Advanced synchrotron characterization techniques for fusion materials science
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99 GENERAL AND MISCELLANEOUS↗
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Assessment of diagenesis in archaeological human second metacarpal bones using the intensity of the small angle X-ray scattering D -period peak
Bone consists mainly of carbonated apatite (cAp) nanoplatelets embedded in a matrix of collagen fibrils. Earlier, high-energy small angle X-ray scattering (SAXS) studies of archaeological adult human second metacarpal bones (mc2) found collagen D-period peaks with high-intensity I D in specimens in which microcomputed tomography (microCT) showed little diagenesis and I D ~ 0 for specimens where microCT revealed severe diagenesis (Park et al. 2022 Int. J. Osteoarchaeol. 32, 170–181 (doi:10.1002/oa.3053); Stock et al. 2022 Int. J. Osteoarchaeol. 32, 120–131 (doi:10.1002/oa.3049)). Here, the present paper uses SAXS at beamline 1-ID, Advanced Photon Source, Argonne National Laboratory and other techniques to study a set of 10 mc2 from an early Medieval cemetery at Greding, Germany. We hypothesized that non-invasive measurement of I D would provide an accurate and rapid (approx. 6 min/specimen) assessment of diagenesis in archaeological mc2. Results of Raman spectroscopy, laboratory microCT and backscattered electron, reflected light and polarized transmitted light microscopies confirmed the SAXS determinations, but lattice parameter values from X-ray diffraction were uncorrelated with I D value. Age-at-death estimates placed the 10 mc2 in three age categories (young adult, middle adult, old adult): lattice parameters from X-ray diffraction were uncorrelated with age at death. Cross-sectional bone area fraction from microCT dropped noticeably for the older age cohort.
Raman spectroscopy↗
Measurement of G-phase volume fraction and number density in duplex stainless steels using transmission electron microscopy
Duplex stainless steels (DSS) have a high toughness and strength due the presence of both austenitic and ferritic phases. These alloys have had limited use in power production applications due to thermal embrittlement caused by spinodal decomposition and development of G-phase precipitates in the ferrite. Lean grade DSS alloys (e.g., 2101, 2003) may offer improved thermal stability due to the reduction of Cr- and Ni-equivalent elements when compared to standard grade compositions (e.g., 2205, 2209). The abundance of the G-phase was measured in five duplex stainless steels, three wrought alloys (2101, 2003, 2205) and their matching filler metals (2101-w, 2209-w), after aging at 427 °C for 1000 h and 10,000 h. The G-phase volume fraction, number density, size, and precipitate spacing were found using quantitative analysis of transmission electron microscopy dark field images and the composition of G-phase precipitates on other clusters were characterized with atom probe tomography (APT). In the welded alloys, the G-phase was found to develop rapidly, relative to the wrought material. A positive correlation was found between the nickel equivalent composition of the alloy and the G-phase volume fraction. The alloys 2205, 2209, and 2101-w, which are higher in Cr and Ni, all showed significant G-phase precipitation, further strengthening the hypothesis that lean grade DSS alloys are more thermally stable against precipitation in the ferrite. Electron diffraction showed a secondary phase present in the 2101 wrought alloy at 10,000 h, but it was not crystallographically consistent with the G-phase; APT showed the presence of nanoclusters rich in both nickel and copper for this alloy. In conclusion, no secondary phases or clusters were found in 2003 after 10,000 h of aging, so it may be a candidate alloy for applications that require long-life times at high operating temperatures.
36 MATERIALS SCIENCE↗
Resolution-enhanced X-ray fluorescence microscopy via deep residual networks
Abstract Multimodal hard X-ray scanning probe microscopy has been extensively used to study functional materials providing multiple contrast mechanisms. For instance, combining ptychography with X-ray fluorescence (XRF) microscopy reveals structural and chemical properties simultaneously. While ptychography can achieve diffraction-limited spatial resolution, the resolution of XRF is limited by the X-ray probe size. Here, we develop a machine learning (ML) model to overcome this problem by decoupling the impact of the X-ray probe from the XRF signal. The enhanced spatial resolution was observed for both simulated and experimental XRF data, showing superior performance over the state-of-the-art scanning XRF method with different nano-sized X-ray probes. Enhanced spatial resolutions were also observed for the accompanying XRF tomography reconstructions. Using this probe profile deconvolution with the proposed ML solution to enhance the spatial resolution of XRF microscopy will be broadly applicable across both functional materials and biological imaging with XRF and other related application areas.
