Sensitivity and Figure of Merit Measurements of EELS vs XEDS in the Analytical Electron Microscope
Abstract not provided.
47 OTHER INSTRUMENTATION↗
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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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Identification of engine oil-derived ash nanoparticles and ash formation process for a gasoline direct-injection engine
Engine oil-derived ash particles emitted from internal combustion (IC) engines are unwanted by-products, after oil is involved in in-cylinder combustion process. Since they typically come out together with particulate emissions, no detail has been reported about their early-stage particles other than agglomerated particles loaded on aftertreatment catalysts and filters. To better understand ash formation process during the combustion process, here differently formulated engine oils were dosed into a fuel system of a gasoline direct injection (GDI) engine that produces low soot mass emissions at normal operating conditions to increase the chances to find stand-alone ash particles separated from soot aggregates in the sub-20-nm size range. In addition to them, ash/soot aggregates in the larger size range were examined using scanning transmission electron microscopy (STEM)-X-ray electron dispersive spectroscopy (XEDS) to present elemental information at different sizes of particles from various oil formulations. The STEM-XEDS results showed that regardless of formulated oil type and particle size, Ca, P and C were always contained, while Zn was occasionally found on relatively large particles, suggesting that these elements get together from an early stage of particle formation. The S, Ca and P K-edge X-ray absorption near edge structure (XANES) analyses were performed for bulk soot containing raw ash. The linear combination approach & cross-checking among XANES results proposed that Ca 5 (OH)(PO 4 ) 2 , Ca 3 (PO 4 ) 2 and Zn 3 (PO 4 ) 2 are potentially major chemical compounds in raw ash particles, when combined with the STEM-XEDS results. Despite many reports that CaSO 4 is a major ash chemical when ash found in DPF/GFP systems was examined, it was observed to be rarely present in raw ashes using the S K-edge XANES analysis, suggesting ash transformation.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Transmission Electron Microscopy Study on the Effect of Thermal and Electrical Stimuli on Ge2Te3 Based Memristor Devices
Memristor devices fabricated using the chalcogenide Ge 2 Te 3 phase change thin films in a metal-insulator-metal structure are characterized using thermal and electrical stimuli in this study. Once the thermal and electrical stimuli are applied, cross-sectional transmission electron microscopy (TEM) and X-ray energy-dispersive spectroscopy (XEDS) analyses are performed to determine structural and compositional changes in the devices. Electrical measurements on these devices showed a need for increasing compliance current between cycles to initiate switching from low resistance state (LRS) to high resistance state (HRS). The measured resistance in HRS also exhibited a steady decrease with increase in the compliance current. High resolution TEM studies on devices in HRS showed the presence of residual crystalline phase at the top-electrode/dielectric interface, which may explain the observed dependence on compliance current. XEDS study revealed diffusion related processes at dielectric-electrode interface characterized, by the separation of Ge 2 Te 3 into Ge- and Te- enriched interfacial layers. This was also accompanied by spikes in O level at these regions. Furthermore, in-situ heating experiments on as-grown thin films revealed a deleterious effect of Ti adhesive layer, wherein the in-diffusion of Ti leads to further degradation of the dielectric layer. This experimental physics-based study shows that the large HRS/LRS ratio below the current compliance limit of 1 mA and the ability to control the HRS and LRS by varying the compliance current are attractive for memristor and neuromorphic computing applications.
Shallcross, Austin↗
Characterization of Properties of Laser Powder Bed Fusion 3D-Printed Inconel 718 for Centrifugal Turbomachinery Applications
Here, this paper presents the results of a comprehensive effort to characterize the properties of Inconel 718 produced by a form of laser powder bed fusion (LPBF) additive manufacturing (AM) or 3D-printing, subsequently subjected to hot isostatic pressing (HIP) and heat treatment according to standards F3055-14a and AMS 5663, respectively. Material property data, while broadly available for traditional Inconel 718 presentations (e.g. forgings or castings), is currently lacking for the 3D-printed material. It is expected that while limited in size, the experimental data sets presented provide sufficient information to glean the capability of LPBF Inconel 718. These include: 1) Chemical composition, electron backscatter diffraction (EBSD), and x-ray energy dispersive spectroscopy (XEDS) characterization of 3D-printed material structure; 2) Tensile properties — 0.2% yield stress, ultimate stress, modulus of elasticity, and elongation to failure — based on 108 samples, as functions of temperature and sample print orientation; 3) Creep rupture data including the Larson-Miller parameter, based on 21 samples; and 4) High cycle fatigue data based on 21 samples as a function of temperature. Results are compared to available standards and/or data for forged, cast, and other AM Inconel 718. A key observation of this study, based on the EBSD results, is that while the material appears to approach full recrystallization following heat treatment, there is a detectable fraction of the material that does not fully recrystallize, resulting in a material with mechanical properties (e.g. yield stress, creep rupture) measurably lower than those of forgings, but higher than those of castings.
