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At least 1,261 records · Page 70
All sourcesNASA NTRSDOE OSTI
NASA NTRS2024

Constraining the Thermal and Textural Evolution of Evolved Achondrite DOM 10100: Implications for Volatile Loss

Identification of evolved achrondritic clasts suggests that some early planetesimals experienced extensive differentiation and formed chemically evolved crusts. Many of these samples contain volatile-bearing phases (i.e., apatite, merrillite, nominally anhydrous minerals), which can be used to constrain volatile budgets and abundancies via in-situ measurements. These ancient crustal rocks are subject to high heat, moderate pressures, potentially hot mineral-rich fluids, and degassing that has likely modified many of these volatiles, and their abundancies do not represent the composition of the primary magma from which these achondrites formed. In this work we attempt to deconvolve the thermal evolution of these samples to provide petrologic information that can be used for making inferences regarding their volatile history, and ultimately constraining volatile budgets on planetary bodies in the early Solar System. Here, we combine in-situ major element geochemistry, thermodynamic modeling, and detailed textural and microstructural observations to reconstruct the thermal and textural evolution of howardite DOM 10100, which contains a dacite within its matrix. Previous analyses of several sections of DOM 10100 suggest that the dacitic clast is evidence for partial melting of Vesta’s differentiated basaltic crust, making it an ideal candidate for evolved crustal studies. While its igneous petrogenesis has been well constrained, there is still opportunity to better characterize its post-crystallization thermal history, including possible thermal metamorphism and cooling.

J S Gorce↗
DOE OSTI2025

Evolution of dislocations during the rapid solidification in additive manufacturing

Materials processed by fusion-based additive manufacturing (AM) typically exhibit relatively high dislocation densities, along with cellular structures and elemental segregation. This representative structural feature significantly influences material performance; however, post-mortem microstructure characterizations of AM materials cannot capture the dynamic evolution of dislocations during the manufacturing process, thereby offering limited mechanism-based guidance for further advancing AM techniques and facilitating the qualification and certification of AM products. In this study, we conduct operando high-energy synchrotron X-ray diffraction experiments on wire-laser directed energy deposition of 316 L stainless steel. Through a unique configuration, our operando synchrotron experiments semi-quantitatively probe the dislocation density in solid phases and their dynamic changes during solidification and subsequent cooling. By integrating this advanced synchrotron technique with multi-physics simulation, in-situ neutron diffraction, and multi-scale electron microscopy characterization, our mechanistic study aims to elucidate the effects of rapid cooling and subsequent thermal cycling on the dislocation generation and evolution.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Investigation of residual stress distribution in wire-arc directed energy deposited refractory molybdenum alloy utilizing numerical thermo-mechanical analysis and neutron diffraction method

Directed energy deposition (DED), a metal additive manufacturing (AM) technique, offers higher deposition rates and energy efficiency, making it suitable for fabricating components from refractory molybdenum alloys, such as molybdenum-titanium-zirconium (TZM). However, large thermal gradients and non-equilibrium thermal cycles in DED could generate high residual stress in the component, potentially deteriorating quality and performance. Thus, this study aims to investigate residual stress generation and its distribution in wire-arc DED of TZM thin-wall, utilizing thermo-mechanical analysis and high-fidelity neutron diffraction (ND) method. Two interpass temperatures (50°C and 200°C) have been considered to investigate their impact on residual stress formation. During experiments, in-situ thermal data has been recorded using thermocouples, which have been utilized for calibrating the thermal model. Thermocouple data shows a good agreement with the simulation results, having a difference of less than 10 %. Post-deposition part deformation has been observed, which is measured using a coordinate measuring machine, showing maximum values of 0.93 mm and 0.78 mm for interpass temperatures of 50°C and 200°C, respectively. Numerical predictions of distortion deviated by less than 15% from the experimental results. ND measurement and simulation results indicate that residual stress magnitude and evolution vary across the TZM deposits, revealing microstructural anisotropy in both conditions. Notably, lower interpass temperatures resulted in higher residual stresses, confirmed by experimental and simulation data. Further, this study demonstrated that an integrated experimental and thermo-mechanical analysis can potentially reveal the temperature history, part deformation, and residual stress formation in wire-arc DED TZM alloy.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Disentangling ferroelectric domain wall geometries and pathways in dynamic piezoresponse force microscopy via unsupervised machine learning

