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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 37 records · Page 2

Grain Boundary Plane Measurement Using Transmission Electron Microscopy Automated Crystallographic Orientation Mapping for Atom Probe Tomography Specimens

Abstract Grain boundaries are critical in determining the properties of materials, including mechanical stability, conductivity, and corrosion resistance. The specific properties of materials depend not only on the misorientation of the crystals, the three most commonly characterized parameters, but also on the angle of the grain boundary plane between the two crystals, the final two parameters in the five-parameter macroscopic description of the grain boundary. The method presented here allows for the direct measurement of all five parameters of the grain boundary in a transmission electron microscopy specimen of various morphologies. This is especially applicable to atom probe specimens, where only a single-tilt axis is generally available, allowing the crystallographic description to be matched to the detailed chemical data available in the atom probe tomography. This method provides a platform for efficient grain boundary analysis in unique samples, saving operator time and allowing for ease of acquisition and interpretation in comparison with traditional electron diffraction methods.

Materials Science↗

The Digital Mirror Langmuir Probe: Field Programmable Gate Array Implementation of Real-Time Langmuir Probe Biasing

High bandwidth, high spatial resolution measurements of electron temperature, density and plasma potential are valuable for resolving turbulence in the boundary plasma of tokamaks. While conventional Langmuir probes can provide such measurements either their temporal or spatial resolution is limited: the former by the sweep rate necessary for obtaining I-V characteristics and the latter by the need to use multiple electrodes, as is the case in triple and double probe configurations. The Mirror Langmuir Probe (MLP) bias technique overcomes these limitations by rapidly switching the voltage on a single electrode cycling between three bias states, each dynamically optimised for the local plasma conditions. The MLP system on Alcator C-Mod used analog circuitry to perform this function, measuring Te, VF, and Isat at 1.1 MSPS. Recently, a new prototype digital MLP controller has been implemented on a Red Pitaya Field Programmable Gate Array (FPGA) board which reproduces the functionality of the original controller and performs all data acquisition. There is also the potential to provide the plasma parameters externally for use with feedback control systems. The use of FPGA technology means the system is readily customisable at a fraction of the development time and implementation cost. A second Red Pitaya was used to test the MLP by simulating the current response of a physical probe using C-Mod experimental measurements. This project is available as a git repository to facilitate extensibility (e.g. real-time control outputs, more voltage states) and scalability through collaboration.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Flight calibration of compensated and uncompensated pitot-static airspeed probes and application of the probes to supersonic cruise vehicles

Static pressure position error calibrations for a compensated and an uncompensated XB-70 nose boom pitot static probe were obtained in flight. The methods (Pacer, acceleration-deceleration, and total temperature) used to obtain the position errors over a Mach number range from 0.5 to 3.0 and an altitude range from 25,000 feet to 70,000 feet are discussed. The error calibrations are compared with the position error determined from wind tunnel tests, theoretical analysis, and a standard NACA pitot static probe. Factors which influence position errors, such as angle of attack, Reynolds number, probe tip geometry, static orifice location, and probe shape, are discussed. Also included are examples showing how the uncertainties caused by position errors can affect the inlet controls and vertical altitude separation of a supersonic transport.

Webb, L. D.↗

Thermal design and development of a planetary probe - Pioneer Venus large probe

The thermal control system developed for the Large Atmospheric Probe of the Pioneer Venus Multiprobe Mission is described. The scope of the thermal control task requires maintaining the probe internal equipment shelf temperatures within a nonoperating range of -40 to 122 F and an operating range of -4 to 122 F during three different mission phases: (1) preseparation, the transit phase of the mission when the probe is attached to the Multiprobe Spacecraft Bus, (2) postseparation, the free-flight cruise phase of the mission following release from the Bus, and (3) descent, the phase of the mission from preentry equipment turn-on to impact on the Venus surface. Thermal control for these phases is achieved by a combination of passive thermal finishes on the probe exterior surfaces and heaters mounted on the equipment shelves. Verification of the adequacy of the total thermal design to meet all mission requirements has been completed.

