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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 1,171 records · Page 65
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Transmission Electron Microscopy Studies of Transition Metal Oxides Employed as Carrier Selective Contacts in Silicon Solar Cells

The focus of this work is on the nano-scale characterization of transition metal oxides employed as carrier selective contacts in crystalline silicon (c-Si) solar cells using crosssectional transmission electron microscopy (TEM). Both electronselective (titanium dioxide, TiO 2 ) and hole-selective (molybdenum oxide, MoO x ; tungsten oxide, WO x ) contacts were investigated. High-resolution TEM (HRTEM) images were obtained with a FEI Tecnai F30 TEM.

Ali, H↗
DOE OSTI2019

In Situ Transmission Electron Microscopy: A Powerful Tool for the Characterization of Carrier-Selective Contacts

© 2019 IEEE. The goal of this paper is to provide an overview of an in situ transmission electron microscopy (TEM) technique used to study the thermal stability of various transition metal oxide-based contacts used as carrier-selective contacts in silicon solar cells. In the present work, MoOx/Al and WOx/Al were investigated as hole-selective rear contacts using a combination of in situ TEM and transmission line measurements (TLM).

Ali, Haider↗
DOE OSTI2020

Operando Microscopy Characterization of Perovskite Solar Cells

In this work, we developed operando Kelvin probe force microscopy (KPFM) to study the electrostatic potential distribution across perovskite cells under light and forward bias to gain a deeper understanding of device operation physics. As a case study, we selected perovskite cells with a SnO 2 -based electron-selective layer (ESL), which showed great potential for fabricating high-efficiency, hysteresis-free devices due to the deeper conduction band and higher electron mobility of SnO 2 . The as-made device showed a main junction at the perovskite/spiro interface. After light soaking and applying forward bias, the junction quality improved, possibly explained by filling trap states at the interfaces and by the perovskite absorber perhaps having a self-poling effect; the main junction is observed at the ESL/perovskite interface. The results are consistent with current-voltage measurements, device performance improves mainly with fill factor enhancement. The operando KPFM results should more closely reflect the real case during current density-voltage measurements or solar cell operation. The operando KPFM technique that we have developed can be a powerful tool to provide a deeper understanding of the device operation mechanism and to further optimize the device.

14 SOLAR ENERGY↗
DOE OSTI2024

Enhancing Electron Microscopy Image Classification Using Data Augmentation

Manual labeling for machine learning tasks such as image classification is tedious and labor-intensive; as a result, scientific datasets suitable for deep learning applications are scarce and limited. While data augmentation techniques have shown promise for extending image datasets, very little work has been done to understand the impact of combining multiple augmentation methods sequentially or the limits of their effectiveness when combined. Our work addresses this gap by examining how standard and combinatorial data augmentation affects the performance of machine learning models when trained on small datasets for label classification tasks. For our analysis, we generate single, double and quadruple-augmented datasets for a microscopy image classification task using six standard augmentation methods, and compare the resultant improvements observed in binary classification accuracy with three standard image classification models (DenseNet169, MobileNetV2, ResNet101V2). Our experiments show a non-monotonic relationship between the number of simultaneous augmentation methods and classification accuracy, indicating that there is a trade-off between the degree of augmentation and the model performance. These findings suggest that the optimal number of augmentation methods will vary by domain and use case. We also find that the order in which augmentation methods are applied to a limited dataset matters when combining augmentation schemes, with our use case showing performance differences up to 2.6% when the augmentation order is reversed for double-augmented datasets. Our work offers insights to the limits of data augmentation when working on image classification tasks with limited datasets.

