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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 757 records · Page 42
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Microstructural investigation of PBX 9501: Comparing wet slurry and resonant acoustic mixing techniques

The microstructure of a high explosive (HE) material directly influences the reactive behavior under a variety of insults. Furthermore, the preparation method of polymer-bonded explosives (PBX), as well as the constituent material particle size distribution and consolidation parameters, will dominate the microstructural features that are observed. Here, we compare batches of PBX 9501 prepared by the typical wet slurry process and those prepared by resonant acoustic mixing. The “prills” produced by the wet slurry process leads to an inherently different microstructure than the coated powder produced by resonant acoustic mixing. Additionally, we observed that the conditions required to consolidate (press) the material to the nominal PBX 9501 density varied depending on the preparation technique, which also dictates the observed binder distribution. Furthermore, X-ray microcomputed tomography and ultra-small-angle X-ray scattering analyses revealed distinct differences in the void structure and distribution.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2021

Microstructure and heteroatom dictate the doping mechanism and thermoelectric properties of poly(alkyl-chalcogenophenes)

Heteroatom substitution can favorably alter electronic transport in conductive polymers to improve their thermoelectric performance. Here we report the spectroscopic, structural, and thermoelectric properties of poly(3–(3',7'-dimethyloctyl) chalcogenophenes) or P3RX doped with 2,3,5,6-tetrafluoro-7,7,8,8-tetracyanoquinodimethane (F4TCNQ), where the heteroatom [X = thiophene (T), selenophene (Se), tellurophene (Te)], the doping methodology, and extent of doping are systematically varied. Spectroscopic measurements reveal that while all P3RX polymers are appreciably doped, the doping mechanism is inherently different. Poly(3-hexylthiophene) (P3HT, used as a control) and poly(3–(3',7'-dimethyloctyl)tellurophene) (P3RTe) are doped primarily via integer charge transfer (ICT), whereas poly(3–(3',7'-dimethyloctyl)selenophene) (P3RSe) and poly(3–(3',7'-dimethyloctyl)thiophene) (P3RT) are doped via charge transfer complex (CTC) mechanisms. Despite these differences, all polymers saturate with roughly the same number of F4TCNQ counterions (1 dopant per 4 to 6 heterocycles), reinforcing the idea that the extent of charge transfer varies with the doping mechanism. Grazing incidence wide-angle x-ray scattering measurements provide insight into the structural driving forces behind different doping mechanisms—P3RT and P3RSe have similar microstructures in which F4TCNQ intercalates between the π-stacked backbones resulting in CTC doping (localized carriers), while P3HT and P3RTe have microstructures in which F4TCNQ intercalates in the alkyl side chain region, giving rise to ICT doping (delocalized carriers). These structural and spectroscopic observations shed light on why P3HT and P3RTe obtain electrical conductivities ca. 3 S/cm, while P3RT and P3RSe have conductivities <10–3 S/cm under the same thin film processing conditions. Ultimately, this work quantifies the effects of heteroatom, microstructural ordering, extent of doping, and doping mechanism, thereby providing rational guidance for designing future thermoelectric polymer-dopant systems.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Charge carrier motion and effect of fixed oxide charge in a microstructured silicon radiation detector

Signal formation in a microstructured semiconductor neutron detector is more complex than in planar diode geometry. Three-dimensional microstructures are laterally smaller than the ionization cloud length, and the electric fields may be weak enough to exhibit plasma time effects. This work is the first detailed treatment of charge carrier motion in these complex semiconductor devices to replicate the time profile and signal magnitude. Simulations were performed using COMSOL Multiphysics to investigate various parameters that affect the propagation of the charge cloud. It was observed that the size of the simulated three-dimensional structure had an impact on the induced current pulse, indicating the importance of simulation geometry optimization to accurately simulate charge cloud expansion. COMSOL Multiphysics was used to replicate accurate charge creation profiles using energy deposition information imported from radiation transport codes. A detailed simulation methodology is presented to benchmark preamplifier event pulses along with complexities in modeling the charge carrier motion along the etched microstructured trenches with Si–SiO 2 boundary conditions, including fixed oxide charge and interface trapping.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2024

Microstructural stability and mechanical properties of the as-cast and heat-treated newly developed TiNbCrTa refractory complex concentrated alloy

