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DOE OSTI2024

Measurement report: The Fifth International Workshop on Ice Nucleation phase 1 (FIN-01): intercomparison of single-particle mass spectrometers

Knowledge of the chemical composition and mixing state of aerosols at a single-particle level is critical for gaining insights into atmospheric processes. One common tool to make these measurements is single-particle mass spectrometry. There remains a need to compare the performance of different single-particle mass spectrometers (SPMSs). An intercomparison of SPMSs was conducted at the Aerosol Interaction and Dynamics in the Atmosphere (AIDA) chamber at the Karlsruhe Institute of Technology (KIT) in November 2014, as part of the first phase of the Fifth International Workshop on Ice Nucleation (FIN-01). In this paper we compare size distributions and mass spectra of atmospherically relevant particle types measured by five SPMSs. These include different minerals, desert and soil dusts, soot, bioaerosol (Snomax; protein granule), secondary organic aerosol (SOA), and SOA-coated mineral particles. Most SPMSs reported similar vacuum aerodynamic diameter (d va ) within typical instrumental ranges from ~100–200 nm (lower limit) to ~2–3 µm (upper limit). In general, all SPMSs exhibited a wide dynamic range (up to ~10 3 ) and high signal-to-noise ratio (up to ~10 4 ) in mass spectra. Common spectral features with small diversities in mass spectra were found with high average Pearson's correlation coefficients, i.e., for average positive spectra r avg-pos =0.74 ± 0.12 and average negative spectra r avg-neg =0.67 ± 0.22. We found that instrument-specific detection efficiency (DE) was more dependent on particle size than particle type, and particle identification favored the use of bipolar, rather than monopolar, instruments. Particle classification from “blind experiments” showed that all instruments differentiated SOA, soot, and soil dust and detected subtle changes in the particle internal mixing but had difficulties differentiating among specific mineral types and dusts. This study helps to further understand the capabilities and limitations of the single-particle mass spectrometry technique in general and the specific performance of the instrument in characterizing atmospheric aerosol particles.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2025

Effect of Plutonium on Uranium Oxide Microstructural Fingerprint

The analysis of particulates from environmental sampling is routinely performed for nuclear forensics applications. In order to increase the tools available for nuclear forensics applications, capability development materials (CDMs), or reference particulates, are necessary for developing and benchmarking new analytical methods. Historically, these CDM particulates have been produced with highly controlled and characterized isotopic and size parameters for applications in developing and benchmarking particle sizers and mass spectrometry analytical methods [1- 4]. However, the development of CDMs with highly characterized particle morphology and phase of the particles is vital for aiding in the development and benchmarking of particle analytical methods for those parameters. In many cases, key properties such as crystallographic phase, morphology, and microstructure, may be correlated to processing history of environmental sampling particulates [5]. To that end, this work investigates determining the structural fingerprint of produced Pu-doped uranium oxide CDMs using transmission electron microscopy (TEM). The particulates, one of which shown in Figure 1, were synthesized to Fig. 1. Single particulate of uranium oxide fabricated using the THESEUS technique. develop capabilities for environmental sampling investigations. These particles are monodisperse at diameter of 1 μm and a range of plutonium concentrations from 0- 1,000 ppm. Given their small diameter, TEM analysis was ideal for studying the particulate structural fingerprint in detail. Previous investigations confirmed the external homogeneity of the particulates at different plutonium concentrations, however this analysis focuses on determining the grain structure, phase distribution, and porosity of the particulates.

Mayer, Jack [Univ. of Florida, Gainesville, FL (Un↗

DOE OSTI2024

Weak shock compaction on granular salt

This study conducted integrated experiments and computational modeling to investigate the speeds of a developing shock within granular salt and analyzed the effect of various impact velocities up to 245 m/s. Experiments were conducted on table salt utilizing a novel setup with a considerable bore length for the sample, enabling visualization of a moving shock wave. Experimental analysis using particle image velocimetry enabled the characterization of shock velocity and particle velocity histories. Mesoscale simulations further enabled advanced analysis of the shock wave’s substructure. In simulations, the shock front’s precursor was shown to have a heterogeneous nature, which is usually modeled as uniform in continuum analyses. The presence of force chains results in a spread out of the shock precursor over a greater ramp distance. With increasing impact velocity, the shock front thickness reduces, and the precursor of the shock front becomes less heterogeneous. Furthermore, mesoscale modeling suggests the formation of force chains behind the shock front, even under the conditions of weak shock. This study presents novel mesoscale simulation results on salt corroborated with data from experiments, thereby characterizing the compaction front speeds in the weak shock regime.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2022

