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NASA NTRSDate not supplied

Variable Pressure - Scanning Electron Microscopy (VP-SEM)

Variable Pressure (or Environmental) Scanning Electron Microscopy (VP-SEM) combined with Energy Dispersive X-ray Spectroscopy (EDS) is one of the most powerful methods for characterizing the sub-micron topography and chemical composition of uncoated samples. Terrestrially, VP-SEM is extensively used to non-destructively study geologic and manufactured materials with high spatial resolution (tens of nanometers) and large depth-of-field. An SEM offers a geologist a first survey of microscopic mineral phases via secondary electron imaging (SEI), which provides a topographic look at a sample, as well as backscattered electron (BEI) imaging, which contrasts the phases present based on their geochemistry (atomic number). A VP-SEM utilizes a gas in the sample chamber as a charge dissipation and signal amplification method, allowing analysis of a sample without preparation in the form of a conductive coating. A miniaturized VP-SEM operating in-situ on a lander or rover would be able to use the CO2-rich Martian atmosphere (e.g., Nier et al., 1976; Williams 2016) as an imaging medium for this purpose. Adaptation of a VP-SEM for in-situ Mars surface studies will provide a new imaging capability (via SEI) that is at least an order of magnitude higher resolution than the Mars Hand Lens Imager (MAHLI) on the Mars Science Laboratory (Williams et al., 2015), and equal to or better than the achieved resolution of the Atomic Force Microscope on the Phoenix Mars lander (Pike et al., 2011). In addition, the MVP-SEM is capable of BSI and simultaneous chemical analysis of the imaged region. In this sense, the MVP-SEM can be regarded as an instrument suite that will provide a new set of information not achievable by any other instrument. The Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) was designed, built, and benchtop tested by a team at NASA’s Marshall Space Flight Center and Jet Propulsion Laboratory (JPL), Jacobs Space Exploration Group, Applied Physics Technologies, Inc. (AP-Tech), and Creare LLC, working with a team of technical and science collaborators. Benchtop testing was successful, proving concept feasibility. To date, the MVP-SEM has achieved an imaging resolution of <100 nm in the lab, and with continued optimization, even better performance (~50 nm resolution) is possible. Use in-situ on the lunar or other planetary surfaces would require some redesign to optimize instrument performance, but such an instrument would be equally useful.

Variable Pressure Scanning Electron Microscopy↗

NASA NTRSDate not supplied

Miniature Variable Pressure - Scanning Electron Microscopy (MVP-SEM)

Variable Pressure Scanning Electron Microscopy↗

DOE OSTI2023

Irradiated Low-Enriched Uranium Fuel Measurements with a Gamma-Ray Scanning System

A gamma-ray scanning system was designed to perform post-irradiation measurements of nuclear fuel at Idaho National Laboratory (INL). The system is composed of a coaxial high-purity germanium (HPGe) detector, a collimator, and mechanical positioning stages that translate the fuel sample across the front of the collimator. A Monte Carlo N-Particle code simulation of the system and the fuel were created with vendor-supplied design specifications, dimensional measurements, and x-ray radiographs of the HPGe detector as well as all available fuel specifications. Benchmark measurements were performed by scanning an irradiated fuel rodlet containing eight pellets of 0.74% enriched UO2 in zirconium alloy. This fuel rodlet was part of the Static Environment Rodlet Transient Test Apparatus (SERTTA) testing campaign in the Transient Reactor Test Facility (TREAT). These results were compared to simulated spectra to help characterize the detector model and establish fidelity. A goal of the system is to determine the number of fissions per gram of UO2 in the fuel. This paper documents the modeling of the system and the calculation of the number of fissions per gram along the axial length of the SERTTA-C rodlet.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2024

Impedance Scan of Inverter-Based Resources and Diesel Generator for Stability Analysis: Preprint

