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All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Universal temperature dependence of the London penetration depth in κ - ( ET ) 2 X superconductors

High-precision radio-frequency magnetic susceptibility measurements were performed on single crystals of fully deuterated $κ-(ET)_2Cu[N(CN)_2]\,Br$, hereafter designated as $κ-(ET)_2Cu[N(CN)_2]\,Br$. This material phase separates into superconducting and antiferromagnetic regions, the degree of which depends strongly upon the cooling rate. Here, we show that the screening fraction $η_{sc}$ varies logarithmically with the cooling rate over nearly five decades. The average size of superconducting regions is estimated to vary from 5 to $40μm$, depending upon cooling rate, consistent with previous infrared microscopy measurements. In the region $T≲T_c/3$, the effective magnetic penetration depth exhibits power-law behavior $λ(T)-λ(0)~T^n$ with $n=1.6$, independent of the cooling rate. Changes in cooling rate and the consequent phase separation evidently do not introduce the kind of disorder that would alter the exponent $n$ in a $d$-wave superconductor. The exponent remains close to $n=$ 1.5, reported in single crystals of $κ-(ET)_2Cu[N(CN)_2]\,Br$ and $κ-(ET)_2Cu(NCS)_2$ [A. Carrington et al., Phys. Rev. Lett 83, 4172 (1999)]. The transition temperature fell linearly with $1-η_{sc}$. Measurements were also made on $κ-(ET)_2Cu[N(CN)_2]\,Cl$ of normal isotopic abundance in which a very small amount of superconducting phase $η_{sc}≈10^{-4}$ developed, presumably through the strain-induced sample mounting. This material showed a power-law exponent of $n=1.64$, independent of the cooling rate.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2023

Thermodynamics of Minerals Stable near Earth's Surface

Project “Thermodynamics of Minerals Stable Near the Earth’s Surface” uses specialized calorimetric techniques to obtain new thermochemical data for solid phases of interest in the Earth’s “critical zone”, the near surface regions of the planet most directly affecting and affected by human activity. Major activity was in three areas: manganese oxide materials, aluminum clusters which are precursors to aluminum oxyhydroxide precipitates, and zeolites. All these classes of minerals are potential carriers of heavy metals and radionuclides in the environment, both within their crystal structures and as adsorbed layers or colloids. Their thermodynamic stability, as well as the sequence of stability of competing phases, governs the aqueous solubility of contaminants (and nutrients) in soil, groundwater, and sediments. The thermodynamics of these phases is strongly affected by particle size and crystallinity, since they often occur as very fine particles which do not coarsen in the near-surface environment. Many of these materials exhibit extensive polymorphism, multicomponent solid solution, and variable hydration states. Thus, one must define and systematize important thermodynamic variables, since one cannot make measurements on each and every possible phase, particle size, and composition. A major finding of the work on manganese oxides was labile water-induced oxidation-reduction reactions. These will be studied further by a combination of thermodynamic and synchrotron-based spectroscopic methods, the latter in collaboration with Peggy O’Day at UC Merced. The adsorption of other species, including simple organics, on such redox-active surfaces will also be investigated by a combination of thermochemical and spectroscopic studies. Studies of the energetics of water adsorption on mineral surfaces will be expanded to emphasize the adsorption of CO2 and small organic molecules, relevant to soil, groundwater, and the subsurface environment. Gas adsorption calorimetry, immersion calorimetry, and solution calorimetry will be combined with appropriate analytical and spectroscopic techniques to obtain a comprehensive picture of the interactions and their energetics. The evolution of aqueous aluminum clusters to form aluminum oxyhydroxide precipitates will be studied in detail by a combination of calorimetric and structural methods applied to aqueous samples aged at room temperature. The energetics of new classes of clusters will be explored. The project addresses several common themes relevant to the broad mission of the Department of Energy. Thermochemical data for minerals stable near the Earth’s surface, though still incomplete, are essential for understanding both natural and anthropogenic processes that affect our very existence on this planet. Such data contribute to the fundamental underpinning for mitigation and management strategies for the extraction and use of energy. Fundamental thermodynamic and mechanistic understanding is required to model processes ranging from heavy metal pollution to nuclear waste disposal to climate change.

