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Defect Characterization of Monocrystalline Silicon Solar Cells with Polysilicon Passivated Contact Using Electrically-Detected Magnetic Resonance (EDMR) Spectroscopy

As the c-Si based solar cell efficiencies are approaching over 26%, it is becoming critical to characterize the low concentrations of the defects – as low as 10^10-10^11 cm-3 (for e.g., iron contamination in high-lifetime Ga-doped wafers3 and n-type wafers), and further reduce them. Also, atomistic level understanding of the mechanisms of the low concentration process-induced-defects and reliability limiting defects (such as light and elevated temperature induced degradation, surface passivation degradation) is needed to design the mitigation strategies. The conventional characterization techniques are limited due to their detection limitations. Some of the techniques based on lifetime spectroscopies can still be used for low concentration characterization however, they are based on estimations and theoretical models and hence, indirect and cannot fully reveal information about the microscopic mechanism of the defects. Thus, we present the application of an ultrasensitive magnetic resonance-based technique for the direct spectroscopic detection of the defects in Si PV - electrically detected magnetic resonance (EDMR). In this work, we aim to focus on establishing a process flow for fabrication of minicells with (miniature replica of the larger-area cells) and setting up the routine for EDMR measurements on them with the EDMR instrumentation capability at NREL. For the EDMR measurements, sample size is limited by the dimensions of sample holder tube (width less than 3.2 mm, active area - 20 mm). Thus, we have designed c-Si based minicells with polysilicon (poly-Si) passivated contacts same as the larger-area cells that we fabricate in our group at NREL. We also modified our minicell process flow for fabricating the textured minicells for preserving the texture during processing and taking care of the laser-ablation edge damage which can significantly affect the performance of such small devices. We have achieved comparable performance on these newly fabricated minicells as that of our 4 cm2 devices with same structure (comparable VOC, JSC, FF). We also conducted EDMR measurements on the minicells and observed a distinct EDMR signal at g-value ~2.005 at temperatures 30K and above, as shown in Fig. 2. We associate this signal to the presence of silicon dangling bonds based on the g-value. We also observed an EDMR signal at g-value ~1.998 at temperature ~5K. The origin of this signal is still being investigated. Thus, we show the proof of concept of minicells and EDMR measurements with which we now aim to study some of the unknown defects in silicon solar cell devices.

EDMR↗

Ultrasonic characterization of Ti-5Al-5Mo-5V-3Cr

Metastable β titanium alloys such as Ti-5Al-5Mo-5V-3Cr are of increasing interest due to their excellent corrosion resistance, high strength, and in particular, the ability to manipulate microstructure to a high degree to control the mechanical properties of the material. It is therefore important to consider how this manipulation of mechanical properties will affect the inspection of this material with ultrasonic testing both for the purposes of flaw detection and material characterization. The connection between material properties and ultrasonic characterization techniques will be discussed and then dissected in the context of Ti-5553. This metastable alloy was shown to exhibit remarkable variation in microstructure as well as ultrasonic velocity and attenuation demonstrating these techniques as potential candidates for characterizing Ti-5553 and Ti-5553 as a good candidate for aiding in future studies aimed at learning more about the role of secondary phases in ultrasonic wave propagation.

Sunderman, Ruth↗

Origin and characterization of single-electron events in Skipper-CCDs for light dark matter searches

