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DOE OSTI2021

Neutron Irradiation Induced Changes in Isotopic Abundance of 6Li and 3D Nanoscale Distribution of Tritium in LiAlO2 Pellets Analyzed by Atom Probe Tomography

Tritium, a radioactive isotope of hydrogen is produced by neutron irradiation of 6Li enriched LiAlO2 pellets in Tritium producing burnable absorber rods (TPBARs). Three-dimensional nanoscale mapping of Tritium in irradiated pellets is critical to understand its spatial variation and its association with various microstructural features in the pellets. Spatially resolved analysis of 6Li isotopic enrichment in such ceramic pellets before and after irradiation can provide insights to heterogeneities in Li isotopic distribution. However, Li being a light isotope, its spatially resolved compositional or isotopic analysis is a challenging task to most analytical methods. Here we used atom probe tomography, to evaluate the Li isotopic enrichment in both the LiAlO¬2 matrix and the Li deficient secondary phase LiAl5O8 before irradiation. These results were then compared with 6Li isotopic ratio measured by APT analysis of neutron irradiated pellets to clearly demonstrate the unique capability of APT to quantitatively analyze the isotopic enrichment of 6Li as well as for other light elements present in these materials. Evidence for heterogenous nanoscale distribution of 3H and O3H within irradiated pellet microstructure is also provided, which is attributed to 3H trapping in irradiation induced vacancy clusters or voids within the LiAlO2 matrix. The characterization results given here, now prove the feasibility for using APT for analyzing nanoscale spatially resolved isotopic enrichment of Li as well as other light elements such as Tritium in TPBARs. This work also paves way to adopt APT for analyzing light elements such as Li and tritium in materials used for nuclear fusion reactor applications, geochemistry, astrophysics as well as for energy storage applications.

Devaraj, Arun↗

DOE OSTI2026

Hoop Tensile Failure Stress of 500 µm-Diameter Ceramic Spheres

The tensile failure stress of a brittle-material sphere is important to the survival of the sphere itself but is particularly relevant to systems that employ such spheres for applications in which the sphere exterior is subjected to tension during system fabrication or operation. That maximum hoop or tangential stress can be measured by diametrally compressing a C-sphere specimen directly machined from such spheres. This combination of specimen geometry and test method was conceived at Oak Ridge National Laboratory around 20 years ago. Although the C-sphere geometry has been tested with larger spheres, the ease and efficacy of its testing are unknown for submillimeter sphere diameters. To consider this, C-sphere specimens were machined from yttria-stabilized zirconia (YSZ) spheres of ∼500 µm diameter. The maximum (hoop or tangential) tensile stress was determined as a function of compressive failure force and specimen dimensions using finite element analysis. Companion effective area and volume as a function of Weibull modulus were computed. Hoop tensile failure stresses were then measured and fractography conducted to examine flaw type and location and to estimate the mirror constant of this YSZ grade. This novel study demonstrates that hoop tensile failure stress can be determined with sub-millimeter brittle-material spheres.

Delia, Daniel [ORNL] (ORCID:0000000209023239)↗

DOE OSTI2021

Room temperature facile synthesis of olivine-Co 2 SiO 4 nanoparticles utilizing a mechanochemical method

Co 2 SiO 4 is a ceramic pigment and promising battery material of significant technological interest, as well as a model end-member of one of the most important mineral families in the Earth's crust and upper mantle. All previously developed methods for synthesis of Co 2 SiO 4 require high-temperature processing, which promotes grain growth, while the nanocrystalline form is required for some important technological applications. Here, we report a successful method for synthesizing nanocrystalline Co 2 SiO 4 via a simple and inexpensive high-energy ball milling mechanochemical process. Products of the synthesis were characterized by a combination of XRD and TEM, and their crystal structures and elemental compositions are reported.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

On Uranium-Zirconium Carbonitride Formation by Direct Casting - A Novel Synthesis Study

