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At least 811 records · Page 45

All sources NASA NTRS DOE OSTI

NASA NTRS2004

Joining and Assembly of Silicon Carbide-based Advanced Ceramics and Composites for High Temperature Applications

Silicon carbide based advanced ceramics and fiber reinforced composites are under active consideration for use in wide variety of high temperature applications within the aeronautics, space transportation, energy, and nuclear industries. The engineering designs of ceramic and composite component require fabrication and manufacturing of large and complex shaped parts of various thicknesses. In many instances, it is more economical to build up complex shapes by joining simple geometrical shapes. In addition these components have to be joined or assembled with metallic sub-components. Thus, joining and attachment have been recognized as enabling technologies for successful utilization of ceramic components in various demanding applications. In this presentation, various challenges and opportunities in design, fabrication, and testing o high temperature joints in ceramic matrix composites will be presented. Silicon carbide based advanced ceramics (CVD and hot pressed), and C/SiC and SiC/SiC composites, in different shapes and sizes, have been joined using an affordable, robust ceramic joining technology (ARCJoinT). Microstructure and high temperature mechanical properties of joints in silicon carbide ceramics and CVI and melt infiltrated SiC matrix composites will,be reported. Various joint design philosophies and design issues in joining of ceramics and composites well be discussed.

Singh, M.↗

DOE OSTI2022

In situ study on heavy ion irradiation induced microstructure evolution in single crystal Cu with nanovoids at elevated temperature

Understanding the response of nanovoids to irradiation damage advances our capability to design radiation tolerant materials. Recent in situ studies reveal the shrinkage of hexagon-shaped nanovoids in (110) textured Cu. However, the evolution of voids with irregular geometries under irradiation is less well understood. Here, in situ Kr ion irradiation was performed at 100 °C on single-crystal Cu (112) that possesses nanovoids with high aspect ratio. In situ studies show these elongated voids fragment into smaller voids and shrink gradually with increasing dose. Phase field simulations confirm that fragmentation of the void is governed by the competing kinetics between atoms diffusing toward and away from the elongated nanovoid. In conclusion, cost irradiation analysis reveals the formation of high-density defect clusters.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2026

Symposium MT02: Statistical Mechanics-Based Computational Tools for the Study of Phase Transformation in Complex Materials (Final Report)

Symposium MT02 brought together a diverse and interdisciplinary community of scientists specializing in Statistical Mechanics-based computational modeling to investigate phase transformations in materials exhibiting complex disordered structures. As the demand for materials with extreme performance metrics grows—from aerospace components to next-generation optical fibers—the ability to predict microstructural evolution under non-equilibrium conditions has become paramount. The primary goal of this symposium was to identify, evaluate, and discuss advanced computational tools capable of designing precise manufacturing conditions to tailor material properties efficiently. By fostering a dialogue between computational theorists and experimentalists, the symposium sought to establish new protocols for predicting how processing history—such as cooling rates or strain paths—dictates the final microstructure.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Synthesis, microstructure and micro-mechanical characterization of metal (Nb, Ti) – MAX phase (Ti 2 AlC) nanolaminates

We utilize elevated temperature physical vapor deposition (PVD) techniques to design metal/MAX multilayered nanocomposite thin films with alternating nanoscale metallic (Nb, Ti) and MAX phase (Ti 2 AlC) layer thicknesses. These metal/MAX nanolaminate architectures attempt to exploit a unique hierarchical topology – as interfaces between the layers are expected to be in direct competition with the internal interfaces within the MAX layers, to drive their tunable macroscopic mechanical behavior. Two metal/MAX nanolaminates – Nb/Ti 2 AlC and Ti/Ti 2 AlC – were deposited. The Nb/Ti 2 AlC metal/MAX system showed highly diffused layer interfaces with distinct Ti – rich and Nb–Al – rich layers, with the presence of MAX phase alongside TiC and other Ti–Al and Nb–Al intermetallic phases. The Nb/Ti 2 AlC system possessed a layered architecture, though the MAX phases were not found to be continuously present in each alternating layer. The second Ti/Ti 2 AlC system showed a non-lamellar nanocomposite microstructure and the formation of mixed Ti n+1 AlC n phases (a mix of n = 1, 2), and no indication of layering. Diffusion occurring between the metal/MAX layers in both cases, likely due to the elevated temperatures during the deposition process, is speculated as the likely cause of these resultant microstructures. The mechanical properties of both systems were evaluated using micromechanical (nanoindentation and micro-pillar compression) techniques, which demonstrated high strengths for both systems (Nb system: yield and instability strengths of 4.88 ± 0.1 GPa and 5.57 ± 0.03 GPa, Ti system: yield and instability strength of 5.61 ± 0.28 GPa and 6.21 ± 0.25 GPa). In conclusion, this work highlights the promising mechanical properties of metal/MAX multilayered depositions and summarizes the challenges in PVD synthesis of metal/MAX multilayered nanolaminates.

