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At least 739 records · Page 41

Helium induced microstructure damage, nano-scale grain formation and helium retention behaviour of ZrC

Transition-metal ultra-high temperature ceramics are promising materials for nuclear structural applications. However, an understanding of their response to high-temperature irradiation and helium is vastly limited. This paper presents a study of helium effects in zirconium carbide (ZrC) by performing room temperature 3 MeV 3 He + ion irradiations up to 5 × 10 20 ions m –2 (~1.8 at.% at peak) and high-temperature annealing (1273–1873 K), coupled with state-of-art characterization using transmission electron microscopy (TEM), scanning electron microscopy (SEM) and nuclear reaction analysis (NRA). We reveal that ZrC is susceptible to irradiation damage in terms of helium bubble formation. After annealing at 1373 K, tiny bubbles (1–2 nm) formed aligned clusters which were highly over-pressurized, producing strain contrast in TEM. At 1773 K, significant bubble growth occurred. Additionally, at 1773 K, a combined TEM/SEM analysis revealed dramatic matrix damage due to helium-induced surface blistering. Underneath blister caps, the microstructure evolved into ultra-fine nano-scale grains similar to high burn-up structures observed in nuclear fuels, but consisting of numerous nano-cracks. We hypothesize that such structures are formed due to high gas pressure build-up and its subsequent release. This phenomenon initiated at the grain boundaries. Blister top surface consisted of inter-granular and trans-granular cracks. NRA depth profiling revealed that helium was present as double peaks with major portion lying at the end-of-the-range (EOR) and the rest as TEM invisible clusters in a shoulder extending to the surface. ZrC started releasing helium after 1373 K. As a result, helium release increased significantly at higher temperatures, with majority helium loss occurring from EOR rather than from near-surface regions.

36 MATERIALS SCIENCE↗

Nano-scale microstructure damage by neutron irradiations in a novel Boron-11 enriched TiB 2 ultra-high temperature ceramic

Ultra-high temperature transition-metal ceramics are potential candidates for fusion reactor structural and plasma-facing components. We reveal the irradiation damage microstructural phenomena in Boron-11 enriched titanium diboride (TiB 2 ) using mixed-spectrum neutron irradiations, combined with state-of-art characterization using transmission electron microscopy (TEM) and high resolution TEM. Irradiations were performed using High Flux Isotope Reactor at ~220 and 620 °C up to 2.4 x 10 25 n.m -2 (E > 0.1 MeV). The calculated dose including contribution from residual Boron-10 ( 10 B) transmutation recoils, was ~4.2 displacements per atom. TiB 2 is susceptible to irradiation damage in terms of dislocation loop formation, cavities and anisotropic swelling induced micro-cracking. At both 220 and 620 °C, TEM revealed dislocation loops on basal and prism planes, with nearly two orders of magnitude higher number density of prism-plane loops. HRTEM, electron diffraction and relrod imaging revealed additional defects on {10$ \overline{1}\ $0} planes, identified as faulted prism-plane dislocation loops. High defect cluster density on prism planes will induce a-lattice parameter swelling of TiB 2 , as reported in literature. This anisotropic lattice parameter swelling induced grain boundary micro-cracking, the extent of which decreased with increasing irradiation temperature. The dominance of irradiation defect clusters on prism planes is different than typical hexagonal ceramics where dislocation loops predominantly form on basal planes, causing c-lattice parameter swelling. Helium generation and temperature rise from the transmutation of residual 10 B resulted in matrix and grain boundary cavities for the irradiation at 620 °C. In conclusion, the study additionally signifies isotopic enrichment as a viable approach to produce transition-metal diborides for potential nuclear structural applications.

36 MATERIALS SCIENCE↗

A deep learning model for automatic analysis of cavities in irradiated materials

Transmission electron microscopy (TEM) is a commonly used technique in materials science for defect investigation. Quantitative analysis of defects is important for understanding the properties of a material, but manual analysis of TEM micrographs can be time-consuming and prone to error, especially when the defects have irregular shapes rather than spherical shapes. Many existing methods or deep learning models do not handle a wide range of sizes for the same object type within a single image. In this work, we present a framework that enables users to train an instance segmentation model called Mask R- CNN on any microstructure dataset, perform multi-detection on the same image at different scales, and obtain properties (e.g., size, area) of the objects based on the desired shape (e.g., circle, ellipse, rectangle). Additionally, we have developed a parallel detection module that uses multiple GPUs to increase the efficiency of the object detection process. We demonstrate the capabilities of our framework using a set of TEM images of cavities with different shapes, size distributions, and background contrasts. Finally, we show that the performance of our model in terms of density, size, and swelling of the cavities is comparable to the human average and that our model achieves the highest recall value compared to existing methods due to the use of image multi-rescaling.

