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Particle Distribution Measurement of Pyrotechnic Mixtures using High Resolution Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopic (EDS) Imaging
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Exploring the Extremes via In-Situ Scanning Electron Microscopy.
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A Novel Experimental Approach to Understand the Transport of Nanodrugs
Nanoparticle-based drugs offer attractive advantages like targeted delivery to the diseased site and size and shape-controlled properties. Therefore, understanding the particulate flow of the nanodrugs is important for effective delivery, accurate prediction of required dosage, and developing efficient drug delivery platforms for nanodrugs. In this study, the transport of nanodrugs including flow velocity and deposition is investigated using three model metal oxide nanodrugs of different sizes including iron oxide, zinc oxide, and combined Cu-Zn-Fe oxide synthesized via a modified polyol approach. The hydrodynamic size, size, morphology, chemical composition, crystal phase, and surface functional groups of the water-soluble nanodrugs were characterized via dynamic light scattering, transmission electron microscopy, scanning electron microscopy-energy dispersive X-ray, X-ray diffraction, and fourier transform infrared spectroscopy, respectively. Two different biomimetic flow channels with customized surfaces are developed via 3D printing to experimentally monitor the velocity and deposition of the different nanodrugs. A diffusion dominated mechanism of flow is seen in size ranges 92 nm to 110 nm of the nanodrugs, from the experimental velocity and mass loss profiles. The flow velocity analysis also shows that the transport of nanodrugs is controlled by sedimentation processes in the larger size ranges of 110–302 nm. However, the combined overview from experimental mass loss and velocity trends indicates presence of both diffusive and sedimentation forces in the 110–302 nm size ranges. It is also discovered that the nanodrugs with higher positive surface charges are transported faster through the two test channels, which also leads to lower deposition of these nanodrugs on the walls of the flow channels. The results from this study will be valuable in realizing reliable and cost-effective in vitro experimental approaches that can support in vivo methods to predict the flow of new nanodrugs.
Effects of electron beam irradiation on CrMnV and CrMnTiV high entropy alloys: Nano-mechanical, structural, and thermodynamic perspectives
Beam exit windows are crucial components of any particle accelerator as they provide an interface between the beamline vacuum and target material at atmospheric media. For high beam power machines, special materials and designs are required to withstand high radiation and mechanical loads, while minimizing energy loss during transition and maximizing window lifetime. This research investigates the impact of electron beam exposure to bulk CrMnV and CrMnTiV high entropy alloys (HEAs) with the primary goal of identifying suitable candidate materials for the design of robust and durable exit window settings. The selection criteria include intrinsic characteristics, power dissipation, and mechanical responses. According to the thermodynamic calculations, both equiatomic CrMnV and the addition of 7% of Ti with equiatomic CrMnV yield solid-solutions phases. The structural and mechanical properties of CrMnV and CrMnTiV samples were tested using field emission scanning electron microscopy, atomic force microscopy, scanning electron microcopy with energy dispersive x-ray spectroscopy, x-ray diffraction, and nanoindentation before and after exposure to a dose of ~66 kGy from a 10 MeV e-beam accelerator. Despite exhibiting beam transmission characteristics comparable to Cr and V, the indentation hardness of HEAs exceeded that of the Cr and V samples by five to six times. The examination of the CrMnTiV irradiated samples revealed organized deformation patterns depicting new features, which we suspect twinning and twin boundaries due to the addition of Ti to CrMnV. Ti, a hexagonal-close-packed crystal structure, is commonly known for deformation twinning behavior.
