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At least 1,711 records · Page 95

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↗

Statistics of High Purity Nickel Microstructure From High Energy X-ray Diffraction Microscopy

We have measured and reconstructed via forward modeling a small volume of microstructure of high purity, well annealed nickel using high energy x-ray diffraction microscopy (HEDM). Statistical distributions characterizing grain orientations, intra-granular misorientations, and nearest neighbor grain misorientations are extracted. Results are consistent with recent electron backscatter diffraction measurements. Peaks in the grain neighbor misorientation angle distribution at 60 degrees ({Sigma}3) and 39 degrees ({Sigma}9) have resolution limited widths of {approx} 0.14 degree FWHM. The analysis demonstrates that HEDM can recover grain and grain boundary statistics comparable to OIM volume measurements; more extensive data sets will lead to full, five parameter grain boundary character distributions. Due to its non-destructive nature, HEDM can then watch, both statistically and through tracking of individual grains and boundaries, the evolution of such distributions with processing of the sample.

43 PARTICLE ACCELERATORS↗

Electron Microscopy Study of Hypo-Stoichiometric Fe-Pd Nanocomposites Resulting from Combined Reaction Thermomechanical Processing

Hypo stoichiometric Fe-Pd binary alloys (35-45 at% Pd) were severely deformed (>90%) and subsequently aged to induce concomitant recrystallization, precipitation, and ordering. This thermomechanical processing strategy was articulated by Hornbogen [1] over thirty years ago. The resulting exchange-coupled ferromagnets contain ferrite precipitates and a complex metastable twophase lamellar transformation product comprised of ordered L10 and a metastable FCC phase. The later duplex microconstituent is suggested to form in conjunction with a so-called pseudospinodal reaction [2] involving emerging cubic and tetragonal phases, whereby phase separation and ordering result from continuous changes in composition and a reduction in symmetry, cubic to tetragonal. The deformation texture of the parent austenite is substantially retained in the transformation product, resulting in anisotropy of the magnetic properties as determined by magnetometry (VSM). This paper presents electron microscopy results elucidating the crystallography and morphology of the phase mixtures including HREM. Magnetic field annealing is also included as a branch of our thermomechanical processing strategy, and we discuss the influence of the external fields on recrystallization, precipitation, and ordering. This work was performed in cooperation with ORNL and the NHMFL and is supported by the NSF DMR.

36 MATERIALS SCIENCE↗

Microstructural characterization of Ti-6Al-4V metal chips by focused ion beam (FIB) and transmission electron microscopy (TEM)

The microstructure of the secondary deformation zone (SDZ) near the cutting surface in metal chips of Ti-6Al-4V formed during machining was investigated using focused ion beam (FIB) specimen preparation and transmission electron microscopy (TEM) imaging. Use of the FIB allowed precise extraction of the specimen across this region to reveal its inhomogeneous microstructure resulting from the non-uniform distribution of strain, strain rate, and temperature generated during the cutting process. Initial imaging from conventional TEM foil preparation revealed microstructures ranging from heavily textured to regions of fine grains. Using FIB preparation, the transverse microstructure could be interpreted as fine grains near the cutting surface which transitioned to coarse grains toward the free surface. At the cutting surface a 10 nm thick recrystallized layer was observed capping a 20 nm thick amorphous layer.

36 MATERIALS SCIENCE↗

CO2 Adsorption, Diffusion and Electron-Induced Chemistry on Rutile TiO2(110) – A Low-Temperature Scanning Tunneling Microscopy Study

Low-temperature scanning tunneling microscopy (STM) has been used to study the adsorption of CO{sub 2} on rutile TiO{sub 2}(110) from 80 to 180 K. For low CO{sub 2} doses, two molecular adsorption sites with different binding energies are identified, which are effectively isolated from one another by an apparent activation barrier to their interconversion. We identify the less tightly bound adsorption site as CO{sub 2} adsorbed atop 5-fold coordinated titanium surface atoms (Ti{sub 5f}), without binding preferentially near oxygen vacancies. CO{sub 2} desorption from Ti{sub 5f} occurs at 140 K. The more strongly bound site involves molecular CO{sub 2} binding at bridging oxygen vacancies (V{sub O,br}). We observe two distinct configurations of V{sub O,br} bound CO{sub 2} molecules. Despite its being bound to the vacancy, CO{sub 2} does not dissociate thermally but remains intact up to the desorption temperature of {approx}175 K. At an elevated tunneling bias, the STM tip can selectively dissociate these CO{sub 2} molecules and thus trigger the healing of individual V{sub O,br}. At higher coverage, CO{sub 2} adsorption occurs predominantly at the more abundant Ti{sub 5f} sites, with the distribution of CO{sub 2} molecules being determined by interactions both along the [001] and [110] directions.

36 MATERIALS SCIENCE↗

Characterization of durable nanostructured thin film catalysts tested under transient conditions using analytical aberration-corrected electron microscopy

The stability of Ru0.1Ir0.9 oxidation evolution reaction (OER) catalysts deposited on Pt-coated nanostructured thin films (NSTFs) has been investigated by aberration-corrected electron microscopy. Accelerated stress tests showed that the OER catalysts significantly improved the durability of the Pt under cell reversal conditions. High-resolution images of the end-of-life NSTFs showed significant Ir loss from the whisker surfaces, while no Pt loss was observed, indicating that the OER catalysts had protected the catalyst coated whisker surfaces from degradation.

