Utilizing Distributional Measurements of Material Characteristics from SEM Images for Inverse Prediction.
Abstract not provided.
Ries, Daniel↗
SEARCH · Engineering Papers
Results for “SEM”
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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2D microstructure reconstruction for SEM via non-local patch-based image inpainting.
Abstract not provided.
Tran, Anh↗
NEUP IMEBM Project: Solubility Experiments on Carbon Fibers, Results from SEM-EDS & XRD.
Abstract not provided.
Jove-Colon, Carlos↗
Slides on AFC-4C-R5 MNT20E destructive PIE :SEM, Micro-tensile testing, Post-test TEM Characterization
Slides containing updated PIE results for AFC-4C-R5 (MNT20E)
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
Microanalysis of Irradiated Metallic Hydride Nuclear Fuel (U{sub 0.17}ZrH{sub 1.6})
Metallic hydride nuclear fuels (U{sub 0.17} ZrH{sub 1.6}) have been under consideration for use in Light Water Reactors (LWRs). The fuel matrix consists of isolated particles of uranium metal within a zirconium hydride matrix. Erbium was also added as a neutron poison enabling higher reactor performance. These fuels were encased in a Zircaloy-2 cladding with a Bi/Pb eutectic liquid metal filled-gap to improve thermal conductivity. The inner and outer cladding surfaces were oxidized to nominal 1 μm thickness to eliminate hydrogen attack. The fuels were termed UCB to note the location of fabrication as the University of California-Berkeley. Irradiations were performed in the MITR research reactor. The details are described elsewhere. We originally reported on post-irradiation analysis of the fuel elements of two of the rodlets using Scanning Electron Microscopy (SEM) and x-ray energy dispersive spectroscopy (EDS). In this further study, funded as a rapid turnaround experiment (RTE) through the Nuclear Science User Facilities (NSUF) program, we performed high-resolution Scanning Transmission Electron Microscopy (STEM) of thin lift-out specimens prepared from specific regions in the fuel matrix using an SEM-Focused Ion Beam (FIB) instrument, and again compared these results to the unirradiated material. Earlier investigations using SEM-EDS showed that ∼8% of the Zircaloy cladding had dissolved in the Pb-Bi eutectic during irradiation over 1000 hrs. However, the SEM-EDS failed to show any detectable evidence of damage of the fuel matrix. There was no obvious swelling or migration of elements; hence, we focused on these specific regions in greater detail. Much of the data on hydride fuels come from the Space Nuclear Auxiliary Power (SNAP) program from the 1960's. The principle difference between oxide and hydride fuel is the high thermal conductivity of the latter. This feature greatly decreases the temperature drop over the fuel during operation, thereby reducing the release of fission gases to the fraction due only to recoil. However, very unusual early swelling due to void formation around the uranium metal particles has been reported in hydride fuels over 700 deg. C. In this investigation, the fuel did not reach these extreme temperatures. Phases formed in this system have been previously experimentally investigated using thermal analysis techniques, and wavelength and energy dispersive spectroscopy (EDS/WDS) in scanning electron microscopes (SEM). Major changes were observed in the liquid metal and cladding components but at the scale of the SEM observations, it was not readily apparent that any major changes had occurred to the fuel matrix (i.e. U metal particles in the zirconium hydride matrix with interdispersed erbium metal). Rapid oxidation of the SEM mechanically polished cross-sections, may have obscured our ability to see major changes. By using the SEM-FIB slices, it was possible to remove oxide coatings and the smoother surfaces were found to be less susceptible to oxidation once removed from the vacuum chamber. The high spatial resolution of STEM allowed characterization of individual matrix phases.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
Direct comparison between X-ray nanotomography and scanning electron microscopy for the microstructure characterization of a solid oxide fuel cell anode
X-ray computed nanotomography (nano-CT) and scanning electron microscopy (SEM) have been applied to characterize the microstructure of a Solid Oxide Fuel Cell (SOFC) anode. A direct comparison between the results of both methods is conducted on the same region of the microstructure to assess the spatial resolution of the nano-CT microstructure, SEM being taken as a reference. A registration procedure is proposed to find out the position of the SEM image within the nano-CT volume. It involves a second SEM observation, which is taken along an orthogonal direction and gives an estimate reference SEM image position, which is then refined by an automated optimization procedure. This enables an unbiased comparison between the cell porosity morphologies provided by both methods. In the present experiment, nano-CT is shown to underestimate the number of pores smaller than 1 μm and overestimate the size of the pores larger than 1.5 μm. - Highlights: ► X-ray computed nanotomography (nano-CT) and SEM are used to characterize an SOFC anode. ► A methodology is proposed to compare the nano-CT and SEM data on the same region. ► The spatial resolution of the nano-CT data is assessed from that comparison.