Hennis, L. A.↗

Outer Planets/Solar Probe Project: Solar Probe

Solar Probe, the first mission to the Sun and the third of three missions in NASA's Outer Solar System/Solar Probe Program, is a voyage of exploration, discovery, and comprehension. This near-Sun flyby will provide in situ measurements in the solar corona and high-resolution pictures and magnetograms of the photosphere and polar atmosphere. These measurements are also needed as "ground truth" for interpreting the many measurements of the Sun and solar activity that have been made from a distance of 1 AU. Solar Probe is scheduled for launch in February 2007. It will arrive at the Sun along a polar trajectory perpendicular to the Sun-Earth line with a perihelion of 4 solar radii (R(sub s)) from the Sun's center. Two perihelion passages will occur, the first in 2010 (near solar sunspot maximum) and the second in 2015 (near solar minimum) ensuring measurement of both coronal hole and streamer-related solar wind properties. To reach the Sun, probe must first fly to Jupiter and use a gravity assist to lose its angular momentum about the Sun. The imaging and in situ miniaturized instruments will provide the first 3-dimensional view of the corona, high spatial- and temporal-resolutions of the magnetic fields, and helioseismic measurements of the polar regions, as well as sporadic high-spatial-resolution local sampling of plasmas and fields at all latitudes.

Tsurutani, B. T.↗

Multiple Deep Jovian Atmospheric Entry Probes: Building on the Galileo Probe

Following on the very successful Galileo Entry Probe mission, studies underway at the Jet Propulsion Laboratory (JPL) address the feasibility and cost of the Jupiter Deep Multi-probes (JDMP) mission to deliver and support multiple deep (100 bar level or deeper) atmospheric entry probes to Jupiter.

JPL Galileo Entry Probe Mission Jupiter Deep Multi↗

Pioneer Jupiter orbiter probe mission 1980, probe description

The adaptation of the Saturn-Uranus Atmospheric Entry Probe (SUAEP) to a Jupiter entry probe is summarized. This report is extracted from a comprehensive study of Jovian missions, atmospheric model definitions and probe subsystem alternatives.

Defrees, R. E.↗

The Subsurface Ice Probe (SIPR): A Low-Power Thermal Probe for the Martian Polar Layered Deposits

The distinctive layering visible in images from Mars Global Surveyor of the Martian polar caps, and particularly in the north polar cap, indicates that the stratigraphy of these polar layered deposits may hold a record of Martian climate history covering millions of years. On Earth, ice sheets are cored to retrieve a pristine record of the physical and chemical properties of the ice at depth, and then studied in exacting detail in the laboratory. On the Martian north polar cap, coring is probably not a practical method for implementation in an autonomous lander. As an alternative, thermal probes that drill by melting into the ice are feasible for autonomous operation, and are capable of reasonable approximations to the scientific investigations performed on terrestrial cores, while removing meltwater to the surface for analysis. The Subsurface Ice Probe (SIPR) is such a probe under development at JPL. To explore the dominant climate cycles, it is postulated that tens of meters of depth should be profiled, as this corresponds to the vertical separation of the major layers visible in the MOC images [1]. Optical and spectroscopic analysis of the layers, presumably demarcated by embedded dust and possibly by changes in the ice properties, would contribute to the construction of a chronology. Meltwater analysis may be used to determine the soluble chemistry of the embedded dust, and to monitor gradients of atmospheric gases, particularly hydrogen and oxygen, and isotopic variations that reflect atmospheric conditions at the time the layer was deposited. Thermal measurements can be used to determine the geothermal gradient and the bulk mechanical properties of the ice.

Cardell, G.↗

Combined Impedance Probe and Langmuir Probe Studies of the Low-Latitude E Region

The EQUIS-2 sounding rocket and radar campaign, launched from Kwajalein Atoll in 2004, included a mission to study low-latitude irregularities and electrodynamics, led by NASA GSFC. This mission included two instrumented rockets launched into the nighttime E region (apogee near 120 km), which included comprehensive electrodynamics and neutral density instrumentation. These rockets carried the first of a new generation of impedance probes, that utilize a wide-band drive signal to simultaneously measure the impedance of an antenna in a plasma as a function of frequency from 7 kEIz to 4 MHz. at a rapid cadence. This technique promises to permit true plasma spectroscopy, and resulted in the identification of multiple plasma resonances and accurate measurements of the plasma density, even in the low density nighttime E region. We present analyses of the technique and resulting spectra, and show how these data may be combined with fixed-bias Langmuir Probe data to infer the temperature structure of the E region as well as providing accurate absolute calibrations for the very high time resolution fixed-bias probe data. The data is shown to agree well with data from ionosonde, the ALTAIR radar, and the Peruvian beacon experiment.

