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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 937 records · Page 52
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Implications of post-processing induced microstructural changes on the deformation and fracture response of additively manufactured Ti–6Al–4V

Ti–6Al–4V parts fabricated via electron beam melting (EBM) powder bed fusion are often subjected to hot isostatic pressing below the β-transus temperature to mitigate defects. During which the pressure aids in pore closure and the thermal exposure results in coarsening of α phase while retaining the columnar prior-β phase grain morphology present in the as-fabricated condition. The same post-processing treatment can also be carried out above β-transus temperature which is an effective way to modify both the grain morphology and the associated α textures. Here, the objective of this work is to correlate thermally induced microstructural changes to the deformation and fracture response of the EBM processed Ti–6Al–4V. To this end, we have carried out both sub-transus and super-transus heat-treatments of the as-fabricated material. The mechanical response of the as-fabricated and all heat-treated materials are characterized by in-situ tensile tests under a high-resolution digital optical microscope. This enabled us to capture large-scale panoramic images of the deforming microstructure, and overcome the trade-off between the image resolution and the field of view during in-situ experiments. The series of images captured throughout the imposed deformation are subsequently used to perform microstructure-based digital image correlation to measure microstructural-scale strains over a large area. The results of the in-situ tests together with detailed fractographic analyses are then used to elucidate how the heterogeneous deformation spanning over multiple microstructural length-scales, for example, at the scale of lamellae, colonies of lamellae and grain boundaries, affect the overall deformation and fracture response of the post-processed materials.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Mechanical rolling and annealing of wire-arc additively manufactured stainless steel plates

Thin walls of 304L stainless steel were fabricated by wire-arc additive manufacturing (WAAM) followed by post build thermomechanical processing to modify the as built microstructure and properties. The walls were made using a high-deposition-rate robotically controlled gas-metal arc welding system and were characterized using optical microscopy and tensile tested for mechanical properties. Post processing consisted of mechanical rolling the walls to 25% and 40% strains, followed by annealing at 1050°C to demonstrate a wide range of properties. Results show that WAAM can be used to build custom sized semi-finished parts or blanks that can later be thermomechanically processed to increase strength and ductility through recrystallization of the as built microstructure, and/or processed into desired shapes with improved mechanical properties.

304L stainless steel↗
DOE OSTI2026

Microstructure prediction for Ti-22Al-25Nb in laser powder bed fusion

This work presents a physics-informed framework for predicting solidification morphology and defect susceptibility in additively manufactured Ti–22Al–25Nb across a broad processing space. The framework integrates solidification microstructure selection (SMS) analysis with a single-track defect-based printability map to establish a unified methodology linking processing parameters to both interfacial morphology and manufacturability. Thermal gradients G and solidification rates R are first computed using the Thermo-Calc Additive Manufacturing (TC-AM) module, a finite-interface-dissipation (FID) phase-field (PF) model coupled with CALPHAD method is then employed to systematically distinguish planar and dendritic regimes as functions of $G$ and $R$. By superimposing the printability map onto the morphology projections, a comprehensive process–structure framework is obtained. Across most processing conditions, the predicted microstructure is predominantly dendritic, while planar growth emerges only under selected laser power $P$ and scan speed $v$ combinations. In addition to morphology classification, the framework quantifies the dendritic area fraction and introduces a width-based morphology descriptor to characterize the spatial extent of planar/dendritic regions within the melt pool. It provides mechanistic insight into the interplay between solidification physics and defect formation, offering practical guidance for parameter selection and microstructural control in Ti–22Al–25Nb additive manufacturing (AM).

36 MATERIALS SCIENCE↗
DOE OSTI2023

Shock state distributions in porous tantalum and characterization with multipoint velocimetry

Heterogenous materials under shock compression can be expected to reach different shock states throughout the material according to local differences in microstructure and the history of wave propagation. Here, in this work, a compact, multiple-beam focusing optic assembly is used with high-speed velocimetry to interrogate the shock response of porous tantalum films prepared through thermal-spray deposition. The distribution of particle velocities across a shocked interface is compared to results obtained using a set of defocused interferometric beams that sampled the shock response over larger areas. The two methods produced velocity distributions along the shock plateau with the same mean, while a larger variance was measured with narrower beams. The finding was replicated using three-dimensional, mesoscopically resolved hydrodynamics simulations of solid tantalum with a pore structure mimicking statistical attributes of the material and accounting for radial divergence of the beams, with agreement across several impact velocities. Accounting for pore morphology in the simulations was found to be necessary for replicating the rise time of the shock plateau. The validated simulations were then used to show that while the average velocity along the shock plateau could be determined accurately with only a few interferometric beams, accurately determining the width of the velocity distribution, which here was approximately Gaussian, required a beam dimension much smaller than the spatial correlation lengthscale of the velocity field, here by a factor of ∼30×, with implications for the study of other porous materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Microstructure and Mechanical Performance of the Friction Stir Welds Made on Neutron-Irradiated Steel with Helium