MAX phase↗

DOE OSTI2024

A mechanistic interpretation of Nelson curves for PVP failures under high temperature hydrogen attack

As an empirically established design criterion, Nelson curves that relate the service temperature and the allowable hydrogen partial pressure have been developed and utilized for more than sixty years in pressure vessels and piping (PVP) safety design. Despite a relatively clear thermodynamic understanding of the high-temperature-hydrogen-attack (HTHA) problem, the detailed fracture process on the microstructural length scales, however, remains elusive, and a quantitative assessment of the PVP lifetime under HTHA from the available creep fracture dataset is still not possible. This work develops a microstructure-informed and micromechanics-based model by incorporating a synergy between hydrogen transport and intergranular-cavity-based fracture process. Based on the available creep lifetime data of C-0.5Mo steels, we are able to calibrate material constitutive parameters, and then conduct nonlinear finite element simulations that reveal a real-time stress-induced hydrogen diffusional transport along grain boundaries, coupled with a microstructure-explicit failure process, from which Nelson curves can be computed. Such failure analyses allow us to delineate two distinct regimes on the Nelson curves, i.e., dislocation-creep-controlled or grain boundary diffusion-assisted cavity growth. More importantly, we found that a small change of the pipe thickness and applied stresses can significantly shift these lifetime curves. However, these two parameters are usually not provided in Nelson curves, thus limiting their usage in material selection and safety design. In conclusion, this discrepancy can clearly be mitigated by extensive parametric studies from our micromechanical modeling/simulation framework.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Enhanced CO 2 Methanation Activity of Sm 0.25 Ce 0.75 O 2-δ –Ni by Modulating the Chelating Agents-to-Metal Cation Ratio and Tuning Metal–Support Interactions

Highly active and selective CO 2 methanation catalysts are critical to CO 2 upgrading, synthetic natural gas production, and CO 2 emission reduction. Wet impregnation is widely used to synthesize oxide-supported metallic nanoparticles as the catalyst for CO 2 methanation. However, as the reagents cannot be homogeneously mixed at an atomic level, it is challenging to modulate the microstructure, crystal structure, chemical composition, and electronic structure of catalysts via wet impregnation. In this work, a scalable and straightforward catalyst fabrication approach has been designed and validated to produce Sm 0.25 Ce 0.75 O 2-δ -supported Ni (SDC–Ni) as the CO 2 methanation catalyst. By varying the chelating agents-to-total metal cations ratio (C/I ratio) during the catalyst synthesis, we can readily and simultaneously modulate the microstructure, metallic surface area, crystal structure, chemical composition, and electronic structure of SDC–Ni, consequently fine-tuning the oxide–support interactions and CO 2 methanation activity. The optimal C/I ratio (0.1) leads to an SDC–Ni catalyst that facilitates C–O bond cleavage and significantly improves CO 2 conversion at 250 °C. A CO 2 -to-CH 4 yield of >73% has been achieved at 250 °C. Furthermore, a stable operation of >1500 hours has been demonstrated, and no degradation is observed. Extensive characterizations were performed to fundamentally understand how to tune and enhance CO 2 methanation activity of SDC–Ni by modulating the C/I ratio. The correlation of physical, chemical, and catalytic properties of SDC–Ni with the C/I ratio is established and thoroughly elaborated in this work. This study could be applied to tune the oxide–support interactions of various catalysts for enhancing the catalytic activity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2015