Deep learning-based noise filtering toward millisecond order imaging by using scanning transmission electron microscopy
Application of scanning transmission electron microscopy (STEM) to in situ observation will be essential in the current and emerging data-driven materials science by taking STEM’s high affinity with various analytical options into account. As is well known, STEM’s image acquisition time needs to be further shortened to capture a targeted phenomenon in real-time as STEM’s current temporal resolution is far below the conventional TEM’s. However, rapid image acquisition in the millisecond per frame or faster generally causes image distortion, poor electron signals, and unidirectional blurring, which are obstacles for realizing video-rate STEM observation. Here we show an image correction framework integrating deep learning (DL)-based denoising and image distortion correction schemes optimized for STEM rapid image acquisition. By comparing a series of distortion corrected rapid scan images with corresponding regular scan speed images, the trained DL network is shown to remove not only the statistical noise but also the unidirectional blurring. This result demonstrates that rapid as well as high-quality image acquisition by STEM without hardware modification can be established by the DL. The DL-based noise filter could be applied to in-situ observation, such as dislocation activities under external stimuli, with high spatio-temporal resolution.
py4DSTEM: A Software Package for Four-Dimensional Scanning Transmission Electron Microscopy Data Analysis
Scanning transmission electron microscopy (STEM) allows for imaging, diffraction, and spectroscopy of materials on length scales ranging from microns to atoms. By using a high-speed, direct electron detector, it is now possible to record a full two-dimensional (2D) image of the diffracted electron beam at each probe position, typically a 2D grid of probe positions. These 4D-STEM datasets are rich in information, including signatures of the local structure, orientation, deformation, electromagnetic fields, and other sample-dependent properties. However, extracting this information requires complex analysis pipelines that include data wrangling, calibration, analysis, and visualization, all while maintaining robustness against imaging distortions and artifacts. In this paper, we present py4DSTEM, an analysis toolkit for measuring material properties from 4D-STEM datasets, written in the Python language and released with an open-source license. We describe the algorithmic steps for dataset calibration and various 4D-STEM property measurements in detail and present results from several experimental datasets. We also implement a simple and universal file format appropriate for electron microscopy data in py4DSTEM, which uses the open-source HDF5 standard. We hope this tool will benefit the research community and help improve the standards for data and computational methods in electron microscopy, and we invite the community to contribute to this ongoing project.
The ABCs of phase retrieval: Connecting the acronyms of scanning transmission electron microscopy
High-resolution scanning transmission electron microscopy (S/TEM) is an indispensable tool for characterizing the structure and properties of materials down to the atomic scale. Conventional S/TEM imaging, however, is limited by the phase problem, whereby the phase of the electron exit wave is lost upon detection. Recent advances in diffractive imaging and 4D-STEM have enabled a range of phase-retrieval techniques that computationally reconstruct the missing information encoded in the phase of the transmission function. These approaches offer improved dose efficiency and enhanced sensitivity to weakly scattering signals, extending quantitative imaging to beam-sensitive materials composed of light elements. In this work, we introduce the phase problem in electron microscopy and survey the diverse landscape of phase-retrieval techniques used in the field. Despite their many acronyms and algorithmic variations, these techniques share a common physical and mathematical foundation. We present a unified framework that connects these seemingly distinct methods, from parallax imaging and tilt-corrected bright-field (tcBF-STEM), to aberration-corrected bright-field (acBF-STEM), optimum bright-field (OBF-STEM) and single-sideband (SSB) ptychography, as well as first-moment integrated center of mass techniques (iCOM) and iterative ptychographic algorithms. Based on these insights, we discuss the opportunities and practical limitations of applying these methods across different materials systems, detector designs, and microscope configurations.Graphical abstractRepresentative electron microscopy configurations used for phase retrieval and diffractive imaging in S/TEM: (a) Zernike phase-contrast transmission electron microscopy (TEM), (b) small-convergence-angle four-dimensional scanning transmission electron microscopy (4D-STEM) for nanobeam-based phase reconstruction methods, and (c) large-convergence-angle 4D-STEM for ptychographic and related diffractive imaging techniques reviewed in this work.