36 MATERIALS SCIENCE↗

Atomic Force Microscopy of Arrays of Asymmetrical DNA Motifs

DNA can easily be assembled into wide and relatively flat nanostructures that lend themselves to study via Atomic Force Microscopy (AFM). It is often important to know which side of an assembly the AFM is imaging. This is particularly crucial for characterizing nanomachines, where the movement must be measured relative to fiducial features visible to the AFM. We have developed a cheap and simple technique for building DNA arrays with distinguishable sides, a technique requiring 10 or fewer strands - dozens or hundreds of strands fewer than used for these purposes previously. Our approach involves constructing arrays out of DNA tiles that have low apparent symmetry when imaged via AFM. We have surveyed the effects of varying degrees of motif asymmetry in AFM micrographs. Even at resolutions where the individual tiles cannot be resolved (either because of sub-optimal tip quality, or very gentle tapping by the AFM tip) the larger scale features of the arrays have predictable structures that allow the determination of which side of the array is facing up. We have used this information to verify that DNA hairpins attached to either the up- or down-facing side of an array on mica can be detected in AFM height scans. We have also characterized differences in appearance between hairpins attached to different sides of the arrays.

59 BASIC BIOLOGICAL SCIENCES↗

MULTISLICE SIMULATION OF TRANSMISSION ELECTRON MICROSCOPY IMAGING OF HELIUM BUBBLES IN IRON

The objective of this task is to establish the size correlation between transmission electron microscopy (TEM) imaged helium (He) bubbles and the actual bubbles in an iron (Fe) matrix. SUMMARY The results of this simulation study show that the size of TEM imaged He bubbles, represented by the inner diameter of the first dark Fresnel ring under defocused condition (Din), deviated from the actual bubble size (Do). Din was found to be larger than Do when imaged with a highly incoherent electron beam, but smaller than Do if the beam is coherent. The deviation of Din from Do increases with increasing defocus. On the other hand, the electron beam accelerating voltage, bubble size, bubble position, and TEM sample thickness do not significantly affect the value of D0/Do. This study also suggests that He bubbles can be differentiated from argon (Ar) bubbles by differences in Fresnel contrast.

36 MATERIALS SCIENCE↗

Cryogenic X-ray Diffraction Microscopy for Biological Samples

X-ray diffraction microscopy (XDM) is well suited for nondestructive, high-resolution biological imaging, especially for thick samples, with the high penetration power of x rays and without limitations imposed by a lens. We developed nonvacuum, cryogenic (cryo-) XDM with hard x rays at 8 keV and report the first frozen-hydrated imaging by XDM. By preserving samples in amorphous ice, the risk of artifacts associated with dehydration or chemical fixation is avoided, ensuring the imaging condition closest to their natural state. The reconstruction shows internal structures of intact D. radiodurans bacteria in their natural contrast.

59 BASIC BIOLOGICAL SCIENCES↗

Direct Measurements of the Penetration Depth in a Superconducting Film using Magnetic Force Microscopy

We report the local measurements of the magnetic penetration depth in a superconducting Nb film using magnetic force microscopy (MFM). We developed a method for quantitative extraction of the penetration depth from single-parameter simultaneous fits to the lateral and height profiles of the MFM signal, and demonstrate that the obtained value is in excellent agreement with that obtained from the bulk magnetization measurements.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Characterization of cell surface and extracellular matrix remodeling of Azospirillum brasilense chemotaxis-like 1 signal transduction pathway mutants by atomic force microscopy

To compete in complex microbial communities, bacteria must sense environmental changes and adjust cellular functions for optimal growth. Chemotaxis-like signal transduction pathways are implicated in the regulation of multiple behaviors in response to changes in the environment, including motility patterns, exopolysaccharide production, and cell-to-cell interactions. In Azospirillum brasilense, cell surface properties, including exopolysaccharide production, are thought to play a direct role in promoting flocculation. Recently, the Che1 chemotaxis-like pathway from A. brasilense was shown to modulate flocculation, suggesting an associated modulation of cell surface properties. Using atomic force microscopy, distinct changes in the surface morphology of flocculating A. brasilense Che1 mutant strains were detected. Whereas the wild-type strain produces a smooth mucosal extracellular matrix after 24 h, the flocculating Che1 mutant strains produce distinctive extracellular fibril structures. Further analyses using flocculation inhibition, lectin-binding assays, and comparison of lipopolysaccharides profiles suggest that the extracellular matrix differs between the cheA1 and the cheY1 mutants, despite an apparent similarity in the macroscopic floc structures. Collectively, these data indicate that disruption of the Che1 pathway is correlated with distinctive changes in the extracellular matrix, which likely result from changes in surface polysaccharides structure and/or composition.