Particle–hole asymmetry and quantum confinement effects on the magneto-optical response of topological insulator thin-films

Intrinsically broken symmetries in the bulk of topological insulators (TIs) are manifested in their surface states. Despite particle–hole asymmetry in TIs, it has often been assumed that their surface states are characterized by a particle–hole symmetric Dirac energy dispersion. In this work, we demonstrate that the effect of particle–hole asymmetry is essential to correctly describe the energy spectrum and the magneto-optical response in TIs thin-films. In thin-films of TIs with a substantial degree of particle–hole symmetry breaking, such as Sb 2 Te 3 , the longitudinal optical conductivity displays absorption peaks arising from optical transitions between bulk and surface Landau levels for low photon energies. The transition energies between the bulk and surface Landau levels exhibit clearly discernable signatures from those between surface Landau levels due to their distinct magnetic field dependence. Furthermore, bulk contributions to the magneto-optical conductivity in a TI thin-film are enhanced via one type of doping while being suppressed by the other. This asymmetric dependence on the type of doping aids in revealing the particle–hole asymmetry in TI thin-films.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Orbit modeling of fast particle redistribution induced by sawtooth instability

Initial tests on the National Spherical Torus Experiment Upgrade (NSTX-U) (Menard et al 2012 Nucl. Fusion 083015) device suggest that introducing energy selectivity for sawtooth induced fast ion redistribution is required to improve the agreement between experimental and simulated quantities such as neutron rate and Fast-Ion D-Alpha profiles. The aim of this work is to assess the requirements to properly describe the behaviour of fast ions during a sawtooth crash for predictive sawtooth simulations. As the first step, in this work, we use the particle-following Orbit code to characterize the redistribution of fast particles. In order for a sawtooth crash to be simulated, a spatial and temporal displacement is implemented into the Orbit code. The perturbation amplitude is determined by comparison with experimental measurement of the neutron rate drop. The characteristics of fast ions with different orbit types are investigated in phase and real space. Due to a sawtooth crash, fast ion energy and angular momentum are modified resulting in the redistribution in phase space and orbit type change. The redistribution of fast ions in real space shows that the sawtooth instability brings different effect on fast particles with different orbit types as observed in experiments. Finally, the initial interpretative Transp simulation using the so-called kick model based on the Orbit modeling result shows an improvement of fast ion redistribution before and after a sawtooth crash but the neutron rate still has discrepancy compared to the experimental measurement.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2019

Plutonium Particles in Samples Extracted from Hanford Tank Waste TX-118 and SY-102 (Interim Report)

This is an interim report on the characterization of plutonium particles from Hanford wastes. Plutonium-bearing particles were located in Hanford Waste Tank solids, SY-102 and TX-118. The particles in SY-102 were small, typically < 5 to 10 µm in length, and were crystalline plutonium oxide with an association of other elements at minor levels, including bismuth, phosphate, and iron based on Sanning Electron Microscopy (SEM) observations. Plutonium particles from SY-102 were extracted from the surface mount using the SEM-Focused Ion Beam (FIB) and prepared for Scanning Transmission Electron Microscopy (STEM). This was the first time that this type of analysis of Hanford tank waste solids has been attempted. The STEM analysis indicated a complex co-precipitation of plutonium oxide with bismuth and phosphate. Diffraction and imaging only partially matched with a PuO 2 phase. Pockets of phosphate and bismuth reside within the plutonium oxide suggesting that these phases formed at the same time. The SEM analysis indicated that the plutonium particles from TX-118 were a mixed bismuth-phosphate phase and plutonium oxide. These particles will be examined with SEM-FIB at a later time and then will undergo more detailed examination in the STEM.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRSDate not supplied

AM Powder Flowability Capabilities at NASA Marshall Space Flight Center (MSFC)

Additive Manufacturing (AM) powder flowability is critical to metal 3D printing, because the more fluid the powder is, the better powder spreads. The NASA MSFC’s Contamination Control Team (CCT) studies density, flow, particle size distribution, and morphology for programs such as Moon-to-Mars Planetary Autonomous Construction Technology (MMPACT), ASTM Proficiency Testing for AM and Powder Metallurgy, and MSFC’s AM team. Examining and measuring powder characteristics is essential for improving flowability of AM powder and ensuring lot-to-lot consistency, which will help to prevent defects in manufactured parts. The CCT uses several methods to characterize AM powder. Optical particle size distribution and morphology analyses determine particle parameters including size, circularity, convexity, and dimensions. The Carney and Hall Flowmeter Funnel measures time it takes powder to flow through a funnel to compare relative flowability (free-flowing and non-free-flowing). In addition to this, the device utilizes a density cup which determines apparent density. Lastly, the Revolution Powder Analyzer measures dynamic powder flowability and behavior over time via digital imaging. Using the CCT’s lab, the team has produced ASTM Powder Proficiency Testing results with flow rates, apparent density, particle size distribution, and tap density on titanium-based and nickel-based powder and compared data with other companies/labs. Morphology data was also collected for various regolith simulant powder for the MMPACT program. Lastly, the CCT used morphology data to examine the flowability of Inconel 718 powder for Selective Laser Melting (SLM) and Directed Energy Deposition (DED) printers at MSFC. The CCT’s essential work in studying and enabling AM powder characterization has helped and will continue to help study new and refined powders in the AM industry.