58 GEOSCIENCES↗
DOE OSTI2021

Performance Validation of Pulsed Thermal Imaging System for In-Service Applications

Additive manufacturing (AM) is an emerging method for cost-efficient fabrication of complex topology nuclear reactor parts from high-strength corrosion resistance alloys, such as stainless steel and Inconel. AM of metallic structures for nuclear energy applications is currently based on laser powder bed fusion (LPBF) process, which has the capability of melting metallic powder and net shaping the structures with relatively high precision. Some of the challenges with using LPBF method for nuclear manufacturing include the possibility of introducing pores into metallic structures. Integrity of AM structures needs to be evaluated nondestructively because material flaws could lead to premature failures in high temperature nuclear reactor environment. Currently, there exist limited capabilities to evaluate actual AM structures non-destructively. Pulsed Thermography Imaging (PTI) provides a capability for non-destructive evaluation (NDE) of subsurface defects in arbitrary size structures. The PTI method is based on recording material surface temperature transients with infrared (IR) camera following thermal pulse delivered on material surface with flash light. The PTI method has advantages for NDE of actual AM structures because the method involves one-sided non-contact measurements and fast processing of large sample areas captured in one image. Following initial qualification of an AM component for deployment in a nuclear reactor, a PTI system can also be used for in-service nondestructive evaluation (NDE) applications. In this report, we describe recent progress in enhancing PTI capabilities in detecting microscopic defects in metallic specimens. SS316 and IN718 specimens were developed with a pattern of subsurface calibrated flat bottom hole (FBH) defects with diameters from 500µm to 200µm. FBH’s were created with EDM (electron discharge machining) drill. PTI imaging data was processed Spatial Temporal Denoised Thermal Source Separation (STDTSS) unsupervised machine learning (ML) algorithm. We show that defects as small as 200µm in SS316 and IN718 can be detected with STDTSS algorithm. To the best of our knowledge, these are the smallest detected defects which are reported in literature.

42 ENGINEERING↗
NASA NTRS1996

A Numerical Simulation of Scattering from One-Dimensional Inhomogeneous Dielectric Random Surfaces

In this paper, an efficient numerical solution for the scattering problem of inhomogeneous dielectric rough surfaces is presented. The inhomogeneous dielectric random surface represents a bare soil surface and is considered to be comprised of a large number of randomly positioned dielectric humps of different sizes, shapes, and dielectric constants above an impedance surface. Clods with nonuniform moisture content and rocks are modeled by inhomogeneous dielectric humps and the underlying smooth wet soil surface is modeled by an impedance surface. In this technique, an efficient numerical solution for the constituent dielectric humps over an impedance surface is obtained using Green's function derived by the exact image theory in conjunction with the method of moments. The scattered field from a sample of the rough surface is obtained by summing the scattered fields from all the individual humps of the surface coherently ignoring the effect of multiple scattering between the humps. The statistical behavior of the scattering coefficient sigma(sup 0) is obtained from the calculation of scattered fields of many different realizations of the surface. Numerical results are presented for several different roughnesses and dielectric constants of the random surfaces. The numerical technique is verified by comparing the numerical solution with the solution based on the small perturbation method and the physical optics model for homogeneous rough surfaces. This technique can be used to study the behavior of scattering coefficient and phase difference statistics of rough soil surfaces for which no analytical solution exists.

Sarabandi, Kamal↗
NASA NTRS1998

An Assessment of Molten Metal Detachment Hazards During Electron Beam Welding in Space