36 MATERIALS SCIENCE↗
Phosphate Textural Diversity in CI Chondrites and C-Type Asteroids
Introduction: Apatite, Ca 5 (PO 4 ) 3 (CL/F/OH-), is a ubiquitous phosphate found throughout the solar system, including the most primitive solids, CI-chondrites [1,2] and related samples of carbonaceous asteroids Ryugu [3] and Bennu [4], returned by JAXA’s Hayabusa2 and NASA’s OSIRIS-REx missions, respectively. Apatite in these primitive solids is found as individual grains or mineral clusters and has been inferred to form from the hydrothermal sequence during cooling of their respective parent body or bodies. To better understand the formation history and reworking of these early phosphates we have undertaken a highly coordinated study of phosphate microstructures, geochemistry and U/Pb geochronology from a suite of CI meteorites and carbonaceous asteroid samples. These data have identified novel phosphate microstructures and complex relationships across a suite of apatite grains from the early solar system, indicating multiple episodes of growth and modification on the CI parent body(ies). Methods: Samples of CI chondrites, Alais, Ivuna, Orgueil, Oued Chebeika 002, Yamato (Y) 82162, Y980115, Y980134, and two chips of Hayabusa2 Ryugu particles (A0262 and C0263) have been acquired for analysis. The bulk texture of the samples were first scanned by X-ray Computed Tomography (XCT) using the Nikon XT H 320 within the XFACT facility at NASA JSC or the Xradia 620 Versa at the UTCT facility. Based on the identification of petrofabrics or features of interest from the XCT data, samples were chipped, oriented, potted in epoxy and thick sections were prepared. After anhydrously polishing the samples with silicon carbide and dry diamond powder down to 1 µm, the samples were ion polished using a Hitachi ArBlade. Energy dispersive Xray spectrometry (EDS) maps were collected to ID phosphates of interest using a JEOL 7900F SEM. The internal microstructures of identified phosphates were then mapped by electron backscatter diffraction (EBSD) using the JEOL 7900F. Based on the EDS and EBSD data, domains of interest were targeted for quantitative chemical analyses using a JEOL 8530 EPMA. Subsequently, in situ U-Pb and 207 Pb/ 206 Pb ages will be collected using a Cameca ims1290 secondary ion mass spectrometer at UCLA across a range of microstructures. Results: Apatite grains are ubiquitous throughout the CI chondrites and carbonaceous asteroid materials, found as individual grains, disseminated clusters or grain aggregates. Apatite grains are associated with serpentine, magnet-ite, and/or carbonate. Of particular interest, we have identified individual and aggregate polycrystalline grains ex-hibiting an internal ‘honeycomb’ texture (Fig. 1). Some of these grains appear overprinted by subsequent alteration while others remain unaltered. Apatite halogen sites are dominated by the missing component, assumed to be OH, and F, comparable to published values from Bennu, Ryugu and CM-chondrites [3-5]. However, the Yamato CI-like meteorites show a broader range of Cl values, and one grain from Alais is dominated by CL. Summary: Apatite growth features indicate a protracted and complex growth history, consistent with precipitation from an evolving fluid system. The ‘honeycomb’ texture identified in some CI meteorites is, to the best of our knowledge, the first report of such a microstructure in meteoritic phosphate. The microtextures and zoning will guide subsequent age analyses, to better constrain the formation and reworking of phosphate in CI(-like) materials. Acknowledgments: We thank the National Institute of Polar Research, Japan for samples of Y82162, 980115 and 980134 meteorites, ASU’s Buseck Center for Meteorite Studies for samples of Ivuna and Alais meteorites, and JAXA curation for chips of Ryugu material. This work was funded by NASA ROSES LARS grant 24-LARS24-0014. References: [1] Morlok et al., 2016, GCA 70:5371-5394. [2] Alfin g et al., 2019, Geochemistry 79:125532. [3] Nakamura et al. (2022) Science 379:1-15. [4] Seifert et al. (2026) MAPS 61:504-521. [5] Piralla et al. (2021) MAPS 56:809-828.
