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DOE OSTI2020

Tuning the Morphology and Electronic Properties of Single-Crystal LiNi 0.5 Mn 1.5 O 4-δ : Exploring the Influence of LiCl–KCl Molten Salt Flux Composition and Synthesis Temperature

Single-crystal materials have played a unique role in the development of high-performance cathode materials for Li batteries due to their favorable chemomechanical stability. The molten salt synthesis method has become one of the most prominent techniques used to synthesize single-crystal layered and spinel materials. In this work, the molten salt synthesis method is used as a technique to tune both the morphology and Mn 3+ content of high-voltage LiNi 0.5 Mn 1.5 O 4 (LNMO) cathodes. The resulting materials are thoroughly characterized by a suite of analytical techniques, including synchrotron X-ray core-level spectroscopy, which are sensitive to the material properties on multiple length scales. Furthermore, the multidimensional characterization allows us to build a materials library according to the molten salt phase diagram as well as to establish the relationship among synthesis, material properties, and battery performance. The results of this work show that the Mn 3+ content is primarily dependent on the synthesis temperature and increases as the temperature is increased. Additionally, the particle morphology is mostly dependent on the composition of the molten salt flux, which can be tailored to obtain well-defined octahedrons enclosed by (111) facets, plates with predominant ($11\tilde{2}$) facets, irregularly shaped particles, or mixtures of these. The electrochemical measurements indicate that the Mn 3+ content has a larger contribution to the battery performance of LNMO than do morphological characteristics and that a significant amount of Mn 3+ could become detrimental to the battery performance. However, with similar Mn 3+ contents, morphology still plays a role in influencing the battery cycle life and rate performance. The insights of molten salt synthesis parameters on the formation of LNMO, with deconvolution of the roles of Mn 3+ and morphology, are crucial to continuing studies in the rational design of LNMO cathode materials for high-energy Li batteries.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1982

Observations of solar particle propagation and solar modulation

The solar wind provides a unique opportunity for a study of the propagation of energetic particles in irregular magnetic fields on scales which are of astrophysical interest. Problems concerning the conduction of such a study are related to the great number of different factors which affect the motion of the solar particles. Observations related to solar particle propagation are considered, taking into account approaches involving the adjustment of parameters in analytical models to produce fits to the observed time-intensity and time-anisotropy profiles, and new classes of solar particle events, long and short-term modulations of galactic cosmic rays are discussed, giving attention to observations of modulation at high energies, a low energy solar cycle modulation, and mechanisms of modulation.

Mckibben, R. B.↗

NASA NTRS1980

Radiation induced rotation of interplanetary dust particles - A feasibility study for a space experiment

Irregular interplanetary dust particles may acquire a considerable spin rate due to two non-statistical dynamical mechanisms induced by solar radiation. These arise from variations in surface albedo discussed by Radzievskii (1954) and from irregularities in surface geometry discussed by Paddack (1969). An experiment is reported which will lead to an evaluation in space of the effectiveness of these two spin mechanisms. The technique of optical levitation in an argon laser beam provides a stable trap for particles 10-60 microns in diameter. The objective is to design an optical trap for dielectric particles in vacuum to study these rotation mechanisms in the gravity-free environment of a Spacelab experiment.

Ratcliff, K. F.↗

DOE OSTI2023

Spheroidization of Nd–Fe–B particles

Spherical powders are required for many advanced manufacturing techniques due to their inherent requirement of flowability, either within feed tubes or during powder spreading. As advanced manufacturing of magnets continues to develop, new production methods for feedstocks are also sought. Plasma spheroidization is a high-yield method to produce spherical Nd–Fe–B powders from irregularly shaped particles, with advantages including high throughput and a well-controlled size distribution. Highly spherical Nd–Fe–B powders with large scale production (i.e., kg) have been demonstrated using an inductively coupled thermal plasma system; however, the magnetic properties of the output powder display significant degradation. The coercivity was decreased from the initial 8 kOe (636 kA/m) of the as-received to 0.7 kOe (55 kA/m) for spheroidized powders. Microstructural investigation reveals 6% Nd depletion caused by the extreme temperatures of the plasma, leading to the formation of low-coercivity α-Fe and a subsequent decrease in energy product. In conclusion, post-spheroidization heat treatments with Nd can partially mitigate the coercivity degradation, increasing to 1.7 kOe (135 kA/m), potentially offering a pathway toward spherical powders for a range of applications.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Confocal Raman Microscopy as a Probe of Material Deconstruction in Processed Low-Density Polyethylene Particles