This manuscript summarizes the work carried out within the SENSEI (Sub-Electron-Noise Skipper-CCD Experimental Instrument) collaboration, an effort focused on the search for light dark matter using Skipper-CCDs. Firstly, it presents the data acquisition and processing protocol developed to establish a selection criteria for events compatible with the dark matter signal. This protocol also enabled the structure and tools used for the study and characterization of phenomena that impact the quality of measurements made in the search for dark matter (measurement of the Fano factor, determination of the Compton background, and characterization of the high-energy surface background), which were carried out during this work. Secondly, it discusses the comprehensive study conducted on the origin of single-electron events in Skipper-CCDs, which allowed for the selection of detector operating parameters and improved the detection sensitivity in the search for dark matter. It is highlighted the characterization of the spatial correlation between single-electron events and high-energy events, among other developed event selection criteria, and the optimization of the output device to reduce sources of luminescence during its operation. As a result of this study, the lowest levels of dark current and spurious charge ever measured in a CCD are reported. Finally, the latest published results from SENSEI are presented. The obtained limits for the scattering of a light mediator are the best reported to date across the entire investigated mass range, while for the heavy mediator, they are the best for masses below 10 MeV. In terms of dark matter absorption, the most restringent limits below 10 eV are reported. These results, achieved with only a very small fraction of the total projected exposure for SENSEI, position Skipper-CCDs as leaders in the search for light dark matter worldwide.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Environmental Characterization Scans Using Sodium-Iodide Gamma Spectroscopy to Determine Ra-226 Concentration in Surface Soil - 16326

The recent natural gas drilling boom has brought heightened attention to the issue of TENORM waste management. Radioactive residues from the extraction, treatment, and purification of materials containing uranium and thorium, or their progeny, pose a public health hazard primarily in the form of ground water contamination. Hydraulic fracturing can liberate formation waters from shale; the high salinity of which can cause radium to move with the water to the surface. The disposal and handling of this water has been a subject of public controversy. For soil remediation projects, radium-226 is generally one of the radionuclides of concern due to its alpha emissions. However performing a survey scan for Ra-226 is difficult because its photon emissions are low energy and have minimal probability of emission per decay (186.2 keV, 3.3% abundance). Additionally resolving its emission from U-235 (185.7 keV, 57% abundance) with field instrumentation is not feasible. Therefore detection of Ra-226 relies on the presence and photon emissions of its progeny. This paper outlines methodology for calculating the minimum detectable concentration of Ra-226 in characterization scans using a sodium-iodide detector array coupled with a multi-channel analyzer. Using progeny ingrowth as a detection proxy requires knowing decay time in order to determine progeny emission rates. Knowledge of site history, process, and prior survey results can be key in determining an accurate decay time. However in the absence of such information in-situ measurements can be used to estimate decay time by comparing observed progeny emission ratios against established values. These values are determined using Oak Ridge National Laboratory's ORIGEN-ARP program to generate photon energy spectra for Ra-226 and its progeny at specified time intervals. Once decay time is established, the detector's minimum detectable concentration can be calculated by synthesizing the expected emission spectra and Los Alamos National Laboratory's Monte Carlo N-Particle transport code to simulate detector response. Traditionally, one of the steps in calculating a system's minimum detectable concentration is to place an appropriate button source under the detector, record the response, and then move the source by a specified increment. This process is repeated until the detector's spatial efficiency has been mapped. Due to the impracticality of performing this with Ra-226 button sources of varying decay times, Monte Carlo N-Particle transport code was utilized to determine the detector's spatial efficiency. A dime sized source with the established emission spectra was placed into the center of a rectangle of soil. This rectangle, including the source, was used as a lattice element to fill the region of space below the detector. The simulation was designed to track the energy distribution of pulses created in the sodium iodide crystal using the F8 tally, and was setup to isolate each source; thereby correlating detector response to source position. The simulation output required post-processing to determine conversion factors from counts per second to disintegrations per second. Post-processing accounted for subtraction of the Compton continuum, and average the data over the scanning pattern to obtain the expected spatial sensitivity during a characterization study. This was performed for the following photo-peaks: 609 keV (Bi-214), and 1764 keV (Bi-214). For calculation of the scan minimum detectable concentration, the surveyor efficiency coefficient from NUREG 1507 was supplanted in favor of a scan speed deviation factor. This was used because the detector utilizes computerized data collection (spatial and spectral). This report finds that, for two shielded 10.16 cm x 10.16 cm x 40.64 cm sodium-iodide crystals with integrated multi-channel analyzers, the minimum detectable concentration in surface soils is less than 1 pCi per gram Ra-226 for a 1 second survey measurement. These results assume a volumetric source with a maximum depth of 15.24 cm and a minimum decay time of 21 days. Verification of the system's capabilities was performed by sending soil samples from scanned areas, and locations where in-situ measurements were performed, to an independent laboratory for analysis. The laboratory results demonstrated that scanned area was principally comprised of soil containing less than 1 pCi per gram Ra-226. This borders the system MDC and it underestimated the concentration of radium in the soil. The probable causes of this is escape of radon gas from the surface soil. Radon is the daughter of radium, and has a high mobility in soil. If the gas escapes, then the progeny used as the detection proxy will be present in lower than expected concentrations. Radionuclide identification using high volume sodium-iodide crystals in low level characterization scans is demonstrated to be possible. Further system refinement will focus on developing a methodology to estimate a radon escape factor for site specific use. Accounting for radon escape in the top 15.24 cm of soil will allow the system to better estimate Ra-226 concentrations in soil. This is a significant advancement over the gross counting statistics used in most studies to satisfy MARSSIM survey requirements, because it will increase stakeholder confidence. (authors)