In this study, a TiNbCrTa refractory complex concentrated alloy (RCCA) was prepared using vacuum arc remelting. The microstructural evolution and mechanical properties of both as-cast and heat-treated RCCA samples were analyzed. Heat treatment (HT) was performed at 800–1200 °C for 1 h in a vacuum-sealed environment. These samples exhibited a formation of Cr 2 Nb and Cr 2 Ti Laves phases. A variation in elemental distribution was observed, with interdendritic (ID) regions showing higher fractions of Ti and Cr, while the dendritic regions had a greater concentration of Ta and Nb. Micro-segregation at the IDs was confirmed through energy dispersive x-ray spectroscopy mapping, which inferred the formation of Cr- and Ti-rich phases during HT at 800–1200 °C. High-temperature HT at 1200 °C for 1 h led to the evolution of the hcp omega phase. Prolonged HT at 1200 °C for 96 h resulted in the evolution of a Cr-rich Laves phase (Cr 2 Ta), which was homogeneously distributed within the microstructure, indicating an unstable microstructure. Furthermore, despite prolonged HT, a variation in the elemental distribution persisted due to the presence of dendritic and ID regions. Electron backscattered diffraction analysis revealed the presence of bcc and hcp phases in the dendritic and ID regions, respectively, of the as-cast and HTed samples. The as-cast samples demonstrated a high compressive strength of approximately 2 GPa. Micro-hardness values increased with the HT temperature up to 1000 °C. Further increases under HT conditions did not significantly reduce the microhardness value, whereas prolonged HT at 1200 °C led to an increase in the microhardness value. Overall, the newly developed TiNbCrTa RCCA exhibited high-strength behavior even after the phase transformation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Strong, ductile, and hierarchical hetero-lamellar-structured alloys through microstructural inheritance and refinement

The strength−ductility trade-off exists ubiquitously, especially in brittle intermetallic-containing multiple principal element alloys (MPEAs), where the intermetallic phases often induce premature failure leading to severe ductility reduction. Hierarchical heterogeneities represent a promising microstructural solution to achieve simultaneous strength−ductility enhancement. However, it remains fundamentally challenging to tailor hierarchical heterostructures using conventional methods, which often rely on costly and time-consuming processing. Here, we report a multiscale microstructural inheritance and refinement strategy to process “structural hierarchy precursors” in as-cast heterogeneous Al 0.7 CoCrFeNi MPEAs, which lead directly to a hierarchical hetero-lamellar structure (HLS) after simple rolling and annealing. Interestingly, it takes only 10 min of annealing time, two orders of magnitude less than that required to render the state-of-the-art properties during conventional processing of Al 0.7 CoCrFeNi, for us to achieve record-high strength−ductility combinations via the hierarchical HLS design that sequentially stimulates multiple unusual deformation and reinforcement mechanisms. In particular, the HLS-enabled high hetero-deformation-induced (HDI) internal stress triggers profuse <111>-type dislocations on over five independent slip systems in the supposedly brittle intermetallic phase and activates extensive stacking faults (SFs) and nanotwinning in the adjoining soft phase with a rather high SF energy. These unexpected, dynamically reinforcing hetero-deformation mechanisms across multiple length scales facilitate high sustained HDI strain hardening, along with a salient microcrack-mediated extrinsic ductilization effect, suggesting that the proposed microstructural inheritance and refinement strategy provides an efficient, fast, and low-cost approach to overcome the strength−ductility trade-off in a broad range of structural materials.

Science & Technology - Other Topics↗
DOE OSTI2024

Accelerate microstructure evolution simulation using graph neural networks with adaptive spatiotemporal resolution

Abstract Surrogate models driven by sizeable datasets and scientific machine-learning methods have emerged as an attractive microstructure simulation tool with the potential to deliver predictive microstructure evolution dynamics with huge savings in computational costs. Taking 2D and 3D grain growth simulations as an example, we present a completely overhauled computational framework based on graph neural networks with not only excellent agreement to both the ground truth phase-field methods and theoretical predictions, but enhanced accuracy and efficiency compared to previous works based on convolutional neural networks. These improvements can be attributed to the graph representation, both improved predictive power and a more flexible data structure amenable to adaptive mesh refinement. As the simulated microstructures coarsen, our method can adaptively adopt remeshed grids and larger timesteps to achieve further speedup. The data-to-model pipeline with training procedures together with the source codes are provided.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Dislocation Networks and the Microstructural Origin of Strain Hardening

In this paper, when metals plastically deform, the density of line defects called dislocations increases and the microstructure is continuously refined, leading to the strain hardening behavior. Using discrete dislocation dynamics simulations, we demonstrate the fundamental role of junction formation in connecting dislocation microstructure evolution and strain hardening in face-centered cubic (fcc) Cu. The dislocation network formed consists of line segments whose lengths closely follow an exponential distribution. This exponential distribution is a consequence of junction formation, which can be modeled as a one-dimensional Poisson process. According to the exponential distribution, two non-dimensional parameters control microstructure evolution, with the hardening rate dictated by the rate of stable junction formation. Among the types of junctions in fcc crystals, we find that glissile junctions make the dominant contribution to strain hardening.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Identifying the microstructural features associated with void nucleation during elevated–temperature deformation of copper