36 MATERIALS SCIENCE↗
Sub-50 nm metrology on extreme ultra violet chemically amplified resist—A systematic assessment
With lithographic patterning dimensions decreasing well below 50 nm, it is of high importance to understand metrology at such small scales. This paper presents results obtained from dense arrays of contact holes (CHs) with various Critical Dimension (CD) between 15 and 50 nm, as patterned in a chemically amplified resist using an ASML EUV scanner and measured at ASML and TNO. To determine the differences between various (local) CD metrology techniques, we conducted an experiment using optical scatterometry, CD-Scanning Electron Microscopy (CD-SEM), Helium ion Microscopy (HIM), and Atomic Force Microscopy (AFM). CD-SEM requires advanced beam scan strategies to mitigate sample charging; the other tools did not need that. We discuss the observed main similarities and differences between the various techniques. To this end, we assessed the spatial frequency content in the raw images for SEM, HIM, and AFM. HIM and AFM resolve the highest spatial frequencies, which are attributed to the more localized probe-sample interaction for these techniques. Furthermore, the SEM, HIM, and AFM waveforms are analyzed in detail. All techniques show good mutual correlation, albeit the reported CD values systematically differ significantly. HIM systematically reports a 25% higher CD uniformity number than CD-SEM for the same arrays of CHs, probably because HIM has a higher resolution than the CD-SEM used in this assessment. A significant speed boost for HIM and AFM is required before these techniques are to serve the demanding industrial metrology applications like optical critical dimension and CD-SEM do nowadays.
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
Chemo-Mechanical Instabilities in Lithium Cobalt Oxide at Higher State-Of-Charge in Li-Ion Batteries
Transition metal oxide cathodes are widely used in commercial Li-ion batteries. However, their practical charge capacity is limited due to severe chemo-mechanical instabilities at higher charge voltage, and state-of-charge condition. Here, in situ stress and strain measurements were synchronized to probe mechanical deformations in the lithium cobalt oxide (LCO) cathode via a multi-beam stress sensor and digital image correlation, respectively. In situ mechanical measurements revealed how Li removal from the electrode structure induces deformations on the LCO composite cathodes during cycling. The structure and morphology of the LCO cathodes were further investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM) studies. Two distinct electrochemical and mechanical behaviors were identified when the LCO was charged up to 4.65 V. The LCO undergoes a compressive stress generation when charged up to 4.2 V and surface fractures on the LCO particles were detected by SEM. LCO cathode experienced significantly large contractions (negative strains) when charged up to 4.65 V, where intergranular crack formation and phase transformation were detected on the LCO particles via SEM and XRD, respectively. Overall, the study bridges complicated structural deformations with in situ analysis of mechanical degradations in LCO cathodes charged at higher voltages. The correlation is vital to understanding instability mechanisms in transition metal oxides at high voltages for alkali metal ion batteries.
higher state-of-charge↗
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↗
Resolving the Electron Plume within a Scanning Electron Microscope
Scanning electron microscopy (SEM), a century-old technique, is today a ubiquitous method of imaging the surface of nanostructures. However, most SEM detectors simply count the number of secondary electrons from a material of interest, and thereby overlook the rich material information contained within them. Here, by simple modifications to a standard SEM tool, we resolve the momentum and energy information on secondary electrons by directly imaging the electron plume generated by the electron beam of the SEM. Leveraging these spectroscopic imaging capabilities, our technique is able to image lateral electric fields across a prototypical silicon p–n junctions and to distinguish differently doped regions, even when buried beyond depths typically accessible by SEM. Intriguingly, the subsurface sensitivity of this technique reveals unexpectedly strong surface band bending within nominally passivated semiconductor structures, providing useful insights for complex layered component designs, in which interfacial dynamics dictate device operation. Further, these capabilities for noninvasive, multimodal probing of complicated electronic components are crucial in today’s electronic manufacturing but is largely inaccessible even with sophisticated techniques. These results show that seemingly simple SEM can be extended to probe complex and useful material properties.