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Characterization and Clearance of m/s Sigyn - 16412

M/s Sigyn was a 2044 ton ship that transported contaminated material between 1982 and 2013. Most of the transports were with spent nuclear fuel between Swedish nuclear power plants and the Swedish fuel repository, Clab. In addition to spent fuel, m/s Sigyn also transported big contaminated components, from nuclear power plants in Europe, to Studsvik for analysis or decontamination and melting. She also transported components from Swedish nuclear power plants to final disposal of short lived waste, SFR. Even though all transported items have been cleaned, checked and wrapped with plastics, some activity ended up as contamination onboard. In December 2013 it was decided that m/s Sigyn was subject for decommissioning due to her age. This Paper describes the method in which the activity onboard m/s Sigyn was characterized and clearance levels were calculated. This method for radiological characterization and clearance has recently been developed in Sweden, the method is efficient in that it does not need a big pre characterization survey. Only the nuclide distribution and history of the object, is needed to start the final survey. In the future there will be further development of the method, making it possible to reduce the number of measurements even more. This will further optimize the method and reduce the cost for final surveys and clearance. (authors)

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Characterization of U(VI)-Bearing Precipitates Produced by Ammonia Gas Injection Technology for Unsaturated Sediments - 16600

The processing of irradiated fuel to extract plutonium for the nuclear arsenal has resulted in a legacy of uranium contamination in the vadose zone (VZ) of the Hanford 200 Area. This contamination is a potential source for groundwater contamination, posing a risk to receptors through water uptake from contaminated wells or discharges to surface water. The injection of reactive gases is an innovative technology being evaluated for reducing the mobility of radionuclide contaminants in the Hanford vadose zone. Ammonia (NH{sub 3}) gas in particular has been used to reduce uranium mobility in laboratory scale studies and is being evaluated for field scale application. The sediment of the Hanford vadose zone is composed of a complex of mineral phases including quartz, feldspar, mica, and calcium carbonates. The silica content in the 200 Area subsurface markedly outweighs the majority of elements, with aluminum following closely. The injection of ammonia gas into the vadose zone is associated with an increase in pH conditions as the gas partitions into the pore water. The resulting alkaline conditions significantly increase the solubility of some aluminum and silicate-containing minerals within the system. As pH decreases to natural conditions, the aluminosilicate minerals will precipitate, potentially coating and sequestering the uranium contaminants. Although previous laboratory scale tests have shown decreased uranium mobility, there are many questions regarding the application of the remediation method to 200 Area vadose zone conditions. In particular, additional testing is required to understand the impact of various environmental factors on the formation of uranium mineral phases with the application of the NH{sub 3} injection method. In order to answer some of the unknowns regarding this remediation technology for the 200 Area vadose zone, an effort was made to characterize the uranium-bearing precipitates being formed with the injection of ammonia gas. Rather than a sediment-water system, a synthetic pore water solution was prepared using the ion concentrations relevant to the 200 Area vadose zone. These solutions were limited to select constituents believed to play a major role in the remediation process. The use of this carefully composed solution allows for the thorough evaluation of the contribution the variable components make to the formation of the solid analyte. The characterization of solid samples was attempted using a host of complementary analytical techniques including scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS) and X-ray diffraction (XRD). Though characterization of the samples is ongoing, the data produced thus far has allowed for the imaging and X-ray spectroscopy of the solid uranium phases produced as well as a tentative identification of cejkaite (Na{sub 4}(UO{sub 2})(CO{sub 3}){sub 3}) as the major uranium mineral phase. (authors)

