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PNNL's Intermediate Characterization Summary for the MP-1 Experiment

Characterization of the as-fabricated fuel is being performed at Pacific Northwest National Laboratory (PNNL) in accordance with Characterization Plan for the Fabrication of U-10Mo for the MP-1 Experiment, hereinafter the MP-1 Characterization Plan. Similar characterization work is also being performed at two other organizations, INL and Los Alamos National Laboratory, to provide a detailed understanding of the as-fabricated fuel that would be irradiated in the MP-1 experiment. Under the MP 1 Characterization Plan, fuel foils with different fabrication parameters (such as rolling condition, rolling thickness reduction, co-rolling with Zr layers) are being studied. Similar samples from master foils were sent to each of the three organizations, so that testing and analysis can be performed independently using similar equipment and a standardized set of measurement and analysis procedures. A final consolidated report will be prepared based on this work and it will summarize all of the information obtained from different labs. The MP-1 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 three-way validation. Currently, PNNL characterized 28 U-10Mo samples, by sectioning six pieces/specimens from each sample/foil, in accordance with the MP-1 Characterization Plan. These 28 samples consist of six types of MP-1 characterization foils from BWXT: 0.047 in. thick hot-rolled samples with and without Zr layers; 0.02 in. thick cold-rolled and annealed samples with and without Zr layers, and 0.01 in. thick cold-rolled and annealed samples with and without Zr layers. During the first year, PNNL completed sectioning of two subsamples per sample/foil and performed the necessary characterization on all 28 U-10Mo samples. This report covers the results of the first year’s analyses of PNNL’s MP-1 fuel characterization samples. 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↗

Measurement Sets and Sites Commonly Used for Characterization

Scientists at NASA's Earth Science Applications Directorate are creating a well-characterized Verification & Validation (V&V) site at the Stennis Space Center. This site enables the in-flight characterization of remote sensing systems and the data they acquire. The data are predominantly acquired by commercial, high spatial resolution satellite systems, such as IKONOS and QuickBird 2, and airborne systems. The smaller scale of these newer high resolution remote sensing systems allows scientists to characterize the geometric, spatial, and radiometric data properties using a single V&V site. The targets and techniques used to characterize data from these newer systems can differ significantly from the techniques used to characterize data from the earlier, coarser spatial resolution systems. Scientists are also using the SSC V&V site to characterize thermal infrared systems and active LIDAR systems. SSC employs geodetic targets, edge targets, radiometric tarps, and thermal calibration ponds to characterize remote sensing data products. This paper presents a proposed set of required measurements for visible through long-wave infrared remote sensing systems and a description of the Stennis characterization. Other topics discussed include: 1) The use of ancillary atmospheric and solar measurements taken at SSC that support various characterizations; 2) Additional sites used for radiometric, geometric, and spatial characterization in the continental United States; 3) The need for a standardized technique to be adopted by CEOS and other organizations.

Pagnutti, Mary↗

Radiological Characterization for Decommissioning: International Good Practice and Experience - 18396

The 'Task Group on Radiological Characterization for Decommissioning (TGRCD)' functions under the umbrella of the Nuclear Energy Agency' (NEA) 'Working Party on Decommissioning and Dismantling (WPDD),' which is currently reporting to NEA Radioactive Waste Management Committee (RWMC). The TGRCD task group, which is composed of international experts, has been working since 2014 on a commitment to provide a high-level guidance for characterization practitioners working in nuclear decommissioning. The work has focused on facility characterization from a waste and materials perspective. Radiological characterization is a key activity enabling planning and implementation of decommissioning of nuclear facilities. Effective characterization allows the extent, location and nature of contamination to be determined providing crucial information to facilitate facility dismantling, the management of material and arising waste, protection of workers, the public, the environment and associated cost estimation. The report is written for characterization practitioners who carry out the tactical planning, preparation, optimization and implementation of characterization to support the decommissioning of nuclear facilities and the management of associated materials and waste. It compiles recent experience of NEA member countries in radiological characterization, including the experience of international experts and practitioners; the learning from international case studies and international conferences; and national approaches to the application of international and national regulations, standards and guidance documents. Using this comprehensive approach and evaluation studies, the report identifies relevant good practices and sets out set out practical guidance covering all stages of the characterization process as related to decommissioning. This paper provides a summary of the work conducted and the main findings from the detailed report. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Measurement Sets and Sites Commonly used for Characterizations