Rowland, D. E.↗

Correlating Nanoscale Secondary Ion Mass Spectrometry and Atom Probe Tomography Analysis of Uranium Enrichment in Metallic Nuclear Fuel

Distribution and enrichment of 235U within nuclear fuels are essential to material performance and reactor safety. With the development of metallic U fuels, understanding 235U homogeneity has become increasingly important, however, it is difficult to map with high spatial, and mass resolution to analyze both matrix and secondary phase precipitates. Here, we analyze 235U enrichment in matrix and carbide phases in LEU-Mo via two chemical imaging modalities: nanoscale secondary ion mass spectrometry (nanoSIMS) and atom probe tomography (APT). NanoSIMS and APT provided consistent results, with no statistically significant difference between measured and nominal enrichment (19.75 % 235U).

U-10Mo, atom probe tomography, nanoscale secondary↗

Probing Heterogeneity in Bovine Enamel Composition through Nanoscale Chemical Imaging using Atom Probe Tomography

Objective: The aim of this study was to determine the heterogeneity in chemical composition of bovine enamel using atom probe tomography, and thereby evaluate the suitability of bovine enamel as a substitute for human enamel in in vitro dental research. Design: Enamel samples from extracted bovine incisor teeth were first sectioned using a diamond saw and then milled into needle-like samples (<100 nm diameter) by focused ion beam (FIB) coupled with a scanning electron microscope (SEM). The samples were then analyzed in the atom probe to acquire three-dimensional (3D) images and quantify the atomic chemistry and distribution in bovine enamel. Results: For the first time, the atomic-level composition and clustering of major constituents and impurities within bovine enamel were determined and imaged. We discovered that the chemical composition of bovine enamel is spatially inhomogeneous at the atomic scale. The average bulk Ca/P ratio, ~1.4, was in agreement with previously reported literature values from alternative conventional methods. When assessed locally at the atomic scale, the Ca/P ratio varied between 1.1 and 2.03. We also discovered that the Mg impurities were significantly segregated throughout the enamel, and such clustering influenced the variation of Ca/P ratios. The increase in Mg concentrations, near the Mg clusters, correlated with increased Ca and decreased P concentrations. Conclusion: In conclusion, the presented findings of variability in local composition should be taken into account when interpreting dental research results from bovine enamel.

59 BASIC BIOLOGICAL SCIENCES↗

Probing Local Optical Fields via Ultralow Frequency Raman Scattering from a Corrugated Probe

Here we revisit nanoscale local optical field imaging via tip-enhanced Raman scattering (TERS). Rather than taking advantage of molecular reporters to probe different aspects of the local fields, we show how ultralow frequency Raman (ULF) scattering from the (nano-corrugated) metallic probe itself can be used for the same purpose. The bright ULF-TERS response we record allows non-invasive (tapping mode feedback) local field imaging, enables visualizing the local fields of small (down to 20 nm) isolated plasmonic particles, and can also be exploited to distinguish between Si and SiO2 domains with 5 nm spatial resolution. We describe our approach and its limitations, particularly when it comes to using all-metallic vs molecular reporters.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

In Situ Probing Potassium-ion Intercalation-induced Amorphization in Crystalline Iron Phosphate Cathode Materials

Na-ion and K-ion batteries are promising alternatives for large-scale energy storage applications due to their abundance and low cost. Intercalation of these large ions could cause irreversible structural deformation and partial to complete amorphization in the crystalline electrodes. The designing of new amorphous electrodes is another route to develop electrodes to store these ions reversibly. Lack of understanding of dynamic changes in the amorphous nanostructures during battery operation is the bottleneck for further developments. Here, we report the utilization of in situ digital image correlation and in-operando X-ray diffraction (XRD) techniques to probe dynamic changes in the amorphous phase of iron phosphate during potassium intercalation. In-operando XRD demonstrates amorphization in the electrode’s nanostructure during the first charge/discharge cycle. Additionally, the ex-situ high-resolution transmission electron microscopy further confirms the amorphization after potassium insertion. In situ strain analysis detects the reversible deformation associated with redox reactions in the amorphous phases. Our approach offers new insights on the mechanisms of ion intercalation in the amorphous nanostructures which are highly potent for development of next-generation batteries.

