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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 1,747 records · Page 97
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Influence of Photoemission Geometry on Timing and Efficiency in 4D Ultrafast Electron Microscopy

Broader adoption of 4D ultrafast electron microscopy (UEM) for the study of chemical, materials, and quantum systems is being driven by development of new instruments as well as continuous improvement and characterization of existing technologies. Perhaps owing to the still-high barrier to entry, the full range of capabilities of laser-driven 4D UEM instruments has yet to be established, particularly when operated at extremely low beam currents (~fA). Accordingly, with an eye on beam stability, we have conducted particle tracing simulations of unconventional off-axis photoemission geometries in a UEM equipped with a thermionic-emission gun. Specifically, we have explored the impact of experimentally adjustable parameters on the time-of-flight (TOF), the collection efficiency (CE), and the temporal width of ultrashort photoelectron packets. The adjustable parameters include the Wehnelt aperture diameter (DW), the cathode set-back position (Ztip), and the position of the femtosecond laser on the Wehnelt aperture surface relative to the optic axis (Rphoto). Notable findings include significant sensitivity of TOF to DW and Ztip, as well as non-intuitive responses of CE and temporal width to varying Rphoto. As a means to improve accessibility, practical implications and recommendations are emphasized wherever possible.

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

In situ and operando force-based atomic force microscopy for probing local functionality in energy storage materials

Electrochemical energy storage is the key enabling component of electric vehicles and solar-/wind-based energy technologies. The enhancement of energy stored requires the detailed understanding of charge storage mechanisms and local electrochemical and electromechanical phenomena over a variety of length scales from atoms to full cells. Classical electrochemical techniques, such as voltammetry, represent the macroscopic electrochemical properties, and consequently do not allow to extract important information about local electrochemical reactions, ions adsorption, intercalations, and transport. Understanding, controlling, and tuning the local electrochemical functionalities in functional energy materials require in situ/operando techniques which limit the use of structural and functional characterization techniques that provide local information. Here, force-based atomic force microscopies (AFMs) have provided novel insights into locally probing electrochemical mechanisms on tens of nanometer and even molecular length scales and provide a viable pathway to probe electrochemical processes in situ/operando. In this review, we highlight the contributions in the development and application of force-based AFM methods to elucidate the local charge storage mechanism in a variety of energy-related materials. We will focus in particular on methods or AFM modalities in a liquid electrolyte environment.

25 ENERGY STORAGE↗
DOE OSTI2021

Quantitative phase microscopy monitors subcellular dynamics in single cells exposed to nanosecond pulsed electric fields

A substantial body of literature exists to study the dynamics of single cells exposed to short duration (<1 μs), high peak power (~1 MV/m) transient electric fields. Much of this research is limited to traditional fluorescence-based microscopy techniques, which introduce exogenous agents to the culture and are only sensitive to a single molecular target. Quantitative phase imaging (QPI) is a coherent imaging modality which uses optical path length as a label-free contrast mechanism, and has proven highly effective for the study of single-cell dynamics. In this work, we introduce QPI as a useful imaging tool for the study of cells undergoing cytoskeletal remodeling after nanosecond pulsed electric field (nsPEF) exposure. In particular, we use cell swelling, dry mass and disorder strength measurements derived from QPI phase images to monitor the cellular response to nsPEFs. We hope this demonstration of QPI's utility will lead to a further adoption of the technique for the study

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2019

In Situ Transmission Electron Microscopy Study of Molybdenum Oxide Contacts for Silicon Solar Cells

Here, a molybdenum oxide (MoO x ) and aluminum (Al) contact structure for crystalline silicon (c-Si) solar cells is investigated using a combination of transmission line measurements (TLM) and in-situ transmission electron microscopy (TEM). Cross-sectional high-resolution TEM (HRTEM) micrographs reveal a ≈2 nm silicon oxide (SiO x ) interlayer at c-Si/MoO x interface in the as-deposited state, indicating that formation of SiO x occurs during deposition of MoO x . Moreover, oxygen diffusion takes place from MoO x toward Al resulting in the formation of a ≈2–3 nm aluminum oxide (AlO x ) interlayer at the MoO x /Al interface. Overall, it is observed that MoO x /Al contact is relatively stable upon annealing up to 200 °C and still retains ohmic transport with sufficiently low contact resistivity.