Scientists with NASA's Earth Science Applications Directorate are creating a well-characterized Verification & Validation (V&V) site at the Stennis Space Center (SSC). This site enables the in-flight characterization of remote sensing systems and the data that they require. The data are predominantly acquired by commercial, high-spatial resolution satellite systems, such as IKONOS and QuickBird 2, and airborne systems. The smaller scale of these newer high-resolution remote sensing systems allows scientists to characterize the geometric, spatial, and radiometric data properties using a single V&V site. The targets and techniques used to characterize data from these newer systems can differ significantly from the earlier, coarser spatial resolution systems. Scientists are also using the SSC V&V site to characterize thermal infrared systems and active Light Detection and Ranging (LIDAR) systems. SSC employs geodetic targets, edge targets, radiometric tarps, and thermal calibration ponds to characterize remote sensing data products. This paper presents a proposed set of required measurements for visible-through-longwave infrared remote sensing systems, and a description of the Stennis characterization. Other topics discussed inslude: 1) use of ancillary atmospheric and solar measurements taken at SSC that support various characterizations, 2) other sites used for radiometric, geometric, and spatial characterization in the continental United States,a nd 3) the need for a standardized technique to be adopted by the Committee on Earth Observation Satellites (CEOS) and other organizations.

Pagnutti, Mary↗

Radioactive Waste Characterization Strategies; Comparisons Between AK/PK, Dose to Curie Modeling, Gamma Spectroscopy, and Laboratory Analysis Methods- 12194

In the coming fiscal years of potentially declining budgets, Department of Energy facilities such as the Los Alamos National Laboratory (LANL) will be looking to reduce the cost of radioactive waste characterization, management, and disposal processes. At the core of this cost reduction process will be choosing the most cost effective, efficient, and accurate methods of radioactive waste characterization. Central to every radioactive waste management program is an effective and accurate waste characterization program. Choosing between methods can determine what is classified as low level radioactive waste (LLRW), transuranic waste (TRU), waste that can be disposed of under an Authorized Release Limit (ARL), industrial waste, and waste that can be disposed of in municipal landfills. The cost benefits of an accurate radioactive waste characterization program cannot be overstated. In addition, inaccurate radioactive waste characterization of radioactive waste can result in the incorrect classification of radioactive waste leading to higher disposal costs, Department of Transportation (DOT) violations, Notice of Violations (NOVs) from Federal and State regulatory agencies, waste rejection from disposal facilities, loss of operational capabilities, and loss of disposal options. Any one of these events could result in the program that mischaracterized the waste losing its ability to perform it primary operational mission. Generators that produce radioactive waste have four characterization strategies at their disposal: - Acceptable Knowledge/Process Knowledge (AK/PK); - Indirect characterization using a software application or other dose to curie methodologies; - Non-Destructive Analysis (NDA) tools such as gamma spectroscopy; - Direct sampling (e.g. grab samples or Surface Contaminated Object smears) and laboratory analytical; Each method has specific advantages and disadvantages. This paper will evaluate each method detailing those advantages and disadvantages including; - Cost benefit analysis (basic materials costs, overall program operations costs, man-hours per sample analyzed, etc.); - Radiation Exposure As Low As Reasonably Achievable (ALARA) program considerations; - Industrial Health and Safety risks; - Overall Analytical Confidence Level. The concepts in this paper apply to any organization with significant radioactive waste characterization and management activities working to within budget constraints and seeking to optimize their waste characterization strategies while reducing analytical costs. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

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)↗

Reservoir Characterization of Bridgeport and Cypress Sandstones in Lawrence Field Illinois to Improve Petroleum Recovery by Alkaline-Surfactant-Polymer Flood