UZrCN has exhibited thermophysical properties beneficial to high temperature reactor applications such as nuclear thermal rockets. The present work investigates a novel liquid phase synthesis method involving the admission of nitrogen gas during arc melting of uranium, zirconium, and carbon. Initial microstructural examinations using SEM indicated that the samples remain heterogenous with zirconium-rich cores in a uranium-rich matrix. Heterogeneity resulted from large differences in melting temperature of the major constituents and rapid solidification. Additional EDS, combustion analysis, and inert gas fusion analysis proved that the core regions have both uranium and zirconium and establish that carbon and nitrogen are retained during the fabrication process. XRD clarifies that the light elements did not form compounds with the uranium matrix but rather incorporated into the core region forming a sub-stoichiometric UZrCN. Heat treatment performed on equimolar U-Zr-C resulted in an increase in the homogenous phase present with an XRD pattern reflecting a ternary UZrCN despite small amounts of segregation in the final button.

36 - MATERIALS SCIENCE↗

DOE OSTI2022

A unified finite strain gradient-enhanced micropolar continuum approach for modeling quasi-brittle failure of cohesive-frictional materials

Here, in this work, a novel framework for modeling quasi-brittle crack propagation and shear band dominated failure of cohesive-frictional materials like concrete, mortar, rock, tough ceramics, energetic materials, but also granular materials like sands or powders in terms of a unified continuum approach is proposed. It is based on a combination of the gradient-enhanced continuum with gradients of internal variables for representing quasi-brittle cracking, and the micropolar continuum, accounting for the deformation of the microstructure. For developing the gradient-enhanced micropolar framework, the set of balance equations and the kinematic relations are derived, and the constitutive relations are established in a general manner. The framework is formulated in a geometrically exact setting, based on the thermodynamically sound theory of hyperelasto-plasticity, and the numerical implementation by means of the finite element method is discussed. For assessing the approach, realizations of this new approach in terms of constitutive models for particular materials are developed. They are applied to numerical benchmark examples, investigating various loading conditions, and the obtained results are validated by means of a comparison with experiments from the literature.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Evaluation of Additively Manufactured Monolithic SiC and SiC-Matrix Ceramic Matrix Composites for Concentrating Solar Receiver Applications - Fabrication and Testing of Receiver Design Feature Specimens in a Simulating Lab Test via Laser Heating

Increasing operating temperatures of solar receivers is paramount to the efficiency of concentrated solar thermal (CST) and solar power (CSP) systems. Owing to its high temperature stability combined with excellent thermal and optical properties, SiC has been the material of choice for application in high-temperature solar receivers. We report the results of our study of the effective heat transfer characteristics of several candidate SiC structure motifs, or feature geometries, which are fabricated via additive manufacturing. The SiC structure motifs studied include different permutations of three-dimensional periodic lattices and defined shapes. A solar-thermal simulating laboratory test setup is constructed using a 4kW CO2 laser system with beam shaping optics to apply concurrent radiative heating power on one face of 2”-diameter cylindrical feature specimens, representing the structure motifs of interest for receiver element design, while flowing through the sample as heat transfer fluid. Using the test setup, simulative test conditions representative of a concentrated solar flux of up to ~2000 suns could be achieved in the lab tests under varying air flow through the test structure. A simple 1D numerical analysis scheme is developed to extract an effective or compound heat transfer coefficient representative of the test structure under steady-state heat flow conditions. The test results and their use to guide the selection and optimization of SiC material and structure motifs for the receiver element design fabrication are discussed.

14 SOLAR ENERGY↗

DOE OSTI2024

Predicting non-linear stress–strain response of mesostructured cellular materials using supervised autoencoder

Recent breakthroughs in advanced manufacturing capabilities have made it possible to design and print sophisticated topologies of cellular structures using diverse engineering materials such as metals, polymers, and ceramics. In these architectured materials, it is often desirable to tailor the mechanical properties by altering the unit cell topology. This necessitates an in-depth understanding of how the topology of the unit cell structure affects the macroscopic behavior of the material in both the linear and the non-linear regimes encountered under large compression. Here, we have developed a machine learning (ML) approach capable of accelerating the prediction of the stress–strain response of a polymer-based cellular structure under uniaxial confined compression. As part of generating the training data for ML, 60,000 mesostructures were generated using a relatively novel approach based on cellular automata, and their corresponding stress–strain responses were obtained from the finite element simulations. Principal component analysis (PCA) was used to reduce the dimensionality of the stress–strain curves. With only 20 principal components, PCA captured 99.89% of the variance in the stress–strain curves while reducing the dimensionality by 5X. ML using supervised autoencoder was able to successfully speed up the prediction of the non-linear stress–strain response of a unit cell by up to 4600X. The proposed method can serve as an efficient data generation tool and a rapid means for predicting the structure–property relationship through accelerated forward modeling of cellular materials under compaction, in cases where the macroscopic stress–strain response is governed by the unit-cell topology.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Development of New Magnetron Sputter Deposition Processes for Laser Target Fabrication