The microstructural-scale mechanisms that produce cracks in metals during deformation at elevated temperatures are relevant to applications that involve thermal exposure. Prior studies of cavitation during high-temperature deformation, for example, creep, suffered from an inability to directly observe the microstructural evolution that occurs during deformation and leads to void nucleation. Here the current study takes advantage of modern high-speed electron backscatter diffraction (EBSD) detectors to observe cavitation in oxygen-free, high-conductivity copper in situ during deformation at 300°C. Most voids formed at the triple junction between a twin boundary and a high-angle grain boundary (HAGB). This finding does not contradict previous studies that suggested that twins are resistant to cracking—it reveals that cracks in HAGBs originate at twin/HAGB triple junctions and that cracks preferentially grow along HAGBs rather than the accompanying twins. Atomistic simulations explored the origins of this observation and suggest that twin/HAGB triple junctions are microstructural weak points.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Oxidation and microstructure of SiC f /SiC composites in moist air up to 1600°C by X‐ray tomographic characterization

Abstract SiC f /SiC composites that possess PyC or BN interface layers were fabricated and then oxidized in moist air at 1000, 1200, 1400, and 1600°C. High‐resolution CT was used for capturing 3D images and quantifying the SiC phase, mesophase, and voids. The oxidation behavior and microstructural evolution of SiC f /SiC with PyC or BN interface are discussed in this study. The microstructure of the SiC f /SiC with a PyC layer was seriously damaged in moist air at high temperature, whereas the BN interface layer enhanced the oxidation resistance of the SiC f /SiC. These results are also confirmed by using XRD, oxidation mass gain, tensile testing, and SEM measurements. The results of the oxidation behavior and microstructural evolution for SiC f /SiC oxidized in dry air are also compared with the results of this study. Comparing the SiC f /SiC with a PyC interface layer, the composite with a BN interface layer oxidized in moist air exhibits a high void growth rate and a low SiO 2 grain growth rate from 1000 to 1600°C. This work will provide guidance for predicting the service life of SiC f /SiC for multiscale damage rate models of materials at a local scale and will also provide guidance on the life service design of SiC f /SiC materials.

Lu, Zilong↗
DOE OSTI2021

Cycling-Induced Microstructural Changes in Alloy Anodes for Lithium-Ion Batteries

Abstract High-capacity electrochemical alloying materials, such as tin and tin-based alloys, present an opportunity for the advancement of lithium-ion batteries. However, the destructive effects of volumetric expansion must be mitigated in order to sustain this high capacity during extended cycling. One way to mitigate these effects is by alloying Sn with more malleable metals to accommodate the strain related to severe volumetric expansion. Ex situ X-ray microtomography data of cycled Cu6Sn5 pellets were used to quantify the microstructural changes that occur during lithiation and delithiation. The microtomography data were segmented into three distinct phases to evaluate phase size distributions, specific surface area, and tortuosity. Electrodes lithiated and then delithiated showed the most substantial reduction in overall phase sizes. This suggests that full lithiation of the Sn followed by partial delithiation of the Li4.4Sn to Li2CuSn can cause substantial microstructural changes related to volume expansion on lithiation and structural collapse upon delithiation. When considering other microstructural characteristics, this subset of the electrodes analyzed showed the highest tortuosity values. These results show that in addition to the mechanical degradation of the electrodes, excessive volume expansion can also influence transport networks in the active material and supporting phases of the electrode. While based on studies of the active–inactive alloy Cu6Sn5 for lithium-ion battery applications, the insights obtained are expected to be applicable to other alloy electrodes and battery chemistries.

Electrochemistry↗
DOE OSTI2022

Effect of electrochemical cycling on microstructures of nanocomposite silicon electrodes using hyperpolarized 129 Xe and 7 Li NMR spectroscopy

