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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 1,513 records · Page 84
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

In-situ investigation of incipient melting in a 319 type Al alloy using laser scanning confocal microscopy

Highlights: • In-situ analysis of incipient melting of ternary eutectic in Al alloy. • Incipient melting occurred in three distinct stages in the eutectic. • Increased heating rate increase rate of liquid film propagation. • Incipient melting transformed initial eutectic structure and caused oxidation. • Study determined incipient melting mechanism for eutectic structures. - Abstract: The modified 319 Al alloy system has been used extensively in precision sand casting of automotive powertrain applications such as engine blocks and cylinder heads, with significant improvement in vehicle fuel efficiency. However, a concern in elevated temperature processing of Al alloys, such as heat treatment and hot working processes, is incipient melting of secondary phases, which is deleterious to mechanical properties. In this study, the laser scanning confocal microscopy (LSCM) technique was used in the analysis of in-situ changes in microstructure as a result of incipient melting. Microstructural analysis was carried out prior to and following elevated temperature exposure in the LSCM using optical microscopy, SEM and EDX. The results suggest that incipient melting of the Al-Al{sub 2}Cu-Al{sub 5}Mg{sub 8}Cu{sub 2}Si{sub 6} ternary eutectic clusters was initiated by the formation of a liquid film which propagated rapidly from the eutectic clusters, coating the Al dendrites in regions adjacent to the eutectic clusters. Following film formation, the ternary eutectic clusters melted completely. Incipient melting also resulted in a localized change in composition in the interdendritic channels as supported by a change in cluster morphology from eutectic to a combination of coarse blocky Al-Cu-Ni and Si particles, and ultra-fine eutectic.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Pore structure refinement of cement paste incorporating nanosilica: Study with dual beam scanning electron microscopy/focused ion beam (SEM/FIB)

Highlights: • The modifying effects of nanosilica on pore structure of cement-based composites are investigated. • Dual beam SEM/FIB is implemented to create the 3D pore structure model and calculate porosity and pore size distribution. • The porosity and pore diameter are found to decrease with the inclusion of nanosilica. - Abstract: Pozzolanic materials, micro- and nano-, have been found to improve the durability properties of cement-based materials by refining their pore structure. As a relatively newer material, the modifying effects of nanosilica on pore structure are still inconclusive in the literature. In this study, this was characterized by implementing dual beam SEM/FIB, which can generate 3D models of porous materials for quantitative analysis. The sample is milled by focused ion beam layer-by-layer, and each surface layer is 2D imaged via scanning electron microscopy. Three types of pores – large capillary pore, medium capillary pore and gel pore – can be observed. A 3D pore structure model is then reconstructed from 1000 of these 2D images, from which porosity and pore size distribution can be calculated. Cement pastes incorporating nanosilica and silica fume were compared. The porosity and pore diameter were found to decrease with the inclusion of nanosilica. Furthermore, reduction in capillary pores and subsequent increase in gel pores were also observed.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2021

A study on the creep behavior of alloy 709 using in-situ scanning electron microscopy

In this research, an experimental evaluation of creep properties of Alloy 709 in the temperature range of 750–850 °C was undertaken. Alloy 709 is a novel austenitic stainless steel with 20% Cr and 25% Ni by wt% that was developed for application in structural components of nuclear power plants. Creep rupture tests were conducted in an in-situ heating-loading and Scanning Electron Microscope (SEM) unit equipped with Electron Backscatter Diffraction (EBSD) detector and Energy Dispersive Spectroscopy (EDS). “Real-time” creep damage mechanisms of Alloy 709 at various stresses and temperatures using a flat, un-notched sample with continuously reducing cross-section is studied so that the failure and maximum creep damage occurred at the center of the sample where the in-situ SEM imaging could be focused. Accelerated creep tests at temperatures and stresses above service conditions were performed by employing multiple blocks of constant loads where the loads were increased once the sample attained constant creep rate, indicating a secondary creep regime. This technique ensures multiple data points can be obtained from the same test, saves the time required for an otherwise long-term creep test and usage of SEM. Further, Coincident Site Lattice (CSL) boundary maps were collected as control maps before testing, and the grain boundaries were observed during the creep test to understand the effect of grain boundary character on the creep damage mechanism. Void growth, grain boundary separation, and sliding were found to be the main creep mechanisms whose rate is dependent on stress and temperature. Failure mechanisms studied on the fracture surface using SEM fractography were correlated to the sample surface observations to create complementary information to better understand the underline creep mechanism of Alloy 709.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Biofouling of filtration membranes in wastewater reuse: In situ visualization with confocal laser scanning microscopy