In this work, domain switching pathways in ferroelectric materials visualized by dynamic piezoresponse force microscopy (PFM) are explored via variational autoencoder, which simplifies the elements of the observed domain structure, crucially allowing for rotational invariance, thereby reducing the variability of local polarization distributions to a small number of latent variables. For small sampling window sizes the latent space is degenerate, and variability is observed only in the direction of a single latent variable that can be identified with the presence of domain wall. For larger window sizes, the latent space is 2D, and the disentangled latent variables can be generally interpreted as the degree of switching and complexity of domain structure. Applied to multiple consecutive PFM images acquired while monitoring domain switching, the polarization switching mechanism can thus be visualized in the latent space, providing insight into domain evolution mechanisms and their correlation with the microstructure.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2020

Multi stage and illumination dependent segregation in MAPb(I,Br)3

© COPYRIGHT SPIE. Downloading of the abstract is permitted for personal use only. An unsolved problem of mixed halide perovskites is the light induced compositional instability. Under illumination microscopic clusters with a higher iodide content form which act as efficient recombination centers reducing device performance. In photoluminescence measurements this leads to the development of a secondary peak at low energies that increases in intensity and shifts towards lower energies. Different theories for about the origin have been developed but the underlying key mechanisms are still under debate. In the presented study the photoluminescence evolution of MAPb(I1.5Br1.5) perovskites with varying microstructure is investigated at various excitation densities and temperatures. We find a more evolved segregation mechanism with an intermediate stage between the commonly reported mixed phase and the appearance of the I-rich clusters (Br content < 50%). In this intermediate stage perovskite domains with nearly pure iodide content form (Br content < 25%). Using low excitation densities, the interplay between the I-rich domains and the I-rich clusters leads to a blue shift of the conjunct I-rich luminescence peak. At high excitation densities the I-rich domains and the I-rich clusters are clearly distinguishable, due to a stronger PL response of the I-rich domains. With continuous illumination more I-rich cluster form acting as carrier traps and recombination centers. Due to this, the influence of the few I-rich domains on the PL signature decreases leaving only the commonly reported red shift of the I-rich clusters at later stages of the segregation. The formation of the I-rich domains is fully reversible in the dark and occurs also at elevated temperatures. Measurements on sample with varying grain size further indicate an enhanced formation of those I-rich domains on samples with high grain boundary density possibly by a faster halide mobility along them.

Babbe, F↗
DOE OSTI2021

Experimental Evaluation of Deformation and Fracture Mechanisms in Highly Irradiated Austenitic Steels

The present report documents recent experimental results of analysis using scanning electron microscopy/electron backscatter diffraction (SEM-EBSD) of plastic deformation mechanisms and strain localization phenomena in austenitic steels irradiated by neutrons. Experiments were performed with specimens irradiated to 125 dpa and, additionally, with specimens that experienced radiation-induced swelling up to 3%. Section 1 briefly analyzes the deformation localization in irradiated steels and its consequences on the material performance. The section describes the advantages and importance of the SEM-EBSD approach combined with in situ mechanical testing capability. Section 2 briefly introduces the experimental tools and methods (i.e., SEM/EBSD in situ tensile frame, electric discharge machine to manufacture irradiated specimens) and describes the investigated materials (i.e., element composition, irradiation conditions, and general microstructure). Section 3 describes the key experimental results and provides a brief analysis and comparison with the datasets obtained earlier within the same task (i.e., low-dose specimens). The discussion focuses on EBSD microstructure maps with strain localization features, misorientation evolution as a function of strain, and observed deformation mechanisms. Section 4 evaluates data collected in recent years on highly irradiated steel and estimates the possible misorientation evolution under irradiation. The section introduces and discusses the concept of in-service-induced damage as an irradiation-assisted stress-corrosion cracking precursor. Section 5 summarizes the work performed. As expected, the present work results are beneficial for exploring and understanding degradation mechanisms in highly irradiated in-core materials found in light water reactors after long-term in-service life.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
NASA NTRS2000