Modeling defect cluster evolution in irradiated structural materials: Focus on comparing to high-resolution experimental characterization studies

Exposure of metallic structural materials to irradiation environments results in significant microstructural evolution, property changes, and performance degradation, which limits the extended operation of current generation light water reactors and restricts the design of advanced fission and fusion reactors. Further, it is well recognized that these irradiation effects are a classic example of inherently multiscale phenomena and that the mix of radiation-induced features formed and the corresponding property degradation depend on a wide range of material and irradiation variables. This inherently multiscale evolution emphasizes the importance of closely integrating models with high-resolution experimental characterization of the evolving radiation-damaged microstructure. Lastly, this article provides a review of recent models of the defect microstructure evolution in irradiated body-centered cubic materials, which provide good agreement with experimental measurements, and presents some outstanding challenges, which will require coordinated high-resolution characterization and modeling to resolve.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

NASA NTRS2000

BUNDLE: A Novel Furnace for Performing Controlled Directional Solidification Experiments in a Microgravity Environment

NASA Marshall Space Flight Center has developed a novel directional solidification furnace prototype for processing metals and alloys experiments in a microgravity environment. The BUNDLE (Bridgman Unidirectional Dendrite in Liquid Experiment) furnace is intended to accommodate the science requirements of Flight Definition Principle Investigators studying cellular/dendritic growth in aluminum and lead alloys at processing temperatures up to 1200 C. The furnace implements a number of innovative features to achieve high thermal gradients and quench rates in a low-power, light-weight design. These include a pyrolytic boron nitride/graphite composite heating element surrounded by layers of self-supporting refractory metal shielding, and a graphite fiber enhanced cold zone allowing high levels of heat extraction from the sample crucible. Novel to the BUNDLE design is an in-situ helium gas quench capability that ensures rapid freezing of the solidifying region (mushy zone) of the metal sample within the furnace without sample disturbance prior to quenching; this is a stringent requirement for subsequent analysis and understanding of microstructural development. The experiment hardware concept features multiple furnaces that may be "bundled" together so many samples, currently up to eight, can be processed at one time. The design of BUNDLE is flexible enough to be implemented on the Shuttle and Space Station in a number of locations (SpaceHab, Express Rack, MPESS, ISPR, etc). BUNDLE prototype furnaces have directionally solidified and quenched 1cm diameter lead - 5.8 weight percent antimony and aluminum - 4 weight percent copper alloys. Quenching of the mushy zone, as recorded by in-situ thermocouples, occurred on the order of 0.5 seconds or less, a rate within the PI's requirements. Subsequent metallographic examination revealed the solidified microstructure to be, as expected, unidirectional. Both the dendrite tips and the eutectic reaction were planar in nature indicating uniform axial heat flow. Delineation between the growing dendrites and eutectic structure with the "quenched-in" liquid was sharp, attesting to the efficacy of the helium quench. BUNDLE's conception, development, capability, and adaptability are presented (in view of Flight PI's needs and science requirements) through viewgraphs depicting actual hardware, generated thermal analysis, and micrographs prepared from BUNDLE processed, flight-like samples.

Carrasquillo, Edgar J.↗

NASA NTRS2001

BUNDLE - A Novel Furnace for Performing Controlled Directional Solidification Experiments in a Microgravity Environment

Carrasquillo, Edgar J.↗

DOE OSTI2016

Investigating Accident Tolerant Fuel Concepts using the BISON Fuel Performance Code