36 MATERIALS SCIENCE↗
Study of Percutaneous Stent Placement with Iodine-125 Seed Strand for Malignant Biliary Obstruction
Purpose: To evaluate the effectiveness and safety of simultaneous placement of a self-expandable metallic stents (SEMS) and iodine-125 seed strand in the management of malignant obstructive jaundice (MOJ). Materials and Methods: This study included 132 patients with MOJ treated from November 2015 to October 2017. Forty-five patients underwent insertion of SEMS with iodine-125 seed strands (Seeds group); the remaining 87 patients underwent SEMS placement alone (Control group). Technical success was defined as accurate, successful deployment of SEMS with or without iodine-125 seed strand; clinical success was defined as 20% reduction in serum bilirubin within 1 week after the procedure, compared with baseline. Complications, duration of primary stent patency, and overall survival were evaluated. Results: Technical success was achieved in all patients in both groups. In the Seeds group, an average of 14 seeds (range 8–22) were implanted in the bile duct as a strand. Clinical success rates were similar between the groups (Seeds group, 93.3%; Control group, 95.4%). Major complications occurred in only one patient, in the Control group. The median period of primary stent patency was significantly longer in the Seeds group (194 days) than in the Control group (86 days; P = 0.049). The median overall survival was also significantly longer in the Seeds group (194 days) than in the Control group (96 days; P = 0.031). Conclusion: SEMS combined with iodine-125 seed strands is effective and safe in the management of MOJ and can improve stent patency and patient survival.
62 RADIOLOGY AND NUCLEAR MEDICINE↗
Paw-Net: Stacking ensemble deep learning for segmenting scanning electron microscopy images of fine-grained shale samples
Segmentation of scanning electron microscopy (SEM) images is critical yet time-consuming for geological analyses, as it needs to differentiate the boundaries for different mineral objects to facilitate subsequent analyses, such as porosity calculation. Recently, various machine learning methods, especially convolutional neural networks (CNNs), have been explored to segment SEM images of fine-grained shale samples. However, we found that general CNNs do not yield optimal performance due to insufficient training data and imbalanced objects in SEM images. This work has revised the U-Net architecture, a popular approach for biomedical image analyses, by incorporating a loss function that addresses the imbalance issue. Furthermore, we used the ensemble learning method to train multiple models and combined the results to improve the overall performance of segmentation. We prepared 2162 sub-images from raw SEM images in our experiments and divided them into training, validation, and testing datasets. The overall results show that our method improves the average Intersection over Union (IOU) of mineral objects from 0.49 to 0.58, compared to the original U-Net model. Our method can clearly distinguish each object from others with boundaries, even in highly imbalanced images. Training our models takes less than three minutes using a single GPU, while manual labeling can take up to three hours for each image. Furthermore, the method helps geoscientists gain insights quickly and effectively by building neural network models from a small dataset of SEM images.
58 GEOSCIENCES↗
Nano-Scale Fission Product Phases in an Irradiated U-7Mo Alloy Nuclear Fuel
Irradiated nuclear fuel is a very difficult material to characterize. Due to the large radiation fields associated with these materials, they are hard to handle and typically have to be contained in large hot cells. Even the equipment used for performing characterization is housed in hot cells or shielded glove boxes. The result is not only a limitation in the techniques that can be employed for characterization, but also a limitation in the size of features that can be resolved The most standard characterization techniques include light optical metallography (WM), scanning electron microscopy (SEM), and electron probe microanalysis (EPMA). These techniques are applied to samples that are typically prepared using grinding and polishing approaches that will always generate some mechanical damage on the sample surface. As a result, when performing SEM analysis, for example, the analysis is limited by the quality of the sample surface that can be prepared. However, a new approach for characterizing irradiated nuclear fuel has recently been developed at the Idaho National Laboratory (INL) in Idaho Falls, Idaho. It allows for a dramatic improvement in the quality of characterization that can be performed when using an instrument like an SEM. This new approach uses a dual-beam scanning microscope, where one of the beams isa focused ion beam (FIB), which can be used to generate specimens of irradiated fuel (-10µm x 10µm) for microstructural characterization, and the other beam is the electron beam of an SEM. One significant benefit of this approach is that the specimen surface being characterized has received much less damage (and smearing) than is caused by the more traditional approaches, which enables the imaging of nanometer sized microstructural features in the SEM. The process details are for an irradiated low-enriched uranium (LEU) U-Mo alloy fuel Another type of irradiated fuel that has been characterized using this technique is a mixed oxide fuel.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
A fine pore-preserved deep neural network for porosity analytics of a high burnup U-10Zr metallic fuel
Abstract U-10 wt.% Zr (U-10Zr) metallic fuel is the leading candidate for next-generation sodium-cooled fast reactors. Porosity is one of the most important factors that impacts the performance of U-10Zr metallic fuel. The pores generated by the fission gas accumulation can lead to changes in thermal conductivity, fuel swelling, Fuel-Cladding Chemical Interaction (FCCI) and Fuel-Cladding Mechanical Interaction (FCMI). Therefore, it is crucial to accurately segment and analyze porosity to understand the U-10Zr fuel system to design future fast reactors. To address the above issues, we introduce a workflow to process and analyze multi-source Scanning Electron Microscope (SEM) image data. Moreover, an encoder-decoder-based, deep fully convolutional network is proposed to segment pores accurately by integrating the residual unit and the densely-connected units. Two SEM 250 × field of view image datasets with different formats are utilized to evaluate the new proposed model’s performance. Sufficient comparison results demonstrate that our method quantitatively outperforms two popular deep fully convolutional networks. Furthermore, we conducted experiments on the third SEM 2500 × field of view image dataset, and the transfer learning results show the potential capability to transfer the knowledge from low-magnification images to high-magnification images. Finally, we use a pre-trained network to predict the pores of SEM images in the whole cross-sectional image and obtain quantitative porosity analysis. Our findings will guide the SEM microscopy data collection efficiently, provide a mechanistic understanding of the U-10Zr fuel system and bridge the gap between advanced characterization to fuel system design.