Ozdogru, Bertan↗

Probing sulphur clusters in a microfluidic electrochemical cell with synchrotron-based photoionization mass spectrometry

We present synchrotron-based mass spectrometry to probe products formed in the lithium sulphide electrolyte. In operando analysis was obtained at two different potentials in a vacuum compatible microfluidic electrochemical cell. Mass spectral observations show that the charged electrolyte formed sulfur clusters under dynamic conditions, demonstrating electrolyte electron shuttling.

sulphur cluster, lithium – sulphur battery electro↗

Development of the materials analysis and particle probe for Proto-MPEX

The Prototype Material Plasma Exposure eXperiment (Proto-MPEX) is a linear plasma device being used in plasma source research and development (R&D) for the proposed MPEX. Once the R&D is completed, this device can also be used to perform plasma–material interaction studies. To perform these studies, a new materials analysis and particle probe (MAPP) has been constructed. The MAPP’s components are a sample holder and manipulator and a custom vacuum chamber with ports to facilitate surface chemistry diagnostics. The MAPP’s overall design enables rapid sample turnaround and in vacuo surface characterization. The surface analysis vacuum chamber has ports for x-ray photoelectron spectroscopy, thermal desorption spectroscopy, back-scatter ion scattering spectroscopy, forward-scatter ion scattering spectroscopy, and direct recoil spectroscopy. The sample manipulator and holder is a Lesker/UHV Multi-Centre Analytical Stage, which is used to place the samples in the exposure region of the Proto-MPEX or the analysis position in the MAPP vacuum chamber. The sample holder has a heating capability of up to 1200 °C for heated exposure and for desorption studies. In this work, we present the MAPP’s design and the first tungsten sample exposure with ex situ analysis that shows a surface deposition layer on the exposed target, highlighting the need for additional in situ measurements on the Proto-MPEX.

Beers, C. J. (ORCID:0000000150985459)↗

Ultrafast x-ray pump x-ray probe transient absorption spectroscopy: A computational study and proposed experiment probing core-valence electronic correlations in solvated complexes

Femtosecond X-ray pump X-ray probe experiments are currently possible at free electron lasers such as the linac coherent light source (LCLS), which opens new opportunities for studying solvated transition metal-ligand complexes. In order to make the most effective use of these kinds of experiments, it is necessary to determine which chemical properties an X-ray pump pulse will measure. In this paper, we have combined electron cascade calculations and excited-state time-dependent density functional theory calculations to predict the initial state prepared by an X-ray pump and the subsequent X-ray probe spectra at the Fe K-edge in the solvated model transition metal complex, K 4 Fe II (CN) 6 . We find several key spectral features that report on the ligand-field splitting, solvent-solute interactions, and the 3p and 3d electron interactions. We then show how these features could be measured in an experiment.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Probing the electronic properties of the electrified silicon/water interface by combining simulations and experiments.

Silicon (Si) is broadly used in electrochemical and photoelectrochemical devices, where the capacitive and Faradaic reactions at the Si/water interfaces are critical for signal transduction or noise generation. However, probing the electrified Si/water interface at the microscopic level remains a challenging task. Here we focus on hydrogenated Si surfaces in contact with water, relevant to transient electronics and photoelectrochemical modulation of biological cells and tissues. We show that by carrying out first principles molecular dynamics simulations of the Si(100)/water interface in the presence of an electric field we can realistically correlate the computed flat-band potential and tunneling current images at the interface with experimentally measured capacitive and Faradaic currents. Specifically, we validate our simulations in the presence of bias by performing pulsed chronoamperometry measurements on Si wafers in solution. Consistent with prior experiments, our measurements and simulations indicate the presence of voltage-dependent capacitive currents at the interface. We also find that Faradaic currents are weakly dependent on the applied bias, which we relate to surface defects present in newly prepared samples.

Ye, Zifan↗