfacial Pressure on Li-Metal Cycling Performance and Morphology in 4 M LiFSI in DME. ACS Applied Materials & Interfaces 2021, 13(27), 31668-31679.

batteries↗

PNNL's Characterization Summary for MP-2 Experiment

Characterization of as-fabricated fuel was performed at Pacific Northwest National Laboratory (PNNL) in accordance with the characterization plan for the fabrication of U 10Mo plate fuel for the U.S. High Performance Research Reactor conversion program’s Fuel Fabrication Pillar (INL 2021). Similar characterization work is also being performed at Idaho National Laboratory to provide a detailed understanding of the as-fabricated foils that would be irradiated in the Mini-Plate 2 (MP 2) experiment. Under the MP 2 characterization plan, foils are studied that have different fabrication parameters (such as rolling condition, rolling thickness reduction, co-rolling with Zr layers). Similar samples from master foils were sent to both the organizations, so that the testing and analysis can be done independently using similar equipment and standardized measurement and analysis procedures. A final, consolidated report will be prepared based on this work and will summarize all the information obtained from the two laboratories. The MP 2 experiment will provide an opportunity to understand the effects of processing conditions on the final fuel microstructure, to compare results obtained independently, and achieve a two-way validation. In Fiscal Year 2022, PNNL received five MP 2 cast (PD STD2) samples to examine the foils’ chemistry and microstructure. For each cast sample, PNNL received samples from three different locations. PNNL also received and characterized 24 U 10Mo foil samples, by sectioning four pieces/specimens from each foil, in accordance with the MP 2 Characterization Plan (INL 2021). These 24 samples consist of four types of foils from BWX Technologies: 0.047 in. thick hot-rolled and annealed samples with Zr layers; 0.025 in. thick cold-rolled and annealed samples with Zr layers; 0.0105 in. thick cold-rolled and annealed samples with Zr layers. Along with these, PNNL also received four plates with Zr layers that were 0.025 in. and 0.0105 in. thick. This report describes the results of PNNL’s MP 2 foil characterization. Microstructure, Mo homogeneity, carbide fraction and morphology, U 10Mo foil thickness, and Zr thickness were evaluated in both the longitudinal and transverse directions for all the foils of the three different thicknesses.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Prelaunch Spectral Characterization of the Operational Land Imager-2

The Landsat-9 satellite, launched in September 2021, carries the Operational Land Imager-2 (OLI-2) as one of its payloads. This instrument is a clone of the Landsat-8 OLI and its mission is to continue the operational land imaging of the Landsat program. The OLI-2 instrument is not significantly different from OLI though the instrument-level pre-launch spectral characterization process was much improved. The focal plane modules used on OLI-2 were manufactured as spares for OLI and much of the spectral characterization of the components was performed for OLI. However, while the spectral response of the fully assembled OLI was characterized by a double monochromator system, the OLI-2 spectral characterization made use of the Goddard Laser for Absolute Measurement of Radiance (GLAMR). GLAMR is a system of tunable lasers that cover 350–2500 nm which are fiber-coupled to a 30 in integrating sphere permanently monitored by NIST-traceable radiometers. GLAMR allowed the spectral characterization of every detector of the OLI-2 focal plane in nominal imaging conditions. The spectral performance of the OLI-2 was, in general, much better than requirements. The final relative spectral responses (RSRs) represent the best characterization any Landsat instrument spectral response. This paper will cover the results of the spectral characterization from the component-level to the instrument-level of the Landsat-9 OLI-2.

Landsat-9↗

Use of CFD in the Design of the 10- by 10-Foot Supersonic Wind Tunnel Characterization Array

At the 10- by 10-Foot Supersonic Wind Tunnel at the NASA Glenn Research Center, a future full test section characterization generated an ideal opportunity to design and build new characterization hardware to improve the understanding of the flow field, including flow quality, uniformity, and uncertainty in primary variables of interest. An array of flow sensing probes, referred to as the Characterization Array, was designed and built to replace 1960’s-era test section characterization hardware. Many references exist to guide wind tunnel characterization practitioners in the design of new hardware to properly measure various aspects of the flow within their wind tunnel facilities. Although reliable sources of information, these references tend to be over 30 years old and are not exhaustive. In scenarios where design decisions needed to be validated, computational simulations of the flow field around the characterization hardware were used. Decisions regarding probe location, probe spacing, and performance of various probes were justified using computational fluid dynamic simulations and rules-of-thumb from the legacy resources available in literature. This paper is intended to serve as an example of the benefits from integrating CFD into the design of wind tunnel hardware, particularly hardware for wind tunnel characterization.

