Using in-situ TEM Triple Ion Beam Irradiations to Study the Effects of Deuterium, Helium, and Radiation Damage on TPBAR Components.
Abstract not provided.
Taylor, Caitlin↗
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Observation of formation and local structures of metal-organic layers via complementary electron microscopy techniques
Abstract Metal-organic layers (MOLs) are highly attractive for application in catalysis, separation, sensing and biomedicine, owing to their tunable framework structure. However, it is challenging to obtain comprehensive information about the formation and local structures of MOLs using standard electron microscopy methods due to serious damage under electron beam irradiation. Here, we investigate the growth processes and local structures of MOLs utilizing a combination of liquid-phase transmission electron microscopy, cryogenic electron microscopy and electron ptychography. Our results show a multistep formation process, where precursor clusters first form in solution, then they are complexed with ligands to form non-crystalline solids, followed by the arrangement of the cluster-ligand complex into crystalline sheets, with additional possible growth by the addition of clusters to surface edges. Moreover, high-resolution imaging allows us to identify missing clusters, dislocations, loop and flat surface terminations and ligand connectors in the MOLs. Our observations provide insights into controllable MOL crystal morphology, defect engineering, and surface modification, thus assisting novel MOL design and synthesis.
36 MATERIALS SCIENCE↗
Dose Rate Effects in the Aging of Nuclear Cable Insulation Subjected to Gamma Radiation
In nuclear power plants (NPPs), the aging of polymer-based electrical cable insulation must be effectively monitored to ensure the safe and reliable operation of NPPs. Gamma radiation is one of the main environmental stressors causing degradation of cable insulation. For a given total dose of absorbed gamma radiation, damage due to gamma irradiation may be dose rate dependent. The purpose of this work is to confirm whether a dose rate effect exists for the cable insulation made by crosslinked polyethylene (XLPE) and ethylene propylene rubber (EPR), quantify the relationship between degradation rate and dose rate, and explore the correlation of different measured properties. The dose rate effects at 1800 Gy/h, 200 Gy/h, and 100 Gy/h using 60Co gamma irradiation on cable aging was studied. Different types of cable insulation, including two XLPEs and one EPR, were irradiated at the different dose rates with a total dose around 300 kGy at 26 °C. The properties of unirradiated and irradiated samples were characterized by mass change, yellowness index, and other ongoing measurements. Dose rate effects were observed for mass change data of XLPE and EPR.
Li, Donghui↗
Development of a robust damage analysis scheme at the National Ignition Facility
The onset of laser-induced damage in optical materials is a limiting factor in the design and operation of most high-energy laser systems. As such, significant effort has been dedicated to developing laser damage testing protocols and procedures to inform laser system design and operating limits. These tests typically rely on multiple laser exposures for statistical validation. Historically, small beam single fluence (N / 1) or ramped fluence (R / 1) tests have been used to quantify the “laser-induced damage threshold” of a material. However, due to various distributions in damage precursor populations, the laser fluence at which damage occurs for a given sample varies with beam size and is therefore better described as the onset of observed damage for that testing geometry. In conclusion, we document the development of irradiation, measurement, and analysis methods for damage testing resulting in damage initiation density as a function of incident fluence or ρ(ϕ) which is suitable for both small and large beam area testing and more conducive to extrapolating from one to the other.
Beam diameter↗
Chemical and physical transformations of carbon-based nanomaterials observed by liquid phase transmission electron microscopy
This article addresses recent advances in liquid phase transmission electron microscopy (LPTEM) for studying nanoscale synthetic processes of carbon-based materials that are independent of the electron beam—those driven by nonradiolytic chemical or thermal reactions. In particular, we focus on chemical/physical formations and the assembly of nanostructures composed of organic monomers/polymers, peptides/DNA, and biominerals. The synthesis of carbon-based nanomaterials generally only occurs at specific conditions, which cannot be mimicked by aqueous solution radiolysis. Carbon-based structures themselves are also acutely sensitive to the damaging effects of the irradiating beam, which make studying their synthesis using LPTEM a unique challenge that is possible when beam effects can be quantifi ed and mitigated. With new direct sensing, high frame rate cameras, and advances in liquid-cell holder designs, combined with a growing understanding of irradiation effects and proper experimental controls, microscopists have been able to make strides in observing traditionally problematic carbon-based materials under conditions where synthesis can be controlled, and imaged free from beam effects, or with beam effects quantified and accounted for. These materials systems and LPTEM experimental techniques are discussed, focusing on nonradiolytic chemical and physical transformations relevant to materials synthesis.
