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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 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Towards a quantitative understanding of bonding in supersonic single particle impacts: A three-dimensional FIB-SEM exploration

Particle bonding is crucial to coating quality in cold spray, but it has been a challenge to accurately quantify bonding even in single particle impacts. This paper uses FIB-SEM to explicitly map the particle-substrate interface for Cu-on-Cu single microparticle impacts in a full 3D rendering that spans a wide range of impact velocities. This approach permits a detailed quantification of the total bonding area and all of its associated components. In addition to revealing why prior 2D characterization efforts have missed important details about impact bonding, these data quantitatively reveal the evolution of bonding from its onset at the “critical velocity” V cr (where bonding is generally poor, ∼6 %) to its peak at around 1.3‧V cr (where almost 90 % of the particle bonds). Further increase in the velocity to 1.5‧V cr and beyond finds the onset of hydrodynamic penetration and a decrease in bonding. These data then support the development of a simple analytical model based on oxide rarefication and extrusion of bare metal through gaps in the oxide layer as driving the development of bonding. As a result, the model reproduces the experiments and provides guidance on optimization of bonding as a function of material and process parameters.

Analytical methods↗
DOE OSTI2018

SOFC Microstructures (PFIB-SEM and synthetic) from JPS 2018

This is the microstructural data used in the publication "Mesoscale characterization of local property distributions in hetergeneous electrodes" by Tim Hsu, William K. Epting, Rubayyat Mahbub, et al., published in the Journal of Power Sources in 2018. (DOI 10.1016/j.jpowsour.2018.03.025). Included are a commercial cathode and anode active layer (Materials and Systems Research, Inc., Salt Lake City, UT) imaged by Xe plasma FIB-SEM (FEI, Hillsboro, OR), and four synthetic microstructures of varying particle size distribution widths generated by DREAM3D (BlueQuartz Software, Springboro, OH). For the MSRI electrodes, both the original greyscale and the segmented versions are provided. Each .zip file contains a "stack" of .tif image files in the Z dimension, and an .info ascii text file containing useful information like voxel sizes and phase IDs. More details can be found in the pertinent publication at http://dx.doi.org/10.1016/j.jpowsour.2018.03.025.

FIB-SEM,SOFC,microstructure↗
DOE OSTI2017

Uncertainty in the use of MAMA software to measure particle morphological parameters from SEM images

The MAMA software package developed at LANL is designed to make morphological measurements on a wide variety of digital images of objects. At LANL, we have focused on using MAMA to measure scanning electron microscope (SEM) images of particles, as this is a critical part of our forensic analysis of interdicted radiologic materials. In order to successfully use MAMA to make such measurements, we must understand the level of uncertainty involved in the process, so that we can rigorously support our quantitative conclusions.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2024

Project ICEBall: Cryo-SEM images of Captured Cirrus Ice Particles. ARM SGP, October 21-November 1, 2021

This dataset includes a unique set of cryo-SEM images of captured cirrus ice particle from ARM Project ICEBall, which was conducted at and around the Southern Great Plains site from October 21- November 1, 2021. The instrument used for particle collection, Ice Crystal Encapsulation by Ball (ICE-Ball), is described in Magee et al. 2021, 'Captured cirrus ice particles in high definition", Atmos. Chem. Phys. The ice particles were captured on balloon flights directly from cirrus cloud formations between 7-12 km on seven ICEBall flights on these dates: October 21, 23, 24, 25, 26, 31, and Nov. 1.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2018

Characterization of uraninite using a FIB–SEM approach and its implications for LA–ICP–MS analyses

Focused ion beam (FIB) coupled with scanning electron microscopy (SEM) investigations were performed here on pristine and altered areas of two uraninite samples in order to better understand their 3-dimensional mineralogical and chemical nature, and their impact on trace element abundances obtained by laser ablation inductively coupled plasma mass spectrometry (LA–ICP–MS) analyses. Trace element contents determined by both LA- and solution mode (SM)–ICP–MS analyses together with FIB results identify Pb as the optimal internal standard for LA–ICP–MS analyses of uraninite since it is a major chemical constituent, part of the structure, and similar in abundance to the trace elements of interest.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2024