Magnetron sputter deposition is an enabling technology for laser target fabrication. Solutions are readily available for the deposition of most sub-micron-thick elemental films on planar substrates. However, major challenges still remain for the development of robust deposition processes in regimes of ultrathick (over ~10 μm) coatings and nonplanar substrates. These challenging deposition regimes are directly relevant to laser target applications, including both sphero-cylindrical hohlraums and spherical ablators for inertial confinement fusion (ICF) targets. Understanding underlying physical mechanisms for a specific material system is crucial for process development, given the overall complexity of the deposition process, its nonlinear dependence on deposition parameters, and a very large process space, often precluding conventional process optimization approaches. Here, we describe our approach to developing new deposition processes and give practical advice with examples of new results from our ongoing studies of glassy boron carbide ceramics for next-generation ICF ablators and nonequilibrium gold-tantalum alloys for hohlraums for magnetized ICF schemes. Emphasis is given to two major challenges of ultrathick coatings related to achieving process stability and reducing residual stress.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Synergic grain boundary segregation and precipitation in W- and W-Mo-containing high-entropy borides

The structures of W- and W-Mo-containing high-entropy borides (HEBs) are systematically studied by combining atomic-resolution transmission electron microscopy imaging, electron diffraction, and chemical analysis. Here, we reveal that W or W-Mo addition in HEBs leads to segregation of these elements to the grain boundaries (GBs). In the meantime, W- or W-Mo-rich precipitates also form along the GBs. Crystallographic analysis and atomic-scale imaging show that the GB precipitates in both W- and W-Mo-containing HEBs have a cube-on-cube orientation relationship with the matrix. With further strain analysis, the coherency of the precipitate/matrix interface is validated. Nanoindentation tests show that the simultaneous GB segregation and coherent precipitation, as a supplement to the grain hardening, provide additional hardening of the HEBs. Our work provides an in-depth understanding of the GB segregation and precipitation behaviors of HEBs. It suggests that GB engineering could be potentially used for optimizing the performance of high-entropy ceramics.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2025

Optimization of overhang printing in ceramic binder jetting additive manufacturing

Cylindrical-shaped horizontally-hanging overhangs with different heights on a solid cubic body were printed via binder jetting additive manufacturing with sililcon carbide powder feedstock. Cracking on the overhang neck and sagging on the overhang body were observed both pre- and post-curing, especially on printed design with a smaller particle size of 10 μm. Here, it was found that the width of cracking and depth of sagging were dependent on the height relative to the solid body in the powder bed, and elevated position of overhang with large volume of underneath loose powder led to increased extend of cracking and sagging. Overhang diameter and weight were varied, which were found with no apparent effects on its deformation extend. To mitigate cracking and sagging, contactless support was designed and tested, which could significantly improve the overhang stability and avoid any overhang deformations. Support gap and support distance were studied for their effects on support capability. The printing processes with and without contactless support were simulated by a finite element modeling approach to understand the stress distribution and evolution of the overhang structures, which revealed stress concentrations on the upper neck point of the designed overhang.