Impedance-based methods are widely used for power system stability analysis with inverter-based resources (IBRs), e.g., assessing dynamic interactions between the power grid and an IBR, control interactions between multiple IBRs, and the sub-synchronous oscillation and damping phenomenon. Since it is difficult to get a numerical model 100% matching with the hardware IBR, using the hardware inverter directly to obtain its output impedance has become a prominent approach nowadays. Therefore, this article presents the impedance scan using hardware IBRs, and also a hardware diesel generator as it still stays with the grid before the grid completely goes to renewable. The devices under test (DuTs) for the impedance scan includes two 3-..phi.., 480 V, 60 Hz commercial grid-forming IBRs (one of 250 kVA and another of 125 kVA rating) in series with ..delta..-Y transformers, one 3-..phi.., 480 V, 60 Hz commercial grid-following IBR (of 125 kVA rating), and a 3-..phi.., 480 V, 60 Hz commercial diesel generator (of 187.5 kVA rating). Using voltage signals perturbed with sub-, inter-, and higher harmonic components, and measuring the current response, the positive-sequence impedances are computed via an offline- based post-analysis. Moreover, best-fit transfer functions are estimated that closely resemble the measured data points of the positive-sequence impedances. Based on the observations from various outcomes of the hardware experiments, this article also provides some fundamental insights on the equivalent positive- sequence impedance of a combination of multiple hardware components by comparing the estimated and the empirically computed impedances. A comparative insight on the damping capability of the DuTs using the positive-sequence impedances of the hardware is also discussed.

grid following inverter↗

DOE OSTI2022

Exploring Physics of Ferroelectric Domain Walls in Real Time: Deep Learning Enabled Scanning Probe Microscopy

The functionality of ferroelastic domain walls in ferroelectric materials is explored in real-time via the in situ implementation of computer vision algorithms in scanning probe microscopy (SPM) experiment. The robust deep convolutional neural network (DCNN) is implemented based on a deep residual learning framework (Res) and holistically nested edge detection (Hed), and ensembled to minimize the out-of-distribution drift effects. The DCNN is implemented for real-time operations on SPM, converting the data stream into the semantically segmented image of domain walls and the corresponding uncertainty. Further the pre-defined experimental workflows perform piezoresponse spectroscopy measurement on thus discovered domain walls, and alternating high- and low-polarization dynamic (out-of-plane) ferroelastic domain walls in a PbTiO 3 (PTO) thin film and high polarization dynamic (out-of-plane) at short ferroelastic walls (compared with long ferroelastic walls) in a lead zirconate titanate (PZT) thin film is reported. This work establishes the framework for real-time DCNN analysis of data streams in scanning probe and other microscopies and highlights the role of out-of-distribution effects and strategies to ameliorate them in real time analytics.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Extracting interface locations in multilayer polymer waveguide films using scanning angle Raman spectroscopy

There is an increasing demand for nondestructive in situ techniques that measure chemical content, total thickness, and interface locations for multilayer polymer films, and SA Raman spectroscopy in combination with appropriate data models can provide this information. A scanning angle (SA) Raman spectroscopy method was developed to measure the chemical composition of multilayer polymer waveguide films and to extract the location of buried interfaces between polymer layers with 7–80-nm axial spatial resolution. The SA Raman method measures Raman spectra as the incident angle of light upon a prism-coupled thin film is scanned. Six multilayer films consisting of poly(methyl methacrylate)/polystyrene or poly(methyl methacrylate)/polystyrene/poly(methyl methacrylate) were prepared with total thicknesses ranging from 330-1260 nm. The interface locations were varied by altering the individual layer thicknesses between 140-680 nm. The Raman amplitude ratio of the 1605 cm -1 peak for PS and 812 cm -1 peak for PMMA was used in calculations of the electric field intensity within the polymer layers to model the SA Raman data and extract the total thickness and interface locations. There is an average 8% and 7% difference in the measured thickness between the SA Raman and profilometry measurements for bilayer and trilayer films, respectively.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Challenge and Solution of Characterizing Glass Transition Temperature for Conjugated Polymers by Differential Scanning Calorimetry