Automated SEM analysis of particles in Hanford tank waste

Multiple bench-scale filtration campaigns of Hanford tank waste supernatant on a backpulseable dead-end filtration skid have provided greater insight into the solids that cause fouling and reduce filter performance. The solids collected during each campaign were concentrated from the backpulse solutions and examined using automated particle analysis (APA) methods with scanning electron microscopy (SEM) and x-ray energy dispersive spectroscopy (EDS), to categorize particle types and their morphological characteristics. Finally, we show that with APA, thousands of particles can be analyzed that can provide accurate insight into the phases that may be impacting filter performance.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2017

SEM characterization of two advanced fuel alloys: U-10Zr-4.3Sn and U-10Zr-4.3Sn-4.7Ln

Tin is being investigated as a potential additive to metallic fuel to control fuel-cladding chemical interaction (FCCI). A primary cause of FCCI is the lanthanide fission products moving to the fuel periphery and interacting with the cladding. This interaction will lead to wastage of the cladding and eventually to a cladding breach. The current paper is a scanning electron microscopy (SEM) characterization of as-cast and annealed U-10Zr-4.3Sn and U-10Zr-4.3Sn-4.7Ln, where Ln = 53Nd-25Ce-16Pr-6La. Finally, the present study shows that tin preferentially binds the lanthanides, which will prevent lanthanide migration and interaction with the cladding.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

AGR-2 irradiated TRISO particle IPyC/SiC interface analysis using FIB-SEM tomography

In this work, the morphology in the interface region between the inner pyrolytic carbon layer (IPyC) and silicon carbide (SiC) layers in tristructural-isotropic (TRISO) particle fuel from the AGR-2 irradiation experiment were studied using focused ion beam-scanning electron microscopy tomography. This work quantitatively described the interface and corresponding relevant metrics to understand how the microstructural features at the IPyC/SiC interface may influence actinide and fission product interactions with the SiC layer. Particles were selected with varied 110m Ag retention rates, and their volumes were reconstructed and analyzed for distributions of pores, fission product/actinide features, SiC, and IPyC. It was found that porosity accommodates fission products in the interface and SiC layers. The largest fission product/actinide precipitates were found in the interface region. This was also where the largest number fraction of fission products/actinides was found, consistent with SEM showing fission product/actinide pileup along selected areas of the interface region.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Plutonium migration and phase evolution in irradiated U-Pu-Zr metallic fuels: An integrated EPMA-SEM-TEM study

Constituent redistribution is a defining feature of irradiated U-Pu-Zr metallic fuels, yet its mechanisms and effects on fuel performance are not sufficiently resolved to guide model development. Although decades of irradiation testing have established broad trends, a true mechanistic understanding of constituent redistribution has not been achieved. Here, in this study, we use electron probe microanalysis (EPMA), scanning electron microscopy (SEM), and transmission electron microscopy-based (TEM) selective area electron diffraction (SAED) on a EBR-II irradiated U-19 wt.% Pu-6 wt.% Zr fuel pin cross-section to correlate the composition, porosity, and crystallographic phases formed after irradiation. Constituent redistribution is thought to consist of three distinct zones, in which uranium and zirconium migrate while plutonium remains relatively unchanged. Our EPMA results resolve eight distinct compositional regions, and more importantly, show that plutonium redistributes alongside zirconium, contrary to historical assumptions. The distribution of fission products was highly asymmetric with a few large lanthanide precipitates observed at isolated sites on the pin periphery instead of a uniform distribution of smaller precipitates around the periphery. Using thermodynamic data from TAF-ID and the measured EPMA compositions, matrix phase fractions were predicted across the fuel radius. Phase predictions based on composition did not match TEM/SAED results, which revealed a much higher fraction of α−U phase than would be expected if phases were retained from reactor temperatures. These findings highlight the need for expanded SAED phase identification to capture post-irradiation and storage effects, as well as rigorous uncertainty quantification in fuel performance and phase diagram modeling to better constrain predictions from compositional data.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2014