The filtration membranes utilized in advanced treatment of municipal wastewater are prone to biological fouling. Permeability loss and water recovery limitations due to fouling necessitate additional pretreatment and membrane cleaning, which raise the cost of water reuse. Better fouling mitigation calls for a deeper understanding of biofilm behavior on water reuse membranes. This study uses confocal microscopy to monitor biofouling under realistic conditions. To simulate water reuse, a miniature flow cell with microfiltration and ultrafiltration membranes was operated under typical filtration conditions using secondary effluent from California's East Bay Municipal Utility District. The growing biofilms were stained for extracellular polymeric substances and live and dead cells, and they were monitored in situ under filtration conditions with a confocal laser scanning microscope to produce 2-D and 3-D images. In situ image series revealed biofilm growth and removal processes including internal and external fouling, extracellular polymeric substance production, wrinkling, delamination, and film re-deposition. Additionally, changes in biofilm morphology between in situ and ex situ images highlighted limitations of ex situ imaging. Here, these results provide insight into the physical and biological mechanisms of biofouling in hopes of informing the development of improved techniques for biofouling mitigation.

ultrafiltration↗
DOE OSTI2023

Explainability and human intervention in autonomous scanning probe microscopy

The broad adoption of machine learning (ML)-based autonomous experiments (AEs) in material characterization and synthesis requires strategies development for understanding and intervention in the experimental workflow. Here, we introduce and realize a post-experimental analysis strategy for deep kernel learning-based autonomous scanning probe microscopy. This approach yields real-time and post-experimental indicators for the progression of an active learning process interacting with an experimental system. We further illustrate how this approach can be applied to human-in-the-loop AEs, where human operators make high-level decisions at high latencies setting the policies for AEs, and the ML algorithm performs low-level, fast decisions. The proposed approach is universal and can be extended to other techniques and applications such as combinatorial library analysis.

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Secondary porosity prediction in complex carbonate reefs using 3D CT scan image analysis and machine learning

Development and preservation of carbonate porosity and permeability are critical to characterizing reservoirs. However, secondary porosity, such as vugs and fractures, are difficult to identify and require collection of expensive wireline tools or core sampling. Wireline logs and cores have traditionally been used to identify the presence of secondary porosity but fail to quantify the contribution to total reservoir porosity. Additionally, advanced wireline logs and core are not readily available for most wells. Dual energy CT scans were collected on whole core from the A-1 Carbonate and Brown Niagaran formations drawn from six wells in northern Michigan. 3D analysis techniques were applied to identify and isolate secondary porosity features. A series of machine learning and data analytics techniques were applied to the dataset to predict secondary porosity features on basic wireline logs. The predictive model successfully predicted secondary porosity with high confidence.

