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At least 1,081 records · Page 60

Arcjet Testing of Micro-Meteoroid Impacted Thermal Protection Materials

There are several harsh space environments that could affect thermal protection systems and in turn pose risks to the atmospheric entry vehicles. These environments include micrometeoroid impact, extreme cold temperatures, and ionizing radiation during deep space cruise, all followed by atmospheric entry heating. To mitigate these risks, different thermal protection material samples were subjected to multiple tests, including hyper velocity impact, cold soak, irradiation, and arcjet testing, at various NASA facilities that simulated these environments. The materials included a variety of honeycomb packed ablative materials as well as carbon-based non-ablative thermal protection systems. The present paper describes the results of the multiple test campaign with a focus on arcjet testing of thermal protection materials. The tests showed promising results for ablative materials. However, the carbon-based non-ablative system presented some concerns regarding the potential risks to an entry vehicle. This study provides valuable information regarding the capability of various thermal protection materials to withstand harsh space environments, which is critical to sample return and planetary entry missions.

Agrawal, Parul↗

Comparison of the Organic Composition of Cometary Samples with Residues Formed from the UV Irradiation of Astrophysical Ice Analogs

The NASA Stardust mission successfully collected material from Comet 81P/Wild 2 [1], including authentic cometary grains [2]. X-ray absorption near-edge structure (XANES) spectroscopy analysis of these samples indicates the presence of oxygen-rich and nitrogen-rich organic materials, which contain a broad variety of functional groups (carbonyls, C=C bonds, aliphatic chains, amines, arnides, etc.) [3]. One component of these organics appears to contain very little aromatic carbon and bears some similarity to the organic residues produced by the irradiation of ices of interstellar/cometary composition, Stardust samples were also recently shown to contain glycine, the smallest biological amino acid [4]. Organic residues produced froth the UV irradiation of astrophysical ice analogs are already known to contain a large suite of organic molecules including amino acids [5-7], amphiphilic compounds (fatty acids) [8], and other complex species. This work presents a comparison between XANES spectra measured from organic residues formed in the laboratory with similar data of cometary samples collected by the Stardust mission

Milam, S. N.↗

The effect of secondary phases on microstructure and irradiation damage in an as-built additively manufactured 316 L stainless steel with a hafnium compositional gradient

Additive manufacturing (AM) or rapid prototyping has become a crucial tool for reducing both cost and time while increasing efficiency in qualifying structural materials for reactor use. In this study, directed energy deposition (DED) was used to develop an as-built 316 L stainless steel sample with three regions of increasing Hf-dopant to study the effects of Hf on the irradiation response of the material. Morphological and microstructural changes were analyzed before and after 2 MeV proton irradiation at 360 °C to a damage of 2.5 dpa at ~ 10 µm below the surface. The addition of Hf effectively suppressed radiation-induced damage (dislocation loops, radiation-induced segregation) due to enhanced point defect recombination. The radiation damage seen in the as-built sample was further compared to a thermo-mechanically treated counterpart of the same fabrication and irradiation parameters which was found to behave superiorly. In conclusion, the increased radiation resistance of this material may be attributed to the as-built microstructure, which includes undissolved Hf particles, delta ferrite grains and cellular sub-grain boundaries that can hinder defect motion.

316L Stainless Steel↗

Development and testing of a superconducting link for an IR detector

The development and testing of a ceramic superconducting link for an infrared detector is summarized. Areas of study included the materials used, the electrical contacts, radiation and temperature cycling effects, aging, thermal conductivity, and computer models of an ideal link. Materials' samples were processed in a tube furnace at temperatures of 840 C to 865 C for periods up to 17 days and transition temperatures and critical current densities were recorded. The project achieved better quality high superconducting transition temperature material through improved processing and also achieved high quality electrical contacts. Studies on effects of electron irradiation, temperature cycling, and aging on superconducting properties indicate that the materials will be suitable for space applications. Various presentations and publications on the study's results are reported.

