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At least 649 records · Page 36

Role of scan strategies and heat treatment on grain structure evolution in Fe-Si soft magnetic alloys made by laser-powder bed fusion

A major goal in printing soft magnetic Fe-Si steels using additive manufacturing is to take advantage of the potential for complex geometric designs and site-specific grain control. One major step in the processing of these alloys is understanding how processing parameters might impact how the as-built microstructure responds to annealing (i.e. the annealing response). The impact of scan strategy on the annealing response for thin wall geometries is specifically explored. Two scan strategies were explored for a thin wall geometry that produced a strongly columnar grain structure and equiaxed grain structure. Additionally, samples from both scan strategies annealed at 1200 °C showed a marked difference in annealing response with the more equiaxed sample seeing full recrystallization and grain growth, while the more columnar grain structure saw little change in microstructure. After analysis through characterization techniques and thermal-mechanical simulations Differences in internal energy within the grains were ruled out because calculated GND density values were similar for both samples. The formation of secondary particles was ruled out as a contributing factor due to the type of oxide formations and their size. It was concluded that the contributing factor to the difference in the annealing response were a difference in the resulting grain size and the density of high angle grain boundaries. These two differences were largely attributed to differences in the thermal gradient conditions due to grains preferentially growing in the direction of the steepest thermal gradient.

36 MATERIALS SCIENCE↗

Lidar Sensor Performance in Closed-Loop Flight Testing of the Morpheus Rocket-Propelled Lander to a Lunar-Like Hazard Field

For the first time, a suite of three lidar sensors have been used in flight to scan a lunar-like hazard field, identify a safe landing site, and, in concert with an experimental Guidance, Navigation, and Control (GN&C) system, help to guide the Morpheus autonomous, rocket-propelled, free-flying lander to that safe site on the hazard field. The lidar sensors and GN&C system are part of the Autonomous Precision Landing and Hazard Detection and Avoidance Technology (ALHAT) project which has been seeking to develop a system capable of enabling safe, precise crewed or robotic landings in challenging terrain on planetary bodies under any ambient lighting conditions. The 3-D imaging Flash Lidar is a second generation, compact, real-time, aircooled instrument developed from a number of components from industry and NASA and is used as part of the ALHAT Hazard Detection System (HDS) to scan the hazard field and build a 3-D Digital Elevation Map (DEM) in near-real time for identifying safe sites. The Flash Lidar is capable of identifying a 30 cm hazard from a slant range of 1 km with its 8 cm range precision (1-s). The Flash Lidar is also used in Hazard Relative Navigation (HRN) to provide position updates down to a 250m slant range to the ALHAT navigation filter as it guides Morpheus to the safe site. The Navigation Doppler Lidar (NDL) system has been developed within NASA to provide velocity measurements with an accuracy of 0.2 cm/sec and range measurements with an accuracy of 17 cm both from a maximum range of 2,200 m to a minimum range of several meters above the ground. The NDLâ€"TM"s measurements are fed into the ALHAT navigation filter to provide lander guidance to the safe site. The Laser Altimeter (LA), also developed within NASA, provides range measurements with an accuracy of 5 cm from a maximum operational range of 30 km down to 1 m and, being a separate sensor from the Flash Lidar, can provide range along a separate vector. The LA measurements are also fed into the ALHAT navigation filter to provide lander guidance to the safe site. The flight tests served as the culmination of the TRL 6 journey for the ALHAT system and included launch from a pad situated at the NASA-Kennedy Space Center Shuttle Landing Facility (SLF) runway, a lunar-like descent trajectory from an altitude of 250m, and landing on a lunar-like hazard field of rocks, craters, hazardous slopes, and safe sites 400m down-range just off the North end of the runway. The tests both confirmed the expected performance and also revealed several challenges present in the flight-like environment which will feed into future TRL advancement of the sensors. Guidance provided by the ALHAT system was impeded in portions of the trajectory and intermittent near the end of the trajectory due to optical effects arising from air heated by the rocket engine. The Flash Lidar identified hazards as small as 30 cm from the maximum slant range of 450 m which Morpheus could provide; however, it was occasionally susceptible to an increase in range noise due to scintillation arising from air heated by the Morpheus rocket engine which entered its Field-of-View (FOV). The Flash Lidar was also susceptible to pre-triggering, during the HRN phase, on a dust cloud created during launch and transported down-range by the wind. The NDL provided velocity and range measurements to the expected accuracy levels yet it was also susceptible to signal degradation due to air heated by the rocket engine. The LA, operating with a degraded transmitter laser, also showed signal attenuation over a few seconds at a specific phase of the flight due to the heat plume generated by the rocket engine.