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Characterizing Natural Attenuation of Cr(VI) in a Chromium Plume at Los Alamos National Laboratory - 18594

Characterization of natural attenuation of hexavalent (Cr(VI)) on aquifer sediments within the Cr plume at Los Alamos National Laboratory has been conducted to (1) refine conceptual and numerical models of chromium fate and transport, (2) evaluate the long-term stability of Cr(III)/Cr(VI) in the complex groundwater system along flow paths from the source to the regional aquifer, and (3) evaluate and develop options for successful remediation. The naturally high chromium abundance in aquifer sediments at Los Alamos pose an unique challenge for characterization of chromium reduction, making conventional approaches such as uptake tests and advanced spectroscopic measurements ineffective in identifying relatively small amounts of anthropogenic Cr(VI) in the sediments. To address this challenge and as complimentary to these conventional methods, sequential leaching tests were conducted on core hole sediments obtained from sonic drilled cores taken from both contaminated and non-contaminated horizons among two mineralogically distinct formations (Puye formation and Miocene Pumiceous Unit) within the Cr plume. A series of three and coherent sequential leaching steps were conducted: 1) an alkaline leach to determine the amount of Cr(VI) sorbed on the sediments. 2) a weak acid leach (using 0.01 M and 0.1 M HNO{sub 3}) to determine the amount of anthropogenic chromium (Cr(III) and Cr(VI)) on aquifer sediment surfaces, and 3) a strong acid leach (using 2 M HNO{sub 3}) to characterize the amount of releasable Cr(III) from aquifer minerals. Additionally we tested the efficiency and detection limit of sequential leaching on bentonite, which consists mainly of smectite, used in drill muds and laboratory-grade biotite spiked with known concentrations of Cr(VI). Smectite and biotite are two phases considered to be potentially important host minerals in aquifer sediments within the plume. Thus, by comparing contaminated and uncontaminated sediment leachate results of chromium and other major and trace elements, the signature and quantity of anthropogenic Cr(VI) can be derived. Our results from the weak acid leaching test indicate that the method detection limit for Cr 'uptake' was about 1 μg/g for biotite and about 0.5 μg/g for bentonite. Our results also indicate that all samples taken from known contaminated horizons in comparison to non-contaminated ones within the Puye formation showed no statistical difference in the amount of Cr leached indicative of its insignificant Cr(VI) attenuation capacity. The amount of excess Cr leached from the magnetic fraction of the contaminated Miocene Pumiceous samples was about 2 μg/g of sediment. Considering that the magnetic fraction was about 11% by mass of the bulk sample, the excess amount of Cr leached from the bulk material would be about 0.2 μg/g of sediment, suggesting the potential for some Cr(VI) attenuation capacity in the Miocene pumice unit. (authors)

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TEM Characterization of U-Mo Irradiated with High-Energy Xe Ions