Thermomechanical properties of polymers greatly depend on their glass transition temperature ( T g ). Differential scanning calorimetry (DSC) is commonly used to measure T g of polymers. Yet, many conjugated polymers (CPs), especially donor–acceptor CPs (D–A CPs), do not show a clear glass transition when measured by conventional DSC using simple heat and cool scan. In this work, we discuss the origin of the difficulty for measuring T g in such type of polymers. The changes in specific heat capacity (Δ c p ) at T g were accurately probed for a series of CPs by DSC. The results showed a significant decrease in Δ c p from flexible polymer (0.28 Jg -1 K -1 for polystyrene) to rigid CPs (10 -3 Jg -1 K -1 for a naphthalene diimide-based D–A CP). When a conjugation breaker unit (flexible unit) is added to the D–A CPs, we observed restoration of the Δ c p at T g by a factor of 10, confirming that backbone rigidity reduces the Δ c p . Additionally, an increase in the crystalline fraction of the CPs further reduces Δ c p . We conclude that the difficulties of determining T g for CPs using DSC are mainly due to rigid backbone and semicrystalline nature. We also demonstrate that physical aging can be used on DSC to help locate and confirm the glass transition for D-A CPs with weak transition signals.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Three-dimensional phenotyping of peach tree-crown architecture utilizing terrestrial laser scanning

Tree training systems for temperate fruit have been developed throughout history by pomologists to improve light interception, fruit yield, and fruit quality. These training systems direct crown and branch growth to specific configurations. Quantifying crown architecture could aid the selection of trees that require less pruning or that naturally excel in specific growing/training system conditions. Regarding peaches [Prunus persica (L.) Batsch], access tools such as branching indices have been developed to characterize tree-crown architecture. However, the required branching data (BD) to develop these indices are difficult to collect. Traditionally, BD have been collected manually, but this process is tedious, time-consuming, and prone to human error. These barriers can be circumnavigated by utilizing terrestrial laser scanning (TLS) to obtain a digital twin of the real tree. TLS generates three-dimensional (3D) point clouds of the tree crown, wherein every point contains 3D coordinates (x, y, z). To facilitate the use of these tools for peach, we selected 16 young peach trees scanned in 2021 and 2022. These 16 trees were then modeled and quantified using the open-source software TreeQSM. As a result, “in silico” branching and biometric data for the young peach trees were calculated to demonstrate the capabilities of TLS phenotyping of peach tree-crown architecture. The comparison and analysis of field measurements (in situ) and in silico BD, biometric data, and quantitative structural model branch uncertainty data were utilized to determine the reconstructive model’s reliability as a source substitute for field measurements. Mean average deviation when comparing young tree (YT) height was approx. 5.93%, with crown volume was approx. 13.26% across both 2021 and 2022. All point clouds of the YTs in 2022 showed residuals lower than 12 mm to cylinders fitted to all branches, and mean surface coverage greater than 40% for both the trunk and primary branching orders.

09 BIOMASS FUELS↗

DOE OSTI2024

Tip-Induced 3D Printing on the Nanoscale with Field Emission Scanning Probes

3D printing down to the nanoscale remains a significant challenge. In this paper, the study explores the use of scanning probes that emit low-energy electrons (<100 eV) coupled with the localized injection and electron-induced decomposition of precursor molecules, for the precise localized deposition of 3D nanostructures. The experiments are performed inside the chamber of a scanning electron microscope (SEM), enabling the use of the in-built gas injector system (GIS) with gaseous naphthalene precursor for carbon deposition, as well as immediate inspection of the deposits by SEM. Substrate materials are planar fused silica with thin conductive coatings and non-planar copper wedges. After investigation of the deposition process parameters, various 2D and 3D carbon deposits are grown. Vertical nanowires several microns in length with a diameter <100 nm are achieved and 3D deposits with a high degree of nanoscale branching are also obtained, presumably due to a charging effect. High aspect ratio carbon nanostructures such as those demonstrated here can be employed as miniaturized electrodes or field emitters. The tip-based approach presented thus paves the way toward 3D nanoscale printing of various materials and functional nanostructures.