The safety issue has been raised with regards to potential molten metal detachments from the weld pool and cold filler wire during electron beam welding in space. This investigation was undertaken to evaluate if molten metal could detach and come in contact with astronauts and burn through the fabric of the astronauts' Extravehicular Mobility Unit (EMU) during electron beam welding in space. Molten metal detachments from either the weld/cut substrate or weld wire could present harm to a astronaut if the detachment was to burn through the fabric of the EMU. Theoretical models were developed to predict the possibility and size of the molten metal detachment hazards during the electron beam welding exercises at Low Earth Orbit (LEO). The primary molten metal detachment concerns were those cases of molten metal separation from the metal surface due to metal cutting, weld pool splashing, entrainment and release of molten metal due to filler wire snap-out from the weld puddle, and molten metal accumulation and release from the end of the weld wire. Some possible ways of obtaining molten metal drop detachments would include an impulse force, or bump, to the weld sample, cut surface, or filler wire. Theoretical models were developed for these detachment concerns from principles of impact and kinetic energies, surface tension, drop geometry, surface energies, and particle dynamics. The surface tension represents the force opposing the liquid metal drop from detaching whereas the weight of the liquid metal droplet represents a force that is tending to detach the molten metal drop. Theoretical calculations have indicated that only a small amount of energy is required to detach a liquid metal drop; however, much of the energy of an impact is absorbed in the sample or weld plate before it reaches the metal drop on the cut edge or surface. The tendency for detachment is directly proportional to the weld pool radius and metal density and inversely proportional to the surface tension of the liquid metal. For a detachment the initial kinetic energy of the weld pool with respect to the plate has to exceed the energy to form the extra surface required for the detachment of the pool. The difficulty is in transferring the energy from the point of impact through the plate and sample to the cut edge. It is likely that not all of the kinetic energy is available for detaching the pool; some may be sequestered in weld pool oscillations. The coefficient of restitution for the collision will be lower than one if irreversible deformation, for example plastic flow deformation, takes place during the collision. Thus determining the amount of energy from an impact that actually reaches the molten metal droplet is critical. Various molten metal detachment scenarios were tested experimentally in an enclosed vacuum chamber using the Ukrainian Universal Hand Tool, an electron beam welder designed for space welding. The experimental testing was performed in a 4 ft. X 4 ft. vacuum chamber at Marshall Space Flight Center, evacuated to vacuum levels of at least 50 microTorr, and also some welding garment material was utilized to observe the effect of the molten metal detachments on the material. A "carillon" apparatus consisting of four pendulum hammer strikers, each weighing approximately 3.65 lbs, raised to predetermined specific heights was used to apply an impact force to the weld sample/plate during electron beam welding and cutting exercises. The strikers were released by switching on an electric motor to rotate a pin holding wires retaining the strikers at desired heights. The specimens were suspended so as to be free to respond to the blows with a sudden velocity increment. The specimens were mounted on a hinged plate for minimizing effective mass with the option to fasten it down so as to raise its effective mass closer to that anticipated for an actual space welding scenario. Measurements were made of the impact energy and the horizontal fling distances of the detached metal drops. It was not particularly easy to generate the detachments for this experiment. This document presents the details of the theoretical modeling effort and a summary of the experimental effort to measure molten metal drop detachments from terrestrial electron beam welding in the enclosed vacuum chamber. The results of the experimental effort have shown that molten metal detachments can occur from the sample/weld plate only if a sufficiently large impact force is applied to the weld plate. A "weld pool detachment parameter" was determined to indicate whether detachment would occur. Detachment can be either full or partial (dripping), Partial detachment means that the weld pool detached from one side of the liquid-solid boundary so as to leave a hole at the puddle site but remained attached over part of the liquid-solid boundary and dripped down the plate with no fully detached material detected. Full detachment, however, does not necessarily mean that the whole pool fully detached; in some cases only a smaller portion of the pool detached, the remainder dripping down the plate. The weld pool detachment parameter according to theory and according to the empirical data allows a determination of whether full detachments might occur. Theoretical calculations indicated titanium alloy would be the most difficult from which to detach molten metal droplets followed by stainless steel and then by aluminum. The experimental results were for the most part consistent with the theoretical analysis and predictions. The above theory is applicable to other situations as desired for assessing the potential for molten metal detachments.

Fragomeni, James M.↗
NASA NTRS2002

Science Objectives of EOS-Aura's Ozone Monitoring Instrument (OMI)