14 SOLAR ENERGY↗
DOE OSTI2016

Impact of membrane-induced particle immobilization on seeded growth monitored by in situ liquid scanning transmission electron microscopy

In situ liquid cell scanning transmission electron microscopy probes seeded growth in real time. The growth of Pd on Au nanocubes is monitored as a model system to compare growth within a liquid cell and traditional colloidal synthesis. Furthermore, different growth patterns are observed due to seed immobilization and the highly reducing environment within the liquid cell.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Decoding the Mechanisms of Phase Transitions from In Situ Microscopy Observations

Abstract Analysis of the temperature‐ and stimulus‐dependent imaging data toward elucidation of the physical transformations is an ubiquitous problem in multiple fields. Here, temperature‐induced phase transition in BaTiO 3 is explored using the machine learning analysis of domain morphologies visualized via variable‐temperature scanning transmission electron microscopy (STEM) imaging data. This approach is based on the multivariate statistical analysis of the time or temperature dependence of the statistical descriptors of the system, derived in turn from the categorical classification of observed domain structures or projection on the continuous parameter space of the feature extraction‐dimensionality reduction transform. The proposed workflow offers a powerful tool for the exploration of the dynamic data based on the statistics of image representation as a function of the external control variable to visualize the transformation pathways during phase transitions and chemical reactions. This can include the mesoscopic STEM data as demonstrated here, but also optical, chemical imaging, etc., data. It can further be extended to the higher dimensional spaces, for example, analysis of the combinatorial libraries of materials compositions.

Valleti, Sai Mani Prudhvi↗
DOE OSTI2018

Synchrotron‐Based X‐ray Absorption Fine Structures, X‐ray Diffraction, and X‐ray Microscopy Techniques Applied in the Study of Lithium Secondary Batteries

Abstract Owing to the recent advance of third‐generation synchrotron radiation (SR) sources, SR‐based X‐ray techniques have been widely applied to study lithium‐ion batteries, lithium–sulfur batteries, and lithium–oxygen batteries to solve material challenges. SR‐based techniques provide high chemical and physical sensitivity and a comprehensive picture of material structure and reaction mechanisms. An in‐depth understanding of batteries is imperative for the development of future energy storage devices with enhanced electrochemical performance to meet societies' growing need for devices with high energy density. Here, recent progress in the application of SR techniques for lithium secondary batteries with a focus on several techniques, including X‐ray absorption fine structure, synchrotron X‐ray diffraction, and synchrotron X‐ray microscopy techniques is reviewed. The working principle for all characterization techniques is introduced to provide context for how the technique is used in the field of energy storage. Through discussing the utilization of SR techniques in different directions of batteries, including electrodes, electrolytes, and interfaces, the practical application strategies of techniques in batteries are clarified. By summarizing and discussing the application of SR techniques in batteries, the aim is to highlight the crucial role of SR characterization in the development of advanced energy materials.

Li, Weihan↗
DOE OSTI2024

Correlation of Processing and Structure in an Ethylene‐Glycol Side‐Chain Modified Polythiophene via Combined X‐Ray Scattering and 4D Scanning Transmission Electron Microscopy