Roback, V. Eric↗

Nanoscale Imaging and Measurements of Grain Boundary Thermal Resistance in Ceramics with Scanning Thermal Wave Microscopy

Material thermal conductivity is a key factor in various applications, from thermal management to energy harvesting. With microstructure engineering being a widely used method for customizing material properties, including thermal properties, understanding and controlling the role of extended phonon-scattering defects, like grain boundaries, is crucial for efficient material design. However, systematic studies are still lacking primarily due to limited tools. In this study, we demonstrate an approach for measuring grain boundary thermal resistance by probing the propagation of thermal waves across grain boundaries with a temperature-sensitive scanning probe. The method, implemented with a spatial resolution of about 100 nm on finely grained Nb-substituted SrTiO 3 ceramics, achieves a detectability of about 2 × 10 –8 K m 2 W –1 , suitable for chalcogenide-based thermoelectrics. The measurements indicated that the thermal resistance of the majority of grain boundaries in the STiO 3 ceramics is below this value. While there are challenges in improving sensitivity, considering spatial resolution and the amount of material involved in the detection, the sensitivity of the scanning probe method is comparable to that of optical thermoreflectance techniques, and the method opens up an avenue to characterize thermal resistance at the level of single grain boundaries and domain walls in a spectrum of microstructured materials.

36 MATERIALS SCIENCE↗

Lidar Sensor Performance in Closed-Loop Flight Testing of the Morpheus Rocket-Propelled Lander to a Lunar-Like Hazard Field

For the first time, a suite of three lidar sensors have been used in flight to scan a lunar-like hazard field, identify a safe landing site, and, in concert with an experimental Guidance, Navigation, and Control (GN&C) system, guide the Morpheus autonomous, rocket-propelled, free-flying test bed to a safe landing on the hazard field. The lidar sensors and GN&C system are part of the Autonomous Precision Landing and Hazard Detection and Avoidance Technology (ALHAT) project which has been seeking to develop a system capable of enabling safe, precise crewed or robotic landings in challenging terrain on planetary bodies under any ambient lighting conditions. The 3-D imaging flash lidar is a second generation, compact, real-time, air-cooled instrument developed from a number of cutting-edge components from industry and NASA and is used as part of the ALHAT Hazard Detection System (HDS) to scan the hazard field and build a 3-D Digital Elevation Map (DEM) in near-real time for identifying safe sites. The flash lidar is capable of identifying a 30 cm hazard from a slant range of 1 km with its 8 cm range precision at 1 sigma. The flash lidar is also used in Hazard Relative Navigation (HRN) to provide position updates down to a 250m slant range to the ALHAT navigation filter as it guides Morpheus to the safe site. The Doppler Lidar system has been developed within NASA to provide velocity measurements with an accuracy of 0.2 cm/sec and range measurements with an accuracy of 17 cm both from a maximum range of 2,200 m to a minimum range of several meters above the ground. The Doppler Lidar's measurements are fed into the ALHAT navigation filter to provide lander guidance to the safe site. The Laser Altimeter, also developed within NASA, provides range measurements with an accuracy of 5 cm from a maximum operational range of 30 km down to 1 m and, being a separate sensor from the flash lidar, can provide range along a separate vector. The Laser Altimeter measurements are also fed into the ALHAT navigation filter to provide lander guidance to the safe site. The flight tests served as the culmination of the TRL 6 journey for the lidar suite and included launch from a pad situated at the NASA-Kennedy Space Center Shuttle Landing Facility (SLF) runway, a lunar-like descent trajectory from an altitude of 250m, and landing on a lunar-like hazard field of rocks, craters, hazardous slopes, and safe sites 400m down-range just off the North end of the runway. The tests both confirmed the expected performance and also revealed several challenges present in the flight-like environment which will feed into future TRL advancement of the sensors. The flash lidar identified hazards as small as 30 cm from the maximum slant range of 450 m which Morpheus could provide, however, it was occasionally susceptible to an increase in range noise due to heated air from the Morpheus rocket plume which entered its Field-of-View (FOV). The flash lidar was also susceptible to pre-triggering on dust during the HRN phase which was created during launch and transported by the wind. The Doppler Lidar provided velocity and range measurements to the expected accuracy levels yet it was also susceptible to signal degradation due to air heated by the rocket engine. The Laser Altimeter, operating with a degraded transmitter laser, also showed signal attenuation over a few seconds at a specific phase of the flight due to the heat plume generated by the rocket engine.