OMI is a UV/VIS nadir solar backscatter spectrograph, which provides near global coverage in one day with a spatial resolution of 13 x 24 sq km. OMI is a new instrument, with a heritage from the European satellite instruments GOME, GOMOS and SCIAMACHY. OMI's unique capabilities for measuring important trace gases with a small footprint and daily global coverage, in conjunction with the other Aura instruments, will make a major contribution to our understanding of stratospheric and tropospheric chemistry and climate change. OMI will measure solar irradiance and Earth radiances in the wavelength range of 270 to 500 nm with spectral resolution of about 0.5 nm and a spectral sampling of about 2-3 per FWHM. From these observations, total columns of O3, NO2, BrO and SO2 will be derived from the back-scattered solar radiance using differential absorption spectroscopy (DOAS). The TOMS total ozone record will also be continued by employing the well established TOMS algorithm. Because of the high accuracy and spatial resolution of the measurements, a good estimate of tropospheric amounts of ozone and NO2 are expected. Ozone profiles will be derived using the optimal estimation method. The spectral aerosol optical depth will be determined from measurements between 340 and 500 nm. This will provide information on aerosol concentration, aerosol size distribution and aerosol type. This wavelength range makes it possible to retrieve aerosol information over both land and sea. OMI observations will also allow retrievals of cloud coverage and cloud heights. From these products, the UV-B flux at the surface can then be derived with high spatial resolution.

Levelt, P. F.↗
DOE OSTI2020

Active Learning A Neural Network Model For Gold Clusters & Bulk From Sparse First Principles Training Data

Small metal clusters are of fundamental scientific interest and of tremendous significance in catalysis. These nanoscale clusters display diverse geometries and structural motifs depending on the cluster size; a knowledge of this size-dependent structural motifs and their dynamical evolution has been of longstanding interest. Given the high computational cost of first-principles calculations, molecular modeling and atomistic simulations such as molecular dynamics (MD) has proven to be an important complementary tool to aid this understanding. Classical MD typically employ predefined functional forms which limits their ability to capture such complex size-dependent structural and dynamical transformation. Neural Network (NN) based potentials represent flexible alternatives and in principle, well-trained NN potentials can provide high level of flexibility, transferability and accuracy on-par with the reference model used for training. A major challenge, however, is that NN models are interpolative and requires large quantities (similar to 10 4 or greater) of training data to ensure that the model adequately samples the energy landscape both near and far-from-equilibrium. A highly desirable goal is minimize the number of training data, especially if the underlying reference model is first-principles based and hence expensive. In this work, we introduce an active learning (AL) scheme that trains a NN model on-the-fly with minimal amount of first-principles based training data. Our AL workflow is initiated with a sparse training dataset (similar to 1 to 5 data points) and is updated on-the-fly via a Nested Ensemble Monte Carlo scheme that iteratively queries the energy landscape in regions of failure and updates the training pool to improve the network performance. Using a representative system of gold clusters, we demonstrate that our AL workflow can train a NN with similar to 500 total reference calculations. Using an extensive DFT test set of similar to 1100 configurations, we show that our AL-NN is able to accurately predict both the DFT energies and the forces for clusters of a myriad of different sizes. Our NN predictions are within 30 meV/atom and 40 meV/angstrom of the reference DFT calculations. Moreover, our AL-NN model also adequately captures the various size-dependent structural and dynamical properties of gold clusters in excellent agreement with DFT calculations and available experiments. We finally show that our AL-NN model also captures bulk properties reasonably well, even though they were not included in the training data.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