Welsman, Jordan A↗
DOE OSTI2023

Three-Dimensional Reconstruction of Nb 3 Sn Films by Focused Ion Beam Cross Sectional Microscopy

Niobium has been the material of choice for SRF cavities for several decades due to its formability and superconducting properties. The accelerating gradient of niobium cavities is, however, rapidly approaching a theoretical limit. To achieve higher accelerating gradients a new material is needed that can sustain high fields. Nb 3 Sn is a promising competitor with a higher superconducting transition temperature and a higher critical field than pure niobium. However, Nb 3 Sn is very brittle and cannot be formed readily into a cavity. The main method for creating Nb 3 Sn cavities is to form a Nb 3 Sn film into a niobium surface using a tin vapor-diffusion method. This technique creates a microcrystalline Nb 3 Sn thin film on the inner surface of the cavity. Tin depleted regions are known to form in the film during this process. Previous studies have analyzed these regions using transmission electron microscopy on cross-sectional lamellae prepared by focused ion beam/scanning electron microscope (FIB/SEM). This method does not provide any three-dimensional (3-D) information about the distribution of tin-deficient regions. In this study we employ a focused ion beam tomographic technique to analyze the 3-D structure of the film. Electron dispersive X-ray spectroscopy is used to image the tin concentration of the film in 3-D. Tin-deficient regions are discovered close to the surface of the Nb 3 Sn film.

Viklund, E.↗
DOE OSTI2025

Investigation of the Anisotropy of Y-Ba-Cu-O Thin Films With Photoemission Electron Microscopy

Understanding the anisotropy in the electrical properties of YBa2Cu3O7-δ (YBCO) is important for understanding the fundamental mechanism of superconductivity in unconventional superconductors. Additionally it is also essential for achieving uniform and controllable critical currents and resistances in YBCO Josephson junctions. Here, this study correlates work function measurements of different intrinsic regions on YBCO thin films, obtained through PhotoEmission Electron Microscopy (PEEM), with in plane tunneling data and helium ion imaging. YBCO thin films, 40 nm in thickness, were selectively irradiated with 300 keV helium using a Pelletron to investigate the effects of irradiation compared to unirradiated regions. Post-irradiation PEEM images revealed distinct contrasts between irradiated and non-irradiated regions, suggesting a metal-to-insulator transition. In non-irradiated areas, a domain pattern was detected, showing a 25 meV difference in work function, attributed to CuO and BaO rich surface regions. A similar domain structure was observed using high-resolution helium ion imaging; however, the helium ion beam can damage the YBCO, making PEEM a valuable non-destructive alternative. This work highlights the correlation between PEEM measurements and in-plane tunneling properties of YBCO, providing insights into material orientation and its impact on Josephson junction performance. Furthermore, it offers a non-destructive approach to understanding the anisotropy of cuprate materials, its superconducting properties, and the factors affecting Josephson junction performance.

Qu, Rochelle Y. [Univ. of California, Riverside, C↗
DOE OSTI2024

Quantitative analysis of three-dimensional fatigue crack path selection in Mg alloy WE43 using high-energy X-ray diffraction microscopy

Fatigue short-cracks in Mg alloys display complex growth behavior due to high plastic anisotropy and crack path dependence on local microstructural features. In this study, the three-dimensional crystallography of short-crack paths in Mg alloy WE43 was characterized by mapping near-field high-energy X-ray diffraction microscopy (HEDM) reconstructed grain maps to high-resolution X-ray CT reconstructions of the fracture surfaces in the crack initiation and short-crack growth regions of six ultrasonic fatigue specimens. Crack–grain–boundary intersections were analyzed at 81 locations across the six crack paths. The basal intragranular, non-basal intragranular, or intergranular character of short-crack growth following each boundary intersection was correlated to crystallographic and geometric parameters of the trailing and leading grains, three-dimensional grain boundary plane, and advancing crack front. The results indicate that crack paths are dependent on the combined crystallographic and geometric character of the local microstructure, and crack path prediction can be improved by use of dimensionality reduction on subsets of high-linear-correlation microstructural parameters.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Ta–Zr carbides: Synthesis advances via carbothermal reduction and defect evolution observed through transmission electron microscopy ion irradiation

