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At least 631 records · Page 35

Combining Spatial and Temporal Resolution in Cryo-TEM of Device Materials: Preprint

Cryogenic transmission electron microscopy (cryo-TEM) has been instrumental to reducing the effects of electron-beam sample interactions and enabling higher spatial resolution studies of beam sensitive materials. However, the process of thinning and freezing samples for cryo-TEM characterization is often complex and frequently involves removing materials from their environment or stimuli of interest for extended times. This can allow for structural relaxation, diffusion, and other dynamic processes to occur prior to characterization; for energy materials like battery electrodes, this makes it difficult to precisely correlate the imaged structure with native structures that evolve in-situ during device processing, operation, or aging. Here, we present methods to prepare cryo-TEM samples from energy materials during these critical processes in the relevant device lifetimes. This offers insights into improving the temporal resolution of cryo-TEM, while still exploiting its ability to achieve high spatial resolutions in characterizing beam sensitive materials.

BASIC BIOLOGICAL SCIENCES,MATERIALS SCIENCE↗

Instrument for in situ hard x-ray nanobeam characterization during epitaxial crystallization and materials transformations

Solid-phase epitaxy (SPE) and other three-dimensional epitaxial crystallization processes pose challenging structural and chemical characterization problems. The concentration of defects, the spatial distribution of elastic strain, and the chemical state of ions each vary with nanoscale characteristic length scales and depend sensitively on the gas environment and elastic boundary conditions during growth. The lateral or three-dimensional propagation of crystalline interfaces in SPE has nanoscale or submicrometer characteristic distances during typical crystallization times. Here, an in situ synchrotron hard x-ray instrument allows these features to be studied during deposition and crystallization using diffraction, resonant scattering, nanobeam and coherent diffraction imaging, and reflectivity. The instrument incorporates a compact deposition system allowing the use of short-working-distance x-ray focusing optics. Layers are deposited using radio-frequency magnetron sputtering and evaporation sources. The deposition system provides control of the gas atmosphere and sample temperature. The sample is positioned using a stable mechanical design to minimize vibration and drift and employs precise translation stages to enable nanobeam experiments. Results of in situ x-ray characterization of the amorphous thin film deposition process for a SrTiO 3 /BaTiO 3 multilayer illustrate implementation of this instrument.

47 OTHER INSTRUMENTATION↗

Seasonal Monitoring and Estimation of Regional Aerosol Distribution over Po Valley, Northern Italy, Using a High-Resolution MAIAC Product

In this work, the new 1-km-resolved Multi-Angle Implementation of Atmospheric Correction (MAIAC) algorithm is employed to characterize seasonal AOD-PM10 correlations over northern Italy. The accuracy of the new dataset is assessed versus the widely used Moderate Resolution Imaging Spectroradiometer (MODIS) Collection 5.1 Aerosol Optical Depth (AOD) data, retrieved at 0.55 microns with spatial resolution of 10 km (MYD04). We focused on evaluating the ability of these two products to characterize both temporal and spatial distributions of aerosols within urban and suburban areas. Ground PM10 measurements were obtained from 73 of the Italian Regional Agency for Environmental Protection (ARPA) monitoring stations, spread across northern Italy, for a three-year period from 2010 to 2012. The Po Valley area (northern Italy) was chosen as the study domain because of severe urban air pollution, resulting from the highest population and industrial manufacturing density in the country, being located in a valley where two surrounding mountain chains favor the stagnation of pollutants. We found that the global correlations between PM10 and AOD are R(sup 2) = 0.83 and R(sup 2) = 0.44 for MYD04_L2 and for MAIAC, respectively, suggesting for a greater sensitiveness of the high-resolution product to small-scale deviations. However, the introduction of Relative Humidity (RH) and Planetary Boundary Layer (PBL) depth corrections gave a significant improvement to the PM AOD correlation, which led to similar performance: R(sup 2) = 0.96 for MODIS and R(sup 2) = 0.95 for MAIAC. Furthermore, the introduction of the PBL information in the corrected AOD values was found to be crucial in order to capture the clear seasonal cycle shown by measured PM10 values. The study allowed us to define four seasonal linear correlations that estimate PM10 concentrations satisfactorily from the remotely sensed MAIAC AOD retrieval. Overall, the results show that the high resolution provided by MAIAC retrieval data is much more relevant than 10km MODIS data to characterize PM10 in this region of Italy which has a pretty limited geographical domain, but a broad variety of land usages and consequent particulate concentrations.