Caton, R.↗

Testing and Characterization to Develop a Mechanistic Explanation for Unsaturated Drift of Fiber Optic Sensors during High-Dose Irradiation

The primary limitation for any optical fiber-based sensor for nuclear reactor applications is radiation-induced attenuation (RIA) of the transmitted and/or reflected signals. Based on several recent studies, RIA is tolerable for some fused silica optical fibers with the proper choice of sensing wavelength and fiber dopants. For extreme temperature applications (> 1000°C), sapphire optical fibers have been proposed; however, recent optical transmission measurements performed on bulk sapphire samples showed prohibitively large RIA. For some sensors, radiation-induced dimensional changes in the fiber materials can also cause significant drift. Moreover, the drift that was observed in numerous experiments performed in the High Flux Isotope Reactor (HFIR), the Advanced Test Reactor, the Massachusetts Institute of Technology Reactor, and other international facilities far exceeded what would be expected based on compaction of fused silica glass. Clearly, additional work is needed to better understand the origins of both RIA and radiation-induced drift in both silica and sapphire optical fiber-based sensors before these sensors can be reliably deployed for nuclear applications. This work evaluated the underlying mechanisms that may be responsible for RIA and drift in silica and sapphire materials. First, detailed characterization was performed on bulk fused silica glass samples that were previously irradiated to different neutron fluences at different temperatures to better understand the structural changes that drive radiation-induced drift in the absence of coating effects that are discussed later. Results show that the non-monotonic compaction that occurs with increasing neutron fluence continues up to fast neutron fluences approaching 10 22 n/cm 2 , which has important implications for physics-based models that may be used to compensate for the sensor drift. Initial Raman spectroscopy and synchrotron x-ray diffraction provide insights into the nature of the structural changes. Next, detailed characterizations were performed on silica fibers with various coatings that were subjected to several different thermal treatments. The hypothesis is that the coatings convert to carbon-rich materials that compact under irradiation, putting a large compressive strain on the fiber. Out-of-pile testing confirms that both polyimide and acrylate fiber coatings convert to glassy carbon (GC) materials when heated under inert conditions, and the degree of order (i.e., graphitization) increases with increasing temperature. The results provide increasingly strong evidence that the combination of polymeric coatings and inert (or vacuum) conditions render fiber optic sensors susceptible to significant radiation-induced drift that would not otherwise exist in uncoated fibers. Finally, transmission electron microscopy was performed on bulk sapphire samples that were irradiated to two neutron fluences at different temperatures to gain insights into the potential mechanisms driving the prohibitive RIA at higher neutron fluences and temperatures. Contrary to previous hypotheses, results show that scattering from radiation-induced voids cannot explain the observed RIA. Similarly, models for scattering losses from dislocation loops also do not agree with the experimental results. Instead, fitting to the experimental data shows that increased absorption from aluminum vacancy centers is the most likely explanation for the the prohibitively large RIA that was observed at high irradiation temperature and dose. In addition, the voids that formed in these single-crystal samples were found to align along the basal plane (a-axis) as opposed to that seen in previous observations of c-axis alignment in polycrystalline samples, which could have important implications for anisotropic swelling and other phenomena that could affect sensor performance at high neutron fluence.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Testing and Characterization to Develop a Mechanistic Explanation for Unsaturated Drift of Fiber Optic Sensors during High-Dose Irradiation