Roback, Vincent E.↗

Identification of Defects and the Origins of Surface Noise on Hydrogen–Terminated (100) Diamond

Near-surface nitrogen vacancy centres are critical to many diamond-based quantum technologies such as information processors and nanosensors. Surface defects play an important role in the design and performance of these devices. The targeted creation of defects is central to proposed bottom-up approaches to nanofabrication of quantum diamond processors, and uncontrolled surface defects may generate noise and charge trapping which degrade shallow NV device performance. Surface preparation protocols may be able to control the production of desired defects and eliminate unwanted defects, but only if their atomic structure can first be conclusively identified. This work uses a combination of scanning tunnelling microscopy (STM) imaging and first-principles simulations to identify several surface defects on H:C(100)—2 × 1 surfaces prepared using chemical vapour deposition (CVD). The atomic structure of these defects is elucidated, from which the microscopic origins of magnetic noise and charge trapping are determined based on the modeling of their paramagnetic properties and acceptor states. Rudimentary control of these deleterious properties is demonstrated through STM tip-induced manipulation of the defect structure. Furthermore, the results validate accepted models for CVD diamond growth by identifying key adsorbates responsible for the nucleation of new layers.

36 MATERIALS SCIENCE↗

Origin of organic matter and organic pores in the overmature Ordovician-Silurian Wufeng-Longmaxi Shale of the Sichuan Basin, China

Organic matter (OM)-hosted pores play important roles in controlling the porosity and gas content of gas shales. However, the control of organic pore development and preservation remains poorly understood, partly because of the inability to distinguish OM types under the scanning electron microscope (SEM). In this study, seven over-mature Wufeng-Longmaxi Shale samples (equivalent vitrinite reflectance 1.93%–3.07%) were investigated with organic petrography and scanning electron microscope to study the origin of OM and development of organic pores in this black shale succession. Correlative light and electron microscopy was employed to examine pore development in individual macerals. Organic petrographic observations show that OM in these over-mature black shales is dominated by pyrobitumen and graptolites (> 90 vol.% of total OM based on point counting). Pyrobitumen mainly occurs as matrix bitumen in the fine-grained matrix, and also as a mixture with clay minerals and fossil cavity infillings. Vitrinite-like particles are minor constituents of OM in the Wufeng-Longmaxi Shale, and their average reflectance, reflectance distribution, and morphology suggest that they may be derived from graptolite fragments lacking diagnostic features and acritarchs. OM type critically controls the development of organic pores. Here, organic pores primarily occur in pyrobitumen, whereas other macerals are mostly non-porous when examined under the SEM. Results of this study provided important insights into OM thermal evolution and organic pore development in source-rock reservoirs, calling for a critical appraisal of OM in black shales with organic petrography in addition to SEM.

03 NATURAL GAS↗

Atomic force microscopy monitoring of subcritical slow crack growth in soda lime silicate glass

Prediction of brittle fracture in silicate glasses requires a fundamental understanding of slow crack growth rates, far below the critical stress intensity (K IC ) of the material. Here, in this study, atomic force microscopy (AFM) was used to characterize slow crack propagation in soda lime silicate glasses. Using large-sample AFM systems with specialized tips and scanners, fractures less than 20 nm wide were measured as a function of relative humidity (RH). The results were found to be sensitive to the type of AFM tip used and to the dryness of the surface. Continuous scanning and image capture over several days allowed the determination of the crack tip velocity. The dependance of crack tip velocity on RH was measured by enclosing the sample and AFM head in a humidity-controlled chamber. The crack tip velocity was measured as low 4.0×10 -12 m/s at 15 % RH and as high as 3.7×10 -10 m/s at 40 % RH. Overall crack growth was smooth during the AFM scan. Additionally, recession of the crack tip was noted as the sample dried, indicating crack tip closure may be occurring. Further studies on alternative compositions will provide details on subcritical fracture processes in a range of different environmental conditions.

Atomic force microscopy↗

Combining four-point bending and corrosion to map stress-dependent corrosion susceptibility of 316H stainless steel in FLiNaK

Understanding the effect of stress on the corrosion of steels in molten salts is important for material screening and safety assessment of molten salt reactors. We present a method that combines four-point bending with corrosion testing, enabling the mapping of corrosion susceptibility as a function of local stress from a single specimen. Guided by finite element analysis, a four-point bending setup was used to bend a 316H stainless-steel bar under controlled elastic stress during a 100-hour exposure in FLiNaK at 700 °C. Post-exposure characterization using scanning electron microscopy and energy-dispersive X-ray spectroscopy revealed a pronounced correlation between stress and corrosion. Regions under tensile stress exhibited significantly deeper attack depths and greater chromium depletion along grain boundaries, whereas compressive zones showed shallower corrosion cracks. The stress effect is attributed to stress concentration under tensile loading, which promotes chromium dissolution and crack propagation. This technique can be readily applied to other structural alloys, enabling quantitative measurement of corrosion susceptibility as a function of local stress.