This report describes new experimental results on the microstructure and mechanical performance of the friction stir welds made on neutron-irradiated steel with helium. The report focuses on helium-related issues, specifically, helium-induced degradation in the welded joint, aiming to repair irradiated components of nuclear power plants (NPPs). The friction stir welds analyzed here were produced at Oak Ridge National Laboratory previously, and limited characterization work was performed, mostly addressing the presence or absence of macroscopic cracks. The present work attempts to perform a more comprehensive study to assess microstructure conditions, grain size, plastic strain gradients, the morphology of the helium-induced damage, and deformation behavior.

42 ENGINEERING↗
DOE OSTI2020

Build Orientation Dependent Microstructure in Polymer Laser Sintering: Relationship to Part Performance and Evolution with Aging

Laser sintering (LS) is widely used to produce functional polymeric parts; however, the resulting parts are often limited by their porous structure, and performance of the part may be strongly anisotropic. Relating the structural features of parts to build process conditions or powder feedstock has been explored previously. In contrast, little is known regarding how the unique internal structures of LS parts evolve and relate to their performance later in their life cycle, for example, after use in a real-world operating environment. In this study, a tightly controlled LS build process and measurement campaign by standard X-ray computed tomography (XCT), supported by high-resolution synchrotron XCT, was used to benchmark the internal microstructure (e.g. porosity) as a function of four different build orientations in printed polyamide-12 (PA-12) parts. The initial performance of the parts after printing was characterized by tensile testing and dynamic mechanical analysis (DMA). Arrays of PA-12 parts in different build orientations were exposed to steam (under pressure) and air across multiple temperature and time points for the purposes of accelerated aging through oxidative and hydrolytic breakdown. Exposing parts to steam dramatically altered the internal microstructure and functional properties such as the glass transition temperature, tensile properties, and damping behavior. Notably, post-aging XCT revealed large microstructural changes after only 40 h of steam treatment relative to the as-printed specimens. Furthermore, pore reorganization and changes in crystallinity occurred regardless of whether the steam temperature was aggressive enough to induce a significant loss in mechanical properties. The build orientation dependence on the aging rate was minimal with the relative trend in performance persisting across most metrics among the different orientations even after aging.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Multiscale in-situ characterization of static recrystallization using dark-field X-ray microscopy and high-resolution X-ray diffraction

Abstract Dark-field X-ray microscopy (DFXM) is a high-resolution, X-ray-based diffraction microstructure imaging technique that uses an objective lens aligned with the diffracted beam to magnify a single Bragg reflection. DFXM can be used to spatially resolve local variations in elastic strain and orientation inside embedded crystals with high spatial (~ 60 nm) and angular (~ 0.001°) resolution. However, as with many high-resolution imaging techniques, there is a trade-off between resolution and field of view, and it is often desirable to enrich DFXM observations by combining it with a larger field-of-view technique. Here, we combine DFXM with high-resolution X-ray diffraction (HR-XRD) applied to an in-situ investigation of static recrystallization in an 80% hot-compressed Mg–3.2Zn–0.1Ca wt.% (ZX30) alloy. Using HR-XRD, we track the relative grain volume of > 8000 sub-surface grains during annealing in situ. Then, at several points during the annealing process, we “zoom in” to individual grains using DFXM. This combination of HR-XRD and DFXM enables multiscale characterization, used here to study why particular grains grow to consume a large volume fraction of the annealed microstructure. This technique pairing is particularly useful for small and/or highly deformed grains that are often difficult to resolve using more standard diffraction microstructure imaging techniques.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Enhancing NDE Reliability for Grade 91 Steel Welds: Ultrasonic Imaging and Microstructural Correlations