The primary limitation for any optical fiber-based sensor for nuclear reactor applications is radiation-induced attenuation (RIA) of the transmitted and/or reflected signals. Based on several recent studies, RIA is tolerable for some fused silica optical fibers with the proper choice of sensing wavelength and fiber dopants. For extreme temperature applications (> 1000°C), sapphire optical fibers have been proposed; however, recent optical transmission measurements performed on bulk sapphire samples showed prohibitively large RIA. For some sensors, radiation-induced dimensional changes in the fiber materials can also cause significant drift. Moreover, the drift that was observed in numerous experiments performed in the High Flux Isotope Reactor (HFIR), the Advanced Test Reactor, the Massachusetts Institute of Technology Reactor, and other international facilities far exceeded what would be expected based on compaction of fused silica glass. Clearly, additional work is needed to better understand the origins of both RIA and radiation-induced drift in both silica and sapphire optical fiber-based sensors before these sensors can be reliably deployed for nuclear applications. This work evaluated the underlying mechanisms that may be responsible for RIA and drift in silica and sapphire materials. First, detailed characterization was performed on bulk fused silica glass samples that were previously irradiated to different neutron fluences at different temperatures to better understand the structural changes that drive radiation-induced drift in the absence of coating effects that are discussed later. Results show that the non-monotonic compaction that occurs with increasing neutron fluence continues up to fast neutron fluences approaching 10 22 n/cm 2 , which has important implications for physics-based models that may be used to compensate for the sensor drift. Initial Raman spectroscopy and synchrotron x-ray diffraction provide insights into the nature of the structural changes. Next, detailed characterizations were performed on silica fibers with various coatings that were subjected to several different thermal treatments. The hypothesis is that the coatings convert to carbon-rich materials that compact under irradiation, putting a large compressive strain on the fiber. Out-of-pile testing confirms that both polyimide and acrylate fiber coatings convert to glassy carbon (GC) materials when heated under inert conditions, and the degree of order (i.e., graphitization) increases with increasing temperature. The results provide increasingly strong evidence that the combination of polymeric coatings and inert (or vacuum) conditions render fiber optic sensors susceptible to significant radiation-induced drift that would not otherwise exist in uncoated fibers. Finally, transmission electron microscopy was performed on bulk sapphire samples that were irradiated to two neutron fluences at different temperatures to gain insights into the potential mechanisms driving the prohibitive RIA at higher neutron fluences and temperatures. Contrary to previous hypotheses, results show that scattering from radiation-induced voids cannot explain the observed RIA. Similarly, models for scattering losses from dislocation loops also do not agree with the experimental results. Instead, fitting to the experimental data shows that increased absorption from aluminum vacancy centers is the most likely explanation for the the prohibitively large RIA that was observed at high irradiation temperature and dose. In addition, the voids that formed in these single-crystal samples were found to align along the basal plane (a-axis) as opposed to that seen in previous observations of c-axis alignment in polycrystalline samples, which could have important implications for anisotropic swelling and other phenomena that could affect sensor performance at high neutron fluence.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Conceptual Designs for Irradiation Creep Testing of SiC in HFIR