MODIS↗

Statistical Modeling of Landscape Pattern and the Effects of Coarse Spatial Resolution

Analysis of classified satellite imagery was conducted to characterize errors in estimates of area based on coarse resolution satellite imagery which are due to distortions in sizes of small fragments, and to explore the feasibility of correcting for these errors using a statistical modeling approach. Sizes of bodies of open water on European Remote-Sensing (ERS-1) synthetic aperture radar (SAR) and fire scars on Landsat Multispectral Scanner (MSS) imagery were measured using geographic information system (GIS) software. Statistical analysis of the smaller scars and ponds as observed with this imagery of relatively fine resolution demonstrated that the distribution of the sizes could be modeled by either of two types of statistical distributions-a power distribution related to fractal processes or a simple exponential distribution. A comparison of the size distribution of small burn scars as observed with Landsat with the distribution observed with the much coarser Advanced Very High Resolution Radiometer (AVHRR) imagery revealed effects of coarse resolution, each of which were associated with a particular size range, and whose net effect accounted for the bias in total burn area due to coarse spatial resolution. Size dependent area correction procedures are therefore feasible. A statistical modeling approach to area estimation, based models of the underlying and observed size distributions of fragments in the scene, may lead to a procedure which requires little or no ancillary data.

Hlavka, C. A.↗

EBIC spectroscopy - A new approach to microscale characterization of deep levels in semi-insulating GaAs

The microscale characterization of electronic defects in (SI) GaAs has been a challenging issue in connection with materials problems encountered in GaAs IC technology. The main obstacle which limits the applicability of high resolution electron beam methods such as Electron Beam-Induced Current (EBIC) and cathodoluminescence (CL) is the low concentration of free carriers in semiinsulating (SI) GaAs. The present paper provides a new photo-EBIC characterization approach which combines the spectroscopic advantages of optical methods with the high spatial resolution and scanning capability of EBIC. A scanning electron microscope modified for electronic characterization studies is shown schematically. The instrument can operate in the standard SEM mode, in the EBIC modes (including photo-EBIC and thermally stimulated EBIC /TS-EBIC/), and in the cathodo-luminescence (CL) and scanning modes. Attention is given to the use of CL, Photo-EBIC, and TS-EBIC techniques.

Li, C.-J.↗

Multi-Sensors Observations of Pre-Earthquake Signals. What We Learned from the Great Tohoku Earthquake?

The lessons learned from the Great Tohoku EQ (Japan, 2011) will affect our future observations and an analysis is the main focus of this presentation. Multi-sensors observations and multidisciplinary research is presented in our study of the phenomena preceding major earthquakes Our approach is based on a systematic analysis of several physical and environmental parameters, which been reported by others in connections with earthquake processes: thermal infrared radiation; temperature; concentration of electrons in the ionosphere; radon/ion activities; and atmospheric temperature/humidity [Ouzounov et al, 2011]. We used the Lithosphere-Atmosphere-Ionosphere Coupling (LAIC) model, one of several possible paradigms [Pulinets and Ouzounov, 2011] to interpret our observations. We retrospectively analyzed the temporal and spatial variations of three different physical parameters characterizing the state of the atmosphere, ionosphere the ground surface several days before the March 11, 2011 M9 Tohoku earthquake Namely: (i) Outgoing Long wave Radiation (OLR) measured at the top of the atmosphere; (ii) Anomalous variations of ionospheric parameters revealed by multi-sensors observations; and (iii) The change in the foreshock sequence (rate, space and time); Our results show that on March 8th, 2011 a rapid increase of emitted infrared radiation was observed and an anomaly developed near the epicenter with largest value occurring on March 11 at 07.30 LT. The GPS/TEC data indicate an increase and variation in electron density reaching a maximum value on March 8. Starting from this day in the lower ionosphere there was also observed an abnormal TEC variation over the epicenter. From March 3 to 11 a large increase in electron concentration was recorded at all four Japanese ground-based ionosondes, which returned to normal after the main earthquake. We use the Japanese GPS network stations and method of Radio Tomography to study the spatiotemporal structure of ionospheric perturbations, and to distinguish ionospheric responses to processes of EQ preparation against the effects of other factors. The 2-D snapshots of the electron density over Japan showed abnormal increase over the maximum stress during the night, a few hours before the main shock. Our results from recording atmospheric and ionospheric conditions during the earthquake indicate the presence of anomalies in the atmosphere and ionospheres occurring consistently over regions of maximum stress near the epicenter. Due to their long duration (hours and days) and spatial appearance (only over the Sendai region) these results do not appear to be caused by meteorological or magnetic activity. They reveal the existence of atmospheric and ionospheric phenomena occurring prior to the earthquake, which indicates new evidence of a distinct coupling between the lithosphere and atmosphere/ionosphere. Similar results have been reported before the catastrophic events in Chile (M8.8, 2010), Italy (M6.3, 2009) and Sumatra (M9.3, 2004).