Ensuring the integrity of Grade 91 (9Cr-1Mo-V) steel welds is vital for the safe and reliable operation of fossil fuel–fired and nuclear power plants. Here, this study applies an imaging technique for the ultrasonic characterization of two Grade 91 steel welds created with cold metal transfer and flux-cored arc welding processes. Ultrasonic immersion testing in the through-transmission configuration was employed to generate shear waves, which helped identify the weld metal, heat-affected zone, and base metal regions. These weld microstructures were also correlated to their ultrasonic images using metallography, ultrasonic amplitude, hardness measurements, and grain size. The findings from this study can assist practitioners in developing new nondestructive evaluation technologies, improving the inspection reliability of creep strength–enhanced ferritic steel welds by potentially identifying weld microstructure regions susceptible to creep-type failures.

Grade 91 steel↗
DOE OSTI2020

Multiscale-Informed Modeling of High Temperature Component Response with Uncertainty Quantification

This report summarizes a joint effort between Argonne National Laboratory, Idaho National Laboratory, and Los Alamos National Laboratory to develop and deploy constitutive models targeted at predicting the life of Grade 91 alloy components subjected to high temperature environments typical of those that structural components in advanced nuclear reactors would experience. Two distinct, but complementary constitutive modeling approaches have been taken here. The first employs a phenomenological viscoplastic model for which parameters have been calibrated based on experimental data for a wide range of Grade 91 alloy that has undergone a variety of processing. A Bayesian approach was used to derive distributions of uncertain parameters for this model based on this data set. The second approach is a reduced order model suitable for engineering-scale analysis that is based on the results of a large set of mesoscale simulations. Mesoscale models allow for the microstructure and composition of a particular alloy to be directly taken into account in the computation of the viscoplastic response, but are computationally expensive, which makes it impractical to directly call those models for the material constitutive response in an engineering-scale simulation. The reduced-order representation of the response of the underlying model used here allows for an engineering-scale model to take into account the characteristics of the underlying microstructure, while only incurring a reasonable computational expense. Both of these approaches have different strengths, and are applicable for different parts of the design/analysis process. The phenomenological models can be readily parameterized based on a set of experimental data for a given class of materials and used for scoping calculations. Once a specific material is chosen and adequately characterized, the reduced order models can accurately predict the response of that specific alloy, and because the models are based on predictive models of the underlying microstructure, they can be used to more confidently predict the response under conditions in regions where there is limited experimental data. Both of these models have been integrated in the Grizzly code, which is used here to perform proof-of-concept uncertainty quantification analyses of a simple component under prototypical conditions. The built- in stochastic analysis capabilities in the MOOSE framework that Grizzly is built on are used here to run large sets of simulations for this uncertainty quantification analysis. As would be expected, because the reduced order models are developed for a much more tightly defined alloy, they predict tighter distributions of the time to failure than the phenomenological models, which are calibrated to a broader set of data. Also important is that these simulations demonstrate that a reduced order modeling approach can be successfully deployed to propagate uncertainties from the material scale to practical engineering-scale component simulations.

42 ENGINEERING↗
DOE OSTI2023

Status of Mechanistic Fission Gas Model in High-Burnup Fuel

A desire to increase fuel burnup to decrease the cost of nuclear power plants has led to significant interest within the nuclear industry to develop improved understanding of high-burnup nuclear fuel microstructure and the potential for fuel fragmentation, relocation, and dispersal that contribute to burnup and safe operating limits. This milestone report describes joint research activities and program planning to develop mechanistic models for high-burnup UO 2 microstructure, including both intra- and intergranular gas bubble populations and fission gas release, specifically associated with transient release. This model development is being extensively leveraged against a rapidly growing experimental database of high-fidelity electron microscopy characterization of commercial, light water reactor fuel in the as-irradiated condition as well as that following simulated loss-of-coolant test conditions. This report describes the status of model development, highlights recent microstructural data, and summarizes the data needs to complete initial development and experimental validation of mechanistic models of fission gas and microstructural evolution at high burnup, as well as transient fission gas release.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

Characterizing Performance of Electrocatalyst Nanoparticles Infiltrated into Ni-YSZ Cermet Anodes for Solid Oxide Fuel Cells