36 MATERIALS SCIENCE↗

Structure of the pellet-cladding interaction layer of a high-burnup Zr-Nb-O nuclear fuel cladding

Here, structure of the pellet/cladding-interaction (PCI) layer of a high-burnup nuclear fuel with niobium-bearing cladding was investigated using modern transmission electron microscopy (TEM) techniques. Morphology of the PCI consisted of uniform zirconia layer on the cladding side and finger-like features towards to the ceramic fuel. The PCI layer showed a complex microstructure that constitutes three distinct zirconia layers formed by two zirconia phases. From cladding to fuel, monoclinic, tetragonal, and another tetragonal phase were determined via TEM diffraction patterns and precession electron diffraction (PED) using ASTAR microscopy platform (AMP). Characterizations showed that monoclinic and tetragonal phases close to the cladding were crack-free, but the tetragonal layer adjacent to the fuel contained cracks and pores. Presence of the monoclinic layer suggested that its formation involved the gaseous diffusion of oxygen below threshold dose of fission product damage before the fuel/cladding contact occurred. Furthermore, high-resolution TEM revealed compound phase of (U,Zr)O 2 at fringes of zirconia fingers on the fuel side.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Precession electron diffraction for SiC grain boundary characterization in unirradiated TRISO fuel

Precession electron diffraction (PED), a transmission electron microscopy-based technique, has been evaluated for the suitability for evaluating grain boundary character in the SiC layer of tristructural isotropic (TRISO) fuel. Although the ultimate goal is to determine the grain boundary characteristics of fission product containing grain boundaries of neutron irradiated SiC, our work reports the effect of transmission electron microscope (TEM) lamella thickness on quality of data and establishes a baseline comparison on grain boundary characteristics determined previously using a conventional EBSD scanning electron microscope (SEM) based technique. In general, it was determined that the lamella thickness produced using the standard FIB fabrication process, is sufficient to provide reliable PED measurements with thicker lamellae (~120 nm) produce higher quality orientation data. Analysis of grain boundary character from the TEM-based PED data showed a much lower fraction of low angle grain boundaries compared to SEM-based EBSD data from the SiC layer of the same TRISO-coated particle as well as a SiC layer deposited at a slightly lower temperature. The fractions of high angle and CSL-related grain boundaries determined by PED are similar to those found using SEM-based EBSD. Since the grain size of the SiC layer of TRSIO fuel can be as small as 250 nm [12], depending on the fabrication parameters, and grain boundary fission product precipitates can be nano-sized, the TEM-based PED orientation data collection method is preferred to determine an accurate representation of the relative fractions of low angle, high angle and CSL-related grain boundaries. It was concluded that although the resolution of the PED data is better by more than an order of magnitude, data acquisition times may be significantly longer or the number of areas analyzed significantly larger than the SEM-based method to obtain a statistically relevant distribution. Also, grain size could be accurately determined but significantly larger analysis areas than those used in this study would be required.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Structural Complexities in Sodium Ion Conductive Antiperovskite Revealed by Cryogenic Transmission Electron Microscopy

Here we use low-dose cryogenic transmission electron microscopy (cryo-TEM) to investigate the atomic-scale structure of antiperovskite Na 2 NH 2 BH 4 crystals by preserving the room-temperature cubic phase and carefully monitoring the electron dose. Via quantitative analysis of electron beam damage using selected area electron diffraction, we find cryogenic imaging provides 6-fold improvement in beam stability for this solid electrolyte. Cryo-TEM images obtained from flat crystals revealed the presence of a new, long-range-ordered supercell with a cubic phase. The supercell exhibits doubled unit cell dimensions of 9.4 Å × 9.4 Å as compared to the cubic lattice structure revealed by X-ray crystallography of 4.7 Å × 4.7 Å. The comparison between the experimental image and simulated potential map indicates the origin of the supercell is a vacancy ordering of sodium atoms. This work demonstrates the potential of using cryo-TEM imaging to study the atomic-scale structure of air- and electron-beam-sensitive antiperovskite-type solid electrolytes.