Ouzonounov, D.↗

Status of Aqua MODIS On-orbit Calibration and Characterization

The MODIS Flight Model 1 (FM1) has been in operation for more than two years since its launch onboard the NASA's Earth Observing System (EOS) Aqua spacecraft on May 4, 2002. The MODIS has 36 spectral bands: 20 reflective solar bands (RSB) with center wavelengths from 0.41 to 2.2 micron and 16 thermal emissive bands (TEB) from 3.7 to 14.5 micron. It provides the science community observations (data products) of the Earth's land, oceans, and atmosphere for a board range of applications. Its primary on-orbit calibration and characterization activities are performed using a solar diffuser (SD) and a solar diffuser stability monitor (SDSM) system for the RSB and a blackbody for the TEB. Another on-board calibrator (OBC) known as the spectro-radiometric calibration assembly (SRCA) is used for the instrument's spatial (TEB and RSB) and spectral (RSB only) characterization. We present in this paper the status of Aqua MODIS calibration and characterization during its first two years of on-orbit operation. Discussions will be focused on the calibration activities executed on-orbit in order to maintain and enhance the instrument's performance and the quality of its Level 1B (L1B) data products. We also provide comparisons between Aqua MODIS and Terra MODIS (launched in December, 1999), including their similarity and difference in response trending and optics degradation. Existing data and results show that Aqua MODIS bands 8 (0.412 micron) and 9 (0.443 micron) have much smaller degradation than Terra MODIS bands 8 and 9. The most noticeable feature shown in the RSB trending is that the mirror side differences in Aqua MODIS are extremely small and stable (<0.1%) while the Terra MODIS RSB trending has shown significant mirror side difference and wavelength dependent degradation. The overall stability of the Aqua MODIS TEB is also better than that of the Terra MODIS during their first two years of on-orbit operation.

Aqua↗

Development of Langmuir and Spatially Resolved OES Diagnostics for Arc Jet Shock and Boundary Layer Measurements Relevant to Atmospheric Re-Entry Environments

The second-generation miniature Arc Jet Research Chamber (mARC) ground testing facility at NASA Ames requires physical characterization of its supersonic plasma flow to verify numerical models and material sample testing. Two types of plasma diagnostics will be utilized: Langmuir probes and optical emission spectroscopy (OES). Several single and triple Langmuir probes have been constructed and will be inserted parallel to the flow via a sweep arm to measure post-shock electron temperature and number density along radial profiles at different axial distances. Due to the high heat flux (200-3000 W/cm2) sweep durations are necessarily short (< 0.1 s). Measuring these properties near the probe surface provide characterization of the post-shock environment. This is an important metric for validating coupled CFD-material codes, and will provide insight into longstanding thermocouple anomalies attributed to charging of heatshield surfaces. An OES system has also been assembled to obtain spatially resolved density and temperature for various flow species. The system consists of a convex lens that forms an image of the plasma onto a 16-channel linear fiber array, which will simultaneously capture the spectra from sixteen different locations. The light emission from the plasma is then focused by a spherical mirror into a spectrometer and recorded with a camera. These measurements non-intrusively provide a new spatially resolved flow characterization capability. This will initially be used to resolve issues with shock radiation interference in pyrometer measurements of material surface temperature. The design of each diagnostic and any initial results will be discussed.