The results of a combined grazing incidence wide-angle X-ray scattering (GIWAXS) and 4D scanning transmission microscopy (4D-STEM) analysis of the effects of thermal processing on poly(3[2-(2-methoxyethoxy)ethoxy]-methylthiophene-2,5-diyl) are reported, a conjugated semiconducting polymer used as the active layer in organic electrochemical transistor devices. GIWAXS provides a measure of overall crystallinity in the film, while 4D-STEM produces real-space maps of the morphology and orientation of individual crystallites along with their spatial extent and distribution. The sensitivity of the 4D-STEM detector allows for collection of electron diffraction patterns at each position in an image scan while limiting the imparted electron dose to below the damage threshold. In conclusion, the effects of heat treatment on the distribution and type of crystallites present in the films is determined.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Photoemission Electron Microscopy of a Plasmonic Silver Nanoparticle Trimer

We present a combined experimental and theoretical study to investigate the spatial distribution of photoelectrons emitted from core-shell silver (Ag) nanoparticles. We use two-photon photoemission microscopy (2P-PEEM) to spatially resolve electron emission from a trimeric core-shell aggregate of triangular symmetry. Finite difference time domain (FDTD) simulations are performed to model the intensity distributions of the electromagnetic near-fields resulting from femtosecond (fs) laser excitation of localized surface plasmon oscillations in the triangular core-shell structure. We demonstrate that the predicted FDTD near-field intensity distribution reproduces the 2P-PEEM photoemission pattern.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2016

Atomic-column scanning transmission electron microscopy analysis of misfit dislocations in GaSb/GaAs quantum dots

The structural quality of GaSb/GaAs quantum dots (QDs) has been analyzed at atomic scale by aberration-corrected high-angle annular dark-field scanning transmission electron microscopy. In particular, we have studied the misfit dislocations that appear because of the high-lattice mismatch in the heterostructure. Our results have shown the formation of Lomer dislocations not only at the interface between the GaSb QDs and the GaAs substrate, but also at the interface with the GaAs capping layer, which is not a frequent observation. The analysis of these dislocations points to the existence of chains of dislocation loops around the QDs. The dislocation core of the observed defects has been characterized, showing that they are reconstructed Lomer dislocations, which have less distortion at the dislocation core in comparison to unreconstructed ones. As a result, strain measurements using geometric phase analysis show that these dislocations may not fully relax the strain due to the lattice mismatch in the GaSb QDs.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Determining anisotropic slip system rate sensitivities of Ti-6Al-4V using high-energy X-ray diffraction microscopy

Variation of strain rate sensitivity among different families of slip systems in the hexagonal close-packed (α) phase of titanium (Ti) alloys has the potential to alter microscale load redistribution during both creep and dwell fatigue loading. However, existing literature contains conflicting reports regarding the degree of anisotropy present in the strain rate sensitives between α slip system families across Ti alloys. Here, we quantify the strain rate sensitivity of α slip system families in Ti-6Al-4V using high-energy X-ray diffraction microscopy (HEDM). We present a novel procedure in which we utilize the HEDM-measured grain-scale stress states during stress relaxation to determine the strain rate sensitivities of the basal $\langle a \rangle$ , prismatic $\langle a \rangle$, and first-order pyramidal $\langle c + a \rangle$ slip system families. In addition, we measure the strain rate sensitivity exponent of the macroscopic response and the α phase for comparison. We find rate sensitivities for the different slip system families to range from 0.02 to 0.04, which—while varied—are relatively isotropic in comparison with some values presented in the literature. We also demonstrate the effects of the measured anisotropic rate sensitivities using crystal plasticity finite element simulations.

Peterson, Kenneth M. [Pennsylvania State Univ., Un↗
DOE OSTI2012

Evaluation of Al3Mg2 precipitates and Mn-rich phase in aluminum-magnesium alloy based on scanning transmission electron microscopy imaging

Scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDS) were used to observe intergranular and intragranular -phase (Al3Mg2) formation and growth in as-received sample and long-term (~ 1 year) thermally treated samples of 5083-H131 alloy. Rod-shaped and equiaxed particles rich in Mn, Fe, and Cr were present in the as-received and heat treated samples. The -phase precipitated along grain boundaries as well as around and between preexisting Mn-Fe-Cr rich particles. The measured thickness of -phase along grain boundaries was lower than Zener Hillert diffusion model predicted value and the potential reasons were theoretically analyzed. Dislocation networks, grain boundaries, and different preexisting particles were observed to contribute to Mg diffusion and -phase precipitation.