Additive Manufacturing↗

DOE OSTI2019

Conformally soft photons and gravitons

The four-dimensional S-matrix is reconsidered as a correlator on the celestial sphere at null infinity. Asymptotic particle states can be characterized by the point at which they enter or exit the celestial sphere as well as their SL(2, C) Lorentz quantum numbers: namely their conformal scaling dimension and spin h±h¯ instead of the energy and momentum. This characterization precludes the notion of a soft particle whose energy is taken to zero. We propose it should be replaced by the notion of a conformally soft particle with h = 0 or h¯ = 0. For photons we explicitly construct conformally soft SL(2, C) try on the celestial sphere. For gravity the generator of celestial conformal symmetry is constructed from a (2, 0) SL(2, C) primary wavefunction. Interestingly, BMS supertranslations are generated by a spin-one weight (3/2, 1/2) operator, which nevertheless shares holomorphic characteristics of a conformally soft operator. This is because the right hand side of its OPE with a weight (h, h¯) operator Oh,h¯ involves the shifted operator Oh+1/2,h¯+1/2. This OPE relation looks quite unusual from the celestial CFT 2 perspective but is equivalent to the leading soft graviton theorem and may usefully constrain celestial correlators in quantum gravity.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2026

Aircraft-derived particle fluxes distinguish entrainment zone and decoupled layer nucleation in marine boundary layers

The vertical distribution of freshly nucleated aerosol particles in the marine boundary layer remains poorly constrained, limiting our ability to represent new particle formation in climate models. Here we characterize 3–10 nm particle events, termed small particle events (SPEs), by deriving their vertical turbulent fluxes from aircraft measurements during the Aerosol and Cloud Experiments in the Eastern North Atlantic (ACE-ENA) campaign. To overcome stationarity limitations of traditional eddy covariance methods, we applied continuous wavelet transform analysis to data collected during June–July 2017 and January–February 2018 flights over the Azores. Our flux-based analysis revealed two distinct SPE scenarios with different vertical structures and spatial extents. The first featured nucleation in the entrainment zone, where free tropospheric air entrains into the boundary layer. The second showed nucleation in the decoupled layer, a stratified region between the well-mixed surface layer and cloud-topped upper boundary layer. In both cases, convergence of air masses from different layers diluted preexisting aerosol surface area to very low levels, creating conditions favorable for nucleation and generating strong downward particle fluxes. SPEs occurred in 15 % of flights, challenging prevailing theoretical expectations that new particle formation should rarely occur in marine boundary layers due to high condensation and coagulation sink capacity of sea spray aerosols. Aircraft-derived particle fluxes provide first observational constraints on the vertical location and source strength of likely nucleation regions in the remote marine boundary layer, improving aerosol source representations in climate models and reducing uncertainties in aerosol-cloud interactions.

Rasheeda Satheesh, Ajmal [North Carolina State Uni↗

DOE OSTI2025

Effects of Particle Mixing and Gravitational Settling on Charge Transport in Carbon Flow-Electrode Cells

Flowable carbon slurries are actively studied and under development for charge transport in various electrochemical systems including flow capacitors, capacitive deionization cells, semi-solid flow batteries, and lithium extraction. However, much less is known about in operando slurry flow dynamics and their corresponding effect on charge transport. We performed an experimental study of mixing and settling dynamics of slurry electrodes within an electrochemical flow cell during continuous operations. The electrochemical cell consisted of two horizontal co-flowing channels, separated by a cation-exchange membrane (CEM). Here we used high-speed optical imaging of planes parallel to gravity and simultaneous electrochemical measurements. At low flow rates, dense yet dynamic particle beds formed on the bottom electrode in each channel, which unexpectedly yielded the highest currents. This approach enables the operation of the flow cell at low system-average particle concentrations while leveraging gravity-driven particle settling to locally enhance carbon concentrations precisely at the current collector sites. Conversely, high flow rates were characterized by thin particle beds and well-mixed particle flows. In the latter case, the electrodes in closest proximity (located on either side of the CEM) achieved a current higher than the other electrode pairs. The observations have implications for slurry control and electrode designs in electrochemical systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2019

Novel amorphous SiOC dispersion-strengthened austenitic steels.