02 PETROLEUM↗
DOE OSTI2020

Mapping the phases of quantum chromodynamics with beam energy scan

We review the present status of the search for a phase transition and critical point as well as anomalous transport phenomena in Quantum Chromodynamics (QCD), with an emphasis on the Beam Energy Scan program at the Relativistic Heavy Ion Collider at Brookhaven National Laboratory. We present the conceptual framework and discuss the observables deemed most sensitive to a phase transition, QCD critical point, and anomalous transport, focusing on fluctuation and correlation measurements. Selected experimental results for these observables together with those characterizing the global properties of the systems created in heavy ion collisions are presented. We then discuss what can be already learned from the currently available data about the QCD critical point and anomalous transport as well as what additional measurements and theoretical developments are needed in order to discover these phenomena.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2018

Analysis of rare earth elements in coal fly ash using laser ablation inductively coupled plasma mass spectrometry and scanning electron microscopy

Reference standard NIST SRM 1633b and FA 345, a fly ash sample from an eastern U.S. coal power plant, were analyzed to determine and quantify the mineralogical association of rare earth elements (REE). These analyses were completed using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and a scanning electron microscope, equipped with an energy-dispersive X-ray spectrometer (SEM-EDS). Internal standardization was avoided by quantifying elemental concentrations by normalizing to 100% oxides. Mineral grains containing elevated REE concentrations were found in diverse chemical environments, but were most commonly found in regions where Al and Si were predominant. Dividing the spot analyses into time segments yielded plots that showed the REE content changing over time as individual mineral grains were being ablated. SEM-EDS images of FA 345 confirmed the trends that were found in the LA-ICP-MS results. Small grains of apatite, monazite, or zircon were frequently observed as free mineral grains or embedded in amorphous aluminosilicate glass and were not associated with ferrous particles. This finding is consistent with previous reports that magnetic enrichment may be an effective way of concentrating non-magnetic REE phases. Moreover, aggressive mechanical and chemical-based separation schemes will be required to separate and recover REE from aluminosilicate glass.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2018

Imaging charge carriers in potential-induced degradation defects of c-Si solar cells by scanning capacitance microscopy

We report on nm-resolution imaging of charge-carrier distribution around local potential-induced degradation (PID) shunting defects using scanning capacitance microscopy. We imaged on cross sections of heavily field-degraded module areas, cored out and selected by mm-scale photoluminescence imaging. We found localized areas with abnormal carrier behavior induced by the PID defects: the apparent n-type carrier extends vertically into the absorber to ~1-2 um from the cell surface, and laterally in similar lengths; in defect-free areas, the n-type carrier extends ~0.5 um, which is consistent with the junction depth. For comparison, we also investigated areas of the same module exhibiting the least PID stress, and we found no such heavily damaged junction area. Instead, we found slightly abnormal carrier behavior, where the carrier-type inversion in the absorber did not occur, but the p-type carrier concentration changed slightly in a much smaller lateral length of ~300 nm. These nano-electrical findings may indicate a possible mechanism that the existing extended defects, which may not be significantly harmful to cell performance, can be changed by PID to heavily damaged junction areas.

14 SOLAR ENERGY↗
DOE OSTI2020

Imaging hole-density inhomogeneity in arsenic-doped CdTe thin films by scanning capacitance microscopy

We report nanometer-scale hole-density imaging in As-doped CdTe films by scanning capacitance microscopy (SCM). The hole-density profiling is validated by contrasting a CdTe cross-section sample made by molecular-beam epitaxy with systematically increased As doping in a staircase pattern over the range of 10 15 -10 18 /cm 3 within a single film. In polycrystalline films, the carrier distribution is significantly nonuniform, with inhomogeneity ranging from several hundred nm to several um and hole density varying by one order of magnitude (low 10^16 to low 10 17 /cm 3 ). This nonuniformity is distributed randomly, independent of the grain structure and grain boundaries (GBs). Kelvin probe force microscopy (KPFM) maps the surface potential and is correlated to cathodoluminescence (CL) and SCM by imaging over identical areas. Higher potential and lower CL intensity are found on GBs but not by SCM contrast; this indicates positive GB charging and recombination, but not GB-specific hole-density changes. The overall KPFM potential image is in rough agreement with the SCM carrier distribution and indicates band-edge potential fluctuations. Nonuniform carrier concentration, potential fluctuations, and defect recombination can all cause voltage and performance loss in As-doped CdTe solar technology.