36 MATERIALS SCIENCE↗

The Use of Graphene and Its Derivatives for Liquid-Phase Transmission Electron Microscopy of Radiation-Sensitive Specimens

We present that one of the key challenges facing liquid-phase transmission electron microscopy (TEM) of biological specimens has been the damaging effects of electron beam irradiation. The strongly ionizing electron beam is known to induce radiolysis of surrounding water molecules, leading to the formation of reactive radical species. In this study, we employ DNA-assembled Au nanoparticle superlattices (DNA-AuNP superlattices) as a model system to demonstrate that graphene and its derivatives can be used to mitigate electron beam-induced damage. We can image DNA-AuNP superlattices in their native saline environment when the liquid cell window material is graphene, but not when it is silicon nitride. In the latter case, initial dissociation of assembled AuNPs was followed by their random aggregation and etching. Using graphene-coated silicon nitride windows, we were able to replicate the observation of stable DNA-AuNP superlattices achieved with graphene liquid cells. We then carried out a correlative Raman spectroscopy and TEM study to compare the effect of electron beam irradiation on graphene with and without the presence of water and found that graphene reacts with the products of water radiolysis. We attribute the protective effect of graphene to its ability to efficiently scavenge reactive radical species, especially the hydroxyl radicals which are known to cause DNA strand breaks. We confirmed this by showing that stable DNA-AuNP assemblies can be imaged in silicon nitride liquid cells when graphene oxide and graphene quantum dots, which have also recently been reported as efficient radical scavengers, are added directly to the solution. Lastly, we anticipate that our study will open up more opportunities for studying biological specimens using liquid-phase TEM with the use of graphene and its derivatives as biocompatible radical scavengers to alleviate the effects of radiation damage.

36 MATERIALS SCIENCE↗

Characterizing the Three-Dimensional Structure of Block Copolymers via Sequential Infiltration Synthesis and Scanning Transmission Electron Tomography

Understanding and controlling the three-dimensional structure of block copolymer (BCP) thin films is critical for utilizing these materials for sub-20 nm nanopatterning in semiconductor devices, as well as in membranes and solar cell applications. Combining an atomic layer deposition (ALD) based technique for enhancing the contrast of BCPs in transmission electron microscopy (TEM) together with scanning TEM (STEM) tomography reveals and characterizes the three-dimensional structures of poly(styrene-block-methyl methacrylate) (PS-b-PMMA) thin films with great clarity. Sequential infiltration synthesis (SIS), a block-selective technique for growing inorganic materials in BCPs films in ALD, and an emerging tool for enhancing the etch contrast of BCPs, was harnessed to significantly enhance the high-angle scattering from the polar domains of BCP films in the TEM. The power of combining SIS and STEM tomography for three dimensional (3D) characterization of BCPs films was demonstrated with the following cases: self-assembled cylindrical, lamellar, and spherical PS-PMMA thin films. In all cases, STEM tomography has revealed 3D structures that were hidden underneath the surface, including: 1) the 3D structure of defects in cylindrical and lamellar phases, 2) non-perpendicular 3D surface of grain boundaries in the cylindrical phase, and 3) the 3D arrangement of spheres in body centered cubic (BCC) and hexagonal closed pack (HCP) morphologies in the spherical phase. The 3D data of the spherical morphologies was compared to coarse-grained simulations and assisted in validating the simulations’ parameters. STEM tomography of SIS-treated BCP films enables the characterization of the exact structure used for pattern transfer, and can lead to better understating of the physics which is utilized in BCP lithography.

Block copolymers↗

Dynamics of soft Nanomaterials captured by transmission electron microscopy in liquid water

In this paper we present in situ transmission electron microscopy (TEM) of soft, synthetic nanoparticles with a comparative analysis using conventional TEM methods. This comparison is made with the simple aim of describing what is an unprecedented example of in situ imaging by TEM. However, we contend the technique will quickly become essential in the characterization of analogous systems, especially where dynamics are of interest in the solvated state. In this case, particles were studied which were obtained from the direct polymerization of an oxaliplatin analog, designed for an ongoing program in novel chemotherapeutic delivery systems. The resulting nanoparticles provided sufficient contrast for facile imaging in situ, and point toward key design parameters that enable this new characterization approach for organic nanomaterials. We describe the preparation of the synthetic micellar nanoparticles to- gether with their characterization in liquid water.