On the importance of FIB-SEM specific segmentation algorithms for porous media

A new algorithmic approach to segmentation of highly porous three dimensional image data gained by focused ion beam tomography is described which extends the key-principle of local threshold backpropagation described in Salzer et al. (2012). The technique of focused ion beam tomography has shown to be capable of imaging the microstructure of functional materials. In order to perform a quantitative analysis on the corresponding microstructure a segmentation task needs to be performed. However, algorithmic segmentation of images obtained with focused ion beam tomography is a challenging problem for highly porous materials if filling the pore phase, e.g. with epoxy resin, is difficult. The gray intensities of individual voxels are not sufficient to determine the phase represented by them and usual thresholding methods are not applicable. We thus propose a new approach to segmentation that pays respect to the specifics of the imaging process of focused ion beam tomography. As an application of our approach, the segmentation of three dimensional images for a cathode material used in polymer electrolyte membrane fuel cells is discussed. We show that our approach preserves significantly more of the original nanostructure than a thresholding approach. - Highlights: • We describe a new approach to the segmentation of FIB-SEM images of porous media. • The first and last occurrences of structures are detected by analysing the z-profiles. • The algorithm is validated by comparing it to a manual segmentation. • The new approach shows significantly less artifacts than a thresholding approach. • A structural analysis also shows improved results for the obtained microstructure.

36 MATERIALS SCIENCE↗
DOE OSTI2016

SEM and TEM characterization of microstructure of stainless steel composites reinforced with TiB{sub 2}

Steel-8TiB{sub 2} composites were produced by two new sintering techniques, i.e. Spark Plasma Sintering (SPS) and High Pressure-High Temperature (HP-HT) sintering. This study discusses the impact of these sintering methods on the microstructure of steel composites reinforced with TiB{sub 2} particles. Scanning electron microscopy (SEM), wavelength dispersive spectroscopy (WDS), X-ray diffraction, electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) were used to analyze the microstructure evolution in steel matrix composites. The results of microscopic examinations revealed a close relationship between the composite microstructure and the methods and conditions of sintering. Substantial differences were observed in the grain size of materials sintered by HP-HT and SPS. It has been demonstrated that the composites sintered by HP-HT tend to form a chromium-iron-nickel phase in the steel matrix. In contrast, the microstructure of the composites sintered by SPS is characterized by the presence of complex borides and chromium-iron phase. - Highlights: •The steel-8TiB{sub 2} composites were fabricated by Spark Plasma Sintering (SPS) and High Pressure-High Temperature (HP-HT). •Sintering techniques has an important effect on changes in the microstructure of steel-8TiB{sub 2} composites. •New phases of different size and morphology were identified.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Microstructural characterization of limestone exposed to heat with XRD, SEM and TG-DSC

Highlights: • The microstructure of limestone (25 °C–800 °C) was analyzed by XRD, SEM and TG-DSC. • The microstructural properties of the crystal are anisotropic in different crystal plane directions. • Microstructure controls the macroscopic properties of limestone. - Abstract: Limestone is a common rock used in many buildings and found in underground engineering projects. After exposure to heat, for example, the occurrence of fires, the stability of limestone structures is mostly affected, which may have safety repercussions. Therefore, the impact of thermal effects on the microstructure of limestone is investigated in this study, in which 8 groups of limestone samples are exposed to different temperatures (25 °C, 100 °C, 200 °C, 300 °C, 500 °C, 600 °C, 700 °C and 800 °C), after which X-ray diffraction, differential scanning calorimetry and scanning electron microscopy are carried out. The mineral composition and the microstructure of the samples are numerically modeled, in which the diffraction peaks, full width at half maximum, integral breadth, microstrain, average domain size and dislocation density are analyzed. The macroscopic properties obtained from the results in other works in the literature including porosity, compressive strength, damage coefficients and modulus of elasticity are also compared with the parameters above. The changes in the crystal structure of two minerals, calcite and dolomite, are found to be anisotropic in the different crystal plane directions. It is also found that the limestone microstructure affects the macroscopic properties. A temperature between 200 °C to 300 °C is the critical temperature at which both the macroscopic properties and macrostructure demonstrate significant changes.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Automated identification of deformation twin systems in Mg WE43 from SEM DIC