A DEEP, WIDE-FIELD, AND PANCHROMATIC VIEW OF 47 Tuc AND THE SMC WITH HST: OBSERVATIONS AND DATA ANALYSIS METHODS

In Hubble Space Telescope (HST) Cycle 17, we imaged the well-known globular star cluster 47 Tucanae for 121 orbits using the Wide Field Channel of the Advanced Camera for Surveys (ACS) and both the UV/visible (UVIS) and IR channels of the newly installed Wide Field Camera 3 (WFC3) instrument (GO-11677, PI: H. Richer). This unique data set was obtained to address many scientific questions that demand a very deep, panchromatic, and panoramic view of the cluster's stellar populations. In total, the program obtained over 0.75 Ms of imaging exposure time with the three HST cameras, over a time span of 9 months in 2010. The primary ACS field was imaged in the two broadband filters F606W and F814W, at 13 orientations, for all 121 orbits. The parallel WFC3 imaging provides a panchromatic (0.4-1.7 {mu}m) and contiguous imaging swath over a 250 Degree-Sign azimuthal range at impact radii of 6.5-17.9 pc in 47 Tuc. This imaging totals over 60 arcmin{sup 2} in area and utilizes the F390W and F606W broadband filters on WFC3/UVIS and the F110W and F160W broadband filters on WFC3/IR. In this paper, we describe the observational design of the new survey and one of the methods used to analyze all of the imaging data. This analysis combines over 700 full-frame images taken with the three HST cameras into a handful of ultra-deep, well-sampled combined images in each of the six filters. We discuss in detail the methods used to calculate accurate transformations that provide optimal alignment of the input images, the methods used to perform sky background offsets in the input stack and the flagging of deviant pixels, and the balance reached between the input-pixel drop size onto an output supersampled pixel grid. Careful photometric, morphological, and astrometric measurements are performed on the stacks using iterative PSF-fitting techniques, and reveal unprecedented color-magnitude diagrams of the cluster extending to >30th magnitude in the optical, 29th magnitude in the UV, and 27th magnitude in the IR. The data set provides a characterization of the complete stellar populations of 47 Tuc, extending from the faintest hydrogen-burning dwarfs through the main-sequence and giant branches down to very cool white dwarf remnants in the cluster. The imaging also provides the deepest probe of the stellar populations of the background Small Magellanic Cloud galaxy, resolving low-mass main-sequence dwarfs with M {approx}< 0.2 M{sub Sun }.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2011

THE RELATIVE ABUNDANCE OF COMPACT AND NORMAL MASSIVE EARLY-TYPE GALAXIES AND ITS EVOLUTION FROM REDSHIFT z {approx} 2 TO THE PRESENT

We report on the evolution of the number density and size of early-type galaxies (ETGs) from z {approx} 2 to z {approx} 0. We select a sample of 563 massive (M > 10{sup 10} M{sub Sun }), passively evolving (specific star formation rate <10{sup -2} Gyr{sup -1}), and morphologically spheroidal galaxies at 0 < z < 2.5, using the panchromatic photometry and spectroscopic redshifts available in the Great Observatories Origins Deep Surveys fields. We combine Advanced Camera for Surveys and Wide Field Camera 3 Hubble Space Telescope images to study the morphology of our galaxies in their optical rest frame in the entire 0 < z < 2.5 range. We find that throughout the explored redshift range the passive galaxies selected with our criteria have weak morphological K-correction, with size being slightly smaller in the optical than in the UV rest frame (by {approx}20% and {approx}10% at z > 1.2 and z < 1.2, respectively). We measure a significant evolution of the mass-size relation of ETGs, with a fractional increment that is almost independent of the stellar mass. ETGs formed at z > 1 appear to be preferentially small, and the evolution of the mass-size relation at z < 1 is driven by both the continuous size growth of the compact galaxies and the appearance of new ETGs with large sizes. We also find that the number density of all passive ETGs increases rapidly, by a factor of five, from z {approx} 2 to z {approx} 1, and then more mildly by another factor of 1.5 from z {approx} 1 to z {approx} 0. We interpret these results as evidence that the bulk of the ETGs are formed at 1 < z < 3 through a mechanism that leaves very compact remnants. At z < 1 the compact ETGs grow gradually in size, becoming normal-size galaxies, and at the same time new ETGs with normal-large sizes are formed.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2016

Unit cell determination of coexisting post-perovskite and H-phase in (Mg,Fe)SiO3 using multigrain XRD: compositional variation across a laser heating spot at 119 GPa

Multigrain X-ray diffraction (XRD) can be used to accurately calculate the unit cell parameters of individual mineral phases in a mineral assemblage contained in a diamond anvil cell (DAC). Coexisting post-perovskite (ppv) and H-phase were synthesized at 119 GPa and 2500 K from (Mg 0.85 Fe 0.15 )SiO 3 in a laser-heated DAC. The unit cell parameters of the ppv and coexisting H-phase were determined using multigrain XRD with a 5 μm spatial resolution, close to the size of the X-ray beam, to understand compositional variations across the center area (20–30 μm) in a laser-heated sample. The ppv phase was Fe-depleted and the unit cell volume of ppv decreased by only 0.16 % (corresponding to ~3 % variation of FeSiO 3 ) from the heating center to 10 μm off the center, while the sample pressure remained at 119 GPa in a Ne quasi-hydrostatic environment. The unit cell volume of the H-phase decreased by 0.54 % (~10 % variation of FeSiO 3 content) over the same 10 μm distance. Both phases were more Fe-enriched in the slightly hotter center. This observation suggests that thermal diffusion may not be the major driver for the compositional variations of ppv and H-phase in the center portion of a laser-heated sample. Instead, these variations could be caused by a temperature effect on the partitioning between the ppv and H-phase over the small gradient.