Environmental Molecular Sciences Laboratory↗

Probing the Degradation Mechanisms in Electrolyte Solutions for Li-ion Batteries by In-Situ Transmission Electron Microscopy

One of the goals in the development of new battery technologies is to find new electrolytes with increased electrochemical stability. In-situ (scanning) transmission electron microscopy ((S)TEM) using an electrochemical fluid cell provides the ability to rapidly and directly characterize electrode/electrolyte interfacial reactions under battery relevant electrochemical conditions. Furthermore, as the electron beam itself causes a localized electrochemical reaction when it interacts with the electrolyte, the breakdown products that occur during the first stages of battery operation can potentially be simulated and characterized using a straightforward in-situ liquid stage (without electrochemical biasing capabilities). In this paper, we have studied the breakdown of a range of inorganic/salt complexes that are used in state-of-the-art Li-ion battery systems. The results of the in-situ (S)TEM experiments matches with previous stability tests performed during battery operation and the breakdown products and mechanisms are also consistent with known mechanisms. This analysis indicates that in-situ liquid stage (S)TEM observations can be used to directly test new electrolyte designs and provide structural insights into the origin of the solid electrolyte interphase (SEI) formation mechanism.

25 ENERGY STORAGE↗

Factors influencing quantitative liquid (scanning) transmission electron microscopy

One of the experimental challenges in the study of nanomaterials in liquids in the (scanning) transmission electron microscope ((S)TEM) is gaining quantitative information. A successful experiment in the fluid stage will depend upon the ability to plan for sensitive factors such as the electron dose applied, imaging mode, acceleration voltage, beam-induced solution chemistry changes, and the specifics of solution reactivity. In this paper, we make use of a visual approach to show the extent of damage of different instrumental and experimental factors in liquid samples imaged in the (S)TEM. Previous results as well as new insights are presented to create an overview of beam-sample interactions identified for changing imaging and experimental conditions. This work establishes procedures to understand the effect of the electron beam on a solution, provides information to allow for a deliberate choice of the optimal experimental conditions to enable quantification, and identifies the experimental factors that require further analysis for achieving fully quantitative results in the liquid (S)TEM.

(S)TEM↗

The structure and crystal chemistry of vernadite in ferromanganese crusts

The structure and crystal chemistry of vernadite in ferromanganese crusts from the Magellan Seamount in the north-west Pacific Ocean have been investigated using synchrotron X-ray diffraction (XRD), X-ray pair distribution function (PDF) and high-resolution transmission electron microscopy (TEM). XRD patterns of vernadite mainly show two strong diffraction peaks at 2.42–2.43 Å and 1.41 Å without or with a broad (001) diffraction peak, indicating thin layer nanophases along the c -direction. TEM images show flat and curved sheet-like nanocrystals with (001) layer thickness of ~7.2 Å and ~9.6 Å, and their interstratified structure. PDF patterns of the vernadite are similar to those from synthetic δ-MnO 2 and defective birnessite, suggesting a phyllomanganate framework. Combined XRD/PDF patterns suggest that vernadite in the outer part is associated with a higher density interlayer species at triple-edge sharing sites. The proportion of the 10 Å phase increases from the outer (young) part to the inner (old) part of the Mn crusts due to aging and sorption of Mn, Co and Ni from ambient seawater. This study suggests that this combined method of synchrotron radiation XRD/PDF and high-resolution TEM is a powerful tool to determine atomic structures of poorly crystallized nano-minerals. The mixture model of vernadite structure will help to understand the partitioning and distribution of trace elements in the ferromanganese crusts.