There has been an increased interest in research of accident tolerant fuels (ATF) and claddings for use in commercial reactors ever since the events that occurred at the Fukushima Daiichi nuclear power plant in 2011. The economic impact of these events on the nuclear energy sector is significant. As a result, the United States Department of Energy's Office of Nuclear Energy accelerated research in nuclear fuel concepts with enhanced accident tolerance as part of its Fuel Cycle Research and Development (FCRD) Advanced Fuels Campaign (AFC). A report produced by the AFC entitled Light Water Reactor Accident Tolerant Fuel Performance Metrics outlines a set of metrics that can be used to guide selection of promising ATF concepts. Moreover, the report specifies that a down-selection is to occur in the 2016-2017 time frame, at which time the program will move from a proof-of-concept to a proof-of-principle stage with continued research and development into a small set of concepts. Given the time necessary for comprehensive irradiation experiments and post-irradiation examination, it is impossible to perform a complete set of experiments for material characterization. Therefore, the AFC is utilizing computational analysis tools in an effort to understand the proposed materials under a variety of normal operating and accident conditions. For some time, the DOE's Nuclear Energy Advanced Modeling and Simulation (NEAMS) program has been developing computational analysis tools for nuclear fuel simulation. These codes include BISON and Marmot which investigate fuel behavior at the continuum and microstructural scales, respectively. In 2014, NEAMS introduced what it calls High Impact Problems (HIPs) into its program plan. These HIPs are intended to make significant advancements in a particular area of nuclear power research in a short period of time (3 years or less). NEAMS has chosen an ATF project, which emphasizes utilizing BISON and Marmot to model proposed materials, as its first HIP. This summary focuses on the methodology being utilized for investigation of ATF concepts using the BISON fuel performance code. First, we give an overview of the model development for two candidate ATF materials, FeCrAl for cladding and uranium silicide (U{sub 3}Si{sub 2}) for fuel. Then, we present the approach for deciding which simulations are necessary given the importance of such simulations in providing a detailed report into the fuel performance behavior of these materials by the conclusion of the HIP. In absence of experimental data and given the aggressive schedule outlined by the AFC for ATF research and development, computational analysis tools are required. These tools are being used to help guide experiment design and to perform bounding and sensitivity studies to gain valuable information for which experimental data is limited. In support of this effort, models have been incorporated into BISON for simulation of U{sub 3}Si{sub 2} and FeCrAl. Continued material model development and engineering analysis will help address questions related to the performance of these ATF materials under normal operating and accident conditions. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2013

Thermomechanical simulation of the DIAMINO irradiation experiment using the LICOS fuel design code

Two separate-effect experiments in the HFR and OSIRIS Material Test Reactors (MTRs) are currently under Post- Irradiation Examinations (MARIOS) and under preparation (DIAMINO) respectively. The main goal of these experiments is to investigate gaseous release and swelling of Am-bearing UO2-x fuels as a function of temperature, fuel microstructure and gas production rate. First, a brief description of the MARIOS and DIAMINO irradiations is provided. Then, the innovative experimental in-pile device specifically developed for the DIAMINO experiment is described. Eventually, the thermo-mechanical computations performed using the LICOS code are presented. These simulations support the DIAMINO experimental design and highlight some of the capabilities of the code. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2019

Complete the Design of Benchtop Fiber-Optic Based Photo-Thermal Radiometry System

Thermal transport properties of nuclear fuels, i.e., thermal conductivity and diffusivity, are critical parameters in the thermal design of a nuclear reactor. It is well known that thermal transport properties change temporally and spatially due to dynamic microstructural evolution as a result of neutron irradiation. A real-time instrument to monitor the local thermal property change, which can survive the harsh in-pile environment, will give researchers unprecedented access to fuel behavior during irradiation. Laser-based photothermal techniques are an ideal candidate to accomplish this specific task, because of the remote, non-contact, and non-destructive features. In this report, we present the progress in the development of a bench-top photothermal radiometry (PTR) system to measure the thermal diffusivity of solid samples, and the preliminary design of a fiber-based PTR instrument to measure the real-time, in-pile thermal diffusivity of nuclear fuels. The PTR technique measures the local temperature response from a modulated heat source by detecting the sample radiation heat flux. Initially a well-developed thermal wave analytical model was fit to the data to obtain the thermal diffusivity. However, systematic errors from the diffraction effect and non-linearity issues resulted in thermal diffusivity measurements higher than literature values. These effects have been studied and an improved analytical model has been developed, and the physics behind the phenomena are still under investigation. A procedure for optimizing measurements from the bench-top system has been provided. The experiences from the bench top measurement were then used to guide the fiber-based system.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2018