3D printing↗

DOE OSTI2023

A Platform for Atomic Fabrication and In Situ Synthesis in a Scanning Transmission Electron Microscope

Here, the engineering of quantum materials requires the development of tools able to address various synthesis and characterization challenges. These include the establishment and refinement of growth methods, material manipulation, and defect engineering. Atomic-scale modification will be a key enabling factor for engineering quantum materials where desired phenomena are critically determined by atomic structures. Successful use of scanning transmission electron microscopes (STEMs) for atomic scale material manipulation has opened the door for a transformed view of what can be accomplished using electron-beam-based strategies. However, serious obstacles exist on the pathway from possibility to practical reality. One such obstacle is the in situ delivery of atomized material in the STEM to the region of interest for further fabrication processes. Here, progress on this front is presented with a view toward performing synthesis (deposition and growth) processes in a scanning transmission electron microscope in combination with top-down control over the reaction region. An in situ thermal deposition platform is presented, tested, and deposition and growth processes are demonstrated. In particular, it is shown that isolated Sn atoms can be evaporated from a filament and caught on the nearby sample, demonstrating atomized material delivery. This platform is envisioned to facilitate real-time atomic resolution imaging of growth processes and open new pathways toward atomic fabrication.

36 MATERIALS SCIENCE↗

DOE OSTI2024

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

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

36 MATERIALS SCIENCE↗

DOE OSTI2024

Automatic Digitization and Orientation of Scanned Mesh Data for Floor Plan and 3D Model Generation

This paper describes a novel approach for generating accurate floor plans and 3D models of building interiors using scanned mesh data. Unlike previous methods, which begin with a high resolution point cloud from a laser range-finder, our approach begins with triangle mesh data, as from a Microsoft HoloLens. It generates two types of floor plans, a “pen-and-ink” style that preserves details and a drafting-style that reduces clutter. It processes the 3D model for use in applications by aligning it with coordinate axes, annotating important objects, dividing it into stories, and removing the ceiling. Its performance is evaluated on commercial and residential buildings, with experiments to assess quality and dimensional accuracy. Our approach demonstrates promising potential for automatic digitization and orientation of scanned mesh data, enabling floor plan and 3D model generation in various applications such as navigation, interior design, furniture placement, facilities management, building construction, and HVAC design.

Sharma, Ritesh↗

DOE OSTI2021

Perseverance’s Scanning Habitable Environments with Raman and Luminescence for Organics and Chemicals (SHERLOC) Investigation

The Scanning Habitable Environments with Raman and Luminescence for Organics and Chemicals (SHERLOC) is a robotic arm-mounted instrument on NASA’s Perseverance rover. SHERLOC has two primary boresights. The Spectroscopy boresight generates spatially resolved chemical maps using fluorescence and Raman spectroscopy coupled to microscopic images (10.1 μm/pixel). The second boresight is a Wide Angle Topographic Sensor for Operations and eNgineering (WATSON); a copy of the Mars Science Laboratory (MSL) Mars Hand Lens Imager (MAHLI) that obtains color images from microscopic scales (~13 μm/pixel) to infinity. SHERLOC Spectroscopy focuses a 40 μs pulsed deep UV neon-copper laser (248.6 nm), to a ~100 μm spot on a target at a working distance of ~48 mm. Fluorescence emissions from organics, and Raman scattered photons from organics and minerals, are spectrally resolved with a single diffractive grating spectrograph with a spectral range of 250 to ~370 nm. Because the fluorescence and Raman regions are naturally separated with deep UV excitation (<250 nm), the Raman region ~ 800 – 4000 cm -1 (250 to 273 nm) and the fluorescence region (274 to ~370 nm) are acquired simultaneously without time gating or additional mechanisms. SHERLOC science begins by using an Autofocus Context Imager (ACI) to obtain target focus and acquire 10.1 μm/pixel greyscale images. Chemical maps of organic and mineral signatures are acquired by the orchestration of an internal scanning mirror that moves the focused laser spot across discrete points on the target surface where spectra are captured on the spectrometer detector. ACI images and chemical maps (< 100 μm/mapping pixel) will enable the first Mars in situ view of the spatial distribution and interaction between organics, minerals, and chemicals important to the assessment of potential biogenicity (containing CHNOPS). Single robotic arm placement chemical maps can cover areas up to 7x7 mm in area and, with the < 10 min acquisition time per map, larger mosaics are possible with arm movements. This microscopic view of the organic geochemistry of a target at the Perseverance field site, when combined with the other instruments, such as Mastcam-Z, PIXL, and SuperCam, will enable unprecedented analysis of geological materials for both scientific research and determination of which samples to collect and cache for Mars sample return.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2012