30 DIRECT ENERGY CONVERSION↗
Structural Characterization of the Platinum Nanoparticle Hydrogen-Evolving Catalyst Assembled on Photosystem I by Light-Driven Chemistry
Directed assembly of abiotic catalysts onto biological redox protein frameworks is of interest as an approach for the synthesis of biohybrid catalysts that combine features of both synthetic and biological materials. In this report, we provide a multiscale characterization of the platinum nanoparticle (NP) hydrogen-evolving catalysts that are assembled by light-driven reductive precipitation of platinum from an aqueous salt solution onto the photosystem I protein (PSI), isolated from cyanobacteria as trimeric PSI. The resulting PSI-NP assemblies were analyzed using a combination of X-ray energy-dispersive spectroscopy (XEDS), high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM), small-angle X-ray scattering (SAXS), and high-energy X-ray scattering with atomic pair distribution function (PDF) analyses. The results show that the PSI-supported NPs are approximately 1.8 nm diameter disk-shaped particles that assemble at discrete sites with 145 Å separation. This separation is too large to be consistent with NP nucleation and growth at a site adjacent to the F B cofactor site. Instead, we suggest a mechanism for NP growth at hydrophobic sites on the PSI stromal surface. The NPs photoreductively assembled on the PSI stromal surface are found to be analogous to the nanostructures produced by successive cycles of atomic layer deposition (ALD) of platinum onto 40 nm porous anodic alumina oxide supports, although the mechanisms for nucleation appear to differ. In conclusion, this work establishes a foundation for the investigation of the reductive assembly of abiotic metal catalysts at sites connected to photochemically reducing equivalent production in PSI.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Applications of analytical electron microscopy to guide the design of boron carbide
Compositional analysis of boron carbide on nanometer length scales to examine or interpret atomic mechanisms, for example, solid-state amorphization or grain-boundary segregation, is challenging. This work reviews advancements in high-resolution microanalysis to characterize multiple generations of boron carbide. First, ζ-factor microanalysis will be introduced as a powerful (scanning) transmission electron microscopy ((S)TEM) analytical framework to accurately characterize boron carbide. Three case studies involving the application of ζ-factor microanalysis will then be presented: (1) accurate stoichiometry determination of B-doped boron carbide using ζ-factor microanalysis and electron energy loss spectroscopy, (2) normalized quantification of silicon grain-boundary segregation in Si-doped boron carbide, and (3) calibration of a scanning electron microscope X-ray energy-dispersive spectroscopy (XEDS) system to measure compositional homogeneity differences of B/Si-doped arc-melted boron carbides in the as-melted and annealed conditions. Overall, the improvement and application of advanced analytical tools have helped better understand processing–microstructure–property relationships and successfully manufacture high-performance ceramics.
36 MATERIALS SCIENCE↗
Searching for Axion-like Particles at DarkQuest
Axion-like particles (ALPs) interacting with photons can be abundantly produced in proton xed target experiments. Once produced, they can travel a macroscopic distance before decaying into photons. We study the sensitivity of the proposed DarkQuest experiment at Fermilab to this signature. We show that the proposed upgrade to install an electromagnetic calorimeter will enable DarkQuest to explore untested parameter space by searching for the displaced decays of ALPs.
72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
Rayleigh-Sommerfield Diffraction vs Fresnel-Kirchhoff, Fourier Propagation and Poisson's Spot
The boundary conditions imposed on the diffraction problem in order to obtain the Fresnel-Kirchhoff (FK) solution are well-known to be mathematically inconsistent and to be violated by the solution when the observation point is close to the diffracting screen 1-3. These problems are absent in the Rayleigh-Sommerfeld (RS) solution. The difference between RS and FK is in the inclination factor and is usually immaterial because the inclination factor is approximated by unity. But when this approximation is not valid, FK can lead to unacceptable answers. Calculating the on-axis intensity of Poisson s spot provides a critical test, a test passed by RS and failed by FK. FK fails because (a) convergence of the integral depends on how it is evaluated and (b) when the convergence problem is xed, the predicted amplitude at points near the obscuring disk is not consistent with the assumed boundary conditions.