Ethan Main-Loam Leong↗

The Joint Agency Commercial Imagery Evaluation (JACIE) Team: Overview and IKONOS Joint Characterization Approach

An overview of the Joint Agency Commercial Imagery Evalation (JACIE) team is presented. JACIE, composed of the National Aeronautics and Space Administration (NASA), the National Imagery and Mapping Agency (NIMA), and the U.S. Geological Survey (USGS), was formed to leverage government agencies' capabilities for the characterization of commercial remote sensing data. Each JACIE agency purchases, or plans to purchase, commercial imagery to support its research and applications. It is critical that the data be assessed for its accuracy and utility. Through JACIE, NASA, NIMA, and USGS jointly characterized image products from Space Imaging's IKONOS satellite. Each JACIE agency performed an aspect of the characterization based on its expertise. NASA and its university partners performed a system characterization focusing on radiometric calibration, geopositional accuracy, and spatial resolution assessment; NIMA performed image interpretability and feature extraction evaluations; and USGS assessed geopositional accuracy of several IKONOS products. The JACIE team purchased IKONOS imagery of several study sites to perform the assessments and presented results at an industry-government workshop. Future plans for JACIE include the characterization of DigitalGlobe's QuickBird-2 image products.

Zanoni, Vicki↗

The complex structural and chemical nature of monolithic U-10Mo fuel and Zr barrier layer

Nanoscale microstructural characterization by advanced transmission electron microscopy techniques on a U-10Mo/Zr barrier layer monolithic fuel plate was performed to evaluate the microstructural evaluation after high burn-up. Gas bubble superlattice evolution, grain restructuring, and evolution of the Zr interaction layer is investigated through detailed electron microscopy characterization. The use of automated crystallographic orientation mapping to irradiated U-10Mo fuel highlights that the restructured ultra-fine grains are separated by high angle grain boundaries at a burn up of 4.42 × 10 21 fissions/cm 3 . Additionally, advanced chemical analysis and multi-variable statistical analysis shows spatial clustering of solid fission product precipitates. Finally, characterization of a newly observed porous nanocrystalline Zr region in the barrier layer is studied. Finally, this work provides insights into the grain subdivision and restructuring process while using advanced microscopy techniques to analyze fission products in neutron-irradiated U-10Mo fuel.

36 MATERIALS SCIENCE↗

Investigating the Spatial and Temporal Limitations for Remote Sensing of Wildfire Smoke Using Satellite and Airborne Imagers During FIREX_AQ

Starting from point sources, wildfire smoke is important in the global aerosol system. The ability to characterize smoke near-source is key to modeling smoke dispersion and predicting air quality. With hemispheric views and 10-min refresh, imagers in Geostationary (GEO) orbit have advantages monitoring smoke over once-per-day sensors in low-earth orbit (LEO). However, both can be inadequate in capturing the characteristics of smoke plumes close to their sources due to too-coarse spatial resolution (both detector and product resolution), too-sparse temporal resolution (from LEO sensors), and too-conservative masking. In addition to satellite observations, the Fire Influence on Regional to Global Environments and Air Quality experiment offered sub-orbital enhanced-MODIS Airborne Simulator (eMAS) imagery at 50 m pixel resolution—including multiple eMAS flight tracks over individual fires in short time periods. It provided opportunity to explore smoke plume characterization at various spatial and temporal scales and quantify the limitations of space sensors for describing smoke magnitude near source as well as its temporal evolution. Here we applied modified aerosol algorithm to different imagers, relaxing its masking to estimate smoke's aerosol optical depth (AOD) as close as possible to its source. We found that GEO sensors with nominal 1 km spatial resolution can match the much finer resolution eMAS retrieved mean plume AOD, as long as the retrieval spatial resolution is finer than the width of the plumes. However, the plume's maximum AOD may be drastically underestimated by satellite products.

remote sensing↗

Spatiotemporal Coherence of Mean and Extreme Aerosol Particle Events over Eastern North America as Observed from Satellite