The infiltration of nanoparticle electrocatalysts into solid oxide fuel cell (SOFC) electrodes has been proven to produce a high density of electrochemically active sites, and reduce charge transfer polarization losses for SOFC electrodes. This is crucial for intermediate temperature operation, as these losses increase greatly at lower temperatures. Nickel-yttria stabilized zirconia (NiYSZ) cermets are low-cost, and exhibit excellent stability, but their main disadvantage stems from nickel coarsening and performance loss over their operational lifetimes. Infiltration of electrocatalyst nanoparticles has been shown to mitigate nickel coarsening and the consequent anode degradation. In this study, the effects of these infiltrants are observed in a standard Ni-YSZ electrode. In addition to nickel, mixed ionic and electronic conducting (MIEC) phases were infiltrated into Ni-YSZ scaffolds and their performances were characterized using electrochemical impedance spectroscopy (EIS). Cross-sectional microscopy of fractured cells was used to compare electrode microstructure and particle statistics. A model is proposed for how the nanoparticle electrocatalysts improve the anode performance.

25 ENERGY STORAGE↗
DOE OSTI2022

Optimizing thermal stability and mechanical behavior in segregation-engineered nanocrystalline Al–Ni–Ce alloys: A combinatorial study

The deliberate use of solute enrichment at grain boundaries, otherwise known as segregation engineering, is a promising approach to tailor the properties of interface-dominated materials such as nanocrystalline alloys. Here, the ensuing chemical and structural evolution at grain boundaries can give rise to thermal stability and excellent mechanical properties, but the interplay between enrichment, phase decomposition, grain growth, and mechanical behavior exists in a vast composition and processing space. In this study, a combinatorial synthesis and rapid characterization approach was applied to segregation-engineered nanocrystalline Al–Ni–Ce alloys to assess the evolution of microstructure and resulting mechanical behavior as functions of alloying content and annealing conditions. In addition to the identification of alloys and processing conditions that give rise to exceptional thermal stability, strength retention, and homogeneous plastic flow, we construct combined thermal stability and deformation mechanism maps that demarcate several important regimes of behavior.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Topological analysis of X-ray CT data for the recognition and trending of subtle changes in microstructure under material aging

X-ray computed tomography (CT) is an established non-destructive tool for 3D imaging of multiphasic composites. Numerous applications of X-ray CT in medical diagnosis and materials characterization have been reported, many involving field-specific innovations in the imaging technology itself. Yet, quantitative summarization to link image features to properties of interest has been rare. Here we address this issue by employing state-of-the-art technics in scalar field topology for the summarization of X-ray CT images of an example biphasic system. By varying processing-parameters we create different microstructures, evolve them through accelerated thermal aging, CT-image them pre- and post-aged, and demonstrate the ability of our image summarization method to systematically track process- and age-related changes, which can often be very subtle. A novel aspect of the algorithm involves recognition over multiple resolution levels, which provides deeper insight into the pattern relationship between grain-like features and their neighbors. The method is general, adaptable to diverse image reconstruction methods and materials systems, and particularly useful in applications where practical constraints on the sample-size limits the reliable use of more complex models, e.g., convolutional neural networks.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Evaluation of In-Situ AM Process Monitoring Techniques and Potential for Detecting Process Anomalies and Undesirable Microstructures

The US Department of Energy’s Advanced Materials and Manufacturing Technologies (AMMT) program is pursuing rapid qualification of new materials for fabrication of nuclear relevant components using advanced manufacturing techniques. Particular interest is placed on code-qualifying stainless steel (SS) 316H processed by laser powder bed fusion (LPBF) additive manufacturing. A paradigm that incorporates data from in-situ sensing during the printing, ex-situ characterization, and advanced artificial intelligence–based models was established under the Transformation Challenge Reactor (TCR) program to develop a pedigree for each fabricated component that could be tracked from the feedstock to the component’s release for application. Under the TCR program, the Peregrine software was developed as a tool for incorporating the vast amounts of in-situ and ex-situ characterization data collected; all data stored on a rapidly growing digital platform. The digital platform allows for users to link site-specific process anomalies to the macro- and microstructure. The platform will eventually be able to predict component performance, which will be crucial to qualifying materials and components in risk-averse industries such as those supporting and building nuclear reactors. Current in-situ process monitoring techniques that are already integrated with software like Peregrine are advantageous for identifying process anomalies including powder spatter, component edge swelling, recoating-build interactions, and so on. However, additional data are required to fully predict the resulting microstructures needed for identifying relationships to component performance. The rapid cooling rates observed in LPBF are some of the highest of any bulk manufacturing process, resulting in heterogenous microstructures and typically causing anisotropy in mechanical properties. Moreover, evolved residual thermal stresses are high, which can cause severe defects such as delamination or cracking. Therefore, other in-situ monitoring methods are warranted for exploration to measure and map the thermal history, and potentially the stress state, of each build. This report summarizes different in-situ monitoring strategies proposed for LPBF with a focus on the more developed sensor systems. Novel capabilities for measuring melt pool temperatures are also addressed to better inform modeling efforts.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Effect of Plutonium on Uranium Oxide Microstructural Fingerprint