RS (RAYLEIGH SOMMERFELD)↗
Investigation of Synthetic Mg(1.3)V(1.7)O4 Spinel with MgO Inclusions: Case Study of a Spinel with an Apparently occupied Interstitial Site
A magnesium vanadate spinel crystal, ideally MgV2O4, synthesized at 1 bar, 1200 C and equilibrated under FMQ + 1.3 log f(sub o2) condition, was investigated using single-crystal X-ray diffraction, electron microprobe, and electron backscatter (EBSD). The initial X-ray structure refinements gave tetrahedral and octahedral site occupancies, along with the presence of 0.053 apfu Mg at an interstitial octahedral site . Back-scattered electron (BSE) images and electron microprobe analyses revealed the existence of an Mg-rich phase in the spinel matrix, which was too small (less than or equal to 3microns) for an accurate chemical determination. The EBSD analysis combined with X-ray energy dispersive spectroscop[y (XEDS) suggested that the Mg-rich inclusions are periclase oriented coherently with the spinel matrix. The final structure refinements were optimized by subtracting the X-ray intensity contributions (approx. 9%) of periclase reflections, which eliminated the interstitial Mg. This study provides insight into possible origins of refined interstitial cations reported in the the literature for spinel, and points to the difficulty of using only X-ray diffraction data to distinguish a spinel with interstitial cations from one with coherently oriented MgO inclusions.
Uchida, Hinako↗
The Fixed-bias Langmuir Probe on the Communication-navigation Outage Forecast System Satellite: Calibration and Validation
A fixed-bias spherical Langmuir probe is included as part of the Vector Electric Field Instrument (VEFI) suite on the Communication Navigation Outage Forecast System (CNOFS) satellite.CNOFS gathers data in the equatorial ionosphere between 400 and 860 km, where the primary constituent ions are H+ and O+. The ion current collected by the probe surface per unit plasmadensity is found to be a strong function of ion composition. The calibration of the collected current to an absolute density is discussed, and the performance of the spherical probe is compared to other in situ instruments on board the CNOFS satellite. The application of the calibration is discussed with respect to future xed-bias probes; in particular, it is demonstrated that some density fluctuations will be suppressed in the collected current if the plasma composition rapidly changes along with density. This is illustrated in the observation of plasma density enhancements on CNOFS.
VEFI↗
Preparation and Integration of ALHAT Precision Landing Technology for Morpheus Flight Testing
The Autonomous precision Landing and Hazard Avoidance Technology (ALHAT) project has developed a suite of prototype sensors for enabling autonomous and safe precision land- ing of robotic or crewed vehicles on solid solar bodies under varying terrain lighting condi- tions. The sensors include a Lidar-based Hazard Detection System (HDS), a multipurpose Navigation Doppler Lidar (NDL), and a long-range Laser Altimeter (LAlt). Preparation for terrestrial ight testing of ALHAT onboard the Morpheus free- ying, rocket-propelled ight test vehicle has been in progress since 2012, with ight tests over a lunar-like ter- rain eld occurring in Spring 2014. Signi cant work e orts within both the ALHAT and Morpheus projects has been required in the preparation of the sensors, vehicle, and test facilities for interfacing, integrating and verifying overall system performance to ensure readiness for ight testing. The ALHAT sensors have undergone numerous stand-alone sensor tests, simulations, and calibrations, along with integrated-system tests in special- ized gantries, trucks, helicopters and xed-wing aircraft. A lunar-like terrain environment was constructed for ALHAT system testing during Morpheus ights, and vibration and thermal testing of the ALHAT sensors was performed based on Morpheus ights prior to ALHAT integration. High- delity simulations were implemented to gain insight into integrated ALHAT sensors and Morpheus GN&C system performance, and command and telemetry interfacing and functional testing was conducted once the ALHAT sensors and electronics were integrated onto Morpheus. This paper captures some of the details and lessons learned in the planning, preparation and integration of the individual ALHAT sen- sors, the vehicle, and the test environment that led up to the joint ight tests.