Understanding irradiation creep of nuclear fuel cladding is important to properly size the initial fuel-cladding gap and understand when pellet-cladding contact is expected to occur due to a combination of fuel swelling and cladding creep-down. Irradiation creep also plays a role in relaxing stresses that develop in-pile. Silicon carbide fiber–reinforced silicon carbide matrix (SiC/SiC) composites are the leading long-term accident-tolerant fuel cladding concept for light-water reactors (LWRs). Although some limited data are available regarding irradiation creep of the individual constituents (fibers, matrix), data regarding irradiation creep of SiC/SiC composites are currently insufficient. Additional data regarding irradiation creep compliance and the rupture lifetime (combination of creep and slow crack growth) are needed to understand material limitations. This work describes the design and development of two irradiation vehicles that are being pursued for testing SiC/SiC concepts in the High Flux Isotope Reactor (HFIR). The first is a passive experiment, referred to as the PRECISE experiment, that leverages the constant coolant pressure of HFIR to compress a metallic bellows and provide a well-characterized load to drive creep in a SiC/SiC dog bone specimen. The total creep strain would be quantified post-irradiation by measuring dimensional changes of the specimen length as well as local dimensional changes within the gauge region. Non-stressed specimens would also be irradiated under the same conditions to provide an indication of dimensional changes due to radiation-induced swelling in the absence of creep. A second, more complex experiment, referred to as the INSITE experiment, is being designed in parallel that would use pneumatics to pressurize a metal bellows and linear variable differential transformers (LVDTs) to measure the specimen displacement in situ during irradiation. Such an experiment would provide significantly more data regarding the evolution of the creep compliance as a function of dose and applied stress within a single experiment but would require significantly more development time and cost to execute. The primary concern with the INSITE experiment is the accuracy, reliability, and expected lifetime of the LVDTs during irradiation at elevated temperatures. Efforts are being made to adjust the experiment design and operating procedure to limit LVDT temperatures and mitigate or otherwise compensate for uncertainties due to factors such as temperature fluctuations, creep in the surrounding structural materials, and drift of the LVDTs. This work describes the experiment designs, thermal and structural analysis that were performed to ensure that the desired temperature and stress conditions can be achieved, some initial sensitivity analyses to predict the evolution of the radiation-induced specimen displacements, and potential sources of uncertainty in the measurements. Out-of-pile testing is being performed in parallel to confirm that the test trains achieve the expected stress states in the specimens and do not result in prohibitive stress concentrators (e.g., in the grip regions) that might risk pre-mature failure. The PRECISE experiments are proceeding toward fabrication and assembly with HFIR insertion planned during fiscal year 2026. The INSITE experiment is progressing toward out-of-pile demonstrations, which will provide more conclusive evidence regarding the feasibility of executing these tests in HFIR or whether alternative displacement monitoring techniques may need to be considered.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Comparison of Ion and Neutron Irradiations to 3 dpa at 500C in Ferritic-Martensitic Alloys

The growing global demand for energy will increasingly call upon advanced nuclear fission reactors to supply safe and reliable electricity. The structural and fuel cladding components of these reactors will be subject to extreme conditions of irradiation damage up to several hundred displacements per atom (dpa) at temperatures as high as 700°C. Ferritic-martensitic (F-M) steels are leading candidates for these challenging conditions due to their strength and dimensional stability under irradiation. In order to accelerate the process for evaluating F-M alloys, charged particles are increasingly being used to emulate neutron irradiations. Charged particle irradiations allow the possibility of conducting irradiation experiments within a shorter time period (i.e. at a rate up to 4 orders of magnitude faster) and with minimal radioactivation of the material, enabling lower cost and faster turnaround of post irradiation examination and analysis. However, the irradiation dose rate, damage cascade morphologies, and irradiation damage depth profiles all differ widely between protons, heavier ions, and neutrons. Currently, there is limited understanding of the significance of these physical differences and how they manifest in the irradiated microstructure and mechanical properties of F-M steels. The objective of this study is to evaluate charged particles as a surrogate for neutron irradiations in F-M alloys by assessing common irradiation conditions using Fe++ ions, protons, and neutrons. Keeping the temperature and dose consistent enables isolation of the effects of each irradiating particle and their respective dose rates and cascade morphologies.

Swenson, M.J.↗

A simplified approach for creep damage and remaining life calculation for materials surveillance in advanced reactors

High temperature reactor materials will experience a combination of mechanical degradation caused by creep and fatigue and environmental degradation caused by neutron irradiation and, in some cases, exposure to corrosive coolants. A materials surveillance program is one option for ensuring the safe, reliable operation of key reactor components under these conditions. Such a program would monitor the degradation in key material properties over time, using this data to predict how changes in the material properties affect components performance. This could then be used to make plant operational decisions and support eventual plant license extensions. Past work de-scribes such a material surveillance program based on passively actuated mechanical test articles that impose creep-fatigue type loading on test materials driven only by changes in temperature, for example those experienced by components under standard operating cycles. This report focuses on two aspects of the proposed material surveillance program: how to design the test articles to mimic the mechanical response of the corresponding component and how to use ex-situ test data to deter-mine the amount of damaged experienced by the test article (and hence the corresponding compo-nent) in service. Specifically, this report derives and validated simplified methods for both tasks, replacing earlier, more complicated approaches based on simulating the test article response and finding the best specimen design or current damage via complex numerical optimization. The sim-plified methods for each task developed here can be implemented in spreadsheet software and are simple enough for practical use in future operating plants. This report derives the methods (one for sizing and two options for damage inference), verifies the simplified approaches versus more so-phisticated methods, and compares the results of applying the simplified methods to previous re-sults using the complex numerical optimization approach. The report also provides a worked sam-pled problem applying the simplified techniques to a realistic high temperature reactor component.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