The thermodynamic stability of six distinct compositions within the Zr—Ta—C ternary system is investigated in this study, marking the first report of their synthesis through carbothermic reduction in vacuum. A prolonged annealing process at 2200°C enabled high densification and phase equilibrium. Detailed phase identification and microstructural characterization through microscopy and X-ray diffraction techniques revealed clear compositional trends and stable phase formations. Two compositions ((Ta 0.2 Zr 0.8 )C 0.6 and (Ta 0.5 Zr 0.5 )C 1 ) were selected for ion irradiation experiments using 200 keV Kr + at 600°C—representing the first-ever irradiation study on the Zr—Ta—C system. The findings indicated defect accumulation and nanoscale cavity formation without any evidence of amorphization, highlighting the system's structural stability under irradiation. Together, the synthesis and irradiation results provide a basis for further investigation of the system and suggest its relevance for applications under extreme environments.

36 MATERIALS SCIENCE↗
DOE OSTI2024

High‐speed 4‐dimensional scanning transmission electron microscopy using compressive sensing techniques

Abstract Here we show that compressive sensing allows 4‐dimensional (4‐D) STEM data to be obtained and accurately reconstructed with both high‐speed and reduced electron fluence. The methodology needed to achieve these results compared to conventional 4‐D approaches requires only that a random subset of probe locations is acquired from the typical regular scanning grid, which immediately generates both higher speed and the lower fluence experimentally. We also consider downsampling of the detector, showing that oversampling is inherent within convergent beam electron diffraction (CBED) patterns and that detector downsampling does not reduce precision but allows faster experimental data acquisition. Analysis of an experimental atomic resolution yttrium silicide dataset shows that it is possible to recover over 25 dB peak signal‐to‐noise ratio in the recovered phase using 0.3% of the total data. Lay abstract : Four‐dimensional scanning transmission electron microscopy (4‐D STEM) is a powerful technique for characterizing complex nanoscale structures. In this method, a convergent beam electron diffraction pattern (CBED) is acquired at each probe location during the scan of the sample. This means that a 2‐dimensional signal is acquired at each 2‐D probe location, equating to a 4‐D dataset. Despite the recent development of fast direct electron detectors, some capable of 100kHz frame rates, the limiting factor for 4‐D STEM is acquisition times in the majority of cases, where cameras will typically operate on the order of 2kHz. This means that a raster scan containing 256^2 probe locations can take on the order of 30s, approximately 100‐1000 times longer than a conventional STEM imaging technique using monolithic radial detectors. As a result, 4‐D STEM acquisitions can be subject to adverse effects such as drift, beam damage, and sample contamination. Recent advances in computational imaging techniques for STEM have allowed for faster acquisition speeds by way of acquiring only a random subset of probe locations from the field of view. By doing this, the acquisition time is significantly reduced, in some cases by a factor of 10‐100 times. The acquired data is then processed to fill‐in or inpaint the missing data, taking advantage of the inherently low‐complex signals which can be linearly combined to recover the information. In this work, similar methods are demonstrated for the acquisition of 4‐D STEM data, where only a random subset of CBED patterns are acquired over the raster scan. We simulate the compressive sensing acquisition method for 4‐D STEM and present our findings for a variety of analysis techniques such as ptychography and differential phase contrast. Our results show that acquisition times can be significantly reduced on the order of 100‐300 times, therefore improving existing frame rates, as well as further reducing the electron fluence beyond just using a faster camera.

Robinson, Alex W.↗
DOE OSTI2026

Simplex‐based model for nanoparticle grain identification in four‐dimensional scanning transmission electron microscopy data