36 MATERIALS SCIENCE↗
Observation of two-dimensional p-type dopant diffusion across a p{sup +}-InP/n{sup -}-InGaAs interface using scanning electron microscopy
Scanning electron microscopy (SEM) with potential calculations has been shown to be effective for the detection of p-type dopant diffusion, even across a Zn doped p{sup +}-InP/non-doped n{sup -}-InGaAs/n{sup +}-InP heterojunction. Heterojunction samples were observed using SEM and the electrostatic potential was calculated from Zn concentration profiles obtained by secondary ion mass spectrometry. The sensitivity of SEM for the potential was derived from the SEM observations and potential calculation results. The results were then used to investigate the dependence of the SEM contrast on the Zn diffusion length across the p{sup +}-InP/non-doped n{sup -}-InGaAs interface. Accurate dopant mapping was difficult when the Zn diffusion length was shorter than 30 nm, because the heterojunction affects the potential at the interface. However, accurate dopant mapping was possible when the Zn diffusion length was longer than 30 nm, because the factor dominating the potential variation was not the heterojunction, but rather Zn diffusion 30 nm distant from the interface. Thus, Zn diffusion further than 30 nm from a Zn-doped p{sup +}-InP/non-doped n{sup -}-InGaAs interface can be effectively detected by secondary electron (SE) imaging. SE imaging with potential calculations can be widely used for accurate dopant mapping, even at heterojunctions, and is, therefore, expected to be of significant assistance to the compound semiconductor industry.
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
Characteristics of different frequency ranges in scanning electron microscope images
We demonstrate a new approach to characterize the frequency range in general scanning electron microscope (SEM) images. First, pure frequency images are generated from low frequency to high frequency, and then, the magnification of each type of frequency image is implemented. By comparing the edge percentage of the SEM image to the self-generated frequency images, we can define the frequency ranges of the SEM images. Characterization of frequency ranges of SEM images benefits further processing and analysis of those SEM images, such as in noise filtering and contrast enhancement.
71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
SU-E-T-30: Absorbed Doses Determined by Texture Analysis of Gafchromic EBT3 Films Using Scanning Electron Microscopy: A Feasibility Study
Purpose: The texture analysis method is useful to estimate structural features of images as color, size, and shape. The study aims to determine a dose-response curve by texture analysis of Gafchromic EBT3 film images using scanning electron microscopy (SEM). Methods: The uncoated Gafchromic EBT3 films were prepared to directly scan over the active surface layer of EBT3 film using SEM. The EBT3 films were exposed at a dose range of 0 to 10 Gy using a 6 MV photon beam. The exposed film samples were SEM-scanned at 100X, 1000X, and 3000X magnifications. The four texture features (Homogeneity, Correlation, Contrast, and Energy) were calculated based on the gray level co-occurrence matrix (GLCM) derived from the SEM images at each dose. To validate a correlation between delivered doses and texture features, an R-squared value in linear regression was tested. Results: The results showed that the Correlation index was more suitable as dose indices than the other three texture features due to higher linearity and sensitivity of the dose response curves. Further the Correlation index of 3000X magnified SEM images with 9 pixel offsets had an R-squared value of 0.964. The differences between the delivered doses and the doses measured by this method were 0.9, 1.2, 0.2, and 0.2 Gy at 5, 10, 15, and 20 Gy, respectively. Conclusion: It seems to be feasible to convert micro-scale structural features of {sub χ}t{sub χχχ}he EBT3 films to absorbed doses using the texture analysis method.