Nonprotective Alumina Growth in Sulfur-Doped NiAl(Zr)

The 1200 C oxidation behavior of NiAl was examined at various levels of sulfur and zirconium dopants to test the possibility of a critical S/Zr ratio required for adhesion. Cyclic furnace testing for 200 1 -hr cycles and interrupted testing for 500 hr were used as screening tests. Pure NiAl and NiAl(Zr) with 0. 14 at.% Zr were chosen as model base compositions; they exhibited normal, slow-growing scales (3 Mg/sq cm) with excellent adhesion for the Zr-doped alloys. NiAl with about 120 ppma S exhibited a substantial weight loss (-20 Mg/sq cm) in cyclic tests and a very large weight gain (+60 Mg/sq cm) in interrupted tests. The major surface phase remained as alpha -Al2O3. Sulfur doping the NiAl(Zr) alloy caused massive weight gains of 80 - 100 Mg/sq cm, swelling, cracking, and nearly complete conversion into NiAl2O4, and alpha- Al2O3. The initial objective of determining critical S/Zr ratios for adhesion was therefore unattainable. Initiation of the catastrophic attack was examined after a 10 hr exposure, revealing a few sites of broad, raised, and cracked ridges. In cross-section, the ridges appeared as modular intrusions, with a complex, fractal, oxide-metal interface. They were primarily alumina (with occasional entrapped islands of NiAl2O4 or pure Ni metal). They possessed a unique microstructure consisting of 0.3 microns lamellae, separated by 0.1 microns open channels. This allowed for rapid growth controlled by gaseous diffusion. The microstructure is discussed in terms of SO2 evolution and a sulfur-driven de-passivation process.

Smialek, James L.↗
DOE OSTI2021

Process Robustness of Friction Stir Dovetailing of AA7099 to Steel with In Situ AA6061 Interlayer Linking

Rolled homogeneous armor (RHA) steel was joined to aluminum alloy AA7099-T7451 with an interlayer of AA6061-T651 by single-pass friction stir dovetailing (FSD). The evolution of the AA7099/AA6061 and AA6061/steel interfacial microstructures and mechanical properties of the joints were examined. The AA6061 interlayer prevented Zn migration from the AA7099 to the steel during FSD and inhibited formation of brittle, Zn-rich, Fe-Al intermetallic compounds within the joint. The flow of the dissimilar aluminum alloys at the interface was controlled with a partially threaded friction stir welding pin and a dovetail geometric configuration optimized in previous work. The process robustness was explored to establish parameter windows by elucidating parametric effects on the relationship between process conditions and the joint’s microstructure and mechanical properties. Ranges of process forge force (50–70 kN) and interface temperature (475°C–515°C) consistently yielded joints with adequate performance. The load-carrying capacity in lap shear tensile tests was 2025 ? 100 N/mm.

Friction Stir Dovetailing, FSW, AA7099, AA6061, Ro↗
DOE OSTI2022

Combined DSC/TGA Analysis to Rationalize the As-Sintered Microstructure in Binder Jet Additively Manufactured H13 Tool Steel

In this study, a combined DSC/TGA analysis has been used to rationalize the constant liquid channel width at higher sintering temperatures in H13 tool steel manufactured by binder jet additive manufacturing. Using enthalpy conservation along with coupled DSC + TGA analysis, the phase fractions of liquid and austenite phases during heating and cooling respectively were estimated. The estimates from the DSC/TGA analysis were compared with equilibrium phase fraction predictions from ThermoCalc. The resulting phase evolution was correlated to the as-sintered microstructure to rationalize the unexpected lack of change in liquid channel width at higher sintering temperatures.