CI chondrites↗
Strain Measurements of Chondrules and Refraction Inclusion in Allende
This study uses traditional strain measurement techniques, combined with X-ray computerized tomography (CT), to evaluate petrographic evidence in the Allende CV3 chondrite for preferred orientation and to measure strain in three dimensions. The existence of petrofabrics and lineations was first observed in carbonaceous meteorites in the 1960's. Yet, fifty years later only a few studies have reported that meteorites record such features. Impacts are often cited as the mechanism for this feature, although plastic deformation from overburden and nebular imbrication have also been proposed. Previous work conducted on the Leoville CV3 and the Parnallee LL3 chondrites, exhibited a minimum uniaxial shortening of 33% and 21%, respectively. Petrofabrics in Allende CV3 have been looked at before; previous workers using Electron Back Scatter Diffraction (EBSD) found a major-axis alignment of olivine inside dark inclusions and an "augen"-like preferred orientation of olivine grains around more competent chondrules
Tait, Alastair W.↗
On the Elevated Temperature Thermal Stability of Nanoscale Mn-Ni-Si Precipitates Formed at Lower Temperature in Highly Irradiated Reactor Pressure Vessel Steels
Atom probe tomography (APT) and scanning transmission electron microscopy (STEM) techniques were used to probe the long-time thermal stability of nm-scale Mn-Ni-Si precipitates (MNSPs) formed in intermediate and high Ni reactor pressure vessel steels under high fluence neutron irradiation at ≈320 °C. Post irradiation annealing (PIA) at 425 °C for up to 57 weeks was used to determine if the MNSPs are: (a) non-equilibrium solute clusters formed and sustained by radiation induced segregation (RIS); or, (b) equilibrium G or Γ 2 phases, that precipitate at accelerated rates due to radiation enhanced diffusion (RED). Note the latter is consistent with both thermodynamic models and x-ray diffraction (XRD) measurements. Both the experimental and an independently calibrated cluster dynamics (CD) model results show that the stability of the MNSPs is very sensitive to the alloy Ni and, to a lesser extent, Mn content. Thus, a small fraction of the largest MNSPs in the high Ni steel persist, and begin to coarsen at long times. These results suggest that the MNSPs remain a stable phase, even at 105 °C higher than they formed at, thus are most certainly equilibrium phases at much lower service relevant temperatures of ≈290 °C.
36 MATERIALS SCIENCE↗
Three-dimensional atomic mapping of hydrogenated polymorphous silicon solar cells
Hydrogenated polymorphous silicon (pm-Si:H) is a nanostructured material consisting of silicon nanocrystals embedded in an amorphous silicon matrix. Its use as the intrinsic layer in thin film p-i-n solar cells has led to good cell properties in terms of stability and efficiency. Here, we have been able to assess directly the concentration and distribution of nanocrystals and impurities (dopants) in p-i-n solar cells, by using femtosecond laser-assisted atom probe tomography (APT). An effective sample preparation method for APT characterization is developed. Based on the difference in atomic density between hydrogenated amorphous and crystalline silicon, we are able to distinguish the nanocrystals from the amorphous matrix by using APT. Moreover, thanks to the three-dimensional reconstruction, we demonstrate that Si nanocrystals are homogeneously distributed in the entire intrinsic layer of the solar cell. The influence of the process pressure on the incorporation of nanocrystals and their distribution is also investigated. Thanks to APT we could determine crystalline fractions as low as 4.2% in the pm-Si:H films, which is very difficult to determine by standard techniques, such as X-ray diffraction, Raman spectroscopy, and spectroscopic ellipsometry. Moreover, we also demonstrate a sharp p/i interface in our solar cells.