Confocal Raman microscopy was applied to detect structural change within individual particles of low-density polyethylene (LDPE) following chemical and electrochemical processing steps that aimed to facilitate material decomposition. A high numerical aperture (NA) oil-immersion objective enabled depth-profiling through the near surface region (20 μm–40 μm) of irregularly shaped particles with an axial spatial resolution < 2 μm estimated from measurements of instrument detection efficiency profiles. Changes in vibrational bands sensitive to polyethylene crystallinity were evident following treatments and linked to the release of low molecular weight compounds present as additives and products of processing. Effects of processing were probed by monitoring the rise of Raman scattering intensity in vibrational modes associated with polyethylene chains in a zig-zag (trans) conformation near 1128 cm –1 , 1294 cm –1 , and 1418 cm –1 , signaling chain clustering and development of organized, crystalline-like assemblies. Pristine LDPE particles displayed a uniform structure across the near surface region, while particles treated initially with chemical extractant and then further processed displayed increasingly enhanced crystallinity up to the maximum depth probed (40 μm). As a step toward measurements on ensembles of particles, least squares modeling was adapted to derive pure component spectra reflecting crystallinity change within spectral datasets. The work demonstrates high spatial resolution Raman depth-profiling for the characterization of processed polymers using a high NA immersion objective to overcome the limitations of air-objectives often used for confocal Raman microscopy.

Wahiduzzaman, Md. [Department of Chemistry and Bio↗

NASA NTRS2002

A New Method for Estimating the Single Scattering Phase Functions of Regolith Grains

Hapke's photometric model has been widely used in solar system remote sensing applications for nearly two decades. Recently, Hapke extended his model to describe the coherent-backscatter opposition effect and multiple-scattering by particles with anisotropic single particle phase functions (SPPF's). A practical difficulty for retrieving Hapke's model parameters from typical planet, satellite, and asteroid photometry data sets is that the model employs a large number of adjustable parameters (at least eight) that can be reliably constrained only for a small number of planetary data sets in which both disk-resolved and whole-disk observations are available from opposition to very large phase angles. The present work aims to reduce the number of adjustable parameters and preserve (or even enhance) the model's accuracy and usefulness by expressing Hapke's parameters in terms of more fundamental physical properties on which they mutually depend. The most difficult part of this task, described here, is to develop a simple method for computing the effective SPPF for structurally complex regolith grains from optical constants, grain-size distribution, and average regolith porosity. The development of light-scattering models for irregularly shaped particles is a large, complex subject and many sophisticated methods, such as Discrete Dipole Approximation (DDA) and Monte-Carlo simulations, have been explored elsewhere. Many of these methods are computationally intensive and probably impractical for routine substitution in Hapke's model. Here, progress is reported in developing a practical, semi-empirical method for estimating the directional scattering behavior (i.e. SPPF) of irregular regolith grains. The method employs Optical Transfer Function (OTF) techniques to model how the structural complexity of regolith particles broaden and attenuate the angular distribution of scattered light relative to that expected from ideal spherical particles of equivalent size and composition.

Helfenstein, P.↗

NASA NTRS1986

Preparation, analysis and release of simulated interplanetary grains into low Earth orbit

Astronomical observations which reflect the optical and dynamical properties of interstellar and interplanetary grains are the primary means of identifying the shape, size, and the chemistry of extraterrestrial grain materials. Except for recent samplings of extraterrestrial particles in near-Earth orbit and in the stratosphere observations were the only method of deducing the properties of extraterrestrial particles. In order to elucidate the detailed characteristics of observed dust, the observations must be compared with theoretical studies, some of which are discussed in this volume, or compared with terrestrial laboratory experiments. The formation and optical characterization of simulated interstellar and interplanetary dust with particular emphasis on studying the properties on irregularly shaped particles were discussed. Efforts to develop the techniques to allow dust experiments to be carried out in low-Earth orbit were discussed, thus extending the conditions under which dust experiments may be performed.