High-Throughput Characterization of (Fe x Co 1–x ) 3 O 4 Thin-Film Composition Spreads
In this study, thin-film continuous composition spreads of Fe–Co–O were fabricated by reactive cosputtering from elemental Fe and Co targets in reactive Ar/O 2 atmosphere using deposition temperatures ranging from 300 to 700 °C. Fused silica and platinized Si/SiO 2 strips were used as substrates. Ti and Ta were investigated as adhesion layer for Pt and the fabrication of the Fe–Co–O films. The thin-film composition spreads were characterized by high-throughput electron-dispersive X-ray spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, atomic force microscopy, scanning electron microscopy, and optical transmission spectroscopy. The Fe-content ranged from 28 to 72 at. %. The spinel phases Fe 2 CoO 4 and FeCo 2 O 4 could be synthesized and stabilized at all deposition temperatures with a continuous variation in spinel composition in between. The dependence of the film surface microstructure on the deposition temperature and the composition was mapped. Moreover, the band gap values, ranging from 2.41 eV for FeCo 2 O 4 to 2.74 eV for Fe 2 CoO 4 , show a continuous variation with the composition.
Effect of Added Gadolinium Oxide on the Thermal Air Oxidation of Uranium Dioxide
To develop a more reliable and stable UO2-based nuclear fuel, the Pacific Northwest National Laboratory (PNNL) investigated modifying fuel with several soluble lanthanides and zirconium. This article provides the results of these studies investigating gadolinium doping at levels up to 10 mass%. The authors characterized and compared commercially- and PNNL-prepared gadolinium-doped UO2 to determine the oxygen-to-metal ratio, elemental distribution, chemical composition, physical appearance, lattice parameters, and grain structure using atomic force microscopy, scanning electron microscopy coupled with energy dispersive spectroscopy, and X-ray diffractometry. After confirming PNNL-prepared UO2 and (Gd,U)O2 were similar to commercially prepared UO2 and (Gd,U)O2, we measured the thermal behavior of these gadolinium-doped UO2 materials to air oxidation using differential scanning calorimetry and thermogravimetric analysis. Addition of gadolinium stabilized the first oxidation product U4¬O9/U3O7 and slowed the subsequent oxidation to U3O8. Comparison of our measured two-step oxidation of UO2 to U3O8 at 325°C to common gas/solid kinetic reaction models found that each oxidation step is best described as a convolution of kinetic behaviors; the gadolinium insertion into the UO2 lattice enforces a significant alteration in mechanism and oxidation rate. Noticeable changes in mechanism become apparent between 1% and 3% gadolinium content.
Assessing Manufacturability of the Oxide Dispersion Strengthened (ODS) 14YWT Alloy Fuel Cladding Tube Using SolidStir™ Technology
The 14YWT (Fe–14Cr–3W–0.4Ti–0.3Y2O3 (wt.%)) alloy is a potential candidatematerial for fabricating fuel cladding tubes and other structural components to be used in next-generation advanced nuclear reactors. Due to inherent limitations of current processing routes, this research explored a new variant of friction stir processing, commercially referred to as SolidStir™ Extrusion (patent pending) technology from Enabled Engineering to consolidate and extrude 14YWT powder into a fuel cladding tube. Several single-layer and multiple-layer consolidation experiments were carried out in an Inconel 625 die to determine the suitable processing parameters for SolidStir™ extrusion of the 14YWT alloy cladding tube. With these processing parameters, a 16–18 mm long tube of the 14YWT alloy with no visible defects was successfully extruded using this novel technology. Microstructural characterization results obtained using optical microscopy, scanning electron microscopy, energy dispersive spectroscopy, electron backscatter diffraction, and transmission electron microscopy will be presented.
Characterization and Rationalization of Microstructural Evolution in GRCop-84 Processed by Laser-Powder Bed Fusion (L-PBF)
In this study, prismatic geometries of GRCop-84 [Cu-8Cr-4Nb (at. pct)] were built with laser-powder bed fusion (L-PBF) process. The samples were sectioned parallel or perpendicular to the build direction and characterized in the as-built and after post-processing with a hot-isostatically pressing (HIP) treatment. The microstructure and phase evolutions were evaluated with optical microscopy, scanning electron microscopy (SEM), electron backscattered diffraction (EBSD), and high-temperature X-ray diffraction (HTXRD) up to 1223 K. The samples in the as-built conditions exhibited predominantly columnar epitaxial and misoriented Cu-FCC grains. The microstructure evolutions are discussed based on locations within the overall build geometry, the dynamics of small melt pool shape and sectioning effects. The above grain structure did not change significantly during post-process HIP treatment. The stability of this FCC grain structure is attributed to the formation of primary stable Cr 2 Nb (Laves phase) during L-PBF, even before the emergence of FCC grains from liquid. The stability of Cr 2 Nb in both as-built and HIPed samples were evaluated using high-temperature X-ray diffraction measurements and compared with that of gas-atomized powder. The significance of these results is discussed with reference to aerospace applications.