58 GEOSCIENCES↗
NASA NTRS2000

High-Frequency Excitation of a Plane Wake

In the early 1990's, Glezer and his co-workers at Georgia Tech made a startling discovery. They found that forcing at frequencies too high to directly affect the production scales led to a dramatic alteration in the development of a turbulent shear layer. An experimental study of this phenomenon is presented in Wiltse and Glezer. They used piezoelectric actuators located near the jet exit plane to force the shear layers of a square low-speed jet. The actuators were driven at a high frequency in the Kolmogorov inertial subrange, much higher than the frequencies associated with the large-scale motion (where the turbulent energy is produced and located) but much lower than those associated with the Kolmogorov scale (where the turbulent energy is dissipated). Measurements of the shear-layer turbulence showed that direct excitation of small-scale motion by high-frequency forcing led to an increase in the turbulent dissipation of more than an order of magnitude in the initial region of the shear layer! The turbulent dissipation gradually decreased with downstream distance but remained above the corresponding level for the unforced flow at all locations examined. The high-frequency forcing increased the turbulent kinetic energy in the initial region near the actuators, but the kinetic energy decreased quite rapidly with downstream distance, dropping to levels that were a small fraction of the level for the unforced case. Perhaps most importantly from the present standpoint, the high-frequency forcing significantly decreased the energy in the large-scale motion, increasingly so with downstream distance. Wiltse and Glezer interpreted this behavior as an enhanced transfer of energy from the large scales to the small scales. The initial work by Wiltse and Glezer has expanded into other applications. To explore the potential of high-frequency forcing for active acoustic suppression, in 1998 the first author proposed a set of experiments involving an edge tone shear layer and an open cavity flow. This work was funded by the US Air Force Research Laboratory, and the experiments were developed and executed at Boeing by Raman and Kibens. These experiments involved high-frequency forcing applied to low-speed flows using wedge piezo actuators and powered resonance tubes. The system is simple, open loop, compact, potentially requires little power, and is easily integrated. Dramatic results, such as reductions of 20 dB in spectral peaks and 5-8 dB in overall levels across the entire acoustic spectrum, were obtained in some cases. Sample results are presented. Following this success in low-speed flows, an international cooperative program continuing this work involved transonic experiments in a mid-size facility in the United Kingdom. Similar reductions in noise level were obtained in these transonic experiments. Discussion of this work is given in Raman et at. and Stanek, Raman, Kibens, and Ross. Other experiments at Georgia Tech have shown significant potential of high-frequency forcing in controlling reaction rates in chemically reacting flows.

Cain, Alan B.↗
DOE OSTI2014

Multiple and fast: The accretion of ordinary chondrite parent bodies

Although petrologic, chemical, and isotopic studies of ordinary chondrites and meteorites in general have largely helped establish a chronology of the earliest events of planetesimal formation and their evolution, there are several questions that cannot be resolved via laboratory measurements and/or experiments alone. Here, we propose the rationale for several new constraints on the formation and evolution of ordinary chondrite parent bodies (and, by extension, most planetesimals) from newly available spectral measurements and mineralogical analysis of main-belt S-type asteroids (83 objects) and unequilibrated ordinary chondrite meteorites (53 samples). Based on the latter, we suggest that spectral data may be used to distinguish whether an ordinary chondrite was formed near the surface or in the interior of its parent body. If these constraints are correct, the suggested implications include that: (1) large groups of compositionally similar asteroids are a natural outcome of planetesimal formation and, consequently, meteorites within a given class can originate from multiple parent bodies; (2) the surfaces of large (up to ∼200 km) S-type main-belt asteroids mostly expose the interiors of the primordial bodies, a likely consequence of impacts by small asteroids (D < 10 km) in the early solar system; (3) the duration of accretion of the H chondrite parent bodies was likely short (instantaneous or in less than ∼10{sup 5} yr, but certainly not as long as 1 Myr); (4) LL-like bodies formed closer to the Sun than H-like bodies, a possible consequence of the radial mixing and size sorting of chondrules in the protoplanetary disk prior to accretion.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2023