Here, a novel amorphous silicon oxycarbide dispersion-strengthened (SiOC-DS) austenitic steel has been fabricated via a powder metallurgy process. The microstructure of dispersion particles has been characterized by transmission electron microscopy (TEM) and electron backscatter diffraction (EBSD), revealing that amorphous SiOC nanoparticles with an average particle size of 30 nm were homogeneously distributed in the austenite grains with a sub-micrometer grain size. The high strength and hardness of SiOC-DS may be attributed to grain boundary strengthening, as well as dispersion strengthening via dislocation–particle interactions that were revealed by TEM investigations. In situ ion irradiation experiments showed that amorphous SiOC particles were stable after irradiation of 3.7 dpa, and the SiOC/steel interface can be an effective sink for the annihilation of irradiation defects. The excellent mechanical and irradiation properties of SiOC-DS austenitic steel make it a promising structural material for nuclear applications.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Phase-field model of precipitation processes with coherency loss

A phase-field model is proposed to simulate coherency loss coupled with microstructure evolution. A special field variable is employed to describe the degree of coherency loss of each particle and its evolution is governed by a Ginzburg-Landau type kinetic equation. For the sake of computational efficiency, a flood-fill algorithm is introduced that can drastically reduce the required number of field variables, which allows the model to efficiently simulate a large number of particles sufficient for characterizing their statistical features during Ostwald ripening. The model can incorporate size dependence of coherency loss, metastability of coherent particles, and effectively incorporate the underlying mechanisms of coherency loss by introducing a so-called differential energy criterion. The model is applied to simulate coarsening of Al 3 Sc precipitates in aluminum alloy and comprehensively compared with experiments. Our results clearly show how the particle size distribution is changed during coherency loss and affects the coarsening rate.

36 MATERIALS SCIENCE↗

NASA NTRS1989

NASA-UVA light aerospace alloy and structures technology program

The report on progress achieved in accomplishing of the NASA-UVA Light Aerospace Alloy and Structures Technology Program is presented. The objective is to conduct interdisciplinary graduate student research on the performance of next generation, light weight aerospace alloys and associated thermal gradient structures in close collaboration with researchers. The efforts will produce basic understanding of material behavior, new monolithic and composite alloys, processing methods, solid and fluid mechanics analyses, measurement advances, and a pool of educated graduate students. The presented accomplishments include: research on corrosion fatigue of Al-Li-Cu alloy 2090; research on the strengthening effect of small In additions to Al-Li-Cu alloys; research on localized corrosion of Al-Li alloys; research on stress corrosion cracking of Al-Li-Cu alloys; research on fiber-matrix reaction studies (Ti-1100 and Ti-15-3 matrices containing SCS-6, SCS-9, and SCS-10 fibers); and research on methods for quantifying non-random particle distribution in materials that has led to generation of a set of computer programs that can detect and characterize clusters in particles.

Gangloff, Richard P.↗

DOE OSTI2022

Analysis of hydrogen fueling, recycling, and confinement at Wendelstein 7-X via a single-reservoir particle balance

Abstract A single-reservoir particle balance for the main plasma species hydrogen has been established for W7-X. This has enabled the quantitative characterization of the particle sources in the standard island divertor configuration for the first time. Findings from attached scenarios with two different island sizes with a boronized wall and turbo molecular pumping are presented. Fueling efficiencies, particle flows and source locations were measured and used to infer the total particle confinement time τ p . Perturbative gas injection experiments served to measure the effective particle confinement time τ p * . Combining both confinement times provides access to the global recycling coefficient R ¯ . Hydrogen particle inventories have been addressed and the knowledge of particle sources and sinks reveals the core fueling distribution and provides insight into the capability of the magnetic islands to control exhaust features. Measurements of hydrogen fueling efficiencies were sensitive to the precise fueling location and measured between 12% and 31% with the recycling fueling at the strike line modeled at only 6%, due to much higher densities. 15% of the total 5.2 × 10 22 a/s recycling flow ionizes far away from the recycling surfaces in the main chamber. It was shown that 60% of recycled particles ionize above the horizontal and 18% above the vertical divertor target, while the remainder of the recycling flow ionizes above the baffle (7%). Combining these source terms with their individual fueling efficiencies resolves the core fueling distribution. Due to the higher fueling efficiency in the main chamber, up to 51% of the total 5.1 × 10 21 s −1 core fueling particles are entering the confined plasma from the main chamber. τ p values in the range of 260 ms were extracted for these discharges. Together with τ p , the global recycling coefficient R ¯ was resolved for every τ p * measurement and a typical value close to unity was obtained. An increase of the island size, resulted in no change of τ p , but doubled τ p * , indicating the feasibility of the control coils as an actuator to control exhaust features without affecting core confinement properties.