316H↗

Microscopic Manipulation of Ferroelectric Domains in SnSe Monolayers at Room Temperature

Two-dimensional (2D) van der Waals ferroelectrics provide an unprecedented architectural freedom for the creation of artificial multiferroics and nonvolatile electronic devices based on vertical and coplanar heterojunctions of 2D ferroic materials. Nevertheless, controlled microscopic manipulation of ferroelectric domains is still rare in monolayer-thick 2D ferroelectrics with in-plane polarization. Here we report the discovery of robust ferroelectricity with a critical temperature close to 400 K in SnSe monolayer plates grown on graphene and the demonstration of controlled room-temperature ferroelectric domain manipulation by applying appropriate bias voltage pulses to the tip of a scanning tunneling microscope (STM). This study shows that STM is a powerful tool for detecting and manipulating the microscopic domain structures in 2D ferroelectric monolayers, which are difficult for conventional approaches such as piezoresponse force microscopy, thus facilitating the hunt for other 2D ferroelectric monolayers with in-plane polarization with important technological applications.

2D ferroelectric↗

Multiphoton and Harmonic Imaging of Microarchitected Materials

Microadditive manufacturing has revolutionized the production of complex, nano- to microscale components across various fields. This work investigates two-photon (2P) and three-photon (3P) fluorescence imaging, as well as third-harmonic generation (THG) microscopy, to examine periodic microarchitected lattice structures fabricated using multiphoton lithography (MPL). By immersing the structures in refractive index matching fluids, we demonstrate high-fidelity 3D reconstructions of both fluorescent structures using 2P and 3P microscopy as well as low-fluorescence structures using THG microscopy. These results show that multiphoton fluorescence (MPF) imaging offers reduced signal decay with respect to depth compared to single-photon techniques in the examined structures. We further demonstrate the ability to nondestructively identify intentional internal modifications of the structure that are not immediately visible with scanning electron microscope (SEM) images and compression-induced fractures, highlighting the potential of these techniques for quality control and defect detection in microadditively manufactured components.

36 MATERIALS SCIENCE↗

Progressive growth of the solid–electrolyte interphase towards the Si anode interior causes capacity fading

The solid–electrolyte interphase (SEI), a layer formed on the electrode surface, is essential for electrochemical reactions in batteries and critically governs the battery stability. Active materials, especially those with extremely high energy density, such as silicon (Si), often inevitably undergo a large volume swing upon ion insertion and extraction, raising a critical question as to how the SEI interactively responds to and evolves with the material and consequently controls the cycling stability of the battery. Here, by integrating sensitive elemental tomography, an advanced algorithm and cryogenic scanning transmission electron microscopy, we unveil, in three dimensions, a correlated structural and chemical evolution of Si and SEI. Furthermore, corroborated with a chemomechanical model, we demonstrate progressive electrolyte permeation and SEI growth along the percolation channel of the nanovoids due to vacancy injection and condensation during the delithiation process. Consequently, the Si–SEI spatial configuration evolves from the classic ‘core–shell’ structure in the first few cycles to a ‘plum-pudding’ structure following extended cycling, featuring the engulfing of Si domains by the SEI, which leads to the disruption of electron conduction pathways and formation of dead Si, contributing to capacity loss. The spatially coupled interactive evolution model of SEI and active materials, in principle, applies to a broad class of high-capacity electrode materials, leading to a critical insight for remedying the fading of high-capacity electrodes.

36 MATERIALS SCIENCE↗

Fixed-target serial crystallography at the Structural Biology Center

Serial synchrotron crystallography enables the study of protein structures under physiological temperature and reduced radiation damage by collection of data from thousands of crystals. The Structural Biology Center at Sector 19 of the Advanced Photon Source has implemented a fixed-target approach with a new 3D-printed mesh-holder optimized for sample handling. The holder immobilizes a crystal suspension or droplet emulsion on a nylon mesh, trapping and sealing a near-monolayer of crystals in its mother liquor between two thin Mylar films. Data can be rapidly collected in scan mode and analyzed in near real-time using piezoelectric linear stages assembled in an XYZ arrangement, controlled with a graphical user interface and analyzed using a high-performance computing pipeline. Here, the system was applied to two β-lactamases: a class D serine β-lactamase from Chitinophaga pinensis DSM 2588 and L1 metallo-β-lactamase from Stenotrophomonas maltophilia K279a.