U-Mo alloys (with 7-10 wt.% Mo) with a low U-235 enrichment (< 20%) have been developed to be used in high-performance research and test reactors, replacing the current highly enriched uranium (HEU) fuels. A number of in-pile irradiation tests of U-Mo fuels show that drastic microstructural changes occurred during reactor irradiation, including the formation of U-Mo-Al interaction products and large gas-filled pores. These microstructural changes might lead to breakaway swelling and deterioration of plate mechanical integrity. Hence, it is critical to understand the underlying mechanisms of these microstructural changes in order to improve the irradiation behavior of UMo fuels. Heavy ion irradiation was employed in this study to investigate separate effects of the irradiation behavior of U-Mo fuels. 1.7 mm diameter disks punched out from UMo/ Al dispersion fuel mini-plates were irradiated with 84 MeV Xe ions at the ATLAS accelerator at Argonne National Laboratory (ANL). This particular ion source was selected for two reasons: (1) to simulate the irradiation response of the fuel to fission fragment bombardments, and (2) to study fission gas behavior, as fission gas bubble formation and growth is the primary cause of U-Mo fuel swelling. The ion-irradiated samples have been characterized with scanning electron microscopy (SEM). This study focuses on the characterization of the samples using transmission electron microscopy (TEM). With the high magnification details, microstructures in U-Mo along the ion penetration depth were revealed. The U-7Mo/Al dispersion fuel sample irradiated with 84 MeV Xe ions to a dose of 2.9 x 10{sup 17} ions/cm{sup 3} was characterized using TEM. The TEM results exhibit that the sample microstructure varies along the ion penetration depth. Near the sample surface (zone A) is a layer of nano-crystalline U-Mo-Al interdiffusion product. After passing through zone A, the Xe ions resided in zone B, where gas bubbles formed in U-Mo. TEM images of this region displayed that large gas bubbles formed on grain boundaries and high-density nano-bubbles lay inside grains. The random distribution of intragranular bubbles indicates that the irradiation conditions of this sample cannot lead to gas bubble superlattice formation. Outside of the Xe penetration depth (zone C), significant amount of α-uranium precipitates were identified. The fact that no α-uranium precipitates were found in zone B suggests that the dose rate in this irradiation is sufficient to facilitate a phase reversal by means of a displacement spike mechanism. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Radiochemical Characterization of PWR Control Rods - 19030

NRG has, in cooperation with the German partner Hoefer and Bechtel, performed a radiochemical characterization of the control rods from a German Pressurized Water Reactor. To perform the cutting and sampling of the spent control rods at the reactor site NRG has developed a dedicated, remotely operated tool. This tool enabled the sampling of both the stainless steel tube and the absorber material from the upper, middle and lower parts of selected rods. The samples were transported from the reactor site to NRG's laboratories at Petten, the Netherlands, were they were analysed chemically and radiologically. Due to the different chemical constitution of the control rod tubes and the absorber, the procedures for the chemical separation of the different compounds, prior to the radiological characterization, varied. The route for the stainless steel tube samples turned out more complex than that for the absorber samples: there are more nuclides to be determined, and therefore more treatment steps and component separations were necessary. Subsequently to the component separations, the radiochemical characterization was performed using alpha and gamma spectrometry and the Liquid Scintillation Counting (LSC) technique. The results of the measurements in combination with simulations performed with a reactor physics code provided for a better understanding about the distribution of radionuclides in absorber rods, both in the rod tubes and the absorber core. In addition, the results of the measurements can be used to validate reactor physics codes. (authors)

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Characterizing 5,000 Properties to Determine which Require Radiological Remediation - 19152