Parent, Lucas R.↗
Joint Development of SAS4A Code in Application to Oxide-fueled LFR Severe Accident Analysis
The scope of this project was to pursue specific SAS4A liquid-metal cooled reactor (LMR) safety analysis software extensions to simulate postulated accidents with fuel failures for oxide-fueled Lead-cooled Fast Reactors (LFRs). Since most U.S. LMR experience is on sodium-cooled fast reactor options based on past testing and operation experience with EBR-II and FFTF, the DOE’s legacy fast reactor safety analysis capabilities were focused on metal-fueled pool-type concepts with sodium coolant. In recent years, Westinghouse Electric Company (WEC) has decided to pursue an LFR design as one of their next generation nuclear technology options because of its favorable safety and economics attributes. Oxide fuel is considered among other fuel options due to previous WEC experience with this fuel form. Development of this new technology requires the availability of adequately accurate computational tools, some of which can be adapted from versions of similar software used for analysis of other LMRs. Although Argonne National Laboratory’s (ANL) SAS4A/SASSYS-1 safety analysis software suite (shortened as SAS4A code hereafter for brevity) has the basic capabilities to model LFR system designs, the SAS4A code modules used in the analysis of accidents with fuel/cladding failures lack appropriate models for the unique phenomena that govern as-irradiated oxide-fuel damage mechanisms in lead coolant. Therefore, the objective of this project was to extend the capabilities of SAS4A with mechanistic oxide-fuel failure models in lead coolant for margin to failure assessments, analysis of failure modes, location and timing of failures under different accident scenarios consistent with the whole-plant dynamic response including the reactivity feedback, and assessment of the potential for fuel damage propagation due to potential fission gas jet and fuel-fragment/molten fuel impingement to neighboring fuel pins in an assembly. This report provides mainly a summary of Argonne’s technical contributions in the joint project, but the reports and publications by the Participant team are included as references at the end of the report.
22 GENERAL STUDIES OF NUCLEAR REACTORS↗
A Multiscale Investigation of the Mechanisms Controlling Materials Degradation in the Fusion Energy Environment (DE-SC0006661: Final Report)
Realizing the promise of fusion as a commercially attractive energy source requires the development of advanced structural materials capable of sustained operation in an incredibly hostile environment. The fusion environment presents many challenges associated with high cyclic thermal-mechanical loadings, welding and joining disparate materials, and achieving chemical compatibility with coolants and tritium breeders. Yet, the overarching concern is the degradation of physical and mechanical properties, resulting from a neutron energy spectrum peaked at 14 MeV. The high-energy fusion neutron irradiation produces both displacement damage and high levels of hydrogen and helium through transmutation reactions. Advanced materials development for use in such a hostile environment is predicated on understanding the underlying mechanisms responsible for physical and material property degradation. This project has closely combined computational, theoretical and experimental techniques within a multiscale materials science paradigm to determine the mechanisms controlling material degradation in the fusion environment.