60 APPLIED LIFE SCIENCES↗
The Combined Detection of Morphological and Molecular Biomarkers: Implications for Astrobiology
Experience gathered by previous researchers during their hunt for evidence of early Earth life has shown the complexity in interpreting observations of possible microfossils and to establish the evidence to be positive. Similarly, the stillsimmering controversy on the nature of the nano-structures in Martian meteorite ALH84001 described by McKay et al. (1996) emphasizes the difficulties of conclusively identifying those structures as (a) fossilized bacterial cells and (b) establish their indigeneity. A better understanding of biological signatures in rocks is needed in order to identify traces of microbial life, which include morphological, mineralogical and chemical traces. It is thus considered crucial to tackle the problems emerging in the search for evidence of early life on Earth and in exopaleontological research with a multidisciplinary approach. With this is mind we applied surface sensitive Time of Flight-Secondary Ion Mass Spectroscopy (ToF-SIMS) to a previously described 25 m.y. old fossil bacterial biofilm. This technique allows in situ analysis with high mass resolution as well as molecular imaging of micron sized structures. As no extraction or derivatisation of the sample is required for ToF-SIMS analysis, electron microscopical investigation of the same samples subsequent to analysis is possible, thus allowing the combination of molecular and morphological biomarkers. The analysed fossil bacterial biofilms were associated with macrofossils from volcanoclastic lacustrine sediments from the Upper Oligocene Enspel formation (Germany). Preliminary scanning electron microscopy (SEM) studies have shown that a fossil structure interpreted as a coprolite purely consisted of fossilized bacterial biofilm. For ToF-SIMS investigation small particles were taken from the fossil biofilm and mounted onto Au-coated In-foil and analysed in a Phi Evans T-2000 TRIFT system. The ToF-SIMS analysed samples were Au/Pd-sputter coated and imaged using a Philips XL40 Field Emission Gun SEM (FEG-SEM). ToF-SIMS analysis of the organic rich fossil biofilm (TOC 29%) in the 0-100 Dalton (Da) range showed significant amounts of inorganic species, confirming the results obtained previously by EDX analysis, clearly showing the bacterial fossils to be mineralised. ToF-SIMS furthermore revealed the presence of a variety of low- and high-mass organic molecules and fragments thereof. These include peaks indicative of alkenes and alkanes, aromatic organic species and the polycyclic aromatic hydrocarbon naphthalene. More tentatively, peaks indicative of alkyl pyrroles and pyridyl-CH2 were identified. Other peaks of interest include peaks indicative of C(n)H(2n)O2 and C(n)H(2n-2)O2, which according to their general formula would suggest the presence of both saturated and unsaturated fatty acids although further in situ derivatisation experiments and GC-MS (Gas Chromatography MS) need to be applied to verify this beyond doubt. Furthermore, peaks at m/z 370, 384, 398, 412, 426, 440, 454 and 468 were identified, which indicate the potential presence of bacterial hopanes, a class of biomarkers indicative of bacteria. The main diagnostic peak for this group of chemicals is the fragment at m/z 191.18. Our studies conducted on purified hopane standards have shown that in the high-mass resolution mode differentiation of this diagnostic hopane peak and polyethylene at m/z 191.05 is possible. However, the spectra discussed here were collected in the lower resolution mapping mode, therefore this differentiation was not possible. The centroids of the possible hopane peaks obtained on the fossil biofilms are well within the range associated with bacterial hopanes. There is a strong possibility therefore that hopanoids may be associated with the fossil bacterial cells. Due to the non-destructive nature of ToF-SIMS, analysed samples can be studied using SEM, thus allowing the combination of morphological and molecular biomarkers. Subsequent SEM analysis of the ToF-SIMS analysed samples confirmed that the analysed material purely consists of fossil bacterial cells. This is thus the first successful effort to demonstrate the combination of spectral and morphological biomarkers. The advantages of highly sensitive non-destructive in situ analysis techniques for biomarker detection are invaluable, particularly with respect to envisaged Mars sample return missions, as it may allow us to identify remains and traces of former microbial life in both ancient terrestrial and extraterrestrial materials. This technique may prove particularly useful in the quest for extraterrestrial life with respect to precious extraterrestrial materials, as minute quantities are sufficient to conduct analysis.
Toporski, J.↗