The microstructural stability of composite electrodes during electrochemical cycling is critically important as it dictates the performance of Li-ion batteries. The issue becomes even more important for the high capacity alloying anode such as silicon that typically exhibits dramatic lithiation–delithiation-induced volume changes. The solid electrolyte interphase (SEI) layer formed on the active electrode surface has a profound effect on the overall microstructural stability of composite electrodes. An ideal SEI layer allows Li+ ions in and out of the electrode, but is an insulator to electrons, preventing the electrolyte from being further reduced. However, the SEI layers formed during initial lithiation may experience changes or degradation with subsequent cycling, adversely affecting the electrode performance. A combination of hyperpolarized 129 Xe and 7 Li nuclear magnetic resonance spectroscopies was applied to probe the microstructures of nanocomposite silicon electrodes at various stages of the lithiation–delithiation cycle. The results obtained from this study shed light on the degradation mechanism of nanocomposite Si electrodes upon electrochemical cycling and should prove useful in the effort to design more robust electrodes in the future.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Quantitative Characterization of the Microstructure-Property Relationships in Ni and MIEC Nanocatalyst-Infiltrated Ni/YSZ Anodes

The performance of solid oxide fuel cell (SOFC) anodes can be improved by infiltration of nanoscale electrocatalysts, which increases triple phase boundary (TPB) density, but only when the added TPBs are active. Quantitative characterization of the microstructure of infiltrated nanocatalysts remains a critical challenge in understanding their role in improved performance. This paper explores the relationship between electrochemical performance and microstructure for Ni/YSZ anodes infiltrated with Ni, gadolinium-doped-ceria (GDC), and Ni/GDC nanocatalysts using a combination of electrochemical impedance spectroscopy (EIS), distribution of relaxation times (DRT) analysis, scanning electron microscopy (SEM) microstructural characterization, and three-dimensional (3-D) anode reconstruction. Estimated polarization resistance improvements as a result of nickel nanoparticle infiltration are discussed.

Rix, Jillian↗
DOE OSTI2018

Tensile and Microstructure Characterization of SNS Target Swirl Bubblers Fabricated by Additive Manufacturing

During operation the mercury facing surfaces of the Spallation Neutron Source target vessel are damaged by cavitation-induced erosion. One option to decrease the erosion damage to the SNS target vessel surfaces is to decrease the intensity of the pressure waves using small bubble mitigation. Injection of small diameter helium bubbles into mercury has been shown in decrease the intensity of proton-induced pressure waves and mitigate erosion damage to mercury/container interface surfaces. Several bubbler designs have been evaluated for implementation in the SNS target. One promising bubbler design is called a swirl bubbler, which is capable of producing a high density of very small diameter helium bubbles in flowing mercury. Due to the complexity of the swirl bubbler design and the geometric restrictions of conventional machining processes, additive manufacturing was considered for fabrication. But there was uncertainty with the mechanical properties of bubblers fabricated with additive manufacturing. A series of experiments were designed to characterize the tensile properties and microstructure of swirl bubblers fabricated using selective laser melting (SLM), both before and after consolidation via hot isostatic pressing (HIPing). This report summarizes the tensile and microstructural characterization of HIPed and non-HIPed swirl bubblers produced via the SLM process. The results show that the as-fabricated material contained appreciable porosity, lack-of-fusion defects, and inconsistent tensile properties with essentially zero ductility. But after a HIPing treatment the microstructure became fully consolidated, and the tensile properties surpassed the requirements specified in the material standard for steel-mill produced 316L plate material used to fabricate the SNS target vessel. While further testing is recommended to evaluate the material’s susceptibility to fatigue fracture, these results indicate 316L bubbler assemblies produced SLM and HIPed are promising candidates for implementation in a future SNS target module.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Development of and initial assessment of microstructurally engineered UN

Fuels with high uranium densities have been considered in the Nuclear Technology Research and Development program’s Advanced Fuels Campaign as potential replacements for uranium(IV) oxide in commercial light water reactors. One such candidate fuel is uranium mononitride, UN, which has been observed to readily oxidize in steam and simulated pressurized water reactor conditions. Thus, it is important to examine methods for waterproofing UN, especially for potential cladding breach scenarios. This can be achieved by controlling the microstructure so as to prevent contact between the UN fuel and coolant. Research so far this FY has focused on screening potential candidate additive materials to control UN microstructure using steam oxidation TGA. From these candidates, yttrium was selected based on corrosion resistance, which led to attempts to develop a method for liquid phase sintering of yttrium with UN. Yttrium in the form of yttrium dihydride (YH 2 ) was mixed with UN, pressed, and heated to temperatures above the melting point of Y metal to dehydride the material and then melt it to enable liquid phase sintering. Results showed no indication of densification, but did show chemical interaction between Y and UN, resulting in the formation of yttrium nitride (YN) and uranium metal. These observations were used to develop a better understanding of microstructure control for UN waterproofing to be addressed in an L2 milestone that is an FY19 deliverable (M2FT-19LA020201021).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2019

Microstructural evolution of thin polycrystalline metallic films under extreme conditions