Evaluation of Electron Tomography Capabilities for Shale Imaging

Despite the advantageous resolution of electron tomography (ET), reconstruction of three-dimensional (3D) images from multiple two-dimensional (2D) projections presents several challenges, including small signal-to-noise ratios, and a limited projection range. This study evaluates the capabilities of ET for thin sections of shale, a complex nanoporous medium. A numerical phantom with 1.24 nm pixel size is constructed based on the tomographic reconstruction of a Barnett shale. A dataset of 2D projection images is numerically generated from the 3D phantom and studied over a range of conditions. First, common reconstruction techniques are used to reconstruct the shale structure. The reconstruction uncertainty is quantified by comparing overall values of storage and transport metrics, as well as the misclassification of pore voxels compared to the phantom. We then select the most robust reconstruction technique and we vary the acquisition conditions to quantify the effect of artifacts. We find a strong agreement for large pores over the different acquisition workflows, while a wider variability exists for nanometer-scale features. Furthermore, the limited projection range and reconstruction are identified as the main experimental bottlenecks, thereby suggesting that sample thinning, advanced holders, and advanced reconstruction algorithms offer opportunities for improvement.

3D scanning transmission electron microscopy↗
DOE OSTI2025

Ruthenium/Carbon Nanocomposites for Efficient Hydrogen Electrocatalysis: Impacts of Halide Residues

Ruthenium has emerged as a promising substitute for platinum toward the hydrogen evolution/oxidation reaction (HER/HOR). Herein, ruthenium/carbon composites are prepared by magnetic induction heating (300 A, 10 s) of RuCl3, RuBr3 or RuI3 loaded on hollow N-doped carbon cages (HNC). The HNC-RuCl3-300A sample consists of Ru nanoparticles (dia. 1.96 nm) and abundant Cl residues. HNC-RuBr3-300A possesses a larger nanoparticle size (≈19.36 nm) and lower content of Br residues. HNC-RuI3-300A contains only bulk-like Ru agglomerates with a minimal amount of I residues, due to reduced Ru-halide bonding interactions. Among these, HNC-RuCl3-300A exhibits the best HER activity in alkaline media, with a low overpotential of only -26 mV to reach 10 mA cm-2, even outperforming Pt/C, and can be used as the cathode catalyst for anion exchange membrane water electrolyzer (along with commercial RuO2 as the anode catalyst), producing 0.5 A cm- 2 at 1.88 V for up to 100 h, a performance markedly better than that with Pt/C. HNC-RuCl3-300A also exhibits the best HOR activity, with a half-wave potential (+18 mV) even lower than that of Pt/C (+35 mV). These activities are ascribed to the combined contributions of small Ru nanoparticles and Ru-to-halide charge transfer that weaken H adsorption.

Yu, Bingzhe↗
DOE OSTI2012

Effect of Ca Doping on the Electrical Conductivity of the High-Temperature Proton Conductor LaNbO4

The sintering properties, crystal structure and electrical conductivity of La1-xCaxNbO4- (x=0, 0.005, 0.01, 0.015, 0.02 and 0.025), prepared by a conventional solid-state method, have been investigated using powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and electrochemical impedance spectroscopy (EIS). In 2.5% Ca doped samples, a small amount of impurities Ca2Nb2O7 were observed from the XRD patterns. Impedance spectra show that the grain boundary resistance increases with increasing Ca content, while the bulk resistance remains essentially constant below 550 C. Despite the higher degree of grain growth was observed for higher Ca-doping levels, the total conductivity of the La1-xCaxNbO4- series decreases with increasing Ca content from 0.5 to 2.0 mol%. The activation energy for the total conductivity decreases with increasing Ca content from 0.71 eV (x=0) to 0.54 eV (x=0.01) for the high temperature tetragonal phase, then it increases to 0.60 eV for x=0.02. For the monoclinic phase, La0.995Ca0.005NbO4- shows the lowest activation energy of 1.26 eV. These results imply that the solubility of CaO in LaNbO4 is in the range from 0.5 to 1.0 mol%. By increasing the sintering temperature from 1500 C to 1550 C, the proton conductivity of the Ca-doped LaNbO4 was improved with enlarged grain size due to a reduction in the resistive grain boundary contribution.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2013