71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
Metalorganic chemical vapor deposition of ZnGeN 2 films on GaN: effects of cation stoichiometry on surface morphology and crystallinity
Novel optoelectronic device designs based on the heterostructures of III-N and II-IV-N 2 are promising to advance device performance significantly. For example, by utilizing InGaN-ZnGeN 2 quantum well (QW) structures instead of pure InGaN, the band structure engineering in the QW active region can lead to improved electron-hole wavefunction overlap, and thus enhance the radiative efficiency for photon generation. These novel heterostructures have great potential to address the current challenge of low quantum efficiency in InGaN QW based light emitting diodes emitting in green and beyond. The materials development of ZnGeN 2 is still at an early stage as compared to the much matured GaN material system. In an ideal octet rule preserving ordered structure of ZnGeN 2 , every N atom is coordinated by exactly two Zn and two Ge atoms. However, local violation of octet rule can be caused by non-ideal coordination of N by the cations. The disordered structure is thermodynamically less favorable but can still be achieved, for example, in kinetics-limited growth regime. The ordered ZnGeN 2 has a bandgap very close to that of GaN (~3.4 eV) and a lattice mismatch of <0.1% with GaN. Interestingly, the valence band of ZnGeN 2 has been predicted to be ~1 eV above that of GaN, which has inspired novel designs for high efficiency light emitters. In this work, we investigated the metalorganic chemical vapor deposition (MOCVD) of ZnGeN 2 films on GaN/c-sapphire templates. Diethylzinc (DEZn), germane (GeH4) and ammonia were used as the precursors for Zn, Ge and N, respectively. A systematic study was conducted to investigate the cation stoichiometry as a function of growth temperature (TG), total reactor pressure (P) and DEZn/GeH 4 molar flow rate ratio (RII/IV). Under the investigated growth window, the Zn/(Zn+Ge) composition in the films, determined from energy dispersive X-ray spectroscopy, decreased monotonically with increase in TG but increased with increase in P and RII/IV. Atom probe tomography data did not indicate the presence of any secondary phases such as Zn 3 N 2 or Ge 3 N 4 . The surface morphology and crystallinity of the grown films had strong correlation with the Zn/(Zn+Ge) composition. The scanning electron microscopy images showed that the near-stoichiometric films have planar surfaces whereas Zn-rich films had crystallites on their surface and the Zn-poor films had faceted surface. Scanning transmission electron microscopy (STEM) imaging revealed that the Zn-rich and Zn-poor films have columnar and filament-like morphology, respectively, whereas the near-stoichiometric films have continuous film-like cross-sectional morphology. TEM nano-diffraction patterns as well as X-ray diffraction 2θ-ω scan profiles indicate that the near stoichiometric films are single crystalline. Nano-diffraction pattern of the stoichiometric films resembled that of a disordered ZnGeN 2 structure. Room temperature Raman spectra of near-stoichiometric films showed only the phonon density of states like features of a cation disordered ZnGeN 2 . Cathodoluminescence and photoluminescence spectra measured at different temperatures had similar features with peak emission wavelength at ~ 2 eV. In conclusion, the stoichiometry of ZnGeN 2 films can be widely tuned by tuning the MOCVD growth parameters. The surface morphology and the crystallinity of the films were found to have strong correlation with the Zn/(Zn+Ge) composition. The stoichiometric ZnGeN 2 films grown on GaN were demonstrated with uniform surface morphology and high crystalline quality. The results from this work will provide pathway to implement ZnGeN 2 in device structures.