The analysis of particulates from environmental sampling is routinely performed for nuclear forensics applications. In order to increase the tools available for nuclear forensics applications, capability development materials (CDMs), or reference particulates, are necessary for developing and benchmarking new analytical methods. Historically, these CDM particulates have been produced with highly controlled and characterized isotopic and size parameters for applications in developing and benchmarking particle sizers and mass spectrometry analytical methods [1- 4]. However, the development of CDMs with highly characterized particle morphology and phase of the particles is vital for aiding in the development and benchmarking of particle analytical methods for those parameters. In many cases, key properties such as crystallographic phase, morphology, and microstructure, may be correlated to processing history of environmental sampling particulates [5]. To that end, this work investigates determining the structural fingerprint of produced Pu-doped uranium oxide CDMs using transmission electron microscopy (TEM). The particulates, one of which shown in Figure 1, were synthesized to Fig. 1. Single particulate of uranium oxide fabricated using the THESEUS technique. develop capabilities for environmental sampling investigations. These particles are monodisperse at diameter of 1 μm and a range of plutonium concentrations from 0- 1,000 ppm. Given their small diameter, TEM analysis was ideal for studying the particulate structural fingerprint in detail. Previous investigations confirmed the external homogeneity of the particulates at different plutonium concentrations, however this analysis focuses on determining the grain structure, phase distribution, and porosity of the particulates.

Mayer, Jack [Univ. of Florida, Gainesville, FL (Un↗
DOE OSTI2022

Characterization of Long-term Service Coal Combustion Power Plant Extreme Environment Materials

The technical goal of this project is to develop a comprehensive database of mechanical properties, alloy microstructures, and to a lesser extent, the oxidation/corrosion behavior of coal-fired power plant components, such as boiler tubing, steam headers and steam piping, which have been in long-term service (at least 100,000 operating hours, and preferably more than 200,000 operating hours) under the operating conditions of high temperatures and high mechanical stresses where creep, fatigue, steam-side oxidation, and fireside corrosion are life-limiting factors. The components included in the database will include the following types of high temperature alloys: creep strength enhanced ferritic (CSEF) steels, 300-series H-grade stainless steels, and dissimilar metal welds (DMWs).

Characterization↗
DOE OSTI2025

PROCESS-STRUCTURE-PROPERTY RELATIONSHIPS IN LASER POWDER BED FUSION PRODUCED 17-4 PH STEEL

Laser powder bed fusion (LPBF) is a metal additive manufacturing method that produces non-traditional microstructures as a result of the rapid solidification and thermal cycling inherent to the process. When using LPBF-produced material in application, these unique microstructures challenge the applicability of well developed mechanical property databases achieved by conventional heat treatments. For wider adoption of this technology, a more holistic understanding is necessary on how process attributes develop material structure, which dictate mechanical properties. This dissertation explores the process– structure–property relationships in LPBF 17-4 PH steel through systematic evaluation of atmospheric processing and heat treatment effects on microstructure and mechanical performance. Specimens were fabricated under controlled build environments, subjected to a range of solutionizing, homogenizing, and aging treatments, and characterized using optical microscopy, electron back scatter diffraction (EBSD), and X-ray diffraction (XRD) to quantify phase evolution. Tensile testing was performed to directly link heat treatment pathway and nitrogen absorption to mechanical performance. This work demonstrates where conventional heat treatment standards are applicable to LPBF 17-4 PH steel and where modifications are required. By directly correlating phase stability, nitrogen effects, and tensile response, this work provides practical guidelines for tailoring post-processing strategies. These findings underscore that successful application of LPBF 17-4 PH steel requires explicit consideration of both build environment and post-processing. By linking processing conditions to microstructure and performance, this work advances understanding of critical variables that govern reliability of additively manufactured precipitation-hardened stainless steels in demanding applications.

Brown, Benjamin [Kansas City National Security Cam↗