Zhu, Yakun↗
DOE OSTI2025

Stimulating β -Series Precipitation in Mg–Nd Alloys Via Microalloying: A Comparison of Electron Microscopy and Small-Angle Scattering Techniques

The Mg–Nd alloy system is of particular interest in the development of high-strength, lightweight structural alloys due to the formation of strengthening metastable Mg–Nd β-series precipitates during heat treatment. The strengthening is primarily provided by a combination of the β''' and β 1 precipitation. It is therefore important to understand how the precipitation behavior can be enhanced by other common alloying elements. In this work, the effects of 0.2 wt pct Zn and Ca on β-series precipitation were studied. Small-angle/ultra-small-angle X-ray scattering (SAXS/USAXS) techniques in combination with scanning transmission electron microscopy (STEM) were used to study the evolution of precipitation microstructure. Here, it is found that the Zn additions refine the precipitates, leading to an increase in hardness with aging at 200 °C. On the other hand, the Ca additions result in an acceleration in the formation of larger β 1 precipitates and chains which provides less strengthening. The β 1 chains are surrounded by precipitate-free zones (PFZs) that further contribute to the decreases in hardness observed in the over-aged condition. This paper demonstrated that SAXS/USAXS provides a powerful tool for an in situ study of the early stages of precipitation in the Mg–Nd-based alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Characterization of Recrystallized Grains During Static Recrystallization of Hot-Compressed Mg–Zn–Ca Alloys Using In Situ Far-Field High-Energy Diffraction Microscopy

In this study, we explored the effect of Zn content on the static recrystallization of three 80 pct hot-compressed alloys, Mg–0.5Zn–0.1Ca wt pct (ZX050), Mg–1Zn–0.1Ca wt pct (ZX10), and Mg–3.2Zn–0.1Ca wt pct (ZX30), using far-field high-energy microscopy (ff-HEDM). Individual recrystallized grains were tracked and their 3D centroid, relative volume, and grain-averaged crystallographic orientation were measured during annealing. These measurements were used to compare the recrystallization kinetics and texture evolution of recrystallized grains in ZX alloys as a function of the Zn content. Fully recrystallized microstructures were observed for the ZX30 and the ZX10 alloys after annealing at 230 °C and 330 °C, respectively. In contrast, only a partially recrystallized microstructure for the ZX050 alloy was observed after > 1 hour of annealing at 430 °C. The resistance to recrystallization with decreasing Zn content was also confirmed by detecting faster growth rates of recrystallized grains in the ZX10 and ZX30 alloys, and slower growth rates in the ZX050 alloy. The significant recrystallization texture weakening of the ZX10 and ZX30 alloys and the development of a basal texture in the ZX05 alloy were described based on the orientation dependency of nucleation and growth of recrystallized grains. The analysis demonstrated that texture weakening was associated with increasing Zn content in Mg–Zn–Ca alloys.

Roumina, Reza [Univ. of Michigan, Ann Arbor, MI (U↗
DOE OSTI2018

Transmission Electron Microscopy (TEM) Study of the Oxide Layers Formed on Fe-12Cr-4Al Ferritic Alloy in an Oxygenated Pb-Bi Environment at 800°C

Liquid lead–bismuth eutectic (LBE) can serve as a heat transfer fluid for advanced nuclear applications as well as concentrated solar power but poses corrosion challenges for the structural materials at elevated temperatures. Oxide passivation of the surfaces of these materials during exposure to liquid LBE can inhibit such material degradation. In this study, transmission electron microscopy of oxides formed on Fe-Cr-Al alloy during exposure to lowoxygenated LBE at 800C has been performed. A complex structure of the oxide film has been revealed, consisting of a homogeneous inner layer of mostly Al 2 O 3 and a heterogeneous outer layer.