CFD↗

Use of CFD in the Design of the 10- by 10-Foot Supersonic Wind Tunnel Characterization Array

At the 10- by 10-Foot Supersonic Wind Tunnel at the NASA Glenn Research Center, a future full test section characterization generated an ideal opportunity to design and build new characterization hardware to improve the understanding of the flow field, including flow quality, uniformity, and uncertainty in primary variables of interest. An array of flow sensing probes, referred to as the Characterization Array, was designed and built to replace 1960’s-era test section characterization hardware. Many references exist to guide wind tunnel characterization practitioners in the design of new hardware to properly measure various aspects of the flow within their wind tunnel facilities. Although reliable sources of information, these references tend to be over 30 years old and are not exhaustive. In scenarios where design decisions needed to be validated, computational simulations of the flow field around the characterization hardware were used. Decisions regarding probe location, probe spacing, and performance of various probes were justified using computational fluid dynamic simulations and rules-of-thumb from the legacy resources available in literature. This paper is intended to serve as an example of the benefits from integrating CFD into the design of wind tunnel hardware, particularly hardware for wind tunnel characterization.

CFD↗

Multi-Modal Characterization of Nuclear Fuels and Materials at the Idaho National Laboratory Materials & Fuels Complex

The Idaho National Laboratory (INL) leads cutting-edge research pertaining to the advancement of nuclear reactor technologies, including nuclear fuels and materials. The INL Irradiated Materials Characterization Laboratory (IMCL), Electron Microscopy Laboratory (EML), and future Sample Preparation Laboratory (SPL) are available to the nuclear research community to assess the behavior of nuclear fuels and materials, efficiently and comprehensively characterizing from the engineering to atomistic scale. The IMCL is a unique, 12,000-square-foot facility located at the INL Materials and Fuels Complex designed for analysis of irradiated materials. The facility operates advanced characterization instruments that are sensitive to vibration, temperature, and electromagnetic interference in modular radiological shielding and confinement systems, granting researchers the ability to assess the microstructural, chemical, mechanical and thermophysical properties of nuclear materials, especially irradiated fuels. The EML is dedicated to advanced characterization of materials with optical and electron microscopy tools, including scanning electron microscopy/focused-ion beam (SEM/FIB) and transmission electron microscopy (TEM). Upon construction, the SPL will be a 3 story, 49,000 sq. ft facility, that is the most modern reactor structural materials testing and analysis facility in the world, designed to investigate reactor structural materials in support of life-extension programs and development of advanced reactor concepts, including mechanical testing and advanced characterization capabilities. This presentation will showcase some of the main capabilities available at both IMCL, EML, and SPL, specifically illustrating how these characterization techniques are incorporated into multi-modal characterization work scopes to elucidate the degradation of nuclear structural materials and irradiated fuels.

36 MATERIALS SCIENCE↗

Using the JCC-71 neutron coincidence collar as a benchmark for detector characterization with PTR-32 list mode data acquisition

Augmenting or interchanging current international safeguards shift registerbased data acquisition systems with list mode data acquisition systems gives nondestructive assay (NDA) systems greater versatility. Neutron list mode data analysis offers comparable analytical results to the more widely used shift register analysis in nuclear material quantification applications and offers several diagnostic tools that are specifically beneficial to in-laboratory characterization and calibration measurements. These benefits include identification of non-ideal behavior, optimization of operational parameters from a single measurement, and an improved understanding of the physics-based behavior of NDA systems for a more precise system representation and more confident assay results. In this work the advantages of using list mode data acquisition for detector characterization are demonstrated experimentally. Two commercial-off-the-shelf International Atomic Energy Agency-supported technologies are used for a typical detector characterization procedure and their performance is compared. Specifically, a 3 He-based Canberra Industries JCC-71 Neutron Coincidence Collar is characterized using the Hungarian Institute of Isotopes’ Pulse Train Recorder-32 (PTR-32) list mode data acquisition system, and the results are compared to those obtained using the standard Canberra Industries JSR-15 model shift register. The quantitative results from the two systems are in agreement, which demonstrates that the PTR-32 is a technically viable alternative to conventional shift register electronics for this task. A suitable procedure for full instrument characterization is described, and the added benefits of list mode for characterization and data collection are discussed. Furthermore, this is an important step toward establishing a procedure for the routine use of list mode data acquisition and analysis for neutron NDA system characterization in safeguards field applications.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Benchmarking characterization methods for noisy quantum circuits