Kannan, Rangasayee↗
DOE OSTI2019

How Microstructure and Pore Moisture Affect Strength Gain in Portlandite-Enriched Composites That Mineralize CO 2

Binders containing portlandite (Ca(OH) 2 ) can take up carbon dioxide (CO 2 ) from dilute flue gas streams (<15% CO 2 , v/v), thereby forming carbonate compounds with binding attributes. While the carbonation of portlandite particulates is straightforward, it remains unclear how CO 2 transport into monoliths is affected by microstructure and pore moisture content. Therefore, this study elucidates the influences of pore saturation and CO 2 diffusivity on the carbonation kinetics and strength evolution of portlanditeenriched composites (“mortars”). To assess the influences of microstructure, composites hydrated to different extents and conditioned to different pore saturation levels (S w ) were exposed to dilute CO 2 . First, reducing saturation increases the gas diffusivity and carbonation kinetics so long as saturation exceeds a critical value (S w,c ≈ 0.10) independent of microstructural attributes. Second, careful analysis reveals that both traditional cement hydration and carbonation offer similar levels of strengthening, the magnitude of which can be estimated from the extent of each reaction. As a result, portlandite-enriched binders offer cementation performance that is similar to traditional materials while offering an embodied CO 2 footprint that is more than 50 % smaller. Furthermore, these insights are foundational to create new “low-CO 2 ” cementation agents via in situ CO 2 mineralization (utilization) using dilute CO 2 waste streams.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Synergistic Evolution of Segmental Motion and Cooperative Relaxation within the Amorphous Phase of Organic Mixed Ionic-Electronic Conductors

Organic mixed ionic-electronic conductors (OMIECs) facilitate a variety of electrochemical processes and feature a heterogeneous microstructure composed of both crystalline and amorphous phases. However, structural evolution in amorphous regions during electrochemical doping remains poorly understood, limiting our understanding of mixed conduction mechanisms. Here, in this work, we develop operando chip calorimetry to probe amorphous phase evolution in poly­(3,4-ethylenedioxythiophene):poly­(styrenesulfonate) (PEDOT:PSS) under swelling and electrochemical (de)­doping. Our results reveal that amorphous regions providing ionic transport pathways and those within electronic transport channels undergo heterogeneous, yet synergistic, evolution during electrochemical modulation. The cooperative interplay between segmental motion and relaxation maintains ionic conductivity and intergrain electronic transport upon electrowetting and doping, while facilitating efficient ion hopping and adaptable chain conformations during dedoping. Such synergies are more pronounced in loose structures featuring a fibrillar morphology, which exhibit lower glass transition temperatures (T g ) and higher fragility (m). High-throughput robotic screening further establishes a strong correlation between elevated m/T g ratios and enhanced mixed conduction. These findings elucidate the role of the amorphous phase in the synthesis of OMIECs and underscore the potential of operando chip calorimetry in uncovering structure–property relationships in electroactive polymers.

amorphous phase↗
DOE OSTI2025

The effect of heat treatment on the defect evolution in LPBF 316H stainless steel

This work investigates the effect of processing and heat treatment on defect evolution and irradiation response of laser powder bed fusion (LPBF) 316H stainless steel, with comparisons to LPBF 316L and wrought 316L/316H. Using in-situ and ex-situ ion irradiations across a wide parameter space—temperature (300–675 °C), dose (0.2–25 dpa), dose rate (10 -3 –10 -5 dpa/s), and helium co-implantation (20–2500 appm)—we correlated void swelling, dislocation loop evolution, and segregation behavior with pre-irradiation microstructures (as-built, stress-relieved, solution-annealed, and cold-worked). Results show that swelling is strongly controlled by dislocation density: intermediate densities maximize swelling, while solution annealing or cold working reduce susceptibility to levels comparable to wrought alloys. Low dose rates and helium both promote cavity nucleation and lower the incubation barrier, with helium suppressing the role of dislocation density and driving swelling behavior toward wrought-like response. Loop evolution in SA LPBF 316H resembles wrought 316L but shows localized denuded zones near low-angle grain boundaries. STEM-EDS mapping further revealed Ni segregation at voids and sparse Al-rich oxides, without evidence of Ni–Si precipitates. Collectively, these findings identify dislocation density, helium content, and dose rate as the factors governing swelling in LPBF 316H and provide mechanistic datasets for model validation, supporting LAIN and the qualification of AM austenitic steels for nuclear service.