Scanning Seebeck Coefficient Measurement System for Homogeneity Characterization of Bulk and Thin-Film Thermoelectric Materials

Larger-scale production of thermoelectric materials is necessary when mass-producing thermoelectric devices at industrial level. Certain fabrication techniques can create inhomogeneity in the material through composition and doping fluctuations throughout the sample, causing local variations in thermoelectric properties. Some variations are in the range of sub-millimeter scale or larger but may be difficult to detect by traditional materials characterization techniques such as x-ray diffraction or scanning electron microscopy when the chemical variation is small but the doping variation, which strongly affects thermoelectric performance, is large. In this paper, a scanning apparatus to directly detect local variations of Seebeck coefficient on both bulk and thin-film samples is used. Results have shown that this technique can be utilized for detection of defective regions, as well as phase separation in the 100-m range or larger.

Iwanaga, S↗

DOE OSTI2019

Prevalence and variability in reporting of clinically actionable incidental findings on attenuation-correction CT scans in a veteran population

Background: Myocardial perfusion imaging (MPI) often employs attenuation-correction computed tomography (CTAC) to reduce attenuation artifacts and improve specificity. While there is no specific guideline on how they should be reported, incidental noncardiac findings identified on these scans may be clinically significant. The prevalence of these findings in veterans is not currently known. In addition, variability in reporting these findings may depend on the interpreting physician’s specialty. Methods: To guide future decision-making, CTACs in veterans referred for MPI were prospectively evaluated in a quality-control project for a set of prespecified actionable incidental findings by cardiologists and a radiologist. Results: On the 771 scans performed over eight months, 285 incidental noncardiac findings were identified by the interpreting cardiologists and 378 were identified by the interpreting radiologist. Pulmonary nodules were the most common occurring in 20% of studies read by the radiologist. Interreader agreements between cardiologists and the radiologist were poor for pulmonary nodules ≥ 10 mm and hiatal hernias; fair for pulmonary nodules < 10 mm, extracardiac masses, and aortic aneurysms; and moderate for pleural plaques. Conclusion: Incidental noncardiac findings on CTACs are common in our veteran population. Overall interobserver agreement in identifying these findings between cardiologists and radiologists is fair. Specific guidelines are needed on how CTACs should be read and reported.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

DOE OSTI2022

Mapping structural heterogeneity at the nanoscale with scanning nano-structure electron microscopy (SNEM)