Quantifying spatiotemporal scales of coherence and variability of aerosol particle properties provides (i) metrics for evaluating observational data sets and model simulations, (ii) inferences regarding dominant causes of variability, and (iii) information that is necessary to determine their climate forcing and air quality impacts. Accordingly, analyses of columnar aerosol optical depth (AOD) and Ångstrom exponent (AE) from the MODerate resolution Imaging Spectroradiometer (MODIS) on the Aqua and Terra satellites, and AErosol RObotic NETwork (AERONET) stations are used to evaluate the spatially averaged (Level-3) MODIS products, and to characterize the spatiotemporal scales of variability (and coherence) of aerosol particles over eastern North America (2000-2013). Results show a high degree of consistency in AOD retrievals from the different data sets but larger discrepancies in AE estimates, highest mean AOD and lowest day-to-day variability during the summer, and largest scales of spatial coherence in summer and fall. Consistent with the scales of spatial coherence from MODIS data, in both data sets power spectra indicate AOD variability is manifest primarily on synoptic and annual time scales. Conversely, AE variability in MODIS data is primarily focused on seasonal, semiannual, and annual time scales, and there is an additional mode of AE variability at approx. 30 days in the AERONET measurements. The frequency of cooccurrence of extreme AOD values (>local 90th percentile) decreases to below 50% at approx. 150 km from a central grid cell, but is above that expected by random chance over almost all of eastern North America, indicating supra-regional scale extreme events.

MODIS↗

Detection and Signal Processing for Near-Field Nanoscale Fourier Transform Infrared Spectroscopy

Researchers from a broad spectrum of scientific and engineering disciplines are increasingly using scattering-type near-field infrared spectroscopic techniques to characterize materials non-destructively with nanoscale spatial resolution. However, a sub-optimal understanding of a technique's implementation can complicate data interpretation and act as a barrier to entering the field. Here the key detection and processing steps involved in producing scattering-type near-field nanoscale Fourier transform infrared spectra (nano-FTIR) are outlined. The self-contained mathematical and experimental work derives and explains: i) how normalized complex-valued nano-FTIR spectra are generated, ii) why the real and imaginary components of spectra qualitatively relate to dispersion and absorption respectively, iii) a new and generally valid equation for spectra which can be used as a springboard for additional modeling of the scattering processes, and iv) an algebraic expression that can be used to extract an approximation to the sample's local extinction coefficient from nano-FTIR. The algebraic model for weak oscillators is validated with nano-FTIR and attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectra on samples of polystyrene and Kapton and further provides a pedagogical pathway to cementing some of the technique's key qualitative attributes.

36 MATERIALS SCIENCE↗

NanoSIP: NanoSIMS Applications for Microbial Biology

High-resolution imaging with secondary ion mass spectrometry (nanoSIMS) has become a standard method in systems biology and environmental biogeochemistry and is broadly used to decipher ecophysiological traits of environmental microorganisms, metabolic processes in plant and animal tissues, and cross-kingdom symbioses. When combined with stable isotope-labeling—an approach we refer to as nanoSIP—nanoSIMS imaging offers a distinctive means to quantify net assimilation rates and stoichiometry of individual cell-sized particles in both low- and high-complexity environments. While the majority of nanoSIP studies in environmental and microbial biology have focused on nitrogen and carbon metabolism (using 15 N and 13 C tracers), multiple advances have pushed the capabilities of this approach in the past decade. The development of a high-brightness oxygen ion source has enabled high-resolution metal analyses that are easier to perform, allowing quantification of metal distribution in cells and environmental particles. New preparation methods, tools for automated data extraction from large data sets, and analytical approaches that push the limits of sensitivity and spatial resolution have allowed for more robust characterization of populations ranging from marine archaea to fungi and viruses. Further, NanoSIMS studies continue to be enhanced by correlation with orthogonal imaging and ‘omics approaches; when linked to molecular visualization methods, such as in situ hybridization and antibody labeling, these techniques enable in situ function to be linked to microbial identity and gene expression. Here we present an updated description of the primary materials, methods, and calculations used for nanoSIP, with an emphasis on recent advances in nanoSIMS applications, key methodological steps, and potential pitfalls.