316 stainless steel↗
DOE OSTI2025

Visualizing diverse lithium growth and stripping behaviors in anode-free solid-state batteries with operando X-ray tomography

Anode-free solid-state batteries (SSBs), which eliminate the need for lithium metal use during cell assembly, have the potential to enable high energy densities and simplified manufacturing. However, the factors that control lithium growth/stripping at the anode current collector are not well understood. Here, we use operando X-ray microcomputed tomography to comprehensively image and quantify lithium deposition and stripping under various conditions in three different Li|Li 6 PS 5 Cl|current collector cells, revealing diverse behavior that depends on interface morphology, cell resistance, and solid-state electrolyte (SSE) microstructure. A cell with high resistance exhibits extensive lithium filament growth across the entire current collector interface, with filaments that grow around pre-existing pores in the SSE rather than lithium filling these pores. Lithium filament formation is partially reversible, with the cracks shrinking as lithium metal is stripped. Uniform lithium deposition is achievable at low current densities in low-resistance cells, whereas higher current densities in these cells cause an increase in interfacial roughness, which is correlated with subsequent filamentary growth at the edges of the cell. These results provide insight into filamentary vs. planar lithium growth and highlight that the evolution of lithium is sensitively dependent on SSE microstructure and electrochemical processes.

25 ENERGY STORAGE↗
DOE OSTI2020

In-Operando Study of Shape Retention and Microstructure Development in a Hydrolyzing Sol–Gel Ink during 3D-Printing

3D printing of amorphous and crystalline ceramics is of paramount importance for the fabrication of a wide range of devices with applications across different technology fields. Printed ceramics are remarkably enabled by the sol-gel synthesis method in conjunction with continuous filament direct ink writing. During printing, multiple processes contribute to the evolution of inks including shape retention, chemical conversion, solidification, and microstructure formation. Traditionally, depending on the ink composition and printing environment, several mechanisms have been associated with the shape retention and solidification of 3D printed structures: gelation, rapid solvent evaporation, energy-driven phase transformation, and chemical-driven phase transformation. Understanding the fundamental differences between these mechanisms becomes key since they strongly influence the spatiotemporal evolution of the materials, as the out-of-equilibrium processes inherent to the extrusion, relaxation, and solidification of printed materials have significant effects on the materials properties. Herein, we investigate the shape retention mechanism and the hydrolysis-induced material conversion and microstructure formation during the 3D printing of a water reactive sol-gel ink that transforms into titanium dioxide-based ceramic. This study aims at identifying characteristic mechanisms associated with the material transformation, establishing connections between the microstructure development and the timescales associated with solidification under operando 3D-printing conditions. The investigation of this material's out-of-equilibrium pathways under processing conditions is enabled by time-resolved coherent X-ray scattering, providing simultaneous access to temporospatially resolved microstructural and dynamics information. Furthermore, we explore X-ray speckle tracking as a tool to resolve deformations of the microstructure in a printed filament associated with the deposition of consecutive filaments. Through this work, we aim at providing a fundamental understanding of the relationships behind these transformative processes in 3D printing and their timescales as the basis for achieving unprecedented control over printed materials microstructure.

36 MATERIALS SCIENCE↗
NASA NTRS1982

Irradiation effects in rapidly and conventionally solidified alloys. Phase stability in rapidly solidified N i-Nb under Ni ion irradiation

Two alloy compositions in the Ni-Nb system (Ni60Nb40 and Ni85Nb15) were produced by rapidly quenching from the melt with the piston anvil technique. The Ni60Nb40 was transformed to a metastable, partially crystalline state by heat treatment in a differential scanning calorimeter. The Ni85Nb15 was fully crystalline, with the majority of the grains composed of collections of primary dendrite arms. Both compositions were irradiated with 4 MeV Ni++ ions. The irradiation induced microstructures were examined by transmission electron microscopy and compared with thermally aged samples. The thermal evolution was arrested by ion irradiation in the temperature range studied, by inhibiting the nucleation of the NiNb phase. No irradiation induced voids were observed. It is found that the ion irradiation drives the microstructure along a different path than thermal evolution.