Stephens, J. R.↗

NASA NTRS2014

Topical Issue on Optical Particle Characterization and Remote Sensing of the Atmosphere: Part I

Increasing our understanding of the Earth-atmosphere system has been a scientific and political priority for the last few decades. This system not only touches on environmental science, but it has applicability to our broader understanding of planetary atmospheres in general. While this issue focuses primarily on electromagnetics, other fundamental fields of science, including fluid and thermodynamics play major roles. In recent years, significant research efforts have led to advances in the fields of radiative transfer and electromagnetic scattering from irregularly shaped particles. Recently, several workshops and small conferences have taken place to promote the fusion of these efforts. Late in 2013, for instance, two such meetings took place. The Optical Characterization of Atmospheric Aerosols (OCAA) meeting took place in Smolenice, Slovakia to promote a better understanding of microphysical properties of aerosol particles, and the characterization of such atmospheric particles using optical techniques. A complementary conference was organized in Nagoya, Japan, the 3rd International Symposium on Atmospheric Light Scattering and Remote Sensing (ISALSaRS), whose goal is to fuse the advances achieved in particle characterization with remote-sensing techniques. While the focus of these meetings is slightly different, they represent the same aspects of this rapidly growing field. This Topical Issue is the first of two parts. Within this issue we analyze different aspects of the problem of atmospheric characterization and present a broad overview of the topical area. Research includes theory and experiment, ranging from fundamental microphysical properties of individual aerosol particles to broad characterizations of atmospheric properties. Since this is an active field, we also have encouraged the submission of ideas for new methodologies that may represent the future of the field.

aerosols↗

DOE OSTI2021

Applicability of discrete element method with spherical and clumped particles for constitutive study of granular materials

Discrete element method (DEM) has been intensively used to study the constitutive behaviour of granular materials. However, to what extent a real granular material can be reproduced by virtual DEM simulations remains unclear. This study attempts to answer this question by comparing DEM simulations with typical features of experimental granular materials. Three groups of models with spherical and clumped particles are investigated from four perspectives: (i) deviatoric stress and volumetric behaviour; (ii) critical state behaviour; (iii) stress-dilatancy relationship; and (iv) the evolution of principal stress ratio against axial strain. The results demonstrate that DEM with spherical or clumped particles is capable of qualitatively describing macroscopic deviatoric stress responses, volumetric behaviour, and critical state behaviour observed in experiments for granular materials. On the other hand, some qualitative deviations between experiments and the investigated DEM simulations are also observed, in terms of the stress-dilatancy behaviour and principal stress ratio against axial strain, which are proven to be critical for constitutive modelling. The results demonstrate that DEM with spherical or clumped particles may not necessarily fully capture experimental features of granular materials even from a qualitative perspective. It is thus encouraged to thoroughly validate DEM with experiments when developing constitutive models based on DEM observations.

58 GEOSCIENCES↗

NASA NTRS2007

Dust in Cometary Comae: Present Understanding of the Structure and Composition of Dust Particles

In situ probing of a very few cometary comae has shown that dust particles present a low albedo and a low density, and that they consist of both rocky material and refractory organics. Remote observations of solar light scattered by cometary dust provide information on the properties of dust particles in the coma of a larger set of comets. The observations of the linear polarization in the coma indicate that the dust particles are irregular, with a size greater (on the average) than about one micron. Besides, they suggest, through numerical and experimental simulations, that both compact grains and fluffy aggregates (with a power law of the size distribution in the -2.6 to -3 range), and both rather transparent silicates and absorbing organics are present in the coma. Recent analysis of the cometary dust samples collected by the Stardust mission provide a unique ground truth and confirm, for comet 81P/Wild 2, the results from remote sensing observations. Future space missions to comets should, in the next decade, lead to a more precise characterization of the structure and composition of cometary dust particles.

Levasseur-Regourd, A. C.↗

DOE OSTI2021

An adaptive masking method for beam halo measurement by a digital micro mirror device

We report that in high intensity particle beams, irregularities in cathode emission, scattering effects, dark current and space charge forces can lead to a common phenomenon termed beam halo with associated emittance growth, beam loss and overall beam quality degradation. It is of fundamental interest and practical importance to precisely monitor such beam halo, which could offer valuable insights into the experimental strategy for the suppression of this undesired feature. A Digital Micro mirror Device (DMD) is a computer-controlled micro-electrical-mechanical system that contains a compact array of physically independent reflective mirrors. Using a standard DMD, we come up with an adaptive masking method for halo measurement, which demonstrates superior robustness and efficiency comparing to the conventional approaches as confirmed by simulation and experimental results. Our development includes an integrated package of hardware, software and a graphic user interface (GUI) that is robust and portable and can be applied as a beam halo diagnostic for electron guns or radiating charged particle beams in general.