Thin films are materials systems that are widely used in applications ranging from electronics and optical devices to industrial and biomedical ones. However, these systems are unstable against various homogenization processes and aging mechanisms (grain growth, coarsening, surface evolution, and diffusion of species) even at low service temperatures. In this work, we examine the role of various aspects of microstructure (grain boundary types and characters, free surfaces, surface diffusion, and thermal grooves) on the thermal aging of such systems. Existing experimental tools will be leveraged to characterize thin films, i.e., in-situ quantitative thermal annealing, and provide direct comparisons to predications emerging from a recently developed meso-scale model via Precession Electron Diffraction (PED). Parametric studies will be conducted to gain insights on the role of each of the aforementioned aspects of microstructure on the dynamics. Herein, we will focus on “hard” gold thin films (with alloying elements like Co, Ni, or Fe) as they are materials of choice in a wide range of applications at Sandia. Initially, pure gold systems are examined and future studies will focus on microstructure evolution in the presence of alloying elements and second-phase particles.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Improving Microstructural Quantification in 3D FIB-SEM Tomography

A detailed understanding of 3D microstructural features is crucial during postprocessing of the acquired data, while determining microstructural properties. Focused ion beam and scanning electron microscopy (fib-sem) is an ideal technique for the acquisition and quantification of 3D microstructures in subsurface features. In this work, we evaluated and implemented approaches to quantify 3D morphological features of plutonium oxalate and oxide particles. Image analysis, as well as statistical analysis were utilized to study the effect of process variables on the pore morphology of plutonium oxalate and oxide particles. The primary results were the creation of morphological maps of particles and identify indicators that correlated parameters allowing for discrimination between direct and reverse strike processes. This enabled us to properly quantify and map particles with their images obtained via sem. For this project, the highest correlation was found to be between Volume and Sphericity (R 2 = 0.7432) for the Revere Strike process, and Volume % and Sphericity (R 2 = 0.7450) for the Direct Strike process.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Microstructural Characterization of Alloy 709 Plate Materials with Additional Heat Treatment Protocol

This report provides the results on microstructural characterization of the first commercial heat of Alloy 709 plate material which has undergone additional heat treatment protocol. The report is a Level 4 deliverable in FY19 (M4AT-19AN020502012), under the Work Package AT19AN0205201, “A709 Development – ANL.” The study involves thermodynamic-kinetic modeling, heat treating of materials, microhardness testing, x-ray diffraction (XRD) study, scanning electron microscopy (SEM), and transmission electron microscopy (TEM) study. Through thermodynamic-kinetic modeling, it is determined that after an 1100°C solutionizing treatment, heat treating of Alloy 709 at 775°C for 10 hours or at 900°C for 10 hours are candidate recipes for promoting desired microstructural features. Both heat treatments were executed on small samples of the AOD-1100°C condition of the commercial heat of Alloy 709. Micro-hardness tests showed that both treatments increases the hardness of the material. XRD showed that both treatments brings out M23C6 and MX phases, though the 775°C/10h-treatment has more profound effect. The TEM study revealed that similar for both conditions, M23C6 precipitated on grain boundaries and within grain interior. In contrast, after the 775°C/10h treatment, the dislocations are decorated with MX nano particles, while after the 900°C/10h treatment, most of the dislocations are free of MX particles. It is thus determined that the 775°C/10h treatment has a better potential to provide enhanced creep properties by pinning the dislocations with nano particles. Following this study, the 775°C/10h treatment was carried out on a large ESR-1100°C plate at Idaho National Laboratory. Hardness testing and microstructural characterization were performed and compared between the two materials being heated treated under the same protocol. The implication on mechanical properties was briefly discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Survey of Modeling and Simulation Techniques for Advanced Manufacturing Technologies Volume I – Predicting Initial Microstructures

This report summarizes the current state of modeling and simulation methods for predicting the initial structure and properties of material in components assembled using advanced manufacturing technologies (AMTs). The report is the first volume in a two-volume series. This first volume focuses on predicting initial microstructures of AM material. The second volume discusses predicting material properties given the initial microstructure. The focus is on technologies of particular relevance to the design and manufacture of nuclear reactor components. The purpose of the report is to help develop the technical knowledge base to support regulatory decisions that will be needed to assess nuclear components manufactured with AMTs as these components are installed at nuclear power plants (NPPs). The report develops a list of AMTs of particular interest to the NRC and summarizes the key microstructural features and corresponding processing parameters relevant to each technology. Further sections describe available physically-based and data-driven prediction methods and survey widely available software tools. The report concludes with a summary of gaps that may be of particular interest to the NRC when evaluating modeling and simulation methods for AMTs.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