The Port Hope Area Initiative (PHAI) is a federal environmental clean-up program. Its mandate is the remediation and local, long-term, safe management of approximately 1.7 million cubic metres of historic low-level radioactive waste (hLLRW) in the adjacent communities of Port Hope and Port Granby in Southern Ontario, Canada. The PHAI is being undertaken by Canadian Nuclear Laboratories (CNL), on behalf of Atomic Energy of Canada Limited, a federal Crown corporation. It is currently one of the largest environmental remediation projects in Canada. Conducting work safely, while delivering the PHAI on time and within budget, is CNL's number one priority. The PHAI is being carried out as two projects - the Port Hope Project and the Port Granby Project. The Port Hope Project is the larger of the two and includes the cleanup of approximately 1.7 million cubic metres of hLLRW from various locations within the community. The Port Hope Project includes a unique and important component - the Property Radiological Survey. This survey involves the interior and exterior investigation of approximately 4,800 small-scale sites (SSS) - primarily residential - in the Municipality of Port Hope for the presence or absence of hLLRW. This paper provides an overview of the characterization, delineation and design for remediation of historic LLRW for the SSS, a grouping of sites within the municipality comprised of residential properties, municipal properties including municipal road allowances, private road allowances and temporary storage sites. Comprising over 4,800 parcels of land, a robust remedial process was designed to identify, characterize, delineate and remediate interior and exterior hLLRW contamination found in soils and building materials. The process adheres to the framework of the Port Hope Project Waste Nuclear Substance Licence (License) and its associated governance frameworks and regulatory requirements [1]. The overall goal is for CNL to be able to issue the owner of each parcel of land a Compliance Letter stating that the site meets the PHAI Clean-up Criteria, either after completion of characterization (if no hLLRW is identified) or after completion of remediation and verification. (authors)

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Non-destructive Material Characterization of Radioactive Waste Packages with QUANTOM{sup R} - 20130

During the last decades, the nuclear and non-nuclear industry has produced a considerable amount of low and intermediate level radioactive wastes. In many countries, it is foreseen to dispose of these waste packages safely in a final repository under strict waste acceptance requirements (e.g. the radiological and material characterization) defined by national licensing and supervisory authorities. The material characterization of waste packages can be performed on the basis of existing documentation or, if the documentation is insufficient, on further destructive or non-destructive analysis. Non-destructive methods are to be preferred to minimize radiation exposures of operating personnel as well as costs. We offer here an innovative non-destructive technology called QUANTOM{sup R} (Quantitative Analysis of Toxic and nontoxic Materials) based on prompt and delayed gamma neutron activation analysis (P and DGNAA). This technology is able to identify, quantify and thus verify the amount of hazardous and non-hazardous substances in 200-l radioactive drums, which is required for a final disposal characterization. (authors)

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Radiological Characterization of Hard to Measure Nuclides Using Accelerator Mass Spectrometry (AMS) - 20140

In this project irradiated heavy concrete was characterized regarding hard to measure nuclides like Ca-41 using Accelerator Mass Spectrometry (AMS). Concrete samples were irradiated with a known neutron flux and the Ca-41 content was investigated via AMS measurements. The comparison of the results with calculations shows a very good agreement in the Ca-41 content. The project revealed that AMS can be used to characterize irradiated concrete and contributes to improve the methodological basis of the radiological characterization and to extending the validation of nuclide vectors. (authors)

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Microstructural Characterization of Irradiated U{sub 0.17}ZrH{sub 1.6} Using Ultrasonic Techniques

In recent years, there has been an increased level of effort to understand the changes in microstructure that occur due to irradiation of nuclear fuel. The primary driver for this increased effort is the potential for designing new fuels that are safer and more reliable, in turn enabling new and improved reactor technologies. Much of the data on microstructural change in irradiated fuels is generated through a host of post irradiation examination techniques such as optical microscopy (OM), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) to determine grain structure, porosity, crack geometry, etc. in irradiated fuels. Such 'traditional' examination techniques were recently used to characterize a novel new fuel consisting of U{sub 0.17}ZrH{sub 1.6} pellets bonded to zircaloy-2 cladded with lead-bismuth eutectic before and after irradiation. In addition to the conventional suite of post-irradiation examination tools, several nondestructive interrogation techniques exist which bring the potential for in-situ assessment of microstructural changes. One such method, ultrasonic examination, was tested on each of the samples. This paper describes the results of this examination. Ultrasonic measurements have a long and successful history of use for nondestructive materials characterization, including nondestructive evaluation (NDE) of degradation and damage, microstructure characterization, and measurement of physical parameters for process control. Ultrasonic NDE is critical to the nuclear power industry's in-service inspection program for maintaining pressure boundary integrity, and is being actively investigated for PIE of fuels. Ultrasonic measurements, typically performed at 10 MHz or higher, performed post irradiation show that fuel microstructural parameters, such as porosity and grain size, can be correlated to ultrasonic velocity. The objective of this examination was to assess the feasibility of using ultrasonic measurements on irradiated fuel to determine sensitivity to microstructural changes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Error Convergence Characterization for Stochastic Transport Methods