Additively manufactured novel Al-Cu-Sc-Zr alloy: Microstructure and mechanical properties
An in-depth understanding of microstructure and resultant properties is paramount in the design of a novel alloy system, especially for additive manufacturing (AM). The present investigation aims to characterize a prototypical AM Al alloy with great potential for structural applications. An Al-1.5Cu-0.8Sc-0.4Zr alloy designed using integrated computational material engineering was printed using the laser powder bed fusion AM process. This novel alloy shows promising combination of strength and ductility in as-built and peak-aged conditions. This improvement in the tensile properties is attributed to the presence of both coherent L1 2 Al 3 Sc/Al 3 (Sc,Zr) precipitates and Cu-rich regions. The microstructures were studied via extensive microscopy at different length scales using X-ray microscopy, scanning electron microscopy, and transmission electron microscopy. Fractography revealed that the columnar grain boundaries in as-built condition allow easy slip transfer as compared to the equiaxed grains, with the apex of the melt pool acting as the crack nucleation site. Furthermore, the peak aged condition resulted in improved strength while marginally sacrificing ductility due to precipitates decorating dislocations, grain boundaries and melt pool boundaries thus acting as obstacles to slip transfer.
On residual stress analysis and microstructural evolution for stainless steel type 304 spent nuclear fuel canisters weld joint: Numerical and experimental studies
Chloride-induced stress corrosion cracking (CISCC) in the weldments of austenitic stainless steel canisters is one of the primary safety concerns during the dry storage of used nuclear fuel at Independent Spent Fuel Storage Installations in coastal areas. In order to evaluate the CISCC behavior in the canister, a 3D sequentially coupled thermo-mechanical finite element model was built to simulate the residual stresses induced by two intersecting longitudinal and circumferential multi-pass welds in austenitic stainless steel mockup canister. Weld-induced residual stresses from simulation were in good agreement with the experimental measurement results by deep-hole drilling and contour methods. Through-wall high tensile axial and hoop stresses were observed in both the fusion zone and heat affected zone (HAZ) in the longitudinal and circumferential weld, respectively. On the other hand, the microstructure within the weldments of 304 stainless steel mockup was characterized using optical microscopy, scanning electron microscopy, electron back-scattered diffraction and energy dispersive X-ray spectroscopy methods. A few amount of MnS inclusions in both the base metal and HAZ, and a lot of (Mn,Si) x O y inclusions in the fusion zone were found. Meanwhile, there is some α'-martensite in the base metal, while the martensite was reversed in the HAZ. In the fusion zone, there is a lot of δ-ferrite. The martensite reversion phenomenon was also verified by the combination of Feritscope test and thermal simulation, which could predict a martensite reversion temperature as 400C°. The welding residual stresses and microstructure analysis results could offer the instructive information for the prediction of CISCC behavior of the spent nuclear fuel canisters.
Microstructural evolution of Mo-UO 2 cermets under high temperature hydrogen environments
Ceramic-metallic (cermet) materials show promise for use in nuclear thermal propulsion applications due to attractive thermophysical properties including high temperature stability and high thermal conductivity. In this work, molybdenum-uranium dioxide (Mo-UO 2 ) cermet fuel elements were fabricated by means of spark plasma sintering (SPS) and were subsequently exposed to hydrogen at high temperatures (2500 K). Mo-UO 2 samples pre- and post-exposure were characterized by means of optical microscopy, scanning electron microscopy, and X-ray diffraction (XRD). Microscopy analyses of the as-produced material displayed microscopic cracking on the interior of the spherical UO 2 fuel particles but confirmed that the fuel particles were fully encapsulated in the Mo matrix. The results further showed mass loss, macroscopic swelling, and cracking in the cermet samples which occurred during high temperature hydrogen testing. Nanoscale swelling was evidenced by XRD in the Mo matrix and UO 2 fuel structure due to the incorporation of defects and accompanied microstrain.