14 SOLAR ENERGY↗
DOE OSTI2020

Denoising atomic resolution 4D scanning transmission electron microscopy data with tensor singular value decomposition

Tensor singular value decomposition (SVD) is a method to find a low-dimensional representation of data with meaningful structure in three or more dimensions. Here, tensor SVD has been applied to denoise atomic-resolution 4D scanning transmission electron microscopy (4D STEM) data. On data simulated from a SrTiO 3 [100] perfect crystal and a Si [110] edge dislocation, tensor SVD achieved an average peak signal-to-noise ratio (PSNR) of ~40 dB, which matches or exceeds the performance of other denoising methods, with processing times at least 100 times shorter. On experimental data from SrTiO 3 [100] and LiZnSb [11 2 ¯ 0]/GaSb [110] samples, tensor SVD denoises multiple GB 4D STEM data sets in ten minutes on a typical personal computer. Denoising with tensor SVD improves both convergent beam electron diffraction patterns and virtual-aperture annular dark field images.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Identification and correction of temporal and spatial distortions in scanning transmission electron microscopy

Scanning transmission electron microscopy (STEM) has become the technique of choice for quantitative characterization of atomic structure of materials, where the minute displacements of atomic columns from high-symmetry positions can be used to map strain, polarization, octahedra tilts, and other physical and chemical order parameter fields. The latter can be used as inputs into mesoscopic and atomistic models, providing insight into the correlative relationships and generative physics of materials on the atomic level. However, these quantitative applications of STEM necessitate understanding the microscope induced image distortions and developing the pathways to compensate them both as part of a rapid calibration procedure for in situ imaging, and the post-experimental data analysis stage. Here, we explore the spatiotemporal structure of the microscopic distortions in STEM using multivariate analysis of the atomic trajectories in the image stacks. Based on the behavior of principal component analysis (PCA), we develop the Gaussian process (GP)-based regression method for quantification of the distortion function. The limitations of such an approach and possible strategies for implementation as a part of in-line data acquisition in STEM are discussed. Here, the analysis workflow is summarized in a Jupyter notebook that can be used to retrace the analysis and analyze the reader's data.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Relation between sampling, sensitivity and precision in strain mapping using the Geometric Phase Analysis method in Scanning Transmission Electron Microscopy

The sensitivity and the precision of the Geometric Phase Analysis (GPA) method for strain characterization is a topic widely discussed in the literature and is usually difficult to quantify. Indeed, the GPA precision is intricately linked to the resolution of the strain maps defined when masking the periodic reflections in Fourier space. In this study an additional parameter, sampling, is proposed to be analyzed regarding the precision of GPA by developing the concept of a phase noise in the GPA equations. Both experimentally and theoretically, the following article demonstrates how the precision, and the sensitivity of the GPA method is improved when using a larger pixel spacing to record an electron micrograph in Scanning Transmission Electron Microscopy (STEM). In conclusion, the counterintuitive concept of increasing the field of view to improve the GPA precision results in an extension of the application of strain characterization methods in STEM towards low deformation levels.

47 OTHER INSTRUMENTATION↗
DOE OSTI2015

Scanning EM of non-heavy metal stained biosamples: Large-field of view, high contrast and highly efficient immunolabeling