Effect of Pore Connectivity on Li Dendrite Propagation within LLZO Electrolytes Observed with Synchrotron X-ray Tomography

Li 7 La 3 Zr 2 O 12 (LLZO) is a garnet type material that demonstrates promising characteristics for all solid-state battery applications due to its high Li-ion conductivity and its compatibility with Li metal. The primary limitation of LLZO is the propensity for short-circuiting at low current densities. Microstructure features such as grain boundaries, pore character, and density all contribute to this shorting phenomenon. Toward the goal of understanding structure-processing relationships for practical design of solid electrolytes, the present study tracks structural transformations in solid electrolytes processed at three different temperatures (1000, 1050 and 1150 °C) using synchrotron x-ray tomography. A sub volume of 300 μm 3 captures the heterogeneity of the solid electrolyte microstructure while minimizing the computational intensity associated with 3D reconstructions. While the porosity decreases with increasing temperature, the underlying connectivity of the pore region increases. In conclusion, solid electrolytes with interconnected pores short circuit at lower critical current densities than samples with less connected pores.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Catalytic water splitting kinetics and optimization

This project was motivated primarily by the opportunity of turning photocatalysis into a cost efficient hydrogen generation method for domestic energy and chemical production, and by the need to provide detailed mechanisms of photocatalytic reactions of broad scientific and technological interest. Specifically, we focused on the development of a new technique for analysis of (photo)catalytic reaction mechanisms to guide photocatalyst design. Our approach was based on applying velocity map imaging (VMI) to surface catalyzed reactions in order to identify photocatalytic reaction products, intermediates, and relate these to photocatalyst composition, dimensions, size and other characteristics. By coupling VMI with other spectroscopic and microstructural characterization, we aimed to reveal the features that limit performance of photocatalysis. As a first step to achieve this goal, we constructed a custom VMI microscope specifically designed for investigation of surface photocatalytic reactions and validated it’s design using a photodissociatinon of MnBr(CO) 5 adsorbed on a metallic surface. Using both 230 nm and 266 nm pulsed laser excitations, we observed that there are likely three main pathways for photodissociation of Mn(CO)5Br: from the gas phase, the surface, and ejected Mn complex from the surface increasing the gas phase concentration.

08 HYDROGEN↗

DOE OSTI2015

First Annual Progress Report on Radiation Tolerance of Controlled Fusion Welds in High Temperature Oxidation Resistant FeCrAl Alloys

The present report summarizes and discusses the first year efforts towards developing a modern, nuclear grade FeCrAl alloy designed to have enhanced radiation tolerance and weldability under the Department of Energy (DOE) Nuclear Energy Enabling Technologies (NEET) program. Significant efforts have been made within the first year of this project including the fabrication of seven candidate FeCrAl alloys with well controlled chemistry and microstructure, the microstructural characterization of these alloys using standardized and advanced techniques, mechanical properties testing and evaluation of base alloys, the completion of welding trials and production of weldments for subsequent testing, the design of novel tensile specimen geometry to increase the number of samples that can be irradiated in a single capsule and also shorten the time of their assessment after irradiation, the development of testing procedures for controlled hydrogen ingress studies, and a detailed mechanical and microstructural assessment of weldments prior to irradiation or hydrogen charging. These efforts and research results have shown promise for the FeCrAl alloy class as a new nuclear grade alloy class.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Evolution of microstructure and strength of a high entropy alloy undergoing the strain-induced martensitic transformation

