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At least 73 records · Page 4

Role of Cations in the Cation-Driven Assembly Process and their Effect on the Charge Storage Properties of Bilayered Vanadium Oxide and Reduced Graphene Oxide Heterostructures in Alkali Ion Systems

Exfoliated δ-Li x V 2 O 5 ·nH 2 O (ex-LVO) and reduced graphene oxide (rGO) heterostructures were constructed using different assembling cations (i.e., Li⁺, Na⁺, and K⁺ ions). The ex-LVO and rGO nanoflakes were stacked together using a concentrated chloride solution of each assembling cation and vacuum annealed at 200 °C to form three distinct two-dimensional (2D) layered architectures. X-ray diffraction and thermogravimetric analysis confirmed that the assembling ions can control the interlayer spacing of the bilayered vanadium oxide (BVO) phase as well as impact the crystallographic water content, which in turn affects the electrochemical performance. Scanning electron microscopy, scanning transmission electron microscopy (STEM), electron energy-loss spectroscopy (EELS), and X-ray photoelectron spectroscopy confirmed that a 2D heterointerface formed between LVO and rGO and that the cations used to assemble the heterostructure are trapped in the interlayer BVO region. High-resolution STEM imaging also showed the rGO dispersion throughout the LVO layers. Moreover, STEM-EELS identified a V 2 O 3 phase that forms along the rGO interface and can stabilize the materials during cycling. A charge storage mechanism analysis, combined with the galvanostatic intermittent titration technique, found that increased interlayer spacings of the BVO phase and using the assembling cations to define intercalation sites for identical charge-carrying ions lead to improved ion diffusion and increased capacities during cycling. Therefore, the Li⁺ and Na⁺ ion assembled heterostructures showed improved charge-carrying ion diffusion and charge storage capacities in each of their respective charge storage systems (i.e., Li-ion and Na-ion half-cells). In total, the cation used for heterostructure assembly can modify the final material structure and tailor the ion diffusion and charge storage capacity to tune its properties for the desired electrochemical system using a variety of 2D materials.

25 ENERGY STORAGE↗

Coaxial carbon plasma gun deposition of amorphous carbon films

A unique plasma gun employing coaxial carbon electrodes was used in an attempt to deposit thin films of amorphous diamond-like carbon. A number of different structural, compositional, and electrical characterization techniques were used to characterize these films. These included scanning electron microscopy, scanning transmission electron microscopy, X ray diffraction and absorption, spectrographic analysis, energy dispersive spectroscopy, and selected area electron diffraction. Optical absorption and electrical resistivity measurements were also performed. The films were determined to be primarily amorphous, with poor adhesion to fused silica substrates. Many inclusions of particulates were found to be present as well. Analysis of these particulates revealed the presence of trace impurities, such as Fe and Cu, which were also found in the graphite electrode material. The electrodes were the source of these impurities. No evidence of diamond-like crystallite structure was found in any of the film samples. Details of the apparatus, experimental procedure, and film characteristics are presented.

Sater, D. M.↗

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↗

Miniature Variable Pressure - Scanning Electron Microscopy (MVP-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↗

Intrinsic Defect-Induced Local Semiconducting-to-Metallic Regions Within Monolayer 1T-TiS2 Displayed by First-Principles Calculations and Scanning Tunneling Microscopy

Using density functional theory (DFT) and scanning tunneling microscopy (STM), the intrinsic point defects, formation energy, and electronic structure of 1T-TiS2 were investigated. Defect systems include single-atom vacancies, interstitial and adatom additions, and direct atomic substitution. Using a collective approach for analyzing realistic systems for point defect investigation, we provide a more straightforward comparison to the experimental measurements, reproducing more realistic environmental conditions related to thin film growth. STM images are compared to computationally simulated electron density images to identify specific geometries that result from favorable point defects. DFT suggests that titanium interstitials are the most energetically favorable intrinsic defect, and sulfur vacancies are more likely to form than titanium vacancies within this realistic analysis, which is in agreement with STM data. A pristine, stoichiometric monolayer system is calculated to have a direct band gap of 0.422 eV, which varies based on local point defects. Local semiconducting-to-metallic electronic transitions are predicted to occur based on the presence of Ti interstitials.