43 PARTICLE ACCELERATORS↗

NASA NTRS1999

Optical Imaging of Flow Pattern and Phantom

Time-resolved optical imaging technique has been used to image the spatial distribution of small droplets and jet sprays in a highly scattering environment. The snake and ballistic components of the transmitted pulse are less scattered, and contain direct information about the sample to facilitate image formation as opposed to the diffusive components which are due to multiple collisions as a light pulse propagates through a scattering medium. In a time-gated imaging scheme, these early-arriving, image-bearing components of the incident pulse are selected by opening a gate for an ultrashort period of time and a shadowgram image is detected. Using a single shot cooled CCD camera system, the formation of water droplets is monitored as a function of time. Picosecond time-gated image of drop in scattering cells, spray droplets as a function of let speed and gas pressure, and model calcification samples consisted of calcium carbonate particles of irregular shapes ranging in size from 0. 1 to 1.5 mm affixed to a microscope slide have been measured. Formation produced by an impinging jet will be further monitored using a CCD with 1 kHz framing illuminated with pulsed light. The desired image resolution of the fuel droplets is on the 20 pm scale using early light through a highly scattering medium. A 10(exp -6)m displacement from a jet spray with a flow speed of 100 m/sec introduced by the ns grating pulse used in the imaging is negligible. Early ballistic/snake light imaging offers nondestructive and noninvasive method to observe the spatial distribution of hidden objects inside a highly scattering environment for space, biomedical, and materials applications. In this paper, the techniques we will present are time-resolved K-F transillumination imaging and time-gated scattered light imaging. With a large dynamic range and high resolution, time-gated early light imaging has the potential for improving rocket/aircraft design by determining jets shape and particle sizes. Refinements to these techniques may enable drop size measurements in the highly scattering, optically dense region of multi-element rocket injectors. These types of measurements should greatly enhance the design of stable, and higher performing rocket engines.

Galland, Pierre A.↗

DOE OSTI2022

Laser Additive Manufacturing Process Development for Bismuth Telluride Thermoelectric Material

Thermoelectric generators have strong potential for aerospace and aircraft applications. However, traditional manufacturing methods for thermoelectric devices severely limit device adaptability and consequently marketability. Laser powder bed fusion is an additive manufacturing method which shows promising potential for producing thermoelectric devices. Thermoelectric materials pose unique challenges compared to metals because of low thermal conductivity, brittle fracture characteristics, and irregular powder particle morphologies. Herein, we communicate processing procedures to fabricate thermoelectric parts of Bi 2 Te 3 through laser powder bed fusion. In this study, we identify the successful combination of key process parameters—laser power, scan speed, hatch distance, and powder layer thickness—to achieve high-quality parts in terms of density and physical properties, and we demonstrate the impact of process parameter variation on built part quality. While it cannot exclusively determine part quality, the volumetric energy density is a useful guide in deciding process parameters for thermoelectric materials, and the optimal value is between 9 and 11 J/mm 3 for Bi 2 Te 3 . We demonstrate successful fabrication of different freeform geometries of Bi 2 Te 3 powders. The results suggest it is possible to extend this method more broadly to other semiconductor materials, including thermoelectric power generation materials applicable for space applications.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Correlating 3D Surface Atomic Structure and Catalytic Activities of Pt Nanocrystals

Active sites and catalytic activity of heterogeneous catalysts is determined by their surface atomic structures. However, probing the surface structure at an atomic resolution is difficult, especially for solution ensembles of catalytic nanocrystals, which consist of heterogeneous particles with irregular shapes and surfaces. In this study, we constructed 3D maps of the coordination number (CN) and generalized CN ($\bar{C}\bar{N}$) for individual surface atoms of sub-3 nm Pt nanocrystals. Our results reveal that the synthesized Pt nanocrystals are enclosed by islands of atoms with nonuniform shapes that lead to complex surface structures, including a high ratio of low-coordination surface atoms, reduced domain size of low-index facets, and various types of exposed high-index facets. 3D maps of $\bar{C}\bar{N}$ are directly correlated to catalytic activities assigned to individual surface atoms with distinct local coordination structures, which explains the origin of high catalytic performance of small Pt nanocrystals in important reactions such as oxygen reduction reactions and CO electro-oxidation.

