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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 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Searching for a route to synthesize in situ epitaxial Pr 2 Ir 2 O 7 thin films with thermodynamic methods

In situ growth of pyrochlore iridate thin films has been a long-standing challenge due to the low reactivity of Ir at low temperatures and the vaporization of volatile gas species such as IrO 3 (g) and IrO 2 (g) at high temperatures and high P O2 . To address this challenge, we combine thermodynamic analysis of the Pr-Ir-O 2 system with experimental results from the conventional physical vapor deposition (PVD) technique of co-sputtering. Our results indicate that only high growth temperatures yield films with crystallinity sufficient for utilizing and tailoring the desired topological electronic properties and the in situ synthesis of Pr 2 Ir 2 O 7 thin films is fettered by the inability to grow with P O2 on the order of 10 Torr at high temperatures, a limitation inherent to the PVD process. Thus, we suggest techniques capable of supplying high partial pressure of key species during deposition, in particular chemical vapor deposition (CVD), as a route to synthesis of Pr 2 Ir 2 O 7 .

Chemistry↗
DOE OSTI2021

Evolution of Metastable Phases During Mg Metal Corrosion: An In Situ Cryogenic X-ray Photoelectron Spectroscopy Study

Magnesium and its alloys are potential structural materials candidates for a wide variety of applications due to their high strength-to-weight ratio. However, ductility and poor corrosion resistance under ambient environmental conditions are the bottleneck for industrial deployment. Designing passivation layers and/or corrosion resistant alloys requires fundamental understanding of the corrosion process. The traditional ex-situ spectroscopic measurements of polycrystalline metal surface with ubiquitous surface impurities and grain boundaries only provided an indistinct view of the corrosion process. To clearly distinguish the mechanism and sequence of corrosion process, we employed in-situ cryo-based x-ray photoelectron spectroscopy (XPS) measurements on Mg single crystal surface exposed to aqueous salt solution. Clean Mg (0001) surfaces were exposed to pure D2O and NaCl aqueous solution (5 wt% NaCl+95 wt% D2O). The interfacial reactions were studied using multimodal analysis including XPS, x-ray diffraction (XRD) and scanning electron microscopy (SEM). In contrast to previous studies, our experiments demonstrated the formation of magnesium chloride hydroxide hydrate during aqueous salt corrosion processes. Evidence of metastable ClO* radicals were also found during the initial aqueous salt solution exposure.

Shutthanandan, Vaithiyalingam↗
DOE OSTI2021

In Situ Transmission Electron Microscopy of High-Temperature Inconel-625 Corrosion by Molten Chloride Salts

This paper describes an approach to monitor high temperature molten chloride (MgCl 2 -NaCl-KCl) salt corrosion of Inconel-625 alloy in real time at high spatial resolution. The approach is based on a micro-environmental-cell assembly integrated into a transmission-electron-microscope goniometer to examine in situ the salt-alloy interface during corrosion, employing real time electron diffraction and imaging. It establishes procedures to minimize incorporation of H 2 O or O 2 from atmosphere in the chloride salts during sample fabrication and corrosion, which is critical to understanding the fundamental corrosion mechanisms. A clustering algorithm and a 2D Gaussian fit function are used to determine diffraction spot intensities in in situ diffraction patterns, to quantify alloy corrosion. This facilitates quantitative observation of the evolution of individual grains, in contrast to conventional macroscopic corrosion rate quantification. The isothermal corrosion rate of Inconel-625 in an anhydrous, unoxidized salt-stack is 220 ± 30 μm year -1 at 700 °C and 350 ± 20 μm year -1 at 800 °C. However, the corrosion rate at 700 °C increases five-fold to 1000 ± 170 μm year -1 when the salt stack is air-exposed, indicating the dominant effects of hydrated or oxidized impurities on corrosion acceleration. Furthermore, real time imaging of the microstructure evolution suggests that corrosion is initiated at grain boundaries.

14 SOLAR ENERGY↗
DOE OSTI2021

Visualizing time-dependent microstructural and chemical evolution during molten salt corrosion of Ni-20Cr model alloy using correlative quasi in situ TEM and in situ synchrotron X-ray nano-tomography

In situ monitoring of corrosion processes is important to fundamentally understand the kinetics and evolution of materials in harsh environments. A quasi in situ transmission electron microscopy technique was utilized to study microstructural and chemical evolution of a Ni-20Cr disc sample 6 exposed to molten KCl-MgCl 2 salt for 60 s in consecutive 20 s iterations. In situ synchrotron X-ray nano-tomography was performed to characterize the morphological evolution of a Ni-20Cr microwire exposed to molten KCl-MgCl 2 . Here, both techniques captured key corrosion events and revealed mechanisms at different time and length scales, potentially bringing greater insights and 10 deeper understanding beyond conventional analysis.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Virtual diffraction simulations using the quasi-coarse-grained dynamics method to understand and interpret plasticity contributions during in situ shock experiments