Within the Illinois Basin, most of the oilfields are mature and have been extensively waterflooded with water cuts that range up to 99% in many of the larger fields. In order to maximize production of significant remaining mobile oil from these fields, new recovery techniques need to be researched and applied. The purpose of this project was to conduct reservoir characterization studies supporting Alkaline-Surfactant-Polymer Floods in two distinct sandstone reservoirs in Lawrence Field, Lawrence County, Illinois. A project using alkaline-surfactantpolymer (ASP) has been established in the century old Lawrence Field in southeastern Illinois where original oil in place (OOIP) is estimated at over a billion barrels and 400 million barrels have been recovered leaving more than 600 million barrels as an EOR target. Radial core flood analysis using core from the field demonstrated recoveries greater than 20% of OOIP. While the lab results are likely optimistic to actual field performance, the ASP tests indicate that substantial reserves could be recovered even if the field results are 5 to 10% of OOIP. Reservoir characterization is a key factor in the success of any EOR application. Reservoirs within the Illinois Basin are frequently characterized as being highly compartmentalized resulting in multiple flow unit configurations. The research conducted on Lawrence Field focused on characteristics that define reservoir compartmentalization in order to delineate preferred target areas so that the chemical flood can be designed and implemented for the greatest recovery potential. Along with traditional facies mapping, core analyses and petrographic analyses, conceptual geological models were constructed and used to develop 3D geocellular models, a valuable tool for visualizing reservoir architecture and also a prerequisite for reservoir simulation modeling. Cores were described and potential permeability barriers were correlated using geophysical logs. Petrographic analyses were used to better understand porosity and permeability trends in the region and to characterize barriers and define flow units. Diagenetic alterations that impact porosity and permeability include development of quartz overgrowths, sutured quartz grains, dissolution of feldspar grains, formation of clay mineral coatings on grains, and calcite cementation. Many of these alterations are controlled by facies. Mapping efforts identified distinct flow units in the northern part of the field showing that the Pennsylvanian Bridgeport consists of a series of thick incised channel fill sequences. The sandstones are about 75-150 feet thick and typically consist of medium grained and poorly sorted fluvial to distributary channel fill deposits at the base. The sandstones become indistinctly bedded distributary channel deposits in the main part of the reservoir before fining upwards and becoming more tidally influenced near their top. These channel deposits have core permeabilities ranging from 20 md to well over 1000 md. The tidally influenced deposits are more compartmentalized compared to the thicker and more continuous basal fluvial deposits. Fine grained sandstones that are laterally equivalent to the thicker channel type deposits have permeabilities rarely reaching above 250 md. Most of the unrecovered oil in Lawrence Field is contained in Pennsylvanian Age Bridgeport sandstones and Mississippian Age Cypress sandstones. These reservoirs are highly complex and compartmentalized. Detailed reservoir characterization including the development of 3-D geologic and geocellular models of target areas in the field were completed to identify areas with the best potential to recover remaining reserves including unswept and by-passed oil. This project consisted of tasks designed to compile, interpret, and analyze the data required to conduct reservoir characterization for the Bridgeport and Cypress sandstones in pilot areas in anticipation of expanded implementation of ASP flooding in Lawrence Field. Geologic and geocellular modeling needed for reservoir characterization and reservoir simulation were completed as prerequisites for design of efficient ASP flood patterns. Characterizing the complex reservoir geology that identifies the geologic conditions that will optimize oil recoveries for expansion of the ASP pilots in the Bridgeport and Cypress sandstones to other areas of Lawrence Field is the primary objective of this project. It will permit evaluation of efficiency of oil recovery from Bridgeport and Cypress sandstone reservoirs using ASP technology. Additionally evaluation of similar Pennsylvanian and Chesterian reservoirs shows that it is likely that ASP flood technology can be successfully applied to similar reservoirs in the Illinois Basin as well as to other U.S. reservoirs. Chemical flooding was introduced in stages with the first flood initiated in 2010 and a second offset pilot project initiated during 2011. Rex Energy Corporation is reporting a positive response on its ASP Middagh pilot project in the Pennsylvanian Bridgeport B reservoir, Lawrence Field. Oil response in the 15 acre flood has continued to show an increase in oil cut from 1% to 12%. Total pattern production increased from 16 BOPD and stabilized at a range of 65-75 BOPD in the last three months of 2011. Peak production rose to 100 + BOPD. Oil cut in the pilot increased for 1.0% to ~ 12.0% with an individual well showing oil cuts greater than 20%. A second, 58 acre pilot (Perkins-Smith) adjacent to and likely in communication with the Middagh pilot has been initiated. Preliminary brine injection has been implemented and ASP injection was initiated in mid-2012. Response is expected by mid-2013 with peak recovery expected by late 2013. Rex Energy is projecting full scale expansion with the next step of development being a 351 acre project scheduled to begin in mid-2013. Preliminary development has been initiated in this Delta Unit area located in the south half of section 32, T4N, R12W.