07 ISOTOPE AND RADIATION SOURCES↗

Emerging Per- and Polyfluoroalkyl Substances in Tap Water from the American Healthy Homes Survey II

Humans experience widespread exposure to anthropogenic per- and polyfluoroalkyl substances (PFAS) through various media, which can lead to a wide range of negative health impacts. Tap water is an important source of exposure in communities with any degree of contamination but routine or large-scale PFAS monitoring often depends on targeted analytical methods limited to measuring specific PFAS. We analyzed 680 tap water samples from the American Healthy Homes Survey II for PFAS using non-targeted analysis (NTA) to expand the range of detectable PFAS. Based on detection frequency and relative abundance, about half of the identified PFAS were found only by NTA. We identified (with varying degrees of confidence) 75 distinct PFAS, including 57 exclusively detected by NTA. The identified PFAS are members of seven structural subclasses differentiated by their head groups and degree of fluorination. Clustering analysis categorized the PFAS into four coabundance groups dominated by specific PFAS subclasses. One group uniquely identified by NTA contains zwitterionic PFAS and other PFAS transformation products which are likely associated with aqueous firefighting foam contaminants in a small number of spatially correlated samples. These results help further characterize the scope of exposure to emerging PFAS experienced by the U.S. population via tap water and augment nationwide targeted-PFAS monitoring programs.

63 RADIATION, THERMAL, AND OTHER ENVIRON. POLLUTAN↗

Ferroelectric Self-Polarization Controlled Magnetic Stratification and Magnetic Coupling in Ultrathin La 0.67 Sr 0.33 MnO 3 Films

Multiferroic oxide heterostructures consisting of ferromagnetic and ferroelectric components hold the promise for nonvolatile magnetic control via ferroelectric polarization, advantageous for the low-dissipation spintronics. Modern understanding of the magnetoelectric coupling in these systems involves structural, orbital, and magnetic reconstructions at interfaces. Previous works have long proposed polarization-dependent interfacial magnetic structures; however, direct evidence is still missing, which requires advanced characterization tools with near-atomic-scale spatial resolutions. Here, extensive polarized neutron reflectometry (PNR) studies have determined the magnetic depth profiles of PbZr 0.2 Ti 0.8 O 3 /La 0.67 Sr 0.33 MnO 3 (PZT/LSMO) bilayers with opposite self-polarizations. When the LSMO is 2–3 nm thick, the bilayers show two magnetic transitions on cooling. However, temperature-dependent magnetization is different below the lower-temperature transition for opposite polarizations. PNR finds that the LSMO splits into two magnetic sublayers, but the inter-sublayer magnetic couplings are of opposite signs for the two polarizations. Near-edge X-ray absorption spectroscopy further shows contrasts in both the Mn valences and the Mn–O bond anisotropy between the two polarizations. Finally, this work completes the puzzle for the magnetoelectric coupling model at the PZT/LSMO interface, showing a synergic interplay among multiple degrees of freedom toward emergent functionalities at complex oxide interfaces.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Helium in Stream Water as a Volcanic Monitoring Tool

Abstract We show that synoptic sampling of streams can be used to characterize volcanic volatiles in groundwater over large spatial scales. Synoptic sampling of dissolved noble gases, 222 Rn, major ions, and stream discharge was carried out along a 30 km reach of the Gibbon River, near Norris Geyser Basin in Yellowstone National Park, USA. Groundwater discharge location, volume, and composition were estimated by constrained calibration of a stream flow and solute transport model. Estimated groundwater composition from stream modeling was compared to shallow groundwater concentrations measured in nearby springs. 3 He, 222 Rn, and Cl signatures in the Gibbon River are indicative of groundwater discharge with a volcanic signature along the study reach. Stream water noble gas isotopic composition has similar isotopic mixing patterns to springs. The model‐estimated composition of groundwater discharging to the Gibbon agrees well with observed groundwater composition from nearby springs for all modeled analytes. We present the first observations of elevated mantle helium in stream water and show that stream water can be used as a convenient collection point to estimate spatially distributed groundwater composition and to monitor changes in volatile flux over large spatial areas. These results offer the possibility that stream surveys in volcanic terrain could be a new method for distributed volcanic monitoring at the catchment scale and beyond.

Gardner, W. Payton↗