36 MATERIALS SCIENCE↗

A scalable multi-process model of root nitrogen uptake

This article is a Commentary on McMurtrie & Näsholm et al., 218: 119–130. Roots are represented in Terrestrial Ecosystem Models (TEMs) in much less detail than their equivalent above-ground resource acquisition organs – leaves. Often roots in TEMs are simply resource sinks, and below-ground resource acquisition is commonly simulated without any relationship to root dynamics at all, though there are exceptions (e.g. Zaehle & Friend, 2010). The representation of roots as carbon (C) and nitrogen (N) sinks without complementary source functions can lead to strange sensitivities in a model. For example, reducing root lifespans in the Community Land Model (version 4.5) increases plant production as N cycles more rapidly through the ecosystem without loss of plant function (D. M. Ricciuto, unpublished). The primary reasons for the poorer representation of roots compared with leaves in TEMs are three-fold: (1) data are much harder won, especially in the field; (2) no simple mechanistic models of root function are available; and (3) scaling root function from an individual root to a root system lags behind methods of scaling leaf function to a canopy. Here in this issue of New Phytologist, McMurtrie & Näsholm (pp. 119–130) develop a relatively simple model for root N uptake that mechanistically accounts for processes of N supply (mineralization and transport by diffusion and mass flow) and N demand (root uptake and microbial immobilization).

59 BASIC BIOLOGICAL SCIENCES↗

Sample Preparation and Experimental Design for In Situ Multi-Beam Transmission Electron Microscopy Irradiation Experiments

We discuss the need to understand materials exposed to overlapping extreme environments such as high temperature, radiation, or mechanical stress. When these stressors are combined there may be synergistic effects that enable unique microstructural evolution mechanisms to activate. Understanding of these mechanisms is necessary for the input and refinement of predictive models and critical for engineering of next generation materials. The basic physics and underlying mechanisms require advanced tools to be investigated. The in situ ion irradiation transmission electron microscope (I 3 TEM) is designed to explore these principles. To quantitatively probe the complex dynamic interactions in materials, careful preparation of samples and consideration of experimental design is required. Particular handling or preparation of samples can easily introduce damage or features that obfuscate the measurements. There is no one correct way to prepare a sample; however, many mistakes can be made. The most common errors and things to consider are highlighted within. The I 3 TEM has many adjustable variables and a large potential experimental space, therefore it is best to design experiments with a specific scientific question or questions in mind. Experiments have been performed on large number of sample geometries, material classes, and with many irradiation conditions. The following are a subset of examples that demonstrate unique in situ capabilities utilizing the I 3 TEM. Au nanoparticles prepared by drop casting have been used to investigate the effects of single ion strikes. Au thin films have been used in studies on the effects of multibeam irradiation on microstructure evolution. Zr films have been exposed to irradiation and mechanical tension to examine creep. Ag nanopillars were subjected to simultaneous high temperature, mechanical compression, and ion irradiation to study irradiation induced creep as well. These results impact fields including: structural materials, nuclear energy, energy storage, catalysis, and microelectronics in space environments.

47 OTHER INSTRUMENTATION↗

Biomass Burning Research Using DOE ARM Single-Particle Soot Photometer (SP2) Field Campaign Report

The focus of this laboratory study was to investigate the chemical and optical properties, and the detection efficiencies, of tar balls generated in the laboratory using the same instruments deployed on the U.S. Department of Energy (DOE) Atmospheric Radiation Measurement (ARM) Climate Research Facility Gulfstream-1 (G-1) aircraft during the 2013 Biomass Burning Observation Project (BBOP) field study, during which tar balls were observed in wildland biomass burning particulate emissions. Key goals of this laboratory study were: (a) measuring the chemical composition of tar balls to provide insights into the atmospheric processes that form (evaporation/oxidation) and modify them in biomass burning plumes, (b) identifying whether tar balls contain refractory black carbon, (c) determining the collection efficiencies of tar balls impacting on the 600oC heated tungsten vaporizer in the Aerodyne Soot Particle Aerosol Mass Spectrometer (SP-AMS) (i.e., given the observed low volatilities, AMS measurements might underestimate organic biomass burning plume loadings), and (d) measuring the wavelength-dependent, mass-specific absorption cross-sections of brown carbon components of tar balls. This project was funded primarily by the DOE Atmospheric System Research (ASR) program, and the ARM Facility made their single-particle soot photometer (SP2) available for September 1-September 31, 2016 in the Aerodyne laboratories. The ARM mentor (Dr. Sedlacek) requested no funds for mentorship or data reduction. All ARM SP2 data collected as part of this project are archived in the ARM Data Archive in accordance with established protocols. The main objectives of the ARM Biomass Burning Observation Period (BBOP, July-October, 2013) field campaign were to (1) assess the impact of wildland fires in the Pacific Northwest on climate, through near-field and regional intensive measurement campaigns, and (2) investigate agricultural burns to determine how those biomass burn plumes differ from those from wildland fires. During BBOP, tar balls, small solid particles of organic substances, were observed downwind from wildland fires (at plume ages of 0-3 hours), but not agricultural burns. Observations of the tar balls on transmission electron microscope (TEM) grids suggest that they formed during atmospheric transport, likely due to the same atmospheric processes that increased the oxidation levels of the organic aerosol. Preliminary analyses suggest that tar balls may account for almost 50% of the total particle number, and 30% of the total organic particle mass, of the aerosol emitted from the burning events. These BBOP observations are described in detail in a manuscript in preparation (Sedlacek et al., 2017). The current laboratory study lasted four weeks and was conducted in the aerosol laboratories located at Aerodyne Research, Inc. in Billerica, Massachusetts. Tar balls were generated from several different biomass fuels, including samples from BBOP-related field sites, following literature procedures (Hoffer, Tóth, Nyirö-Kósa, Pósfai, and Gelencsér, 2016; Tóth, Hoffer, Nyirö-Kósa, Pósfai, and Gelencsér, 2014), and they were characterized using the same equipment used during the 2013 BBOP study, specifically the SP-AMS, SP2 and TEM. This study determined that laboratory-generated tar balls (1) are refractory with respect to TEM analysis in a similar manner to those collected during BBOP from wildland fires, (2) are composed of organic material with some refractory carbon components, (3) can be measured quantitatively by the SP-AMS, strengthening observations during BBOP, (4) absorb visible light, and (4) are dominated by unsaturated hydrocarbons that may be responsible for their light-absorbing properties. The results from this project are already being incorporated into our analysis of the formation processes and emission rates of tar balls as a function of fuel and combustion conditions from wildland fires.