The dynamic deformation response of metallic materials has contributions from dislocations, deformation twinning, and plastic deformation. The current state-of-art techniques can detail the complex mechanistic history of deformation modes under shock loading in real-time using in situ X-ray diffraction (XRD). However, the capability of these experiments to unravel plasticity contributions is challenging due to limitations in interpreting results and the lack of validation from atomistic simulations. Molecular dynamics (MD) simulations can successfully capture various deformation modes in metals and complement experiments using simulated diffractograms at various stages of evolution. However, the difference in length and time scales of MD simulations and experiments is a substantial obstacle in completing and interpreting in situ diffractograms. Therefore, the existing modeling methods require various approximations to model defect evolution and interaction at the mesoscales. However, while using approximations to correlate the peak broadening behavior to the density of dislocations or the shifts/splitting due to the presence of twins, the interpretations of the plasticity contributions from diffractograms are non-trivial, especially when multiple modes of deformation may be operating. This viewpoint discusses combining a mesoscale modeling method called quasi-coarse-grained dynamics and virtual XRD to characterize the plasticity contributions in BCC metals from slip, twinning, and phase transformation behavior. Furthermore, the combined approach shows promise in bridging the mesoscale gap between the capabilities of atomic-scale simulations and in situ experiments to characterize the dynamic deformation of materials.

36 MATERIALS SCIENCE↗
DOE OSTI2025

A co-registered in-situ and ex-situ dataset from wire arc additive manufacturing process

Recent progress in sensing techniques and data analytics tools have significantly accelerated the development of Wire Arc Additive Manufacturing (WAAM) systems. This data-centric approach emphasizes leveraging sensor data available throughout the production process to optimize performance. Integration of extensive data analysis provides opportunities for improving precision, reducing waste, and enhancing the quality of produced parts. This method relies on AI/ML models and optimization techniques, which are developed using the data collected from various sources, including in-situ sensors, ex-situ imaging, and manufacturing process parameters. The quality and diversity of this data, along with the alignment between different data streams (achieved through spatiotemporal registration) are critical for the successful development of AI/ML and optimization models. In this work, we present a spatiotemporally registered dataset generated during the WAAM process of deposition of a rectangular block. The dataset includes a comprehensive description of the deposition process, process parameters, welding characteristics and acoustic data collected in-situ, and X-Ray Computed Tomography data of the build.

42 ENGINEERING↗
DOE OSTI2023

In-situ and ex-situ characterization of ion-irradiated AM materials

Additive manufacturing (AM) has attracted increasing attention in recent years as a new way of making high-quality components for nuclear reactors. While AM materials are compositionally similar to their conventionally produced counterparts, they do possess different microstructures, such as dislocation cells and chemical inhomogeneity, that can lead to different mechanical properties and performance behavior. In this study, the irradiation response of AM materials was investigated. In-situ and ex-situ ion irradiations were performed on AM316L and AM316H stainless steels (SS) at 300 and 600°C. The influence of the dislocation cell structure on the evolution of irradiation-induced dislocation loops was evident at 600ºC, but was much weaker at 300ºC. No voids were observed with the in-situ ion irradiation up to 10 dpa at both temperatures. Post-irradiation energy dispersive spectroscopy showed radiation-induced segregation (RIS) near grain boundaries and the formation of Cr-rich oxides throughout the matrix. The extent of segregation at dislocation cell walls varies with dose. Nanoindentation tests performed on the AM316L SS irradiated at 600ºC showed a complex dose dependence with softening at low doses and hardening at high doses.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2024

In-situ and ex-situ characterization of irradiated AM materials

This study investigates the irradiation performance of laser powder bed fusion (LPBF) 316L and 316H stainless steels (SS), and their wrought counterparts. While LPBF 316L has been more studied, LPBF 316H is relatively new, with little prior data on its irradiation behavior. The research involved fabricating, preparing, irradiating, and characterizing six materials: LPBF 316L (two variants), LPBF 316H (two variants), and wrought 316L and 316H. LPBF materials were subjected to various heat treatments, including solution annealing and stress relief, and were irradiated using in-situ and ex-situ ion techniques at temperatures of 300°C and 600°C, with doses ranging from 0.2 dpa to 25 dpa. Under ex-situ irradiation with 4 MeV Ni 2+ ions at 600°C, the dislocation cell structures in LPBF316L-1 and LPBF316H-1 gradually evolved into a uniform dislocation network. At a low irradiation dose (0.2 dpa), the cell structures were still partially visible. At 2 dpa, a uniform dislocation network formed, though remnants of the original cell structure were still discernible as contrast domains. At 5 dpa and 10 dpa, even the contrast domains vanished. For irradiation at 300°C, the cell structure was still clearly visible at 0.2 dpa for LPBF316L-1. For LPBF316H-1, the dislocation cell structure was less apparent at the same dose but was still recognizable. With further increase in dose at 300°C, the dislocation cell walls were completely replaced by irradiation-induced defects and no longer visible. Void formation was observed for irradiation at 600°C. At 2 dpa, no evident voids were observed in either LPBF316L-1 or LPBF316H-1.