Phase stability and microstructure of neutron-irradiated substoichiometric yttrium dihydrides
The impact of the neutron-displacement damage on phase stability and microstructure of substoichiometric yttrium dihydrides (YH x , x <2) were investigated to assess their use as solid moderator in high-temperature nuclear reactors. YH x specimens were, thus, subjected to neutron irradiations in the range of 0.1–2 displacements per yttrium atom (dpa-Y) in the temperature range of 536–878°C at the Oak Ridge National Laboratory's (ORNL's) High Flux Isotope Reactor (HFIR). YH x specimens were initially prepared at stoichiometry (H/Y) ratios of 1.69 and 1.83. HFIR-irradiated specimens were characterized by variety of techniques to investigate H retention characteristics including dimensional analysis, optical microscopy, scanning electron microscopy electron back scatter diffraction (EBSD), transmission electron microscopy, thermal desorption spectroscopy (TDS), and high-energy x-ray diffraction (HE-XRD) characterizations. Overall, YH x exhibited notable structural and phase stability under short-term neutron-irradiation, except for the samples with significant silicon carbide (SiC) interaction at high doses and temperatures. Basic dimensional and mass measurements were misleading for accurate assessment of H retention, as confirmed by EBSD phase maps, XRD line profiles, and TDS signals. Thus, it was discussed that a robust H retention metric is needed to assess irradiated hydrides. Further, nanoscale cavities were observed as a result of the neutron irradiation in all samples. Although no clear impact of dose and irradiation temperature was determined, the initial H/Y ratio had an impact on the cavity number density where low H/Y specimens had high-resistance to cavity formation. The Y-vacancy cluster formation at the collision stage of the displacement cascade and their stabilization by H were considered to be the likely underlying mechanisms for the observed cavity microstructure.
Evaluation of corrosion coupons exposed to molten-chloride electrorefiner salts long term
Corrosion mitigation has long been considered a challenge in long-term service of both pyrochemical reprocessing and molten salt reactor applications. Corrosion coupons consisting of 2.25Cr 1Mo ASME SA387 Grade 22 Class 2 steel, were installed in a uranium electrorefiner containing molten chloride salt at 500°C. This electrorefiner went into service at Idaho National Laboratory in 1994. Seven of these coupons were removed in 2019 (i.e., submerged in molten salt for 25 years) for analysis and characterization including neutron imaging, optical microscopy, scanning electron microscopy, and wave/energy dispersive x-ray spectroscopy. The results showed that all seven coupons experienced between 30 to 175 µm of surface degradation without evidence of brittle fracture. Meaning there was no evidence of accelerated corrosion or fractures, and the average steel surface loss was of less than 5 µm per year. All indications were that the environmental conditions inside the electrorefiner were favorable for the steel alloy.
Laser glazing of cold sprayed coatings for the mitigation of stress corrosion cracking in light water reactor (LWR) applications
The effect of laser power, traverse speed, and cold spray coating thickness were examined with the goal of mitigating and repairing stress corrosion cracking (SCC) in light water reactor (LWR) environment. For this purpose, SCC-susceptible Alloy 600 substrate material was coated with SCC-resistant Alloy 690 via the cold spray technique. The cold spray coated substrate was then laser-glazed using various laser parameters. Single pass and multiple pass laser glazed regions were created to determine the effects. For this purpose, the area of the fusion zone, depth of the fusion zone, and elemental composition of the cross section were examined by optical microscopy, scanning electron microscopy, and energy dispersive spectroscopy. Additionally, it was shown that chromium dilution from the laser glazed region into the substrate is not a significant factor in laser glazed cold spray coated samples. Separate laser glazed samples were subjected to ASTM 633C to determine coating adhesion. Finally, by using interrupted SCC crack growth rate tests, it was shown that low traverse speeds and high laser powers produce deep fusion zones within the cold sprayed coating and substrate that can be used to seal pre-existing cracks, thus stopping SCC growth.