In this study, the application of machine learning and computer vision approaches to microscale deformation data for the automated identification of deformation twinning systems, and their associated twin area, is introduced. Deformation data was obtained during in-situ SEM compression testing of a WE43 Mg alloy using digital image correlation (DIC) modified for use with electron microscopy. A 5.7 mm × 3.4 mm area of interest was analyzed, generating ~100 million data points of deformation. Experimental twin trace directions were determined by applying k-means clustering, morphological thinning, and Hough transforms to the deformation data. The identification of deformation twinning was achieved by consideration of the twin trace direction, its strain value, and its evolution. The deformation map was divided into areas corresponding to individual active twin systems, enabling the analysis of microstructure dependence of deformation behavior and twinning activity. The performance of the proposed twinning identification approach was evaluated by accuracy, precision, and sensitivity metrics. The effect of the tuning parameters used in the algorithm on the performance is also discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2018

The roles of interfaces and other microstructural features in Cu/Nb nanolayers as revealed by in situ beam bending experiments inside an scanning electron microscope (SEM)

Interfaces and their interactions with other microstructural features, such as grain boundaries or twin structures, have been widely viewed as parameters for designing metallic nanolayers. These interfaces could play a role in hindering cracks from propagating across the nanolayers while in operation. To date, many studies have focused on the roles of interfaces in affecting the plasticity mechanisms and thus the deformability of nanolayers. However, no studies have investigated on the subsequent mechanisms of fracture leading to the final failure. In this study, in situ microfracture bending tests inside a scanning electron microscope (SEM) were performed on the notched clamped beams of Cu/Nb nanolayers with a similar layer thickness using two different fabrication processes: physical vapor deposition (PVD) and accumulative roll bonding (ARB). Due to the columnar grains of the Cu/Nb PVD beams, a sudden catastrophic linear elastic, brittle fracture phenomenon was observed; in the Cu/Nb ARB beams, fracture events of notch widening phase and crack initiation and fracture along the shear instability were observed. Detailed examinations showed the presence of competing mechanisms between the multilayered interface, columnar grain boundary, and experimental factors of beam geometry and the position of the tip. With this newfound knowledge, new types of metallic nanolayers can be designed with enhanced strength and fracture resistant properties.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Site-specific plan-view (S)TEM sample preparation from thin films using a dual-beam FIB-SEM

To fully evaluate the atomic structure, and associated properties of materials using transmission electron microscopy, examination of samples from three non-collinear orientations is needed. This is particularly challenging for thin films and nanoscale devices built on substrates due to limitations with plan-view sample preparation. In this work, a new method for preparation of high-quality, site-specific, plan-view TEM samples from thin-films grown on substrates, is presented and discussed. Here, it is based on using a dual-beam focused ion beam scanning electron microscope (FIB-SEM) system. To demonstrate the method, the samples were prepared from thin films of perovskite oxide BaSnO 3 grown on a SrTiO 3 substrate and metal oxide IrO 2 on a TiO 2 substrate, ranging from 20–80 nm in thicknesses using molecular beam epitaxy. While the method is optimized for the thin films, it can be extended to other site-specific plan-view samples and devices build on wafers. Aberration-corrected STEM was used to evaluate the quality of the samples and their applicability for atomic-resolution imaging and analysis.

BaSnO3↗
DOE OSTI2025

Generalizable Image Segmentation for Microstructure Characterization Through Integrated SEM and EBSD Analysis

We demonstrate generalizable semantic segmentation using minimal ground truth data. Correlated scanning electron microscopy (SEM) images and electron backscatter diffraction (EBSD) measurements of frictionstir processed 316L stainless steel plates were used to train deep learning models for grain boundary segmentation. Secondary electron (SE) imaging taken at an accelerating voltage of 10 keV correlated to EBSD-derived grain boundaries produced the best performing model. Notably, an ensemble of three models trained on a single SE image produced accurate segmentation over a series of BSE images of samples manufactured under different processing parameters, with a resultant mean absolute error in grain size of 0.34 µm. The striking generalizability of the models likely results from the similar escape depths of the SE training input and the EBSD training output and the reduced probability of dislocation artifacts appearing in the image. This finding highlights the importance of considering the physical principles behind imaging in the development of robust segmentation models for microstructure characterization.

Taufique, Mohammad Fuad Nur↗