Source record↗
DOE OSTI2024

Development of a MOOSE-based crystal plasticity model with irradiation defect evolution for irradiation creep in 316

Irradiation creep and irradiation swelling are two of the lifetime limiting factors for structural materials in nuclear reactors. These mechanical effects are driven by irradiation defect evolution and the interaction of those defects with dislocations in the microstructure. We present here a coupled cluster dynamics – crystal plasticity approach to model irradiation swelling and creep behavior in 316 SS. The time-dependent evolution of irradiation defects is calculated with a cluster dynamics approach and passed to the crystal plasticity model to compute the dislocation evolution. We show the impact of the irradiation defect evolution on the stress state in the material, which drives inelastic deformation through dislocation motion. The inelastic deformation in the 316 SS is dependent on the dose rate, where the inelastic deformation driven by the early-stage irradiation defect evolution determines the mechanical behavior of the 316 SS.

316 Stainless Steels↗
DOE OSTI2022

Virtual texture analysis to investigate the deformation mechanisms in metal microstructures at the atomic scale

Understanding the deformation behavior of metallic materials at high strain rates requires the characterization of plasticity contributors such as twins, phase transformed regions, and dislocations. However, predicting the contributions from phase transformation and twinning relies on a complete understanding of the selection of variants for various loading orientations and the evolution of their volume fractions. This manuscript presents a new virtual texture (VirTex) analysis approach to characterize phase transformation and twinning variants in deformed microstructures generated using molecular dynamics (MD) simulations. Furthermore, the VirTex method involves the construction of a rotation matrix to calculate the angle/axis pairs and misorientation angles for each atom in the microstructure. Any changes in the orientation angle from angle/axis pairs and/or structure types are analyzed to determine the nucleation and evolution of variants in the microstructure. The study uses shock deformed single-crystal Fe, Ta, and Cu to analyze the variant selections for phase transformation or twinning or both in BCC and FCC systems. In addition, the VirTex analysis is able to characterize the phase transformation and twinning variants in nanocrystalline Fe and Ta microstructures. Besides characterizing variants, orientation mapping also provides an accelerated and on-the-fly approach for quantifying twin fractions in MD microstructures.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Report on Evolution of Inconel 718 Following HFIR Irradiation

The report presents the microstructure and mechanical properties of 3D printed Inconel 718 after irradiation in the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory (ORNL) to assess its potential use as a structural material. The structural components near the outlets of several proposed reactor cores will experience significant neutron fluxes and outlet coolant temperatures ranging from the hot standby temperature of 300 °C to nearly 550 °C at the center of the part. These components must support the core in appropriate loading conditions and require structural analysis at relevant temperatures. In FY21, three heat treatments were designed and conducted to simplify the microstructure and to determine how each precipitating phase contributed to the overall strength. In FY21, baseline mechanical properties were measured from uniaxial tensile tests on subsize SS-J2 specimens at room temperature and at elevated temperatures of 300, 450, and 600 °C to serve a comparison to the irradiated properties. Four capsules containing 3D printed Inconel 718 were inserted into HFIR in FY21 for a matrix of two temperatures and two doses. The lower of the two doses was available for characterization in FY22. Multiple heat treatments of Inconel 718 irradiated to nominal conditions of 2 displacements per atom (dpa) at either 300 or 600 °C were strained with uniaxial tensile tests at the Irradiated Material Examination and Testing (IMET) Facility to discern the mechanical properties. Transmission electron microscopy was performed to correlate the observed mechanical properties with nanoscale features. The initially homogenous AM718-HM increased in strength at both irradiation temperatures based on a high density of nanometer-scale radiation-induced cavities at lower temperature and nucleation and growth of γ" precipitates at higher temperatures. The precipitate-hardened AM718-HT2 showed very small differences in strength before and after irradiation: the contribution to strength from γ" precipitates was replaced with dislocation loops. Because the radioactivity of the nickel superalloys from neutron activation limited the scope of the analysis, a feasibility study examined the possibility of an ultra-miniature specimen geometry, colloquially SS-Tiny (SS-T), for mechanical property determination using the nonirradiated Inconel 718. This study found an overestimation of ductility from the SS-T geometry with yield strength and ultimate tensile strength slightly above the SS-J2 geometry: this could be contributed to a reduction in specimen thickness.

36 MATERIALS SCIENCE↗