Binder jetting↗

DOE OSTI2020

A thermodynamics-based damage model for the non-linear mechanical behavior of SiC/SiC ceramic matrix composites in irradiation and thermal environments

A damage model is developed and validated with experimental data for the non-linear mechanical behavior of SiC/SiC composite materials in nuclear applications. Cyclic thermal and mechanical loading associated with neutron irradiation effects of these composites leads to wide-spread and progressive micro-cracking that leads to loss of thermal conductivity and further enhancement of thermo-mechanical damage. A physics-based model of wide-spread micro-cracking is developed within the thermodynamic framework of continuum damage mechanics. Evolution equations for damage parameters that describe the growth of continuum damage are developed, where the material variables are obtained from experiments. The model novelty is in coupling mechanical, thermal, and irradiation damage through a consistent thermodynamic framework, including loss of thermal conductivity due to the evolution of mechanically induced micro-cracks. A number of thermo-mechanical experiments were conducted to confirm model assumptions. The model is shown to be validated with out-of-pile experiments, and then implemented using commercial finite element code COMSOL to the fuel cladding problem with normal and high radiation dose cases.

Materials Science↗

DOE OSTI2020

Corrosion interactions between stainless steel and lead vanado-iodoapatite nuclear waste form part II

This paper studied the release of iodine from lead vanado-iodoapatite (I-APT, Pb 9.85 (VO 4 ) 6 I 1.7 ), a potential nuclear waste form for the radioactive waste element of I-129, which can be enhanced when crevice corrosion of stainless steel (SS) occurring nearby. Reference corrosion studies of I-APT were performed in different bulk solutions including DI water, 0.6 M and 6 M NaCl, and 0.1 M HNO 3 without metal crevice corrosion interactions. The localized enrichment of Cl – , one of the major consequences of SS crevice corrosion, was found to be the decisive factor that led to the enhanced release of iodine. A surface alteration layer consisting of a mixture of nanocrystalline I-APT and Cl-rich apatite (Cl-APT) formed on I-APT surface. Meanwhile, large Cl-APT crystals formed at the crevice mouth on the I-APT surface. This study reveals a new near-field corrosion mechanism for ceramic waste forms when they are exposed to aggressive local corrosive conditions created by the electrochemical reactions of nearby metals. The insight gained in this study could be beneficial for a more accurate prediction of waste form degradation.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Reactive flash sintering and characterization of bulk high entropy nitrides

Over the past decade, numerous high-entropy ceramics have been synthesized, often displaying attractive properties. However, the study on facile preparation of bulk high entropy nitrides (HEN) are limited, despite its broad potential applications. This research demonstrates for the first time rapid fabrication (within ∼6 min) of bulk high-entropy nitrides, especially (Al 0.17 Nb 0.17 Ta 0.17 Ti 0.32 Zr 0.17 )N, from binary nitride powder mixtures using a highly efficient reactive flash sintering (RFS) technique. X-ray diffraction (XRD) shows the HENs from RFS are near single-phase solid solutions with a rock salt crystal structure, while in situ synchrotron study carried out during RFS captured in real time the formation of HEN, which was preserved upon cooling, suggesting thermodynamic stability of the HEN phase, even up to extreme pressure (∼35.6 GPa). Microscopic analyses using SEM, STEM, and EDS reveal decent uniformity for HEN with no obvious segregation of elements, even to submicron scale. Some properties of the obtained bulk HENs are consistent with expectations. For example, their hardness and bulk modulus are close to estimates based on rule-of-mixture (ROM) values from the constituent binary nitrides. Meanwhile, some other measured properties seem to show surprises. For example, the fracture toughness for the HENs (e.g., 7.81 ± 1.40 MPa•m 1/2 or higher) turns out to be more than double of the expected ROM estimates. The significantly improved fracture toughness is attributed to the observed nano-layered structure of the HENs, despite the HEN’s cubic crystal structure and high hardness. In addition, the oxidation resistance shows improvement up till ∼800°C, possibly due to Ta doping that suppress oxygen vacancy formation in the oxide shell, while the 5-metal HEN of (Al 0.17 Nb 0.17 Ta 0.17 Ti 0.32 Zr 0.17 )N displays superconductivity (T c of ∼5–7 K from magnetism and resistivity measurements, slightly lower than ROM estimate), despite insulating property of starting AlN. Furthermore, future study combining experimental investigation using larger samples to confirm the observed increase in fracture toughness and oxidation resistance, theoretical modeling at different length scale, and more detailed structural/chemical characterization, especially at the atomic scale, are all needed to fully understand the inter-relationships between composition, processing, structure, and novel properties for these HENs and the development of related new materials for different applications.