36 MATERIALS SCIENCE↗
DOE OSTI2021

In situ TEM observation of calcium silicate hydrate nanostructure at high temperatures

Fire poses a substantial threat to concrete structures because calcium silicate hydrate (C-S-H) is not thermally stable at high temperatures. Herein, in situ TEM at temperatures from 20 to 800 °C was conducted to study the thermal-induced structural changes in C-S-H. We captured C-S-H shrinks at an average rate of 0.02 μm{sup 2}/{sup o}C upon heating with three stages observed, including induction, constant, and rapid periods. Our observation revealed that an 800 nm pore could be healed during pore structure evolution owing to the reconstruction and deformation among C-S-H blocks. The Ca/Si ratio was dropped at higher temperatures because of the leakage of calcium ions from the C-S-H structure to form CaO precipitates. The temperature-driven phase transformation and degradation were also detected using electron diffraction that C-S-H was transformed into metastable calcium silicate minerals above 800 °C. This work provides insights into the nanoscale transformation of C-S-H at high temperatures.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Direct Observation of Tungsten Oxidation Studied by In Situ Environmental TEM

In this study, in situ environmental transmission electron microscopy (ETEM) was applied, for the first time, to investigate the thermal oxidation of a pristine and a self-ion irradiated polycrystalline tungsten, using a MEMS-based gas cell at 500 oC to 900 oC in a 1 bar 2%O2/N2 gas mixture. By tracking the dynamic evolution of the tungsten oxide scale as it initiates, grows, and sublimates during a consecutive thermal oxidation experiment, we observed two distinctive tungsten oxide microstructure – one nanocrystalline o-WO3 scale grown on W{27-1 } and W{1-1 8} and another o-WO3 scale exhibits a novel highly textured nanostructure. While the two oxide microstructures shared a similar thickness of ~200 nm after 40-minute early-stage oxidation, the nanocrystalline scale on the W{27-1 } grew much more rapidly at 800 oC than the highly textured oxide at a higher temperature of 900 oC. This suggests both the microstructure of these tungsten oxide scales as well as their oxidation kinetics are highly sensitive to the tungsten surface orientation, and such correlations also change dynamically in the course of oxidation. We also discuss the tungsten oxidation mechanism, the effects of the TEM foil thickness, and the focused ion beam (FIB) Ga+ damage on in situ ETEM oxidation.

In situ ETEM, Tungsten, Thermal oxidation, Orienta↗
DOE OSTI2021

Electrochemical and In Situ Spectroscopic Study of the Effect of Prussian Blue as a Mediator in a Solid-State Supercapacitor

In situ X-ray absorption spectroscopy (XAS) along with electrochemical measurements were used to explore the redox activity of Prussian blue (PB) and its contribution to pseudocapacitance in an asymmetrical solid-state supercapacitor (SC). The SC, with a configuration of (activated carbon)/polymer electrolyte membrane/(activated carbon + PB), was fabricated with an embedded KCl saturated Ag/AgCl reference electrode. The potentials of the two electrodes were generally displaced proportionally with increase in the cell voltage. Upon negative polarization from the open circuit voltage (OCV) condition to -3 V, the charge capacity was greater than that upon positive polarization from the OCV condition to +3 V, in agreement with the higher fraction of Fe(III) than that of Fe(II) and the low concentration of K ions in PB. Detailed analysis of cyclic voltammetry data in the range between 0 and -3 V indicates that the battery-like contribution to the charge current was 96% that of the capacitor-like contribution at a scanning rate of 2.5 mV s -1 but only 15% at 100 mV s -1 . The in situ XAS characterization results indicate that the majority of Fe was reversibly charged and discharged between Fe(III) and Fe(II) during positive and negative polarizations with minimal changes in local atomic structure.