14 SOLAR ENERGY↗
DOE OSTI2023

Small Scale Creep Testing of 14YWT via In-situ Transmission Electron Microscopy Irradiation and Nanoindentation

The next generation of nuclear materials must withstand harsh operating conditions such as high temperatures and irradiation doses. Nanostructured ferritic alloys like oxide dispersion strengthened steels, especially 14YWT, have shown promise as a structural material to withstand these harsh operating conditions. For application, understanding the irradiation enhanced creep of the structural components is fundamental to evaluating the service life in a reactor. Challenges with evaluating irradiation enhanced creep are related to the limited space in nuclear reactors and the expense of conducting post irradiation experiments on irradiated cladding. Ion irradiations are considered to expedite irradiation testing, but such experiments have restricted depth of penetration into the material, limiting the ability to characterize changes to material properties after irradiation. Small scale mechanical testing can be used with ion beam irradiations as a potential avenue to evaluate the irradiation enhanced creep of materials. In this study, in-situ transmission electron microscopy nanopillar creep studies on 14YWT were performed and simultaneously ion beam irradiated with 2.8 MeV Au4+ ions. It was observed that the ion beam irradiation did increase the measured strain rate of the materials. In addition, ex-situ nanoindentation creep studies were performed over a range of temperatures on control 14YWT, and it was observed that there was a change in the deformation mechanism between 873 K and 1073 K that agrees well with macro-scale mechanical testing. Furthermore, these results show promise for applying these techniques to nuclear materials in the future.

14 YWT↗
DOE OSTI2022

Revealing the dynamics of the alloying and segregation of Pt-Co nanoparticles via in-situ environmental transmission electron microscopy

Thermal treatment is a general and efficient way to synthesize intermetallic catalysts and may involve complicated physical processes. So far, the mechanisms leading to the size and composition heterogeneity, as well as the phase segregation behavior in Pt-Co nanoparticles (NPs) are still not well understood. Here, via in-situ environmental transmission electron microscopy, the formation dynamics and segregation behaviors of Pt-Co alloyed NPs during the thermal treatment were investigated. It is found that Pt-Co NPs on zeolitic imidazolate frameworks-67-derived nanocarbon (NC) are formed consecutively through both particle migration coalescence and the Ostwald ripening process. The existence of Pt NPs is found to affect the movement of Co NPs during their migration. With the help of theoretical calculations, the correlations between the composition and migration of the Pt and Co during the ripening process were uncovered. Herein, these complex alloying processes are revealed as key factors leading to the heterogeneity of the synthesized Pt-Co alloyed NPs. Under oxidation environment, the Pt-Co NPs become surface faceted gradually, which can be attributed to the oxygen facilitated relatively higher segregation rate of Co from the (111) surface. This work advances the fundamental understanding of design, synthesis, and durability of the Pt-based nanocatalysts.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Analysis of passivated A-286 stainless steel surfaces for mass spectrometer inlet systems by Auger electron and X-ray photoelectron spectroscopy and scanning electron microscopy

In this study, various commercially available surface treatments are being explored for use on stainless steel components in mass spectrometer inlet systems. Type A-286 stainless steel coupons, approximately 12.5 mm in diameter and 3 mm thick, were passivated with one of five different surface treatments; an untreated coupon served as a control. The surface and near-surface microstructure and chemistry of the coupons were investigated using sputter depth profiling using Auger electron spectroscopy, x-ray photoelectron spectroscopy, and scanning electron microscopy (SEM). All the surface treatments studied appeared to change the surface morphology dramatically, as evidenced by lack of tool marks on the treated samples in SEM images. In terms of the passivation treatment, Vendors A-D appeared to have oxide layers that were very similar in thickness to each other (0.7–0.9 nm thick), as well as to the untreated samples (the untreated sample oxide layers appeared to be somewhat larger). Vendor E’s silicon coating appears to be on the order of 200 nm thick.

36 MATERIALS SCIENCE↗