02 PETROLEUM↗

Gulf of Mexico miocene CO₂ site characterization mega transect

This project characterized the Miocene-age sub-seafloor stratigraphy in the near-offshore portion of the Gulf of Mexico adjacent to the Texas coast. The large number of industrial sources of carbon dioxide (CO₂) in coastal counties and the high density of onshore urbanization and environmentally sensitive areas make this offshore region extremely attractive for long-term storage of carbon dioxide emissions from industrial sources (CCS). The study leverages dense existing geologic data from decades of hydrocarbon exploration in and around the study area to characterize the regional geology for suitability and storage capacity. Primary products of the study include: regional static storage capacity estimates, sequestration “leads” and prospects with associated dynamic capacity estimates, experimental studies of CO₂-brine-rock interaction, best practices for site characterization, a large-format ‘Atlas’ of sequestration for the study area, and characterization of potential fluid migration pathways for reducing storage risks utilizing novel high-resolution 3D (HR3D) seismic surveys. In addition, three subcontracted studies address source-to-sink matching optimization, offshore well bore management and environmental aspects. The various geologic data and interpretations are integrated and summarized in a series of cross-sections and maps, which represent a primary resource for any near-term commercial deployment of CCS in the area. The regional study characterized and mapped important geologic features (e.g., Clemente-Tomas fault zone, the regionally extensive Marginulina A and Amphistegina B confining systems, etc.) that provided an important context for regional static capacity estimates and specific sequestration prospects of the study. A static capacity estimate of the majority of the Study area (14,467 mi 2 ) was estimated at 86 metric Gigatonnes. While local capacity estimates are likely to be lower due to reservoir-scale characteristics, the offshore Miocene interval is a storage resource of National interest for providing CO₂ storage as an atmospheric emissions abatement strategy. The natural petroleum system was used as an analog to infer seal quality and predict possible migration pathways of fluids in an engineered system of anthropogenic CO₂ injection and storage. The regional structural features (e.g., Clemente-Tomas fault zone) that exert primary control on the trapping and distribution of Miocene hydrocarbons are expected to perform similarly for CCS. Industrial-scale CCS will require storage capacity utilizing well-documented Miocene hydrocarbon (dominantly depleted gas) fields and their larger structural closures, as well as barren (unproductive, brine-filled) closures. No assessment was made of potential for CO₂ utilization for enhanced oil and gas recovery. The use of 3D numerical fluid flow simulations have been used in the study to greatly assist in characterizing the potential storage capacity of a specific reservoir. Due to the complexity of geologic systems (stratigraphic heterogeneity) and inherent limitations on producing a 3D geologic model, these simulations are typically simplified scenarios that explore the influence of model property variability (sensitivity study). A specific site offshore San Luis Pass (southern Galveston Island) was undertaken successfully, indicating stacked storage potential. Downscaling regional capacity estimates to the local scale (and the inverse) has proven challenging, and remains an outstanding gap in capacity assessments. In order to characterize regional seal performance and identify potential brine and CO₂ leakage pathways, results from three high-resolution 3D (HR3D) seismic datasets acquired by the study using novel HR3D (P-Cable) acquisition system showed steady and significant improvements in data quality because of improved acquisition and processing technique. Finely detailed faults and stratigraphy in the shallowest 1000 milliseconds (~800 m) of data allowed for the identification and mapping of unconformable surfaces including what is probably a surface associated with the last Pleistocene glacial lowstand. The identification of a previously unrecognized (in commercial seismic data) gas chimney that was clearly defined in the 2013 HR3D survey, indicates that HR3D surveys may be useful as both a characterization tool for the overburden of a potential carbon sequestration site and as an additional monitoring tool for future engineered injection sites. Geochemical modeling indicated that injection of CO₂ would result in minor dissolution of calcite, K-feldspar and albite. In addition, modeling of typical brines in Miocene age rocks indicate that approximately 5% of injection capacity would result from CO₂ dissolution into the brine. After extensive searches, no rock samples of the Marginulina A and Amphistegina B seals (“caprocks”) were obtained, but analyses of available core samples of other Miocene age mudrocks (seals or caprocks) indicate that they have sealing ability sufficient for potential CO 2 storage in underlying sandstone units.