Flash sintering↗

DOE OSTI2020

Mechanism-Based Energy Regularization in Computational Modeling of Quasibrittle Fracture

Abstract Quasibrittle materials are featured by a strain-softening constitutive behavior under many loading scenarios, which could eventually lead to localization instability. It has long been known that strain localization would result in spurious mesh sensitivity in finite element (FE) simulations. Previous studies have shown that, for the case of fully localized damage, the mesh sensitivity can be mitigated through energy regularization of the material constitutive law. However, depending on the loading configuration and structural geometry, quasibrittle structures could exhibit a complex damage process, which involves both localized and diffused damage patterns at different stages of loading. This study presents a generalized energy regularization method that considers the spatial and temporal evolution of damage pattern. The method introduces a localization parameter, which describes the local damage pattern. The localization parameter governs the energy regularization of the constitutive model, which captures the transition from diffused to localized damage during the failure process. The method is cast into an isotropic damage model, and is further extended to rate-dependent behavior. The energy regularization scheme is directly incorporated into the kinetics of damage growth. The model is applied to simulate static and dynamic failures of ceramic specimens. It is shown that the present model is able to effectively mitigate the spurious mesh sensitivity in FE simulations of both types of failure. The present analysis demonstrates the essential role of mechanism-based energy regularization of constitutive relation in FE simulations of quasibrittle fracture.

Mechanics↗

DOE OSTI2025

3D pore structure reconstruction of fluff region in top of EBR-II irradiated fuel by X-ray micro-computed tomography

Metallic fuels comprised of U-Zr binary and U-Pu-Zr ternary alloys are a promising fuel candidate for sodium-cooled fast reactors and possess many advantages over ceramic fuels such as higher uranium density and improved thermal conductivity. Fluff is a highly porous structure forming at the top of metallic fuel slugs during irradiation and was extensively observed in past sodium-cooled fast reactor (SFR) experiments such as Idaho National Laboratory’s Experimental Breeder Reactor II (EBR-II). Previous investigations have shown that fluff is rich in fissile atoms and hence could have neutronics implications, but its formation mechanisms are not understood. In this work, two cube-shaped lift outs were taken from the fluff and bulk fuel regions of a high burnup U-19Pu-10Zr composition EBR-II fuel slug and characterized by micro computed tomography (Micro-CT) and energy dispersive x-ray spectroscopy (EDS). This was used to characterize differences in microscale porosity and composition between fluff and bulk fuel, and to support or oppose postulated fluff formation mechanisms. Surface EDS showed minimal differences between the elemental compositions of the fluff and fuel cubes. However, three-dimensional (3D) pore analysis from the tomography scans showed significant differences between the fluff and fuel cube pore size distributions at the microscale level. The high porosity and irregular pore distribution seen in macroscale fluff was also present within the micro-scale fluff cube, having a much higher porosity than the fuel cube which was concentrated in a few large pore networks. In conclusion, these results indicate support for a creep driven mechanism of fluff formation.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

High-Efficiency and Low-Carbon Energy Storage and Power Generation System for Electric Aviation

This report summarizes the work performed by University of California San Diego (UCSD) – Honeywell Aerospace (Honeywell) team for the U.S. Department of Energy/Advanced Research Projects Agency-Energy (DOE/ARPA-E) under Phase 1 (April 2021 – October 2023) project, Cooperative Agreement DE-AR0001347 entitled “High-Efficiency and Low-Carbon Energy Storage and Power Generation System for Electric Aviation”. The main objective of this project is to develop and demonstrate an energy storage and power generation (ESPG) system operating on bio liquid natural gas (LNG) for electric aviation applications. The ESPG system concept in this project is a fuel cell, battery, and gas turbine hybrid system that incorporates an innovative solid oxide fuel cell (SOFC) technology. This SOFC technology has two main novel elements: (i) a lightweight and compact stack architecture that consists of cells and cell modules in electrical parallel and series connections (the module design) and (ii) exceptionally high performance, direct methane thin-film cells on porous substrate made by sputtering deposition process. This fuel cell has the specific power and volumetric power density suitable for electric aviation applications. Based on the current status of the SOFC technology, the Phase 1 work focused on the following activities: (i) ESPG System Modeling – to design and optimize an aircraft SOFC-based ESPG system concept that met the performance, weight and cost targets; (ii) Cell Material Development and Scaleup – to demonstrate scalability of the sputtering process for manufacture of thin-film SOFC cells of practical sizes, confirm the exceptional performance of sputtered cells, improve cell stability and durability for operation with hydrogen and methane fuel, and develop a suitable electrically conducting porous substrate to replace the current non-conducting ceramic substrate; (iii) Stack Development – to design and manufacture stack components for the stack architecture, evaluate and select a suitable sealant, and build and operate multi-cell stacks to demonstrate stack operation, and (iv) Technology to Market – to develop business models and commercialization plans, conduct various market and technology analysis and estimate SOFC and ESPG system costs.