Karim, Md Rezaul↗
A New Coordinated NanoSIMS, Transmission Electron Microscopy and Atom Probe Tomography Approach For the Characterization of Primitive Astromaterials
Presolar grains are remnants of evolved stellar systems preserved within primitive extraterrestrial materials. They are important for studying physical and chemical processing, and formation mechanisms occurring within the interstellar medium, Solar Nebula and their parent stellar environments [1]. Our recent work has shown coordinated nano-scale Secondary Ion Mass Spectrometry (NanoSIMS) and Atom Probe Tomography (APT) can show isotopic and chemical signatures at major to trace levels, morphological signatures, and regional contextual relationships [2,3]. Previous studies have shown Transmission Electron Microscopy (TEM) of Focus Ion Beam (FIB) TEM lamella, can provide localized contextual relationships, crystallographic information and chemical information [1]. Coordinating NanoSIMS, TEM, and APT could gain access to almost all contextual, structural and geochemical signatures within each presolar grain. However, this has proved challenging owing to the preparation requirements for TEM and APT. For example, studying specimen prepared as APT needles in TEM removes the local context, the higher degree of surface exposure can alter the chemistry of beam sensitive materials, and the shank angle of the needle can impact the quality of TEM diffraction images. We designed a new FIB method which takes a 100 nm thick FIB-TEM lamella and sandwiches it between two indium slices (5 μm x ~300 nm x 3 μm). The indium is melted onto the lamella surface using the electron beam (Fig 1). This process adds bulk to the lamella, making it more amenable to APT needle formation (Fig 2). Consequently, samples can be prepared per the optimal requirements for each technique improving data quality, acquisition stability, and access to the signatures and relationships summarised earlier. This technique can be used for measuring multiple phases across a TEM lamella and targeting an individual phase. For example, a presolar grain identified in NanoSIMS could be targeted, studied in TEM and then indium sandwiched with its precise location in the TEM lamella marked using a Pt button for preparation of an APT needle and atomic scale acquisition. [1] A. M. Davis (2014) Meteorites and cosmochemical processes, 1. [2] Nevill N. et al. (2023) LPSC, 54, #1707. [3] Nevill N. et al. (2023) LPSC, 54, #1714.
NanoSIMS↗
Thermal equation of state for zoisite: Implications for the transportation of water into the upper mantle and the high-velocity anomaly in the Farallon plate
Seismic tomography studies have revealed a high-velocity anomaly at depths between 100 km and 300 km in the Farallon plate. However, the reasons for the high-velocity anomaly continue to be debated. An analysis of the mineral proportions of eclogites exhumed from the Farallon plate shows that the average amount of zoisite in eclogite is ∼16.0 vol%. Therefore, the presence of zoisite eclogite needs to be considered to explain the high-velocity anomaly of the Farallon plate. However, the thermal equation of state and stability of zoisite have not been fully investigated under high pressure−temperature (P-T) conditions. We investigated the high-pressure and high-temperature behavior of natural zoisite utilizing synchrotron single crystal-X-ray diffraction (XRD). The results indicate that zoisite is metastable up to 24.8 GPa and 700 K. We obtained the ambient unit-cell volume V0 = 901.26(3) Å3 by synchrotron single crystal-XRD measurement. We also fitted the pressure-volume-temperature data to a high-temperature Birch-Murnaghan equation of state and obtained the zero-pressure bulk modulus K0 = 134.7(8) GPa, the temperature derivative of the bulk modulus (∂K/∂T)P = −0.011(4) GPa/K, and the thermal expansion coefficients α0V = 1.9(7) × 10−5 K−1 and α1V = 3(2) × 10−8 K−2 when the pressure derivative of bulk modulus (K′0) is fixed at 4. By incorporating the results from previous studies, we calculated the density and bulk sound velocity profiles of zoisite eclogite along the Farallon plate geotherm. Finally, we infer that zoisite could carry water to depths of ∼300 km within cold subducting slabs and that the bulk sound velocity of typical zoisite eclogite with ∼61.0 vol% omphacite, ∼23.0 vol% garnet, and ∼16.0 vol% zoisite could cause the high-velocity anomalies at depths of 100−300 km in the Farallon plate.
Geology↗
Nondestructive ultrasonic characterization of a triple-weld-bead wire arc additively manufactured ER70S-6 S-curved wall
Understanding build-scale microstructural variation in wire arc additive manufacturing (WAAM) of low-carbon steels is essential for ensuring consistent structure–property relationships throughout large components. Conventional destructive characterization techniques, such as scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD), are time-intensive and limited to localized regions, making comprehensive evaluation of large WAAM structures challenging. In this study, a nondestructive ultrasonic approach was employed to characterize a 252 mm tall ER70S-6 S-curved WAAM wall produced using a triple-bead deposition strategy. Optical and SEM analysis revealed a repeating dual-region microstructure consisting of uniform polygonal ferrite at melt pool centers and heterogeneous ferrite with coarse and fine grains near melt pool boundaries, attributed to cyclic thermal conditions. Longitudinal ultrasonic backscatter imaging was used to evaluate the continuity of this periodicity along the full build height. The ultrasonic response exhibited a consistent repeating pattern that correlated with the observed layer-wise microstructural variation. X-ray computed tomography confirmed the absence of detectable porosity, indicating that ultrasonic contrast is primarily governed by grain morphology. Overall, the results indicate that longitudinal backscatter ultrasound is a promising nondestructive characterization technique for validating microstructural variations along the s-curved WAAM wall, with significant potential for microstructure optimization and process control.