01 COAL, LIGNITE, AND PEAT↗

Improved Characterization and Modeling of Tight Oil Formations for CO 2 Enhanced Oil Recovery Potential and Storage Capacity Estimation

Tight oil formations such as those in the Bakken petroleum system are known to hold hundreds of billions of barrels of oil in place; however, the primary recovery factor for these plays is typically less than 10%. Tight oil formations, including the Bakken Formation, therefore, may be attractive candidates for enhanced oil recovery (EOR) using CO 2 . Multiphase fluid behavior and flow in fluid-rich shales can vary substantially depending on the size of pore throats, and properties such as fluid viscosity and density are much different in nanoscale pores than in macroscale pores. Thus it is critical to understand the nature and distribution of nano-, micro-, and macroscale pores and fracture networks. To address these issues, the Energy & Environmental Research Center (EERC) has been conducting a research program entitled “Improved Characterization and Modeling of Tight Oil Formations for CO 2 Enhanced Oil Recovery Potential and Storage Capacity Estimation.” The objectives of the project are 1) the use of advanced characterization methods to better understand and quantify the petrophysical and geomechanical factors that control CO 2 and oil mobility within tight oil formation samples, 2) the determination of CO 2 permeation and oil extraction rates in tight reservoir rocks and organic-rich shales of the Bakken, and 3) the integration of the laboratory-based CO 2 permeation and oil extraction data and the characterization data into geologic models and dynamic simulations to develop predictions of CO 2 storage resource and EOR in the Bakken tight oil formation. A combination of standard and advanced petrophysical characterization techniques were applied to characterize samples of Bakken Formation tight reservoir rock and shales from multiple wells. Techniques included advanced computer tomography (CT) imaging, scanning electron microscopy (SEM) techniques, whole-core and micro x-ray CT imaging, field emission (FE) SEM, and focused ion beam (FIB) SEM. Selected samples were also analyzed for geomechanical properties. X-ray CT imaging yielded information on the occurrence of fractures, bedding planes, fossils, and bioturbation in core, as well as data on bulk density and photoelectric factor logs, which were used to interpret porosity, organic content, and mineralogy. FESEM was used for characterization of nano- and microscale features, including nanoscale pore visualization and micropore and pore throat mineralogy. FIBSEM yielded micro- to nanoscale visualization of fracture networks, porosity and pore-size distribution, connected versus isolated porosity, and distribution of organics. Results from the characterization activities provide insight on nanoscale fracture properties, pore throat mineralogy and connectivity, rock matrix characteristics, mineralogy, and organic content. Laboratory experiments demonstrated that CO 2 can permeate the tight matrix of Bakken shale and nonshale reservoir samples and mobilize oil from those samples. Geologic models were created at scales ranging from the core plug to the reservoir, and dynamic simulations were conducted. The data from the characterization and laboratory-based activities were integrated into modeling research activities to determine the fundamental mechanisms controlling fluid transport in the Bakken, which support EOR scheme design and estimation of CO 2 storage potential in tight oil formations. Simulation results suggest a CO 2 storage resource estimate range of 169 million to 1.5 billion tonnes for the Bakken in North Dakota, possibly resulting in 1.8 billion to 16 billion barrels of incremental oil.

04 OIL SHALES AND TAR SANDS↗

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↗

Lessons Learned from the Application of Bulk Characterization to Individual Containers on the Brookhaven Graphite Research Reactor Decommissioning Project at Brookhaven National Laboratory - 12056

When conducting environmental cleanup or decommissioning projects, characterization of the material to be removed is often performed when the material is in-situ. The actual demolition or excavation and removal of the material can result in individual containers that vary significantly from the original bulk characterization profile. This variance, if not detected, can result in individual containers exceeding Department of Transportation regulations or waste disposal site acceptance criteria. Bulk waste characterization processes were performed to initially characterize the Brookhaven Graphite Research Reactor (BGRR) graphite pile and this information was utilized to characterize all of the containers of graphite. When the last waste container was generated containing graphite dust from the bottom of the pile, but no solid graphite blocks, the material contents were significantly different in composition from the bulk waste characterization. This error resulted in exceedance of the disposal site waste acceptance criteria. Brookhaven Science Associates initiated an in-depth investigation to identify the root causes of this failure and to develop appropriate corrective actions. The lessons learned at BNL have applicability to other cleanup and demolition projects which characterize their wastes in bulk or in-situ and then extend that characterization to individual containers. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

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)

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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)

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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.

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