25 ENERGY STORAGE↗

DOE OSTI2021

Immobilization of cesium and iodine into Cs 3 Bi 2 I 9 perovskite-silica composites and core-shell waste forms with high waste loadings and chemical durability

Cs$_3$Bi$_2$I$_9$, a defect perovskite derivative, is a potential host phase to immobilize iodine and cesium with high waste loadings. In this work, two strategies were explored to form Cs$_3$Bi$_2$I$_9$-silica composites and a core-shell structure in order to improve chemical durability of waste form materials meanwhile maintaining high waste loadings. Cs$_3$Bi$_2$I$_9$ loadings as high as 70 wt.% were incorporated into a silica matrix to form silica-ceramic composites, and 20 wt.% Cs$_3$Bi$_2$I$_9$ was encapsulated into silica to form a core–shell structure by low temperature spark plasma sintering. Chemical durability of the composite and core-shell waste forms was evaluated by semi-dynamic leaching experiments, and Cs and I were incongruently released from waste form matrices. A BiOI alteration layer formed, acting as a passivation layer to reduce the release of radionuclides. The long-term iodine release rate was low (30 mg m$^{-2}$ day$^{-1}$) for the 70 wt.%Cs$_3$Bi$_2$I$_9$–silica composite leached in deionized water at 90 °C, which can be further reduced to 5 × 10$^{-3}$ mg m$^{-2}$ day$^{-1}$ for the 20 wt.% core-shell structure. This work highlights a robust way to immobilize the highly mobile radionuclides with high waste loadings through encapsulation into durable matrices and a surface passivating mechanism that can greatly reduce the elemental transport from waste form materials and significantly enhance their chemical durability.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Stresses within rare-earth doped yttria-stabilized zirconia thermal barrier coatings from in-situ synchrotron X-ray diffraction at high temperatures

There is a growing interest for smart coatings that can be integrated into turbine engines for in-situ temperature measurements or health monitoring. The addition of rare-earth dopants into standard thermal barrier ceramic top coat materials is used to obtain luminescent coatings that enable spectral measurements, for real-time temperature or health monitoring. The thermomechanical performance and durability of such novel coating compositions in extreme environments still remains to be evaluated. Consequently, the ability to manufacture sensor coatings which present suitable thermal properties needs to be demonstrated. For this study, highly luminescent erbium and europium doped yttria-stabilized zirconia and state-of-the-art yttria-stabilized zirconia coatings manufactured by air plasma spray were characterized to determine the effects of the embedded rareearth dopants on coating internal strain and stress and to quantify and compare their high temperature response using synchrotron X-ray diffraction. In-situ depth-resolved strain measurements were performed at 15 μm intervals along the depth of the coatings to evaluate materials response at key locations, specifically at layer interfaces. In-plane stress was calculated for the coatings and a finite element model was implemented to supplement the results and enable further predictions. The results show that the sensor coatings that were manufactured in this work revealed only minor variations in the strain response of sensor coatings under a typical thermal cycle and especially at temperatures closer to that of gas turbine operating conditions, compared to state-of-the-art coatings. This work demonstrates the viability of manufacturing rare-earth doped yttria-stabilized zirconia coatings that provide beneficial spectroscopic monitoring capabilities while having minimal impact on the thermomechanical response of the thermal barrier coatings.

Air plasma spray↗