Scanning electron microscopy (SEM) is increasing its application in life sciences for electron density measurements of ultrathin sections. These are traditionally analyzed with transmission electron microscopy (TEM); by most labs, SEM analysis still is associated with surface imaging only. Here we report several advantages of SEM for thin sections over TEM, both for structural inspection, as well as analyzing immuno-targeted labels such as quantum dots (QDs) and gold, where we find that QD-labeling is ten times more efficient than gold-labeling. Furthermore, we find that omitting post-staining with uranyl and lead leads to QDs readily detectable over the ultrastructure, but under these conditions ultrastructural contrast was even almost invisible in TEM examination. Importantly, imaging in SEM with STEM detection leads to both outstanding QDs and ultrastructural contrast. STEM imaging is superior over back-scattered electron imaging of these non-contrasted samples, whereas secondary electron detection cannot be used at all. We conclude that examination of ultrathin sections by SEM, which may be immunolabeled with QDs, will allow rapid and straightforward analysis of large fields with more efficient labeling than can be achieved with immunogold. The large fields of view routinely achieved with SEM, but not with TEM, allows straightforward raw data sharing using virtual microscopy, also known as nanotomy when this concerns EM data in the life sciences. - Highlights: • High resolution and large fields of view via nanotomy or virtual microscopy. • Highly relevant for EM‐datasets where information density is high. • Sample preparation with low contrast good for STEM, not TEM. • Quantum dots now stand out in STEM‐based detection. • 10 Times more efficient labeling with quantum dots compared to gold.

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

A Fast Algorithm for Scanning Transmission Electron Microscopy Imaging and 4D-STEM Diffraction Simulations

Scanning transmission electron microscopy (STEM) is an extremely versatile method for studying materials on the atomic scale. Many STEM experiments are supported or validated with electron scattering simulations. However, using the conventional multislice algorithm to perform these simulations can require extremely large calculation times, particularly for experiments with millions of probe positions as each probe position must be simulated independently. Recently, the plane-wave reciprocal-space interpolated scattering matrix (PRISM) algorithm was developed to reduce calculation times for large STEM simulations. Here, we introduce a new method for STEM simulation: partitioning of the STEM probe into “beamlets,” given by a natural neighbor interpolation of the parent beams. This idea is compatible with PRISM simulations and can lead to even larger improvements in simulation time, as well requiring significantly less computer random access memory (RAM). We have performed various simulations to demonstrate the advantages and disadvantages of partitioned PRISM STEM simulations. We find that this new algorithm is particularly useful for 4D-STEM simulations of large fields of view. We also provide a reference implementation of the multislice, PRISM, and partitioned PRISM algorithms.

97 MATHEMATICS AND COMPUTING↗
DOE OSTI2022

An Automated Scanning Transmission Electron Microscope Guided by Sparse Data Analytics

Abstract Artificial intelligence (AI) promises to reshape scientific inquiry and enable breakthrough discoveries in areas such as energy storage, quantum computing, and biomedicine. Scanning transmission electron microscopy (STEM), a cornerstone of the study of chemical and materials systems, stands to benefit greatly from AI-driven automation. However, present barriers to low-level instrument control, as well as generalizable and interpretable feature detection, make truly automated microscopy impractical. Here, we discuss the design of a closed-loop instrument control platform guided by emerging sparse data analytics. We hypothesize that a centralized controller, informed by machine learning combining limited a priori knowledge and task-based discrimination, could drive on-the-fly experimental decision-making. This platform may unlock practical, automated analysis of a variety of material features, enabling new high-throughput and statistical studies.

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Isotope-Resolved Electron Energy Loss Spectroscopy in a Monochromated Scanning Transmission Electron Microscope

The development and implementation of high-stability monochromators in state-of-the-art aberration-corrected scanning transmission electron microscopes has enabled materials characterization with an energy resolution as good as 3 meV. This allows the vibrational modes, which would otherwise be obscured by the energy spread of the electron beam, to be probed with very high precision in molecular materials. Since the vibrational energies depend on the weight of the atomic nuclei, vibrational spectroscopy can distinguish isotopes whose only difference lies in their neutron content. This opens up isotopic analysis and mapping in transmission electron microscopy as two important new research areas. In this paper, we review the monochromated electron energy loss spectroscopy (EELS) instrumentation, discuss optimal methods for probing beam-sensitive materials without destroying them, and review key nanoscale isotope-resolved results.

47 OTHER INSTRUMENTATION↗