59 BASIC BIOLOGICAL SCIENCES↗

Topography and Mechanical Property Mapping of International Simple Glass Surfaces with Atomic Force Microscopy

Quantitative Nanomechanical Peak Force (PF-QNM) TappingModeTM atomic force microscopy measurements are presented for the first time on polished glass surfaces. The PF-QNM technique allows for topography and mechanical property information to be measured simultaneously at each pixel. Results for the international simple glass which represents a simplified version of SON68 glass suggests an average Young s modulus of 78.8 15.1 GPa is within the experimental error of the modulus measured for SON68 glass (83.6 2 GPa) with conventional approaches. Application of the PF-QNM technique will be extended to in situ glass corrosion experiments with the goal of gaining atomic-scale insights into altered layer development by exploiting the mechanical property differences that exist between silica gel (e.g., altered layer) and pristine glass surface.

alteration layer↗

Characterizing Dislocation Defects in Dark Field X-ray Microscopy Images of Bulk Aluminum

Material defects play a large role in material response under shock loading, yet the process of how these defects initiate, propagate, and annihilate is not well understood. Using a newly developed diagnostic, dark field X-ray microscopy (DFXM), we can now visualize the behavior of dislocation defects in materials at the mesoscale under varying conditions. Using data from the European Synchrotron Radiation Facility, we apply a variety of image processing techniques to capture relevant features to locate and characterize size and orientation of dislocation defects in bulk aluminum DFXM images. Beyond simple visualization, this analysis drives statistical characterization of the defects and their dynamic response to further improve the relevant physics models.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Examining Bioethanol-Producing Ultrastructures with Electron Microscopy and Molecular Dynamics

A longstanding goal in the biofuel sector is to increase the efficiency of the circularization of the use of materials (1). One such instance is the degradation of plant material, such as cellulose, and converting it to biofuel via bacterial digestion (2). The bifunctional aldehyde-alcohol dehydrogenase (AdhE) from the anaerobic thermophile C. thermocellum seems to be vital for the production and cellular tolerance of bioethanol; however, it lacks the efficiency to produce ethanol at industry standards (3). Therefore, to understand how C. thermocellum AdhE functions, we used cryo-electron microscopy (cryo-EM) to obtain a 3.2 A structure of the AdhE complex. When compared to previously published structures from E. coli (4-6), we identified potential regions that control the native conformation of the ultrastructure, as well as located channels that isolate the intermediate aldehyde from the cellular milieu. This high-resolution structure, in combination with molecular dynamics simulations, provides insight into one example of substrate channeling and establishes a basis for future mutagenesis studies.

AdhE↗

Leveraging Super High Optical Resolution Microscopy to Probe the Interaction Zone Between Clostridium thermocellum and Biomass

This poster, part of the Pacific Northwest National Laboratory-sponsored Integration 2020: Visualizing the Proteome virtual conference, discusses super high optical resolution microscopy to probe the interaction zone between Clostritium thermocellum and biomass. Clostridium thermocellum is one of the most efficient microorganisms for the deconstruction of biomass. To achieve this high level of cellulolytic activity, C. thermocellum uses large multienzyme complexes known as cellulosomes to sugars in 4-5 break down polysaccharides found in plant cell walls. The attachment of bacterial switchgrass 70% cells to the nearby substrate via the cellulosome has been hypothesized to be the reason for this high efficiency. The region lying between the cell and the substrate has shown great variation and dynamics that are affected by the growth stage of cells and the substrate used for growth.

bacteria↗

Initial results from electron microscopy from AGR 5/6/7 Capsule 1 fuel and

Initial results from electron microscopy from AGR 5/6/7 Capsule 1 fuel and applications of other microanalysis techniques to irradiated TRISO fuel. Includes detail on characterization of particles from AGR 5/6/7 Capsule 1, which include background and motivation, x-ray computed tomography on four particles from compact 1-7-9, SEM/EDS of particles from compacts 1-7-9 and 1-7-4, and Summary. Local thermal conductivity measurement on AGR-2 particles also discussed.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

XRD, Electron Microscopy and Vibrational Spectroscopy Characterization of Simulated SB6 HLW Glasses - 13028

Sample glasses have been made using SB6 high level waste (HLW) simulant (high in both Al and Fe) with 12 different frit compositions at a constant waste loading of 36 wt.%. As follows from X-ray diffraction (XRD) and optical and scanning electron microscopy (SEM) data, all the samples are composed of primarily glass and minor concentration of spinel phases which form both isometric grains and fine cubic (∼1 μm) crystals. Infrared spectroscopy (IR) spectra of all the glasses within the range of 400-1600 cm{sup -1} consist of the bands due to stretching and bending modes in silicon-oxygen, boron-oxygen, aluminum-oxygen and iron-oxygen structural groups. Raman spectra showed that for the spectra of all the glasses within the range of 850-1200 cm{sup -1} the best fit is achieved by suggestion of overlapping of three major components with maxima at 911-936 cm{sup -1}, 988-996 cm{sup -1} and 1020-1045 cm{sup -1}. The structural network is primarily composed of metasilicate chains and rings with embedded AlO{sub 4} and FeO{sub 4} tetrahedra. Major BO{sub 4} tetrahedra and BO{sub 3} triangles form complex borate units and are present as separate constituents. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