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

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

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Oak Ridge Response to Versatile Test Reactor Environmental Impact Statement Data Request

The Versatile Test Reactor (VTR) is a fast-spectrum test reactor being developed in the United States under the direction of the US Department of Energy Office of Nuclear Energy (DOE-NE). The VTR mission is to enable accelerated testing of advanced reactor fuels and materials required for advanced reactor technologies. The conceptual design of the 300 MWth sodium-cooled metallic-fueled pool-type fast reactor has been led by the US National Laboratories in collaboration with General Electric–Hitachi and Bechtel National, Inc. In support of the VTR project, DOE issued a Notice of Intent (NOI) in the Federal Register on August 5, 2019, announcing the intent to prepare an Environmental Impact Statement (EIS) in accordance with the National Environmental Policy Act (NEPA) and its implementing regulations. The EIS will evaluate alternatives for a versatile reactor–based fast-neutron source facility and associated facilities for the preparation, irradiation, and post-irradiation examination (PIE) of test/experimental fuels and materials. Specifically, the NOI identified two siting alternatives for the VTR reactor facility: Idaho National Laboratory (INL) or Oak Ridge National Laboratory (ORNL). In addition, the NOI also specified two siting alternatives for VTR fuel fabrication: INL and the Savannah River Site (SRS). This report provides information in response to data requests made to ORNL to fill in site-specific knowledge gaps to develop a high-quality EIS. The responses provided are not required to provide full details in every aspect; instead, they adequately bound possible environmental impacts or provide sufficient information to adequately assess likely environmental impacts. This work is being performed under a subcontract from INL to ORNL using DOE-NE funds and is directed by DOE-NE and DOE-ID. Leidos has been contracted by DOE-NE to write the VTR EIS, so most data requests have come from Leidos but were often routed through INL or DOE-ID. DOE-ID is overseeing the NEPA and EIS processes for the VTR project. Leidos will use the information provided in this report to inform the VTR EIS and will also cite this document to establish a clear, publicly available source of the information. Section 2 of this report briefly describes the proposed ORNL VTR Alternative and illustrates the location of the proposed site for the ORNL VTR Alternative. Sections 3 through 7 provide direct responses to data requests received by ORNL. These sections use a tabular format in which data requests are divided into separate items to be addressed; the items are numbered, the data requests are restated with more topical information included, and then the responses are provided. Initial data requests and follow-on requests for additional information (RAIs) are combined under the original data request fields. Finally, Section 8 presents summarized conclusions and describes future work.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Yttrium Hydride Post-Irradiation Examination Plan

Micro nuclear reactors are expected to use metal hydride moderators to ensure thier compact design for the flexible operational purposes. Department of Energy’s Microreactor program therefore aims to provide infrasture and qualification bed for the development of micro nuclear reactors. Because micro nuclear reactors must be compact to offer a flexible operational purposes, metal hydrides are expected to be used as neutron moderator materials due to their high hydrogen number density. Los Alamos National Laboratory (LANL) directed by the DOE to provide a qualified fabrication techniques of metals hydride, especially the yttrium hydride (YHx) which provides advantages over other metal hydride candiates. Qualification of YHx involves fabrication, property, and performance pillars, which must be met for the deployment of microreactors. In the support of the qualification process metal hydride, LANL has developed fabrication techniques based in direct hydriding and powder compacting. For both manufacturing techniques, fresh material properties of metal hydrides have been reported in the literature. To establish the performance limits and the qualification parameters, an irradiation campaign has been initated at Idaho National Laboratory (INL). The irradation campaign aims to investigate the critical irradiated YHx properties as a function of neutron fluence and temperaute. The first phase of the irradiation campaign includes the effect of the operating temperature under neutron irradiation which provides initial data on the metal hydrides and informs the manufacturing processes. So that, drop-in irradations in Advanced Test Reactor (ATR) has been designed. This document depicts the post-irradation examination (PIE) plan of the ATR irradiated YHx. Objective of the PIE plan is to serve as a qualification basis for YHx as a neutron moderator material by understanding the impacts irradiation has on the physical and thermophysical properties; to establish a link between fabrication and the irradiated YHx properties; to institute a PIE strategy for other solid-state neutron moderator candidates, and; to inform micro nuclear reactor fuel performance and safety codes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Laser Ablation of Materials for Propulsion of Spacecraft