Metrological characterization of X-ray diffraction methods at different acquisition geometries for determination of crystallite size in nano-scale materials

Crystallite size values were determined by X-ray diffraction methods for 183 powder samples. The tested size range was from a few to about several hundred nanometers. Crystallite size was calculated with direct use of the Scherrer equation, the Williamson–Hall method and the Rietveld procedure via the application of a series of commercial and free software. The results were statistically treated to estimate the significance of the difference in size resulting from these methods. We also estimated effect of acquisition conditions (Bragg–Brentano, parallel-beam geometry, step size, counting time) and data processing on the calculated crystallite size values. On the basis of the obtained results it is possible to conclude that direct use of the Scherrer equation, Williamson–Hall method and the Rietveld refinement employed by a series of software (EVA, PCW and TOPAS respectively) yield very close results for crystallite sizes less than 60 nm for parallel beam geometry and less than 100 nm for Bragg–Brentano geometry. However, we found that despite the fact that the differences between the crystallite sizes, which were calculated by various methods, are small by absolute values, they are statistically significant in some cases. The values of crystallite size determined from XRD were compared with those obtained by imaging in a transmission (TEM) and scanning electron microscopes (SEM). It was found that there was a good correlation in size only for crystallites smaller than 50 – 60 nm. Highlights: • The crystallite sizes for 183 nanopowders were calculated using different XRD methods • Obtained results were subject to statistical treatment • Results obtained with Bragg-Brentano and parallel beam geometries were compared • Influence of conditions of XRD pattern acquisition on results was estimated • Calculated by XRD crystallite sizes were compared with same obtained by TEM and SEM.

36 MATERIALS SCIENCE↗
NASA NTRS1988

Improved canopy reflectance modeling and scene inference through improved understanding of scene pattern

The Li-Strahler reflectance model, driven by LANDSAT Thematic Mapper (TM) data, provided regional estimates of tree size and density within 20 percent of sampled values in two bioclimatic zones in West Africa. This model exploits tree geometry in an inversion technique to predict average tree size and density from reflectance data using a few simple parameters measured in the field (spatial pattern, shape, and size distribution of trees) and in the imagery (spectral signatures of scene components). Trees are treated as simply shaped objects, and multispectral reflectance of a pixel is assumed to be related only to the proportions of tree crown, shadow, and understory in the pixel. These, in turn, are a direct function of the number and size of trees, the solar illumination angle, and the spectral signatures of crown, shadow and understory. Given the variance in reflectance from pixel to pixel within a homogeneous area of woodland, caused by the variation in the number and size of trees, the model can be inverted to give estimates of average tree size and density. Because the inversion is sensitive to correct determination of component signatures, predictions are not accurate for small areas.

Franklin, Janet↗
DOE OSTI2018

Production of monodisperse cerium oxide microspheres with diameters near 100 µm by internal-gelation sol–gel methods

Cerium dioxide microspheres with uniform diameters between 65 – 211 µm were fabricated using internal gelation sol-gel methods. Although uniform microspheres are produced for nuclear fuel applications with diameters above 300 µm, sol-gel microspheres with diameters of 50 - 200 µm have historically been made by emulsion techniques and had poor size uniformity [1, 2]. An internal gelation, sol-gel apparatus was designed and constructed to accommodate the production of small, uniform microspheres whereby cerium-containing solutions were dispersed into flowing silicone oil and heated in a gelation column to initiate solidification [3, 4]. Problems with premature feed gelation and microsphere coalescence were overcome by equipment modifications unique among known internal gelation setups. Microspheres were fabricated and sized in batches as a function of dispersing needle diameter and silicone oil flow rate in the two-fluid nozzle in order to determine the range of sizes possible and corresponding degree of monodispersity. Initial experiments with poor size uniformity were linked to microsphere coalescence in the gelation column prior to solidification as well as excessive flow rates for the cerium feed solution. Average diameter standard deviations as low as 2.23% were observed after optimization of flow rates and minimization of coalescence reactions.

cerium oxide↗