recycling↗

DOE OSTI2025

Development and characterization of an aerosol-generated multi-method analytical particle test material

Ceria (CeO 2 ) particles with low to ultra-low loading of nickel dopant were produced using an aerosol-based, droplet-to-particle synthesis via an in-line calcination technique. This aerosol-based synthesis method enables the production of particles with a monodisperse size distribution. These produced and well-characterized, multi-element, ceria-based particles demonstrate a material exemplar for multi-method analytical testing. They were prepared from a cerium nitrate feedstock where low loading nickel dopant was added at target Ni/(Ni + Ce) atomic percents of 1 %, 0.1 %, and 0.01 %, using a nickel nitrate spike. This methodology proved to produce ceria particles doped with a dynamic range of low to ultra-low loadings of nickel over a 24-h period, with consistent size distribution, morphology, and composition. The successful incorporation of nickel was demonstrated with bulk and single particle inductively coupled plasma mass spectroscopy and revealed notable particle-to-particle elemental homogeneity. X-ray photoelectron spectroscopy demonstrated the presence of a high concentration of nickel dopant incorporated preferentially toward the surface of the particles, and that this dopant aided oxidation of surface Ce(III) atoms to Ce(IV). These particle test materials were then validated through X-ray absorption near edge spectroscopy, comparing the ultra-low 0.01 % Ni and low 1 % Ni-doped ceria samples. This revealed a more-reduced oxidation state of the nickel with an increase in dopant concentration. Finally, this work demonstrates a synthesis and systematic characterization scheme to produce multi-method analytical test particulates.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Spectro-Microscopic Investigation of the Aerosol Impact on Hydrological Processes

This project investigated physico-chemical characteristics of atmospheric particles collected during DOE ARM field campaigns and how they are involved in the hydrological cycle. Our efforts were focused on multi-modal chemical imaging and molecular characterization of atmospheric particles and snow samples collected during the Surface-Atmosphere Integrated Field Laboratory (SAIL) campaign and particle samples from the Tracking Aerosol Convection Interactions ExpeRiment (TRACER) campaign.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2003

Solar Particle Events Observed by the Odyssey MARIE Instrument at Mars: Dose and Model Calculations

One of the primary concerns prior to human exploration of Mars is the need to accurately characterize the charged particle radiation environment both for the surface stay, and for the transit period to and from the planet. The Odyssey spacecraft, currently in Mars orbit includes a charged particle radiation detector, MARIE, which can measure particle fluxes with energies above approx. 30 MeV and charges between 1 and 10. Two classes of particles are of particular interest: the Galactic Cosmic Rays, (GCR), and those charged particles associated with Solar Particle Events, (SPE). The GCR are present continuously throughout the solar activity cycle, and their numbers vary inversely with the level of solar activity. They are characteristically more energetic than those particles originating from solar activity, and hence less influences by the solar magnetic field.

Cleghorn, T. F.↗

NASA NTRS2007

Measurement of Primary Ejecta From Normal Incident Hypervelocity Impact on Lunar Regolith Simulant

The National Aeronautics and Space Administration (NASA) continues to make progress toward long-term lunar habitation. Critical to the design of a lunar habitat is an understanding of the lunar surface environment. A subject for further definition is the lunar primary ejecta environment. The document NASA SP-8013 was developed for the Apollo program and is the latest definition of the primary ejecta environment. There is concern that NASA SP-8013 may over-estimate the lunar primary ejecta environment. NASA's Meteoroid Environment Office (MEO) has initiated several tasks to improve the accuracy of our understanding of the lunar surface primary ejecta environment. This paper reports the results of experiments on projectile impact into pumice targets, simulating lunar regolith. The Ames Vertical Gun Range (AVGR) was used to accelerate spherical Pyrex projectiles of 0.29g to velocities ranging between 2.5 km/s and 5.18 km/s. Impact on the pumice target occurred at normal incidence. The ejected particles were detected by thin aluminum foil targets placed around the pumice target in a 0.5 Torr vacuum. A simplistic technique to characterize the ejected particles was formulated. Improvements to this technique will be discussed for implementation in future tests.

Edwards, David L.↗