Grain identification in polycrystalline nanoparticles, for example, determining which crystal phases are present at each spatial location, is fundamental to materials characterisation. This is particularly challenging when grains overlap extensively, as commonly occurs in four-dimensional scanning transmission electron microscopy (4D-STEM) datasets. We propose a simplex-based model (SBM) in which each simplex vertex represents the diffraction pattern (DP) of a pure grain, and the simplex edges and interior represent overlapping grains. Our SBM grain identification algorithm operates on the Bragg disk (BD) data matrix distilled from the 4D-STEM data to identify the grain membership at each scan position, together with a BD feature matrix whose columns represent the DPs for each constituent grain, which is important for identifying the crystal structure of each grain. We solve the model using a two-stage algorithm. In Stage 1, we adapt a linear mixing algorithm to estimate an initial BD feature matrix whose columns represent DPs of potentially overlapping grains. Our Stage 2 algorithm incorporates sparsity considerations to transform the initial BD feature matrix so that its columns represent DPs of pure grains. Using simulated datasets with various grain configurations, we demonstrate that SBM recovers both the BD feature matrix and membership maps more accurately than existing methods, even when a grain lacks any pure region and completely overlaps with other grains.

4D-STEM segmentation↗
DOE OSTI2022

X-Ray Induced Chemical Reaction Revealed by In Situ X-Ray Diffraction and Scanning X-Ray Microscopy in 15 nm Resolution

The detection sensitivity of synchrotron-based X-ray techniques has been largely improved due to the ever-increasing source brightness, which has significantly advanced ex situ and in situ research for energy materials such as lithium-ion batteries. However, the strong beam–material interaction arising from the high beam flux can substantially modify the material structure. The beam-induced parasitic effect inevitably interferes with the intrinsic material property, making the interpretation of the experimental results difficult and requiring comprehensive assessments. Here, we present a quantitative study of the beam effect on an electrode material Ag 2 VO 2 PO 4 using four different X-ray characterization methods with different radiation dose rates. The material system exhibits interesting and reversible radiation-induced thermal and chemical reactions, further evaluated under electron microscopy to illustrate the underlying mechanism. Further, the work will provide a guideline for using synchrotron X-rays to distinguish the intrinsic behavior from extrinsic structure change of materials induced by X-rays.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Hyperspectral fluorescence microscopy detects autofluorescent factors that can be exploited as a diagnostic method for Candida species differentiation

Fungi in the Candida genus are the most common fungal pathogens. They not only cause high morbidity and mortality but can also cost billions of dollars in healthcare. To alleviate this burden, early and accurate identification of Candida species is necessary. However, standard identification procedures can take days and have a large false negative error. The method described in this study takes advantage of hyperspectral confocal fluorescence microscopy, which enables the capability to quickly and accurately identify and characterize the unique autofluorescence spectra from different Candida species with up to 84% accuracy when grown in conditions that closely mimic physiological conditions.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2024

Enhancing Diagnosis through AI-driven Analysis of Reflectance Confocal Microscopy

Reflectance Confocal Microscopy (RCM) is a non-invasive imaging technique used in biomedical research and clinical dermatology. It provides virtual high-resolution images of the skin and superficial tissues, reducing the need for physical biopsies. RCM employs a laser light source to illuminate the tissue, capturing the reflected light to generate detailed images of microscopic structures at various depths. Recent studies explored AI and machine learning, particularly CNNs, for analyzing RCM images. Our study proposes a segmentation strategy based on textural features to identify clinically significant regions, empowering dermatologists in effective image interpretation and boosting diagnostic confidence. This approach promises to advance dermatological diagnosis and treatment.

Yoon, Hong-Jun↗
DOE OSTI2019

Building and exploring libraries of atomic defects in graphene: Scanning transmission electron and scanning tunneling microscopy study

The presence and configurations of defects are primary components determining materials functionality. Their population and distribution are often nonergodic and dependent on synthesis history, and therefore rarely amenable to direct theoretical prediction. Here, dynamic electron beam–induced transformations in Si deposited on a graphene monolayer are used to create libraries of possible Si and carbon vacancy defects. Deep learning networks are developed for automated image analysis and recognition of the defects, creating a library of (meta) stable defect configurations. Density functional theory is used to estimate atomically resolved scanning tunneling microscopy (STM) signatures of the classified defects from the created library, allowing identification of several defect types across imaging platforms. This approach allows automatic creation of defect libraries in solids, exploring the metastable configurations always present in real materials, and correlative studies with other atomically resolved techniques, providing comprehensive insight into defect functionalities.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Ultrahigh-resolution scanning microwave impedance microscopy of moiré lattices and superstructures