Effective methods for characterizing the noise in quantum computing devices are essential for programming and debugging circuit performance. Existing approaches vary in the information obtained as well as the amount of quantum and classical resources required, with more information generally requiring more resources. Here we benchmark the characterization methods of gate set tomography, Pauli channel noise reconstruction, and empirical direct characterization for developing models that describe noisy quantum circuit performance on a 27-qubit superconducting transmon device. We evaluate these models by comparing the accuracy of noisy circuit simulations with the corresponding experimental observations. Here, we find that the agreement of noise model to experiment does not correlate with the information gained by characterization and that the underlying circuit strongly influences the best choice of characterization approach. Empirical direct characterization scales best of the methods we tested and produced the most accurate characterizations across our benchmarks.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Multiscale Characterization of Photovoltaic Modules—Case Studies of Contact and Interconnect Degradation

The current popularity of photovoltaic (PV) systems is due in large part to their exceptional reliability and significantly lower cost than other energy sources. Studying cell and module degradation is key to promote further development in the state of the art. Fielded or accelerated aged modules exhibit different failure modes, of which metallization degradation (contacts and interconnections) is prevalent. In this work, we discuss how multiscale characterization methods can be applied to a variety of module technologies that have been field exposed and have undergone accelerated age testing. These methods include performing characterization on the module level, cell level, and finally the materials level. The observed performance losses from the module- and cell-level characterization can be correlated with materials properties to find out the root cause of degradation. We recommend an initial nondestructive characterization suite, including module- and cell-level current-voltage ( I--V ), Suns-V OC , photoluminescence and electroluminescence imaging, quantum efficiency, ultraviolet fluorescence imaging, and thermal infrared imaging. Samples are then extracted from particularly degraded regions of the module and prepared for materials characterization techniques, such as top-down and cross-sectional scanning electron microscopy, energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, secondary ion mass spectrometry, Raman spectroscopy, and transmission electron microscopy, allowing a deeper look into the mechanism behind the metallization degradation. This article serves as an instructional review to introduce the different multiscale characterization methods and how they can be effectively applied to perform PV degradation studies. Furthermore, we also share some of our examples and discuss the strengths, limitations, and best practices for each of the characterization techniques.

14 SOLAR ENERGY↗

Multiscale Characterization of the Caney Shale — An Emerging Play in Oklahoma

From a hydrocarbon perspective, the Caney Shale has historically been evaluated as a sealing unit, which resulted in limited studies characterizing the rock properties of the Caney Shale and its suitability for hydraulic fracturing. The objective of our research is to help bridge the current knowledge gap through the integration of multiscale laboratory techniques and to characterize the macro- and microscale rock properties of the Caney Shale. We employed an integrated approach for the characterization of the Caney using 200 ft (61 m) of Caney core from a target well in southern Oklahoma. Core observation and petrographic analysis of thin sections were combined to characterize the general rock types and associated fabrics and textures. Mineralogical composition, pore system architecture, and rock fabric were analyzed using x-ray diffraction (XRD), scanning electron microscopy/energy dispersive x-ray spectroscopy (SEM/EDS), and focused ion beam (FIB)-SEM. In addition, rebound hardness and indentation testing were carried out to determine rock hardness (brittleness) and elasticity, respectively. With the integrated multiscale characterization, three mixed carbonate-siliciclastic rock types were identified — mudstone, calcareous siltstone, and silty carbonate — likely representing a spectrum of deposition from low to relatively high energy environments in the distal portions of a ramp system. Silty carbonate contains mostly interparticle pores. The calcareous siltstones and silty mudstones contain a combination of organic matter pores and interparticle pores. Each of the rock types shows unique mineralogical compositions based on XRD. The mudstone lithofacies has the highest clay content and the least carbonate content. Calcareous siltstones show moderate carbonate and clay content. Silty carbonate indicates the highest carbonate content with the least clay content. In an order of mudstone, calcareous siltstone, and silty carbonate, rebound hardness and Young’s modulus show an increasing trend. As a result of rock-fluid interactions, there are potential scaling reactions during completion and production that could ultimately affect permeability and production rates. Overall, the proposed multiscale integration approach is critical for the geologic characterization of most rocks. However, in shale reservoirs dominated by microporosity and microstructure where engineered fractures are expected to provide permeability at a reservoir scale, successful integration is essential. An optimized, integrated geological characterization of the Caney Shale that is well aligned with the engineering designs in drilling, completing, and producing wellbores will ultimately lead to optimal production while providing safe and environmentally responsible operations.

Wang, Yulun↗