36 MATERIALS SCIENCE↗
NASA Tech Briefs, July 2013
Dielectrophoresis-Based Particle Sensor Using Nanoelectrode Arrays; Multi-Dimensional Damage Detection for Surfaces and Structures; ULTRA: Underwater Localization for Transit and Reconnaissance Autonomy; Autonomous Cryogenic Leak Detector for Improving Launch Site Operations; Submillimeter Planetary Atmospheric Chemistry Exploration Sounder; Method for Reduction of Silver Biocide Plating on Metal Surfaces; Silicon Micromachined Microlens Array for THz Antennas; Forward-Looking IED Detector Ground Penetrating Radar; Fully Printed, Flexible, Phased Array Antenna for Lunar Surface Communication, Battery Charge Equalizer with Transformer Array; An Efficient, Highly Flexible Multi-Channel Digital Downconverter Architecture; Dimmable Electronic Ballast for a Gas Discharge Lamp; Conductive Carbon Nanotube Inks for Use with Desktop Inkjet Printing Technology; Enhanced Schapery Theory Software Development for Modeling Failure of Fiber-Reinforced Laminates; High-Performance, Low-Temperature-Operating, Long-Lifetime Aerospace Lubricants; Carbon Nanotube Microarrays Grown on Nanoflake Substrates; Differential Muon Tomography to Continuously Monitor Changes in the Composition of Subsurface Fluids; Microgravity Drill and Anchor System; 20 Granular Media-Based Tunable Passive Vibration Suppressor; 21 Miga Aero Actuator and 2D Machined Mechanical Binary Latch; Micro-XRF for In Situ Geological Exploration of Other Planets; Hydrogen-Enhanced Lunar Oxygen Extraction and Storage Using Only Solar Power; Uplift of Ionospheric Oxygen Ions During Extreme Magnetic Storms; Miniaturized, High-Speed, Modulated X-Ray Source; Hollow-Fiber Spacesuit Water Membrane Evaporator 25 High-Power Single-Mode 2.65-micrometers InGaAsSb/AlInGaAsSb Diode Lasers; Optical Device for Converting a Laser Beam Into Two Co-aligned but Oppositely Directed Beams; A Hybrid Fiber/Solid-State Regenerative Amplifier with Tunable Pulse Widths for Satellite Laser Ranging; X-Ray Diffractive Optics; SynGenics Optimization System (SynOptSys); 29 CFD Script for Rapid TPS Damage Assessment; radEq Add-On Module for CFD Solver Loci-CHEM; Science Opportunity Analyzer (SOA) Version 8; 30 Autonomous Byte Stream Randomizer; Distributed Engine Control Empirical/Analytical Verification Tools; Dynamic Server-Based KML Code Generator Method for Level-of-Detail Traversal of Geospatial Data; Automated Planning of Science Products Based on Nadir Overflights and Alerts for Onboard and Ground Processing; Linked Autonomous Interplanetary Satellite Orbit Navigation; Risk-Constrained Dynamic Programming for Optimal Mars Entry, Descent, and Landing; Scheduling Operations for Massive Heterogeneous Clusters; Deepak Condenser Model (DeCoM); Flight Software Math Library; Recirculating 1-K-Pot for Pulse-Tube Cryostats; 35 Method for Processing Lunar Regolith Using Microwaves; Wells for In Situ Extraction of Volatiles from Regolith (WIEVR); and Estimating the Backup Reaction Wheel Orientation Using Reaction Wheel Spin Rates Flight Telemetry from a Spacecraft.