In a recent work, we have reported outstanding strength and work hardening exhibited by a metastable high entropy alloy (HEA), Fe 42 Mn 28 Co 10 Cr 15 Si 5 (in at. %), undergoing the strain-induced martensitic transformation from metastable gamma austenite (γ) to stable epsilon martensite (ε). However, the alloy exhibited poor ductility, which was attributed to the presence of the brittle sigma (σ) phase in its microstructure. The present work reports the evolution of microstructure, strength, and ductility of a similar HEA, Fe 38.5 Mn 20 Co 20 Cr 15 Si 5 Cu 1.5 (in at. %), designed to suppress the formation of σ phase. A cast and then rolled plate of the alloy was processed into four conditions by annealing for 10 and 30 min at 1100 °C and by friction stir processing (FSP) at tool rotation rates of 150 and 400 revolutions per minute (RPM) to facilitate detailed examinations of variable initial grain structures. Neutron diffraction and electron microscopy were employed to characterize the microstructure and texture evolution. The initial materials had variable grain size but nearly 100% γ structure. Diffusionless strain induced γ→ε phase transformation took place under compression with higher rate initially and slower rate at the later stages of deformation, independent on the initial grain size. The transformation facilitated part of plastic strain accommodation and rapid strain hardening owing to a transformation-induced dynamic Hall-Petch-type barrier effect, increase in dislocation density, and texture. Here, the peak strength of nearly 2 GPa was achieved under compression using the structure created by double pass FSP (150 RPM followed by 150 RPM). Remarkably, the tensile elongation exhibited by the alloy was nearly 20% with fracture surfaces featuring a combination of ductile dimples and cleavage.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Comparison on the properties of ITZs in fly ash-based geopolymer and Portland cement concretes with equivalent flowability

Highlights: • Modelled ITZs can effectively avoid the effects caused by different factors and test locations of ITZ. • ITZ properties of PC and geopolymer concretes are compared based on equivalent flowability of binders. • Geopolymer ITZ exhibits stronger bonding than that of PC, and higher mechanical properties than geopolymer paste. • Strong ITZs in geopolymer concrete are attributed to the layer of gel-rich paste with dense microstructures. • Elastic modulus and hardness properties of ITZs in PC concrete are increased due to the CH crystals. This paper aims to compare the properties of interfacial transition zones (ITZs) in Portland cement (PC) concrete and geopolymer concrete. Portland cement and geopolymer pastes were designed with the equivalent flowability to provide similar mix and casting condition of ITZs. Two types of modelled ITZs were prepared to facilitate the nanoindentations across ITZs, microstructural characterization, and comparison on the properties of ITZs with less influential factors. The results showed that the interfacial bonding of ITZs between geopolymer matrix and aggregate is relatively stronger than the counterpart in the PC concrete. There is a high amount of crystalline hydration products in the ITZs of PC concrete, but a layer gel-rich paste with denser microstructures in the ITZs of geopolymer concrete. Additionally, the interface morphology and nanoindentation analysis indicate that the property of ITZs in the modelled geopolymer concrete is not poorer than that of the corresponding geopolymer paste.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Microstructure and mechanical behavior of a TiC nanoprecipitate strengthened V Alloy

The V-4Cr-4Ti (V44) alloys have been proposed as the prime candidate structural material for self-cooled liquid Li blanket and other designs for fusion energy applications. However, the applications of the V44 alloy are limited to a narrow operation temperature window, due to reduction in creep strength at or above 700 °C and susceptibility to irradiation hardening and embrittlement when irradiated below 400 °C. Here, in this work, we explore the feasibility of designing a novel V alloy to form a high number density of TiC nanoprecipitates, in order to simultaneously improve creep strength and provide defect sinks to mitigate irradiation hardening. Computational thermodynamics was used to design a new alloy (V44C) to achieve our goal of high TiC nanoprecipitates density within the alloy V44 matrix. To ensure scalability, the new alloy was made through arc-melting and ingot-casting followed by hot forging, cold rolling and heat treatments of homogenization and precipitation aging. The microstructure was characterized by SEM, TEM, XRD and APT, confirming the existence of nanoprecipitates predicted in the thermodynamic calculations. In addition to microstructural evaluation tensile properties at room temperature and 700 °C, and Charpy impact energy at room temperature were measured. The microstructure and mechanical properties were then compared with those from a historic reference V44 alloy. The tensile strength improvement in V44C was rationalized based on particle and solid solution strengthening mechanism. The fracture behavior was discussed based on the fractography results and necking deformation behavior.

Alloys development↗