There has been increased interest in reliably and efficiently solving engineering systems involving uncertainty in recent years. Characterization of the convergence of errors within the problem, including statistical and bias errors, increases confidence that chosen solution methods are appropriate for a particular problem and quantity of interest (QoI), that implementation errors have not been made, and can aid users or algorithms in solving problems within a tolerance efficiently. We demonstrate a method for characterizing error convergence in a simple stochastic transport problem. Though the approach is applicable to problems with more complicated physics, our simple problem enables analytic QoI solutions so that error convergence behavior and the identification of limiting errors can be presented with high precision. A one-dimensional, two-material, neutral-particle, and absorption-only transport problem involving uniformly distributed uncertain total cross sections is presented. Random sampling (RS) and stochastic collocation (SC) are used as stochastic solvers which sample from the uncertain space and Monte Carlo (MC) transport is employed to solve transport results on the resulting realizations. Probability density functions (PDFs) are created using either RS solutions or samples taken from a polynomial chaos expansion (PCE) constructed with SC solutions. The convergence of each solver is characterized with respect to the QoI against analytic solutions, convergence behavior is used to efficiently solve a QoI within a tolerance, and convergence plots are used to identify dominant solution errors.

42 ENGINEERING↗

Microstructural characterization of the oxidation of nuclear graphite under chronic and accident conditions via XCT and synchrotron XCT

Graphite is a candidate material to moderate fast neutrons and for structural components in the US next-generation graphite-moderated reactors. A graphite core is conceived as a large formation of interconnected bricks that primarily serves as the moderator of fast neutrons, holds instrumentation, fuel elements, control rods, and is a receptacle for molten salts for Molten Salt Reactors (MSRs) designs. During the operation of a graphite-moderated power plant, graphite components might be subjected to chronic oxidation during normal operating conditions or aggressive oxidation as a result of accidental ingress of air that reacts vigorously with the graphite core. Using synchrotron, x-ray computed tomography (XCT), this research systematically characterized microstructural changes that accompanied these two oxidation scenarios. Chronic oxidation was studied by characterizing IG-110, PCEA, and NBG-18 specimens that were gradually oxidized in air at a low temperature (520°C). The accidental ingress of air into the graphite reactor was simulated by subjecting the grades mentioned above to high-temperature oxidation at approximately 750°C. This research is the first, in situ, systematic characterization of nuclear graphite microstructural evolution that can be associated with the two possible oxidation scenarios and provide insight into related repercussions. The results show that the microstructure and pore connectivity influence the rate of oxidation and evolution of the microstructure under the two oxidation regimes. These results are crucial to understanding which grades are more resilient to each type of oxidation and documenting the damage created in the graphite.

Arregui Mena, Jose'↗

Fabrication and Characterization of Iron-Based Catalysts for the Dehydrogenation of Fossil Fuels