Source record↗
Argon Milling of Bulk and Post-FIB Specimens for Multi-Length Scale Analyses by EBSD, TEM, and APT under Controlled Environments
Correlative investigations involve structural characterization by transmission electron microscopy (TEM) combined with compositional analysis by atom probe tomography (APT) using the same specimen. A critical component of successful correlative analyses is specimen preparation; probing individual atoms requires a surface and subsurface with minimal defects, beginning with the bulk material through to the prepared specimen for TEM or APT analysis. Our previous work showed that low-energy concentrated ion beam Ar ion milling improves TEM [1] and APT [2,3] specimen quality by removing surface oxides and Ga damage caused by focused ion beam (FIB) preparation. Further enhancement in specimen quality of APT specimens is achieved in the established workflow under controlled environments, as shown in [4]. In this work, we present specimen preparation using Ar ion milling techniques not only for the APT specimen, but also the bulk sample for subsequent multi-length scale analyses by electron backscatter diffraction (EBSD), TEM, and APT under controlled environments. The removal of surface damage and oxidation, which is crucial for probing atomic layer specimens by broad and concentrated Ar ion beam milling techniques under controlled environments, is highlighted.
36 MATERIALS SCIENCE↗
Morphology and composition of Goldeye (Hiodontidae; Hiodon alosoides) otoliths
In this work, we provide up-todate morphological and compositional data on otoliths of the osteoglossomorph Goldeye (Hiodon alosoides). Using computed tomography (CT) X-ray, we documented the location of each of the three pairs of otoliths (lapilli, sagittae, and asterisci) in relation to the swim bladder, which extended forward in close proximity to the sagittae and asterisci. The lappili were the largest otoliths in terms of surface area and volume, but the sagittae were highly modified, appearing spiral in shape when viewed dorsally, with a surface area to volume ratio more than double that of the lapilli. Using scanning electron microscopy, the surface of each otolith was viewable in great detail, and small otoconia (~10.5 μm diameter) were observed on each, but were most numerous on the sagittae. Additionally, on scanning electron micrographs, the sagittae appeared to be bi-lobed, with asymmetrical lobes each oriented in the same general direction. Using neutron and X-ray diffraction methods, we found three polymorphs of calcium carbonate crystals (aragonite, vaterite, and calcite), sometimes all within the same otolith. However, in general, lapilli and sagittae were composed predominately of aragonite whereas asterisci were composed chiefly of vaterite. With these results, we provide information on a unique species, whose inclusion in future studies would benefit our understanding of fish hearing, fish evolution, and fisheries ecology.
59 BASIC BIOLOGICAL SCIENCES↗
Three-dimensional structure of buried heterointerfaces revealed by multislice ptychography
Here, we report on the three-dimensional (3D) structure determination of a twisted hexagonal boron nitride (h-BN) heterointerface from a single-view dataset using multislice ptychography. We identify the buried heterointerface between two twisted h-BN flakes with a lateral resolution of 0.57 Å and a depth resolution of 2.5 nm. The latter represents a significant improvement (∼2.7 times) over the aperture-limited depth resolution of incoherent imaging modes, such as annular-dark-field scanning transmission electron microscopy. This improvement is attributed to the diffraction signal extending beyond the aperture edge, with the depth resolution set by the curvature of the Ewald sphere. Future advancements in this approach could enhance the depth resolution to the subnanometer level and enable the identification of individual dopants, defects, and color centers in twisted heterointerfaces and other materials.