70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
Understanding In-Situ Structure and Chemistry at Battery Interfaces Through Time-Resolved Cryo-EM
Transmission and scanning transmission electron microscopy are vital tools for characterizing interfacial structure and chemistry at high spatial resolutions but are limited by the fact that many materials are quickly damaged by electron beam irradiation. This is a challenge particularly for materials relevant to energy applications, such as lithium-containing battery materials, organic-inorganic hybrids, and liquid electrolytes. Cryogenic electron microscopy (cryo-EM) offers a partial solution to this issue by stabilizing beam-sensitive solid-solid or solid-liquid interfaces for characterization, but typical cryo-EM sample preparations are ex situ and thus cannot capture interfaces in their electrified state of interest to applications. Here, we present a method to prepare cryo-EM samples of electrified battery interfaces in situ to preserve the time-resolved structures and chemistry that arise under applied current or bias.
batteries↗
Layer dissolution in accumulative roll bonded bulk Zr/Nb multilayers under heavy-ion irradiation
In this work, the heavy-ion irradiation behavior of bulk zirconium-niobium multilayered composites was investigated up to large doses. Multilayers with an average individual layer thicknesses ranging between 15 and 80 nm were synthesized by accumulative roll bonding technique. The irradiation was performed with a defocused 7 MeV Zr 2+ ion beam at 500 °C. The maximum dose achieved was ~145 dpa at the depth of ~1.5 μm from the irradiated surface. Sub-surface microstructural damage and the chemical redistribution were characterized by transmission electron microscopy and energy dispersive spectroscopy, respectively. Irrespective of the layer thicknesses, the irradiation condition caused layer instability and the extent of damage varied with the dose levels. Doses lesser than ~60 dpa caused layer fragmentation and greater than ~60 dpa resulted in layer dissolution. The chemical mixing of layers occur to a depth of ~1 μm, consuming multiple bi-layer periods. Despite the elevated irradiation temperature (500 °C) and a slightly positive heat of mixing (+6 kJ/mol), no phase separation was observed and single-phase was retained in the mixed region. The results demonstrate that chemical mixing was facilitated by the liquid phase miscibility of Zr and Nb, which propelled the interdiffusion within the thermal spikes towards mixing.
36 MATERIALS SCIENCE↗
Analysis of attenuation data from the decommissioned ZIon unit 1 reactor pressure vessel beltline weld
In order to examine the attenuation of radiation damage through the thickness of an irradiated reactor pressure vessel (RPV), four segments were acquired from the Zion Unit 1 power plant RPV after the plant was decommissioned. The Zion Unit 1 RPV Beltline Weld Segment 1 was cut into seven blocks, consisting of five base metal and two beltline welds from the high fluence region of the segment. Through-wall test specimens were machined and tested. Specimens included those used for Charpy impact, Master Curve fracture toughness testing, and chemical analysis. The observed through-thickness ductile-to-brittle transition temperatures in the beltline weld deviated significantly from the expected behavior based on the attenuation of fast fluence as a function of depth into the RPV. Beginning at the inside surface, the 41-J Charpy transition temperature was either flat or slightly increasing until the ¾ -T location. The results of a simple, model-based analysis of the Zion beltline weld material that included the irradiation conditions and material chemistry were generally consistent with industry trend curves and the standard attenuation model, rather than the observed data. Although there was no archive material from the RPV available to permit measurement of the unirradiated properties, fracture toughness specimens fabricated from archive surveillance weld were used to obtain an estimate of the initial through-thickness values of the Charpy transition temperature. The Charpy shifts obtained using this approach were similarly in disagreement with the predictions of the US NRC Regulatory Guide 1.99, Rev. 2. However, testing of irradiated Charpy specimens taken from the RPV following post-irradiation annealing (10 hr. at 500 °C) provided a quite different estimate of the unirradiated properties which improved the agreement between the inferred through-thickness Charpy shifts and exponential attenuation model included in Regulatory Guide 1.99/2. In conclusion, the analysis of the Zion data and data obtained in previous post-mortem examinations of decommissioned RPVs indicates that more work is needed to understand the through-thickness properties of RPV materials in order to properly assess through-wall damage attenuation.