Keeney, P. J.↗

Potential Challenges in Near-Field Scanning Optical Microscopy for Space Applications

Near-field scanning optical microscopy is a relatively new but very powerful technique for obtaining several metrological parameters at nanometer range spatial resolution. It is logical to think deploying it into space applications like diagnostics of protein crystal growth under microgravity conditions. One may attempt to deploy existing instrumentation and expect some results. However, the existing technology and commercial instrumentation is tailored to ground based laboratory situations. Even in those laboratory conditions, the role of fluids (common in crystal growth), rough objects (such as a crystal under growth), etc. on the instrumentation is only recently being investigated. These aspects combined with effects of reduced gravity environment are going to make the problem more complex. These technological challenges must be tackled for meaningful system operation in space. Since the microscopy concept has not been attempted so far in space, all of the actual problems are unknown. Nevertheless, based on current literature, some possible problems and potential solutions are described here. One may use the discussion for system modification/optimization during initial use of this kind of microscopy in space.

Vikram, C. S.↗

Scanning Tunneling Microscopy methods for spectroscopic imaging of subsurface interfaces

A new method for spatially-resolved, spectroscopic investigation of subsurface interface structure has been developed. The method, Ballistic Electron Emission Microscopy (BEEM), is based on Scanning Tunneling Microscopy (STM) techniques. BEEM combines STM vacuum tunneling with unique ballistic electron spectroscopy capabilities. BEEM enables, for the first time, direct imaging of subsurface interface electronic properties with nanometer spatial resolution. STM topographic images of surface structure and BEEM images of subsurface properties are obtained simultaneously. BEEM capabilities are demonstrated by investigation of important metal-semiconductor interfaces.

Bell, L. D.↗

Deep learning for electron and scanning probe microscopy: From materials design to atomic fabrication

Machine learning and artificial intelligence (ML/AI) are rapidly becoming an indispensable part of physics research, with applications ranging from theory and materials prediction to high-throughput data analysis. In parallel, the recent successes in applying ML/AI methods for autonomous systems from robotics through self-driving cars to organic and inorganic synthesis are generating enthusiasm for the potential of these techniques to enable automated and autonomous experiment in imaging. Here, we discuss recent progress in application of machine learning methods in scanning transmission electron microscopy and scanning probe microscopy, from applications such as data compression and exploratory data analysis to physics learning to atomic fabrication.

36 MATERIALS SCIENCE↗

In situ plasmonic tip preparation and validation techniques for scanning tunneling microscopy

Among the many parts constituting a scanning tunneling microscope, the metallic tip is the component that directly interacts with the specimen and plays a critical role in visualizing the physical quantity of interest. While tip materials such as W and Pt–Ir are commonly used for topographic imaging and their preparation is well-documented, the preparation of plasmonic materials such as Ag for tip-enhanced Raman spectroscopy is relatively less standardized. Furthermore, we present several in situ Ag tip preparation and validation techniques for the microscopist to use depending on their intended application, including atomic resolution imaging, scanning tunneling spectroscopy (STM), and tip-enhanced Raman spectro-microscopy in ultrahigh vacuum. Besides optical applications, these methods are not limited to Ag but also applicable to other STM tip materials.

47 OTHER INSTRUMENTATION↗

Experimental and analytical study of fatigue damage in notched graphite/epoxy laminates

Both tension and compression fatigue behaviors were investigated in four notched graphite/epoxy laminates. After fatigue loading, specimens were examined for damage type and location using visual inspection, light microscopy, scanning electron microscopy, ultrasonic C-scans, and X-radiography. Delamination and ply cracking were found to be the dominant types of fatigue damage. In general, ply cracks did not propagate into adjacent plies of differing fiber orientation. To help understand the varied fatigue observations, the interlaminar stress distribution was calculated with finite element analysis for the regions around the hole and along the straight free edge. Comparison of observed delamination locations with the calculated stresses indicated that both interlaminar shear and peel stresses must be considered when predicting delamination. The effects of the fatigue cycling on residual strength and stiffness were measured for some specimens of each laminate type. Fatigue loading generally caused only small stiffness losses. In all cases, residual strengths were greater than or equal to the virgin strengths.