Aerodyne Soot Particle Aerosol Mass Spectrometer↗

Final Technical Report for the SciDAC Center for the Study of Plasma Microturbulence

This final technical report for the SciDAC Center for the Study of Plasma Microturbulence documents contributions from MIT to the project over the period of the award (February 15, 2011 to February 14, 2020). This project focused on the development of neoclassical and gyrokinetic simulation capabilities relevant for the description of particle, momentum and energy transport in tokamak fusion plasmas. Extensive validation against experimental results from Alcator C-Mod and DIII-D experiments was performed. Overall areas of emphasis included gyrokinetic simulations, experiments, and observation of density gradient driven Trapped Electron Mode (TEM) turbulence relevant to burning plasmas; theory and gyrokinetic simulations of the parametric variation of the nonlinear upshift of the TEM critical density gradient; identification of a new mechanism for the isotope effect due to density gradient driven TEM turbulence; new synthetic diagnostics based on full-wave simulations which enabled unprecedented agreement between gyrokinetic simulations and measured fluctuation spectra with and without strong electron heating; development of new continuum pedestal neoclassical and turbulence codes; formulation and implementation of the first gyrokinetic exact Fokker-Planck collision operator in gyrokinetic turbulence simulations; development of new spectral approaches in velocity space for highly efficient treatments of collisions; new model collision operators implemented in the discontinuous Galerkin gyrokinetic edge turbulence code GKEYLL; and a new model and spectral code to study the interaction of ion- and electron-scale turbulence, which will serve as an efficient test-bed for multi-rate and multi-scale methods. These fundamental advances contribute to the development of a validated, predictive capability for turbulent and collisional particle, momentum and energy transport in both the core and edge of magnetically confined fusion plasmas.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Advanced Electron Microscopy Characterization of the Fuel-Cladding Chemical Interaction Region in a High Burnup U-10Zr Fuel

To support the development of U-10Zr metallic fuel, advanced characterization techniques have been applied to the fuel-cladding chemical interaction (FCCI) region in a Na-bonded solid U-10Zr fuel cross-section that was irradiated to a burnup of ~13.1 at.% at the Fast Flux Test Facility. 17 phases were identified in the FCCI region through a combination of high-resolution scanning transmission electron microscopy (STEM), STEM based energy dispersive X-ray spectroscopy (STEM-EDS), and TEM based selective area electron diffraction (TEM-SAED) analysis. In this talk, we will also discuss the implications of results on metallic fuel FCCI by focusing on the formation of Zr rind, fission product migration, and HT-9 cladding integrality under the investigated thermal irradiation conditions. This work complements our previous study on the TEM characterization of the fuel region of this high burnup fuel sample and serves as scientific basis to support metallic fuel development and qualification.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