Charpy impact↗
Self-Learning Kinetic Monte Carlo Simulations of Radiation Damage in Nuclear Fuels
Understanding how irradiation affects the thermo-physical and mechanical properties of nuclear materials, such as thermal conductivity degradation in fuels and embrittlement of structural components, is critical to the safety and efficiency of nuclear reactors. These effects are largely governed by the formation and evolution of atomic-scale point defects and defect clusters. Due to their small sizes, however, these defects are invisible under high-resolution scanning transmission electron microscopy. This project aims to fill this experimental knowledge gap by integrating density functional theory (DFT), machine learning interatomic potential (MLIP), and kinetic Monte Carlo (KMC) techniques to predict longtime evolution of irradiation-induced defects in nuclear fuels.
36 - MATERIALS SCIENCE↗
Radiation damage study of POCO ZXF-5Q graphite for neutrino production targets using 4.5 MeV helium ions
To address the challenges of increased beam power and target survivability associated with next-generation particle production beam lines, high dose, high-energy proton beam conditions are simulated using irradiation from low-energy ion beams. A low-energy ion irradiation study of POCO ZXF-5Q graphite under conditions similar to those of the NuMI NT-02 neutrino production target at the Fermi National Accelerator Laboratory is reported. Helium ion irradiation was performed at 100 ∘ C to a maximum damage level of 0.9 displacements per atom (DPA). Irradiation induced hardening, swelling of the irradiated region, inter-plane lattice expansion, and intraplane lattice contraction with increasing ion fluence was observed using micromechanical (nanoindentation, atomic force microscopy) and electron microscopy (high-resolution imaging, selected area diffraction) characterization. Similar changes were also observed in post irradiation examination of the NT-02 target indicating that ion irradiation can be a valuable tool for estimating radiation damage in proton beam targets. Caution must be exercised though, because the hardening, lattice alteration, and swelling occur to different magnitudes for a given damage level. The observed hardening and embrittlement were greater for ion irradiated graphite. For He ion irradiated samples the lattice spacing changes were smaller at low damage levels (78% less expansion and 71% less contraction at 0.1 DPA) and larger at high damage levels (38% more expansion and 5% more contraction at 0.9 DPA) relative to that observed in the NT-02 target. The magnitude of swelling was 8.5× greater under ion irradiation which is influenced by the differing damage gradients and inclusion of implanted He ions in the region of interest.
43 PARTICLE ACCELERATORS↗
A concurrent irradiation-mechanics multiscale coupling model
The vast majority of our current knowledge regarding the basic mechanisms controlling irradiation effect on mechanical properties is based almost entirely on the results of post-irradiation experiments or theoretical models. However, the concurrent effects of irradiation, mechanical stress, and thermal damage on the failure phenomena of materials and components remain largely unexplored due to its internal multiscale-multiphysics coupling nature. Here, we present here a concurrent irradiation-mechanics multiscale coupling model. The concurrent evolutions of nanoscale irradiation defect clusters, microscale dislocation configurations, and mechanical responses are well captured based on coupling cluster dynamics, discrete dislocation dynamics, and the finite element methods using an effective time marching scheme. Model predictions of defect densities and size are in general agreement with experimental observations. Irradiation hardening is shown to take place also in samples undergoing concurrent irradiation-mechanical loading, similar to samples tested post-irradiation. However, the occurrence of plastic flow localization and dislocation channel formation is not accompanied with apparent yield drop (softening) under concurrent irradiation-mechanical loading conditions, which is different from the post-irradiation case.
42 ENGINEERING↗
Evidence of Morphological Change in Sulfur Cathodes upon Irradiation by Synchrotron X-rays
While the development of lithium–sulfur battery cathodes has benefited substantially from the use of in situ and ex situ X-ray absorption studies, the degree of undesired influence from synchrotron radiation has not been studied. In this study, we present evidence of severe beam damage on sulfur cathodes under irradiation by synchrotron X-rays. Specifically, X-ray fluorescence mapping with relatively low dosage was conducted to observe the morphological changes after conducting X-ray absorption spectroscopy (XAS). Under open-circuit conditions, the morphology of the sulfur spontaneously changes and tends to migrate out of the region of XAS sampling. Our work indicates that effort should be placed in first obtaining a no-change/stable open-circuit baseline when attempting to conduct in operando studies of lithium–sulfur batteries using synchrotron radiation with an energy of <7.7 keV and a flux of >6 × 10 12 photons s –1 .