59 BASIC BIOLOGICAL SCIENCES↗

AutoEMX v1.

The invention consists in the full automation of compositional analysis of inorganic powder samples by scanning electron microscopy (SEM) with energy-dispersive X-ray spectroscopy (EDS). The measurements and analysis are controlled via python-based software, Auto-SEMEDS. Auto-SEMEDS fully automates the SEM-EDS measurements, and analyses the collected data via the use of machine-learning (ML) algorithms, which have never been used before for such scope. Auto-SEMEDS enables the identification in fully-automated fashion of the individual material phases present in a powder sample. Similar technologies, such as commercial SEM-EDS software, can automatically classify particles based on their composition, but they have significant limitations. These solutions typically provide inaccurate composition measurements and struggle to identify single phases in lab samples, where phases are often closely intermixed. In contrast, Auto-SEMEDS achieves unprecedented accuracy in composition measurements of powder samples, and furthermore leverages machine learning algorithms to effectively discern intermixed phases. Notably, while previous studies have demonstrated accurate measurements on individual particles, Auto-SEMEDS stands out by successfully analyzing mixture of different phases, a capability that has not been reported in the literature until now.

Giunto, Andrea [Lawrence Berkeley National Laborat↗

SpacerExtractor v0.9

The SpacerExtractor tool is meant to robustly identify and extract CRISPR spacers from metagenome short reads. Working from a database of known CRISPR repeats, SpacerExtractor quickly scans short reads for the corresponding repeat sequences, extract the potential spacer between two repeats, apply several quality control, denoising, and clustering steps, and provides a full non-redundant complement of spacers for each detected repeat. Because of the high variability observed at CRISPR loci, this read mining approach typically recovers a much larger diversity of spacers than can be found in assembled contigs. SpacerExtractor also includes commands to run CRISPR-Cas Typer on a new set of genomes or MAGs, and add newly predicted repeats to the repeat database.

Bushnell, Brian↗

Optical to optical interface device

The development, fabrication, and testing of a preliminary model of an optical-to-optical (noncoherent-to-coherent) interface device for use in coherent optical parallel processing systems are described. The developed device demonstrates a capability for accepting as an input a scene illuminated by a noncoherent radiation source and providing as an output a coherent light beam spatially modulated to represent the original noncoherent scene. The converter device developed under this contract employs a Pockels readout optical modulator (PROM). This is a photosensitive electro-optic element which can sense and electrostatically store optical images. The stored images can be simultaneously or subsequently readout optically by utilizing the electrostatic storage pattern to control an electro-optic light modulating property of the PROM. The readout process is parallel as no scanning mechanism is required. The PROM provides the functions of optical image sensing, modulation, and storage in a single active material.

Oliver, D. S.↗

Fluid flow effects on crystalline perfection

Optimum solidification parameters for the production of highly perfect copper crystals by Czochralski growth are sought along with the documentation of crystal imperfections under various growth conditions. X-ray techniques which do not in their application produce defects and which allow the characterization of imperfections in single crystals are chosen to assess crystal perfection. The X-ray techniques employed ranged from ordinary Laue photography through Borrmann topography to double-crystal scanning diffractometry, thus allowing crystals with a wide variation in perfection to be studied. As a set of controllable solidification parameters, the rotation of the seed and of the melt and the diameter of the bottleneck are chosen. X-ray diffraction topographs are analyzed along with the data obtained from rocking curve measurements. Tables of growth conditions and quantitative data of rocking curve widths are presented.

Kuriyama, M.↗

Applications of digital image acquisition in anthropometry

A description is given of a video kinesimeter, a device for the automatic real-time collection of kinematic and dynamic data. Based on the detection of a single bright spot by three TV cameras, the system provides automatic real-time recording of three-dimensional position and force data. It comprises three cameras, two incandescent lights, a voltage comparator circuit, a central control unit, and a mass storage device. The control unit determines the signal threshold for each camera before testing, sequences the lights, synchronizes and analyzes the scan voltages from the three cameras, digitizes force from a dynamometer, and codes the data for transmission to a floppy disk for recording. Two of the three cameras face each other along the 'X' axis; the third camera, which faces the center of the line between the first two, defines the 'Y' axis. An image from the 'Y' camera and either 'X' camera is necessary for determining the three-dimensional coordinates of the point.

Woolford, B.↗