Whitcomb, J. D.↗

Experimental and analytical study of fatigue damage in notched graphite/epoxy laminates

Fatigue damage development in notched graphite/epoxy laminates is investigated in both compression and tension, with tested specimens being examined for damage type and location using light microscopy, scanning electron microscopy, ultrasonic C-scans, and X-radiography. Delamination and ply cracking were found to be the dominant types of fatigue damage. Comparison of observed delamination locations with finite element calculations indicates that both interlaminar shear and peel stresses must be considered when predicting delamination. Fatigue loading generally caused only small stiffness losses, and residual strengths were in all cases greater than, or equal to, the virgin strengths.

Whitcomb, J. D.↗

Scanning electron microscopy of the vestibular end organs

The vestibular end organs, after chemical fixation, were freeze dried, coated with gold and palladium, and studied in the scanning microscope. Scanning microscopy gives a good three dimensional view of the sensory areas and allows study of both gross anatomy and microstructures. Cross anatomical features of the structure of the ampullae are demonstrated. The form of the statoconia in different species of animals is shown. New aspects of the structure of the sensory hairs are revealed. The hair bundles in the central areas of the cristae and in the striola of the maculae differ structurally from the hair bundles at the periphery of the sensory regions. Furthermore, some hair bundles consisting of very short stereocilia were observed. The relationship between the cupula and the statoconial membrane to the epithelial surface is discussed.

Lindeman, H. H.↗

Method for error correction in scanning probe microscopy

Disclosed here is a scanning probe microscope system and method for operating the same for producing scanning probe microscope images at fast scan rates and reducing oscillation artifacts. In some embodiments, an inverse consistent image registration method is used to align forward and backward scan traces for each line of the scanning microscope image. In some embodiments, the aligned forward and backward scan traces are combined using a weighting factor favoring the scan trace with higher smoothness. In some embodiments, the scanning probe microscope image is a potentiometry map and a method is provided to extract from the potentiometry map a conductivity map.

47 OTHER INSTRUMENTATION↗

Scanning electron microscopy of lunar regolith from the Sea of Fertility

Scanning electron microscopy was used in studying the morphology and cathodoluminescence of lunar regolith particles. Surface and structure of two groups of particles are differentiated: (1) Crystalline with well defined facets and spalling surfaces, which are grains of minerals and rock fragments: and (2) amorphous, fused, and partially or entirely glazed particles. Local melting of particles and the round openings on their surfaces are attributed to secondary influence on the regolith of factors of lunar weathering and above all micrometeoric impacts.

Antoshin, M. K.↗

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.

36 MATERIALS SCIENCE↗

Investigation of KC-135 flight samples solidified in near-zero gravity

An analysis was conducted of three KC-135 flight samples that had been solidified in near-zero gravity. These samples had been generated during near-zero gravity testing of M553 experiment Skylab flight hardware. The samples evaluated were all Star-J Satellite, a cobalt base alloy. The analytical procedures (optical microscopy, scanning electron microscopy, electron microprobe, X-ray diffraction, differential scanning calorimetry, and microhardness) to be use on the Skylab flight samples were optimized and the analytical results are presented.

Larson, D., Jr.↗

Bayesian inference in band excitation scanning probe microscopy for optimal dynamic model selection in imaging

The universal tendency in scanning probe microscopy (SPM) over the last two decades is to transition from simple 2D imaging to complex detection and spectroscopic imaging modes. The emergence of complex SPM engines brings forth the challenge of reliable data interpretation, i.e., conversion from detected signals to descriptors specific to tip–surface interactions and subsequently to material’s properties. In this work, we implemented a Bayesian inference approach for the analysis of the image formation mechanisms in band excitation SPM. Compared to the point estimates in classical functional fit approaches, Bayesian inference allows for the incorporation of extant knowledge of materials and probe behavior in the form of corresponding prior distribution and return the information on the material functionality in the form of readily interpretable posterior distributions. We explore the nonlinear mechanical behaviors spatially in a classical ferroelectric material, PbTiO 3 . We observe the non-trivial evolution of the Duffing stiffness term and the nonlinearity of the sample surface, determine spatial clustering of the nonlinear response, and perform a Landau analysis on predicting the nonlinear coefficient, which indicates that ferroelectric behavior can be a cause of the observed results. These observations suggest that the spectrum of anomalous behaviors at the ferroelectric domain walls may be broader than previously believed and can extend to non-conventional mechanical properties in addition to static and microwave conductance.

36 MATERIALS SCIENCE↗