25 ENERGY STORAGE↗
Effects of radiation damage and precipitate distribution on micro-pillar compression testing of irradiated CuCrZr
The results of small-scale mechanical tests are convoluted by the so-called size effect, whereby materials appear stronger when the scale of the test is reduced to the order of microns or less. The dimensional range over which this occurs has been shown to be linked to a change in sample microstructure, such as the addition of defects induced by irradiation. To investigate this response, a CuCrZr alloy was subjected to proton irradiation and mechanically tested using micro compression of pillars with a range in size. It was found that irradiation defects dominate over the extrinsic size effect and the sensitivity to differences in precipitate microstructure was also somewhat reduced, suggesting that size-independent results could be obtained from much smaller test volumes in irradiated material compared to their non-irradiated counterparts. Lastly, comparison was made between the increase in yield strength predicted by models and the experimentally measured values to establish the key parameters driving the strengthening behaviour.
36 MATERIALS SCIENCE↗
Positron Emission Tomography Imaging of Functional Transforming Growth Factor β (TGFβ) Activity and Benefit of TGFβ Inhibition in Irradiated Intracranial Tumors
Transforming growth factor β (TGFβ) promotes cell survival by endorsing DNA damage repair and mediates an immunosuppressive tumor microenvironment. Thus, TGFβ activation in response to radiation therapy is potentially targetable because it opposes therapeutic control. Strategies to assess this potential in the clinic are needed.
62 RADIOLOGY AND NUCLEAR MEDICINE↗
Assessment of thermal and radiation induced creep in the dual cooled lead lithium blanket
The creep in recently designed blanket for the fusion nuclear science facility is described by decomposing it into thermal, irradiation and cavity swelling creep. Initial estimates of thermal creep using elastic high temperature rules showed that the recent heat transfer improvements at the first wall (FW) is feasible, and the FW can withstand heat flux of 0.35 MW/m 2 at 3000 hrs without rupture. A viscoplastic model that is based on Norton's power law and relies on Multiphysics coupling of solid mechanics and heat transfer modules is used to capture the inelastic deformation in the blanket. Results showed that the design peak heat flux of 0.25 MW/m 2 produced maximum thermal creep strain of 0.45 % and the relaxation of the thermal stress at the FW. Irradiation creep is prescribed to be proportional to the displacement damage dose and applied stress. The displacements from irradiation creep radially decrease from the FW to the back wall, but the maximum deformation is found at the back wall that is connected to the Helium manifold due to the high stresses at the region. In conclusion, cavity swelling creep is dominant at steady state and combined with radiation creep to produce displacement of about 8 mm at the FW.
70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
Fusion Materials Semiannual Progress Report for the Period Ending December 31, 2020
Three ferritic/martensitic alloys; F82H, Fe8Cr2W and CNA3 were studied for the effect of H and He on swelling. Single ion beam (Fe 2+ ), dual ion beam (Fe 2+ +He 2+ ), and triple ion beam (Fe 2+ +He 2+ +H + ) irradiations were conducted at 500°C to a damage level of 50 dpa and dual and triple beam irradiation experiments were conducted at 450°C to 50 dpa. Cavity distribution and swelling were comparable in dual ion beam and triple ion beam irradiated F82H at 500°C, indicating that the role of hydrogen in swelling in triple beam irradiated F82H appeared to be insignificant compared to the role of helium. Swelling in Fe8Cr2W and CNA3 at 500°C was approximately 3-4X greater than that at 450°C. In F82H, the average cavity size and swelling were minimally larger at 500°C than at 450°C. The significant role of hydrogen in swelling has yet to be confirmed. Future efforts will focus on separate effects experiments to understand the role of hydrogen in cavity swelling.
70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