For a prosperous and sustainable future, hydrogen is an encouraging solution due to its simple transition for industrial decarbonization and synergy for economic development. Paradoxically, current hydrogen production pathways release substantial amount of greenhouse gases into the atmosphere contributing to climate change. To keep up with increasing demand, hydrogen could be produced through microwave-assisted thermocatalytic dehydrogenation of fossil fuels without emitting carbon dioxide. This requires specified catalysts to meet the requirements of hydrogen yield and selectivity. The objective of the present research is to fabricate, characterize, and compare iron-based alumina (FeAlxOy) catalysts produced via solution combustion synthesis and iron-based catalysts on silicon carbide support (Fe/SiC) produced via incipient wetness impregnation. Heat mode, fuel type, and oxidizer mole ratio were varied for FeAlxOy catalysts, and metal loading was varied for Fe/SiC catalysts. Each resultant product was characterized by X-ray diffraction analysis, scanning electron microscopy, laser diffraction particle size analysis, and Brunauer-Emmett-Teller (BET) surface area analysis. Characterization suggests that fabrication of iron-based alumina nanocomposites through solution combustion synthesis in a muffle furnace using citric acid as the fuel yields the most promising catalyst.

Reyes, Victoria Isabel↗

Review of the synergies between computational modeling and experimental characterization of materials across length scales

With the increasing interplay between experimental and computational approaches at multiple length scales, new research directions are emerging in materials science and computational mechanics. Such cooperative interactions find many applications in the development, characterization and design of complex material systems. This manuscript provides a broad and comprehensive overview of recent trends in which predictive modeling capabilities are developed in conjunction with experiments and advanced characterization to gain a greater insight into structure–property relationships and study various physical phenomena and mechanisms. The focus of this review is on the intersections of multiscale materials experiments and modeling relevant to the materials mechanics community. After a general discussion on the perspective from various communities, the article focuses on the latest experimental and theoretical opportunities. Emphasis is given to the role of experiments in multiscale models, including insights into how computations can be used as discovery tools for materials engineering, rather than to “simply” support experimental work. This is illustrated by examples from several application areas on structural materials. In conclusion this manuscript ends with a discussion on some problems and open scientific questions that are being explored in order to advance this relatively new field of research.

3-D microstructure characterization↗

Characterizing Technetium in Subsurface Sediments for Contaminant Remediation

Technetium-99 (Tc) contamination remains a major environmental problem at legacy nuclear reprocessing sites, including the Hanford Site (Washington State, USA) where ~700 Ci of Tc has been released into the subsurface. The environmental risk associated with Tc is due to its long half-life (213,000 years) and high mobility of the oxidized anionic pertechnetate species, Tc(VII)O 4 - , which warranted the US Department of Energy to identify Tc as a primary contaminant of concern. This risk generates a critical need to resolve scientific and technical issues underpinning the ability to safely, cost-effectively, and efficiently remediate Tc-contaminated vadose zone sediments and groundwater and mitigate risk to human health and the environment. Developing enhanced attenuation and efficient remediation strategies for released Tc requires a complete understanding of retardation processes and Tc mass flux, including the different mechanisms by which Tc is immobilized in the subsurface and the effect of localized subsurface conditions. Selection of over 30 sediments from Hanford waste disposal sites, based on historical information and sediment characterization, for analysis by autoradiography revealed that Tc concentrations were generally below the detection limit of 5 mg Tc/g sediment. When Tc was measurable in vadose zone sediments, it was predominantly present as TcO 4 - in water films associated with fine-grained sediments, with a maximum of 12 % of the total Tc present in the acid-extractable fraction, defined here as the immobile fraction. However, beneath one waste disposal site, where sediments containing minerals with reducing capacity intercepted miscellaneous fission product recovery waste and waste from the bismuth phosphate process, the amount of Tc present in the immobile fraction was 53 % of the total. Characterization of Tc-containing phases present in these field-contaminated sediments for the first time using Tc K-edge X-ray absorption near edge structure spectroscopy revealed that, as well as Tc present as Tc(VII)O 4 - in pore water associated with fine-grained sediments, Tc was also: (i) physically encapsulated within solid phases precipitated from other waste components and in multi-component phosphate minerals; and (ii) present as mixed Tc(VII)/Tc(IV) in localized reducing zones. These results will be used to develop improved long-term Tc remediation strategies optimized for field application, through stimulation of conditions that enhance Tc attenuation.

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