3D atomic structure↗

NASA NTRS1992

Debris and micrometeorite impact measurements in the laboratory

A method was developed to simulate space debris in the laboratory. This method, which is an outgrowth of research in inertial confinement fusion (ICF), uses laser ablation to accelerate material. Using this method, single 60 micron aluminum spheres were accelerated to 15 km/sec and larger 500 micron aluminum spheres were accelerated to 2 km/sec. Also, many small (less than 10 micron diameter) irregularly shaped particles were accelerated to speeds of 100 km/sec.

Resnick, J.↗

NASA NTRS2004

Optical Levitation of Micro-Scale Particles in Air

Success has been achieved using a radiation pressure gradient to levitate microscale particles in air for as long as four hours. This work is performed as a precursor to the development of a vacuum based optical tweezers interrogation tool for nanotechnology research. It was decided to first proceed with solving the problem of achieving optical levitation of a micro-scale particle in air before trying the same in a vacuum environment. This successful optical levitation in air confirms the work of Ashkin and Dziedzic. Levitation of 10 and 13.8 microns diameter polystyrene spheres was achieved, as well as the levitation of 10 and 100 microns diameter glass spheres. Particles were raised and lowered. A modicum of success was achieved translating particles horizontally. Trapping of multiple particles in one laser beam has been photographed. Also, it has been observed that particles, that may be conglomerates or irregular in shape, can also be trapped by a focused laser beam. Levitated glass beads were photographed using laser light scattered from the beads. The fact that there is evidence of optical traps in air containing irregular and conglomerate particles provides hope that future tool particles need not be perfect spheres.

Wrbanek, Susan Y.↗

NASA NTRS1992

Extracellular vesicles of calcifying turkey leg tendon characterized by immunocytochemistry and high voltage electron microscopic tomography and 3-D graphic image reconstruction

To gain insight into the structure and possible function of extracellular vesicles in certain calcifying vertebrate tissues, normally mineralizing leg tendons from the domestic turkey, Meleagris gallopavo, have been studied in two separate investigations, one concerning the electron microscopic immunolocalization of the 66 kDa phosphoprotein, osteopontin, and the other detailing the organization and distribution of mineral crystals associated with the vesicles as determined by high voltage microscopic tomography and 3-D graphic image reconstruction. Immunolabeling shows that osteopontin is related to extracellular vesicles of the tendon in the sense that its initial presence appears coincident with the development of mineral associated with the vesicle loci. By high voltage electron microscopy and 3-D imaging techniques, mineral crystals are found to consist of small irregularly shaped particles somewhat randomly oriented throughout individual vesicles sites. Their appearance is different from that found for the mineral observed within calcifying tendon collagen, and their 3-D disposition is not regularly ordered. Possible spatial and temporal relationships of vesicles, osteopontin, mineral, and collagen are being examined further by these approaches.

NASA Discipline Musculoskeletal↗

NASA NTRS2020

Differences in the Evolution of Pyrocumulonimbus and Volcanic Stratospheric Plumes as Observed by CATS and CALIOP Space-Based Lidars

Recent fire seasons have featured volcanic-sized injections of smoke aerosols into the stratosphere where they persist for many months. Unfortunately, the aging and transport of these aerosols are not well understood. Using space-based lidar, the vertical and spatial propagation of these aerosols can be tracked and inferences can be made as to their size and shape. In this study, space-based CATS and CALIOP lidar were used to track the evolution of the stratospheric aerosol plumes resulting from the 2019–2020 Australian bushfire and 2017 Pacific Northwest pyrocumulonimbus events and were compared to two volcanic events: Calbuco (2015) and Puyehue (2011). The pyrocumulonimbus and volcanic aerosol plumes evolved distinctly, with pyrocumulonimbus plumes rising upwards of 10 km after injection to altitudes of 30 km or more, compared to small to modest altitude increases in the volcanic plumes. We also show that layer-integrated depolarization ratios in these large pyrocumulonimbus plumes have a strong altitude dependence with more irregularly shaped particles in the higher altitude plumes, unlike the volcanic events studied.

Kenneth Christian↗