A report describes experiments performed as part of a continuing investigation of the feasibility of laser ablation of materials as a means of propulsion for small spacecraft. In each experiment, a specimen of ablative material was mounted on a torsion pendulum and irradiated with a laser pulse having an energy of 5 J. The amplitude of the resulting rotation of the torsion pendulum was taken to be an indication of the momentum transferred from the laser beam. Of the ablative materials tested, aluminum foils yielded the smallest rotation amplitudes of the order of 10 degrees. Black coating materials yielded rotation amplitudes of the order of 90 degrees. Samples of silver coated with a fluorinated ethylene propylene (FEP) copolymer yielded the largest rotation amplitudes 6 to 8 full revolutions. The report presents a theory involving heating of a confined plasma followed by escape of the plasma to explain the superior momentum transfer performance of the FEP specimens. It briefly discusses some concepts for optimizing designs of spacecraft engines to maximize the thrust obtainable by exploiting the physical mechanisms of the theory. Also discussed is the use of laser-ablation engines with other types of spacecraft engines.

Edwards, David L.↗

In-Situ Helium Implantation and TEM Investigation of Radiation Tolerance to Helium Bubble Damage in Equiaxed Nanocrystalline Tungsten and Ultrafine Tungsten-TiC Alloy

The use of ultrafine and nanocrystalline materials is a proposed pathway to mitigate irradiation damage in nuclear fusion components. Here, we examine the radiation tolerance of helium bubble formation in 85 nm (average grain size) nanocrystalline-equiaxed-grained tungsten and an ultrafine tungsten-TiC alloy under extreme low energy helium implantation at 1223 K via in-situ transmission electron microscope (TEM). Helium bubble damage evolution in terms of number density, size, and total volume contribution to grain matrices has been determined as a function of He+ implantation fluence. The outputs were compared to previously published results on severe plastically deformed (SPD) tungsten implanted under the same conditions. Large helium bubbles were formed on the grain boundaries and helium bubble damage evolution profiles are shown to differ among the different materials with less overall damage in the nanocrystalline tungsten. Compared to previous works, the results in this work indicate that the nanocrystalline tungsten should possess a fuzz formation threshold more than one order of magnitude higher than coarse-grained tungsten.

36 MATERIALS SCIENCE↗

Energy-Dispersive X-ray Spectroscopy and Atom-probe Tomography Data Quantifying Component-Ratios of Multicomponent Nano-Precipitates in Ion-Irradiated Ceria

Samples of ~1 µm films of CeO2 doped with 2 wt% Mo, 1.5 wt% Ru, 0.75 wt% Pd, 0.5 wt% Re and 0.25 wt% Rh grown with pulsed laser deposition were irradiated with I2+ ions (610°C and 730°C, 1016 and 5×1016 I2+/cm2). For selected samples post-irradiation heat treatment was conducted (900°C, 1100°C). The specimens were sectioned with focussed ion beam milling and characterized in a transmission electron microscope with energy dispesive x-ray spectroscopy, and with atom-probe tomography. Energy dispersive x-ray spectroscopy was used to obtain elemental maps showing the distribution of dopants in the specimen after exposure. Some of these maps are discussed in detail in our companion article “Formation of multicomponent alloy particles in doped ceria under I2+ ion irradiation and thermal annealing” in the Journal of Nuclear Materials [REF]. Advanced computational analysis could be used to more accurately quantify local compositions. Data is provided for additional regions of interest and one additional irradiation condition. The doped Ceria film that was heat treated at 1100 °C delaminated from the substrate in most places. Samples were extracted from the underside of a delaminated piece and analyzed with atom-probe tomography. The resulting data show Ceria and a Mo-rich particle and demonstrate that this approach is feasable in principle to study local compositions in a sample exposed to such extreme conditions.