Carson, John M., III↗
Characterization of Plasma Synthesized Vertical Carbon Nanofibers for Nanoelectronics Applications
We report on the material characterization of carbon nanofibers (CNFs) which are assembled into a three-dimensional (3D) configuration for making new nanoelectromechanical systems (NEMS). High-resolution scanning electron microscopy (SEM) and x-ray electron dispersive spectroscopy (XEDS) are employed to decipher the morphology and chemical compositions of the CNFs at various locations along individual CNFs grown on silicon (Si) and refractory nitride (NbTiN) substrates, respectively. The measured characteristics suggest interesting properties of the CNF bodies and their capping catalyst nanoparticles, and growth mechanisms on the two substrates. Laser irradiation on the CNFs seems to cause thermal oxidation and melting of catalyst nanoparticles. The structural morphology and chemical compositions of the CNFs revealed in this study should aid in the applications of the CNFs to nanoelectronics and NEMS.
carbon nanomaterials↗
Conceptual Design Optimization of an Augmented Stability Aircraft Incorporating Dynamic Response Performance Constraints
This research focused on incorporating stability and control into a multidisciplinary de- sign optimization on a Boeing 737-class advanced concept called the D8.2b. A new method of evaluating the aircraft handling performance using quantitative evaluation of the sys- tem to disturbances, including perturbations, continuous turbulence, and discrete gusts, is presented. A multidisciplinary design optimization was performed using the D8.2b transport air- craft concept. The con guration was optimized for minimum fuel burn using a design range of 3,000 nautical miles. Optimization cases were run using xed tail volume coecients, static trim constraints, and static trim and dynamic response constraints. A Cessna 182T model was used to test the various dynamic analysis components, ensuring the analysis was behaving as expected. Results of the optimizations show that including stability and con- trol in the design process drastically alters the optimal design, indicating that stability and control should be included in conceptual design to avoid system level penalties later in the design process.
Welstead, Jason↗
Static Wind Tunnel Testing of a Legged Venus Lander
A static wind tunnel test was conducted to determine the static aerodynamic coe cients of the surface lander design proposed by the Venus In-Situ Atmospheric and Geochemical Explorer (VISAGE). The baseline design of the lander consists of a spherical pressure vessel with a top-mounted circular drag plate for aerodynamic deceleration, and three xed landing legs. A modular subscale lander model, which allowed testing of several drag plate and landing leg con gurations, was fabricated using rapid-prototyping techniques. The model was tested with four di erent drag plates and three di erent leg con gurations, at a dynamic pressure of 1610 Pa and Mach number of 0.15. Testing was conducted using legs of varying diameter in order to determine the appropriate scaling of the results to Reynolds numbers representative of terminal descent at Venus. The static aerodynamic force (axial, normal, and side), and moment (rolling, pitching, yawing) coe cients for each lander con guration were determined as a function of model orientation. All model con gurations were found to be statically stable in the range of total angles of attack considered (0 to 30 deg). However, the drag performance and degree of static stability of the model were dependent on the dihedral angle of the circular drag plate. The results will enable the creation of a preliminary aerodatabase for the VISAGE lander concept, and allow the e ect of design changes on aerodynamic performance to be evaluated.
Rabinovitch, Jason↗
Simulation of Axion-like Particles at DarkQuest
DarkQuest is a collaboration at Fermilab searching for beyond the StandardModel (SM) physics using a xed target beam dump experiment. This experiment featuresa proton beam colliding with a target and creating particles, possibly theoretical ones,from the interactions that occur. A popular theoretical particle is the axion, an elementaryparticle that explains the breakage of symmetry that occurs in our current model of physics,called the strong CP problem. An axion-like particle (ALP) is similar to an axion in itsresolution of the strong CP problem, but has mass, and so is detectable by experimentation.By simulating the production and decay of an ALP, we can estimate the region of parameterspace of ALP mass and SM coupling that DarkQuest could make a discovery.
72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
Quantitative Assessment and Measurement of X-ray Detector Performance and Solid Angle in the Analytical Electron Microscope
A wide range of X-ray detectors and geometries are available today on transmission/scanning transmission analytical electron microscopes. While there have been numerous reports of their individual performance, no single experimentally reproducible metric has been proposed as a basis of comparison between the systems. In this paper, we detail modeling, experimental procedures, measurements, and specimens which can be used to provide a manufacturer-independent assessment of the performance of an analytical system. Using these protocols, the geometrical collection efficiency, system peaks, and minimum detection limits can be independently assessed and can be used to determine the best conditions to conduct modern hyperspectral and/or spectrally resolved tomographic analyses for an individual instrument. Here, a simple analytical formula and specimen is presented which after suitable system calibrations can be used to experimentally determine the X-ray detector solid angle.
47 OTHER INSTRUMENTATION↗