Two-dimensional heterostructures composed of layers with slightly different lattice vectors exhibit new periodic structure known as moiré lattices, which, in turn, can support novel correlated and topological phenomena. Moreover, moiré superstructures can emerge from multiple misaligned moiré lattices or inhomogeneous strain distributions, offering additional degrees of freedom in tailoring electronic structure. High-resolution imaging of the moiré lattices and superstructures is critical for understanding the emerging physics. Here, we report the imaging of moiré lattices and superstructures in graphene-based samples under ambient conditions using an ultrahigh-resolution implementation of scanning microwave impedance microscopy. Although the probe tip has a gross radius of ~100 nm, spatial resolution better than 5 nm is achieved, which allows direct visualization of the structural details in moiré lattices and the composite super-moiré. We also demonstrate artificial synthesis of novel superstructures, including the Kagome moiré arising from the interplay between different layers.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Picosecond carrier dynamics in InAs and GaAs revealed by ultrafast electron microscopy

Understanding the limits of spatiotemporal carrier dynamics, especially in III-V semiconductors, is key to designing ultrafast and ultrasmall optoelectronic components. However, identifying such limits and the properties controlling them has been elusive. Here, using scanning ultrafast electron microscopy, in bulk n-GaAs and p-InAs, we simultaneously measure picosecond carrier dynamics along with three related quantities: subsurface band bending, above-surface vacuum potentials, and surface trap densities. We make two unexpected observations. First, we uncover a negative-time contrast in secondary electrons resulting from an interplay among these quantities. Second, despite dopant concentrations and surface state densities differing by many orders of magnitude between the two materials, their carrier dynamics, measured by photoexcited band bending and filling of surface states, occur at a seemingly common timescale of about 100 ps. This observation may indicate fundamental kinetic limits tied to a multitude of material and surface properties of optoelectronic III-V semiconductors and highlights the need for techniques that simultaneously measure electro-optical kinetic properties.

42 ENGINEERING↗
DOE OSTI2026

Discovery of spontaneous mesoscopic strain waves in nematic domains using dark-field x-ray microscopy

Electronic nematic order arises when correlated electrons spontaneously break the rotational symmetry of a crystal lattice. When electronic nematic order couples bilinearly to symmetry-breaking lattice strain, both appear together at a single ferroelastic phase transition, producing structural twin domains with distinct orientations of the nematic director. While the effects of applied strain on these domains are well established, the intrinsic behavior of spontaneous subdomain strain fields has remained unexplored. Here, we report the discovery of spontaneous mesoscopic strain waves within individual nematic domains of an iron-based superconductor, observed using dark-field x-ray microscopy (DFXM). Using this advanced full-field imaging technique, we visualize subdomain strain modulations emerging concurrently with nematic order. Elastic compatibility relations governing inhomogeneous strains provide a natural mechanism for the strain waves. Our findings reveal a broadly relevant form of strain self-organization and position DFXM as a powerful probe of the local interplay between lattice strain and electronic order.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Atomic structure of sensitive battery materials and interfaces revealed by cryo–electron microscopy

Whereas standard transmission electron microscopy studies are unable to preserve the native state of chemically reactive and beam-sensitive battery materials after operation, such materials remain pristine at cryogenic conditions. It is then possible to atomically resolve individual lithium metal atoms and their interface with the solid electrolyte interphase (SEI). We observe that dendrites in carbonate-based electrolytes grow along the < 111 > (preferred), < 110 >, or < 211 > directions as faceted, single-crystalline nanowires. These growth directions can change at kinks with no observable crystallographic defect. As a result, we reveal distinct SEI nanostructures formed in different electrolytes.

36 MATERIALS SCIENCE↗