Here, in this work, we explore the use of scanning electron diffraction (also known as 4D-STEM) coupled with electron atomic pair distribution function analysis (ePDF) to understand the local order (structure and chemistry) as a function of position in a complex multicomponent system, a hot rolled, Ni-encapsulated, Zr 65 Cu 17.5 Ni 10 Al 7.5 bulk metallic glass (BMG), with a spatial resolution of 3 nm. We show that it is possible to gain insight into the chemistry and chemical clustering/ordering tendency in different regions of the sample, including in the vicinity of nano-scale crystallites that are identified from virtual dark field images and in heavily deformed regions at the edge of the BMG. In addition to simpler analysis, unsupervised machine learning was used to extract partial PDFs from the material, modeled as a quasi-binary alloy, and map them in space. These maps allowed key insights not only into the local average composition, as validated by EELS, but also a unique insight into chemical short-range ordering tendencies in different regions of the sample during formation. The experiments are straightforward and rapid and, unlike spectroscopic measurements, don’t require energy filters on the instrument. We spatially map different quantities of interest (QoI’s), defined as scalars that can be computed directly from positions and widths of ePDF peaks or parameters refined from fits to the patterns. We developed a flexible and rapid data reduction and analysis software framework that allows experimenters to rapidly explore images of the sample on the basis of different QoI’s. The power and flexibility of this approach are explored and described in detail. Because of the fact that we are getting spatially resolved images of the nanoscale structure obtained from ePDFs we call this approach scanning nano-structure electron microscopy (SNEM), and we believe that it will be powerful and useful extension of current 4D-STEM methods.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Influence of scan pattern and geometry on the microstructure and soft-magnetic performance of additively manufactured Fe-Si

The influence of geometry and scan pattern on the microstructure evolution and magnetic performance of additively manufactured Fe-3Si components was investigated. To reduce eddy current losses, novel geometries were designed and built and the microstructure and properties of these samples were characterized. The laser scan pattern was shown to strongly influence both the as-built grain structure and strength of the crystallographic texture, resulting in measurable changes in the as-built magnetic performance. In thin wall samples, heat treatment resulted in an increase in the maximum relative magnetic permeability and decrease in power losses in most samples, consistent with grain growth. However, decreases in the spacing between thin walls to increase the stacking factor of the cross-section was shown to result in unwanted electrical shorting between walls and an increase in eddy current losses. Compared to simple parallel plate construction and a mesh structure, a novel cross-section design based on the Hilbert space filling curve was found to produce the lowest power losses. The mechanisms behind these results were explored using a combination of heat conduction and electromagnetic simulations, providing a route for future component and process optimization.

36 MATERIALS SCIENCE↗

DOE OSTI2011

Assessment of Early Toxicity and Response in Patients Treated With Proton and Carbon Ion Therapy at the Heidelberg Ion Therapy Center Using the Raster Scanning Technique

Puropose: To asses early toxicity and response in 118 patients treated with scanned ion beams to validate the safety of intensity-controlled raster scanning at the Heidelberg Ion Therapy Center. Patients and Methods: Between November 2009 and June 2010, we treated 118 patients with proton and carbon ion radiotherapy (RT) using active beam delivery. The main indications included skull base chordomas and chondrosarcomas, salivary gland tumors, and gliomas. We evaluated early toxicity within 6 weeks after RT and the initial clinical and radiologic response for quality assurance in our new facility. Results: In all 118 patients, few side effects were observed, in particular, no high numbers of severe acute toxicity were found. In general, the patients treated with particle therapy alone showed only a few single side effects, mainly Radiation Therapy Oncology Group/Common Terminology Criteria grade 1. The most frequent side effects and cumulative incidence of single side effects were observed in the head-and-neck patients treated with particle therapy as a boost and photon intensity-modulated RT. The toxicities included common radiation-attributed reactions known from photon RT, including mucositis, dysphagia, and skin erythema. The most predominant imaging responses were observed in patients with high-grade gliomas and those with salivary gland tumors. For skull base tumors, imaging showed a stable tumor outline in most patients. Thirteen patients showed improvement of pre-existing clinical symptoms. Conclusions: Side effects related to particle treatment were rare, and the overall tolerability of the treatment was shown. The initial response was promising. The data have confirmed the safe delivery of carbon ions and protons at the newly opened Heidelberg facility.

62 RADIOLOGY AND NUCLEAR MEDICINE↗