multicomponent alloys, epsilon phase, EDS, atom pr↗

Freeze It or Leave It? Evaluating the Role of Cryo-Electron Microscopy in Battery Research

Cryogenic electron microscopy (cryo-EM) continues to gain prominence in materials science, particularly in battery research where it has enabled high-resolution, multimodal characterization of electrode materials and interfaces that otherwise degrade quickly under electron beam irradiation. But as anyone who has attempted cryo-EM techniques knows, freezing comes at a cost; cryo-EM experiments are time-consuming, highly sensitive, and carry an increased risk of artifacts due to issues such as frost contamination. Thus, when planning new characterization of battery materials or other beam-sensitive samples, it is critical to consider whether (and which) cryo-EM techniques are appropriate, based on study goals and an understanding of electron beam-sample interactions. Here we review such considerations for battery materials to elucidate the questions of when, why, and how to freeze to achieve high-quality characterization.

25 ENERGY STORAGE↗

Defining Probe Closure Offset and Scan Stitching Methodology for Element Contact Profilometry in the Hot Fuel Examination Facility

The Element Contact Profilometer (ECP) is a non-destructive post-irradiation examination (PIE) method established in the Materials and Fuels Complex (MFC) Hot Fuel Examination Facility (HFEF). The ECP suspends a fuel rod with a standard end-fitting in a vertical orientation and draws it between two opposed Sony probes with sapphire rod tips, which measure the diameter directly as a function of vertical stage position through contact profilometry. The ECP is equipped with concave rollers, which pinch the rod to maintain a consist position between these sapphire probe tips. A schematic of the analysis head is shown in Figure 1. The gripper that suspends the rod end-fitting is able to rotate to allow measuring of any azimuthal angle around the rod. This system is used to characterize the diameter of full-length light water reactor (LWR) irradiated fuel rods at multiple azimuthal angles in support of the Advanced Fuels Campaign (AFC).

22 - GENERAL STUDIES OF NUCLEAR REACTORS↗

In-Cell Deployment and First Use of Digital Image Correlation for In-Situ Strain Analysis of Irradiated Nuclear Fuel Rods During LOCA Transient

Digital image correlation (DIC) is a noncontact, optical method increasingly used across industries and research environments for acquiring multidimensional strain data. At Oak Ridge National Laboratory’s (ORNL’s) Severe Accident Test Station (SATS), DIC has been extensively applied to study the thermomechanical response of nuclear fuel claddings, yielding fundamental insights into material behavior. However, these efforts have focused exclusively on unirradiated materials and relied on the SATS out-of-cell infrastructure. Efforts over the past two years have been made to extend these capabilities to ORNL’s Irradiated Fuels Examination Laboratory SATS system within the hot-cells to enable testing of irradiated fuel cladding materials. Integrating DIC into the hot-cell SATS infrastructure presents unique challenges, including enabling remote operation of optical equipment and adapting auxiliary hot-cell systems for DIC implementation. This report discusses design, stand-up testing, and application of DIC to an irradiated nuclear fuel cladding segment. A DIC testing rig was successfully built and validated out-of-cell through extensive surrogate tests and calibrations. The rig and specialized DIC furnace were installed in the hot-cell, and a DIC test was successfully conducted. Results from that test correspond to expectations for Zr-based alloys and showed similar uncertainties compared to out-of-cell tests.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