71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
NASA Tech Briefs, May 2009
Topics covered include: Valve-"Health"-Monitoring System; Microstrip Antenna for Remote Sensing of Soil Moisture and Sea Surface Salinity; Biomedical Wireless Ambulatory Crew Monitor; Wireless Avionics Packet to Support Fault Tolerance for Flight Applications; Aerobot Autonomy Architecture; Submillimeter Confocal Imaging Active Module; Traveling-Wave Maser for 32 GHz; System Synchronizes Recordings from Separated Video Cameras; Piecewise-Planar Parabolic Reflectarray Antenna; Reducing Interference in ATC Voice Communication; EOS MLS Level 1B Data Processing, Version 2.2; Auto-Generated Semantic Processing Services; Geospatial Authentication; Maneuver Automation Software; Event Driven Messaging with Role-Based Subscriptions; Estimating Relative Positions of Outer-Space Structures; Fabricating PFPE Membranes for Capillary Electrophoresis; Linear Actuator Has Long Stroke and High Resolution; Installing a Test Tap on a Metal Battery Case; Fabricating PFPE Membranes for Microfluidic Valves and Pumps; Room-Temperature-Cured Copolymers for Lithium Battery Gel Electrolytes; Catalysts for Efficient Production of Carbon Nanotubes; Amorphous Silk Fibroin Membranes for Separation of CO2; "Zero-Mass" Noninvasive Pressure Transducers; Radial-Electric-Field Piezoelectric Diaphragm Pumps; Ejector-Enhanced, Pulsed, Pressure-Gain Combustor; Suppressing Ghost Diffraction in E-Beam-Written Gratings; Target-Tracking Camera for a Metrology System; Polarimetric Imaging using Two Photoelastic Modulators; Miniature Wide-Angle Lens for Small-Pixel Electronic Camera; Modal Filters for Infrared Interferometry; Mo(3)Sb(7-x)Te(x) for Thermoelectric Power Generation; Two-Dimensional Quantum Model of a Nanotransistor; Scanning Miniature Microscopes without Lenses; Manipulating Neutral Atoms in Chip-Based Magnetic Traps; Expansion Compression Contacts for Thermoelectric Legs; Processing Electromyographic Signals to Recognize Words; Physical Principle for Generation of Randomness; DSN Beowulf Cluster-Based VLBI Correlator; Hybrid NN/SVM Computational System for Optimizing Designs; Criteria for Modeling in LES of Multicomponent Fuel Flow; Computerized Machine for Cutting Space Shuttle Thermal Tiles; Orbiting Depot and Reusable Lander for Lunar Transportation; FPGA-Based Networked Phasemeter for a Heterodyne Interferometer; Aquarius Digital Processing Unit; Three-Dimensional Optical Coherence Tomography; Benchtop Antigen Detection Technique using Nanofiltration and Fluorescent Dyes; Isolation of Precursor Cells from Waste Solid Fat Tissue; Identification of Bacteria and Determination of Biological Indicators; Further Development of Scaffolds for Regeneration of Nerves; Chemically Assisted Photocatalytic Oxidation System; Use of Atomic Oxygen for Increased Water Contact Angles of Various Polymers for Biomedical Applications; Crashworthy Seats Would Afford Superior Protection; Open-Access, Low-Magnetic-Field MRI System for Lung Research; Microfluidic Mixing Technology for a Universal Health Sensor; Microfluidic Extraction of Biomarkers using Water as Solvent; Microwell Arrays for Studying Many Individual Cells; Droplet-Based Production of Liposomes; and Identifying and Inactivating Bacterial Spores
Source record↗
Fatigue performance of laser powder bed fusion hydride-dehydride Ti-6Al-4V powder
We report hydride-dehydride (HDH) Ti-6Al-4V alloy with particle size distribution of 50–120 µm is laser powder bed fusion (L-PBF) processed using optimum processing parameters and a near-fully dense structure with a density of 99.9 % is achieved. Microstructural observations and phase analyses indicate formation of columnar β grains with acicular α/α' phases in as-built condition. The roughness of the as-fabricated samples is significant with an average roughness of R a = 15.71 ± 3.96 µm and a root mean square roughness of R rms = 108.4 ± 24.9 µm, however, both values are reduced to R a = 0.19 ± 0.04 µm and R rms = 4.9 ± 0.6 µm after mechanical grinding. Mechanical tests are carried out on as-fabricated specimens followed by stress relief treatment. All samples are tested to failure in fatigue, under fully-reversed tension-compression conditions of R = –1. The as-built samples failed from the surface with crack initiation mainly at micro-notches, whereas after mechanically grinding, crack initiation changed to subsurface defects such as pores. Minimizing surface roughness by mechanically grinding eliminates surface micro-notches which improves fatigue strength in the high cycle fatigue region. Fatigue notch factor calculations showed that the effect of surface roughness was significantly lower when HDH powder is used compared to standard spherical powder. X-ray diffraction analysis revealed an in-plane compressive stress, micro-strain and grain refinement on the surface of the mechanically ground samples. Fractography observations (macroscale) revealed a fully brittle fracture in the first stage of crack growth with a transition to a dominantly ductile fracture in the third stage of crack growth. On the other hand, at the micro scale, even the brittle fracture regions showed evidence of ductile fracture within the α' martensite laths.
36 MATERIALS SCIENCE↗