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

Evaluating Entrainment–Mixing Characteristics through Direct Comparisons of Drop Size Distributions Using In Situ Observations from ACE-ENA

Abstract Constraining the impacts of entrainment and associated mixing (i.e., entrainment–mixing) on cloud properties continues to be difficult, partly due to observational uncertainties as well as a lacking consensus of which methodologies for diagnosing entrainment–mixing are most appropriate. This study introduces a novel method to evaluate the presence and degree of inhomogeneous and homogeneous mixing using ∼100 h of in situ observations from a research aircraft over the northeastern Atlantic. Specifically, drop size distributions are compared between regions containing negligible and significant entrainment for select flight legs, making a direct characterization of the degree of homogeneous and inhomogeneous mixing possible. A measure of drop concentration variance is used as a proxy variable to diagnose entrainment–mixing. Results correspond well with entrainment–mixing metrics, showing lower Damköhler numbers where drop size distributions shift toward smaller drop sizes (i.e., inhomogeneous mixing) and greater transition length scales where drop size distributions do not (i.e., homogeneous mixing). Inhomogeneous mixing occurs in most samples from Aerosol and Cloud Experiment in the Eastern North Atlantic (ACE-ENA) (regardless of homogeneous mixing frequencies increasing with increasing spatial resolution from ∼100 to ∼10 m) and is associated with decreased drop size relative dispersion and both greater aerosol and drop concentrations compared with homogeneous mixing. Precipitating clouds have a greater frequency of homogeneous mixing compared with nonprecipitating clouds. The proposed methodology is similarly applied to in situ observations of southeast Pacific stratocumulus, shallow convective clouds over central Oklahoma and low-level clouds over the Southern Ocean. All four locations are primarily dominated by inhomogeneous mixing with minimal variability among each region.

Clouds↗
DOE OSTI2024

Spatiotemporally Registered In-Situ and Ex-Situ Datasets for Laser-based Blown Powder Directed Energy Deposition

This dataset is comprised of in situ sensing data collected during laser-based, blown powder directed energy deposition (DED) of Inconel 718 representing eight different printing conditions: (1) nominal, (2) +15% scan speed, (3) +12% laser power, (4) +42% powder feed rate, (5) +100% jerk limit, (6) +10% layer height, (7) +20% hatch spacing, (8) +20% carrier gas flow. All eight DED builds constructed an identical test coupon geometry consisting of geometric features representative of industrial print requirements (e.g., bulk deposition, thin walls, overhangs). In situ data consists of xyz-coordinates (100 Hz) and on-axis melt pool camera video (60 Hz), both of which have been temporally synchronized to spatially map the melt pool camera data. In addition, post-build X-ray computed tomography (XCT) data for each of the eight test geometries have been spatially registered to the recorded xyz-coordinates, allowing for comparisons between melt pool camera data and flaws identified in the XCT data.

additive manufacturing↗
DOE OSTI2025

Characterization of in-situ and ex-situ ion-irradiated additively manufactured 316L and 316H stainless steels

Additively manufactured (AM) 316 stainless steel (SS) differs from its wrought counterpart in its unique dislocation cell structure and the presence of segregation and oxide particles at the cell walls. This work investigated the evolution of the microstructure in laser powder bed fusion (LPBF) 316L and 316H SS under in-situ 1 MeV Kr ion irradiation at 600 °C to 5 dpa, and ex-situ 4 MeV Ni ion irradiation at 300 °C and 600 °C from 0.2 dpa to 10 dpa, with a dose rate for all experiments of 10 -3 dpa/s. The results reveal that the dislocation cell structure results in heterogeneous formation of dislocation loops and voids, particularly at 600 °C, where loops tend to form within the cell interiors while voids form at the cell boundaries. LPBF 316H has a reduced level of swelling compared to LPBF 316L due to prolonged incubation. Energy Dispersive X-ray Spectroscopy (EDS) mapping indicates Ni and Si segregation at void surfaces due to radiation-induced segregation. At 300 °C, where voids are absent, the distribution of dislocation loops and stacking fault tetrahedra appears to be uniform. Dislocation cell structures mostly disappeared by 2 dpa for all conditions in this work. M 23 C 6 carbides were observed in LPBF 316H at 600 °C as early as 0.2 dpa, but not in LPBF 316L. Nanoindentation was performed to obtain the hardness of irradiated materials. In conclusion, this work illustrated the influence of additive manufacturing processes on microstructure evolution under irradiation, revealing the differences as well as the similarities as compared with wrought 316 SS, and the AM-related phenomenon that can potentially occur under neutron irradiation in nuclear reactors.

36 - MATERIALS SCIENCE↗
DOE OSTI2021

In situ friction and wear behavior of rubber materials incorporating various fillers and/or a plasticizer in high-pressure hydrogen

Polymers are used routinely for equipment and infrastructure in hydrogen vehicle refueling stations, but significant gaps remain in understanding their hydrogen compatibility. The tribological properties of these materials in a high-pressure hydrogen environment is important in preventing component failure and the need for frequent replacement. We present in situ tribological studies on model rubbers, which include common fillers and plasticizer, using an in situ tribometer developed previously. Results suggest a clear, yet complicated, combined effect of the high-pressure hydrogen and the additives on the tribological performance of the chosen materials, as compared to matching experiments performed in ambient air. We find that the additives improved wear resistance in EPDM but deteriorated that in NBR due to disparate additive-polymer interactions.

Kuang, Wenbin↗