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DOE OSTI2025

Nanotomography for Quantitative 3D Particle Reconstruction

Particulates are ubiquitous across fuel cycle operations and carry critical information about particle formation, processing, and potential proliferation-related activities. Traditional analytical techniques, including micro-Raman spectroscopy and standard electron microscopy, are often limited in spatial resolution or dimensionality, particularly when used to examine metallic or submicron-scale features. Understanding particle morphology, phase distribution, and internal porosity is essential for constraining formation conditions, thermodynamic environments, and material transport behavior. In this report, we demonstrate the application of plasma focused ion beam nanotomography to reconstruct micron-scale particulates at nanoscale resolution. Using high-resolution backscattered electron imaging and Avizo software, we obtained 3D reconstructions that enabled quantitative analysis of particle morphology, phase composition, and internal voids. Representative examples include a Ta particle with a large central void and a composite particle with embedded tetrahedral crystalline structures. These reconstructions reveal structural and compositional details that are inaccessible through conventional 2D imaging. The results demonstrate that nanotomography provides both qualitative and quantitative insights into particle formation and behavior. Using nanotomography, porosity and phase distributions can be quantified to inform models of particle density, transport, and solidification conditions. Beyond technical insights, the workflow developed here establishes a transferable capability for analyzing heterogeneous particles and has potential applications in bulk materials studies via x-ray computed tomography or other volumetric imaging modalities. Ongoing efforts are focused on optimizing the workflow to process multiple particles simultaneously, increasing throughput and statistical robustness. Overall, this work illustrates the power of nanotomography as a tool for connecting particulate morphology to formation mechanisms, composition, and transport, thereby strengthening analytical capabilities for nuclear forensics, fuel cycle analysis, and related scientific investigations.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2020

Collaborative Research: Understanding Nanoparticle-Plasma Interactions in Dusty Non-Thermal Plasmas by Nanoparticle Probes and Online Aerosol Characterization (Final Technical Report)

This report describes results from the University of Minnesota’s contribution to studies performed under the award DE-SC0018202 (principal Investigator: Christopher J. Hogan Jr.. This award is a collaborative research grant with support equally provided to Case Western Reserve University and to the University of Illinois (with principal investigator R. Mohan Sankaran). To date ten peer-reviewed published papers have resulted from the studies performed with University of Minnesota personnel contributing; this report describes the results of these studies as well as several unpublished studies, grouped into seven separate study types. The overarching goal of the carried out studies was to understand nanoparticle behavior and dynamics in non-thermal plasma synthesis reactors, specifically adapting aerosol measurement technology to provide online measurements of particle size, charge, and structure in plasma reactor systems.

42 ENGINEERING↗

DOE OSTI2023

FY23 Update: Aerosol Sampling for the Canister Deposition Field Demonstration

This report describes the results of preliminary testing of aerosol monitoring equipment that will be used to continuously monitor the aerosol source term for the multi-year Canister Deposition Field Demonstration (CDFD). These data are required inputs for the development and validation of models for the deposition of dust and potentially corrosive salts on the surface of spent nuclear fuel (SNF) dry storage canisters. Surface salt loads correlate with the extent of corrosion damage on a metal surface, and potentially to the likelihood and timing of initiation of stress corrosion cracks. Aerosols will be monitored at the CDFD site using three instruments. A Dekati ® ELPI+ cascade impactor will be used for real-time monitoring of aerosol particle sizes. It will also collect dust in 14 size bins on impactor targets that can be chemically analyzed to determine the soluble salts present as a function of particle size. However, this instrument can only measure dried aerosols, with a diameter of <10 µm. The second instrument is a Topas laser particle size spectrometer, which provides real-time monitoring of aerosol particle sizes up to ~40 µm in size. It monitors both the ambient (potentially deliquesced) aerosol particle size distributions required for the dust deposition models and the distributions of the equivalent dried particles, allowing correlation with the Dekati ® data. However, it does not discriminate between inert dust particles and salt aerosols, and it does not retain samples of the different particle sizes for later analysis. The third instrument that will monitor aerosols at the CDFD site is a Clean Air Status and Trends Network (CASTNET) tower, which uses a multiple canister system to collect weekly samples for analysis to total suspended aerosol particle compositions and atmospheric gas concentrations. This status report describes work in FY23 to develop the capabilities for using these tools. In two training exercises, the cascade impactor and laser particle sizer were deployed in two different testing environments, one indoor and one outdoor. For the cascade impactor, the tests provided opportunities for the operators to familiarize themselves with impactor substrate preparation, and post-test sample removal and analysis. For the laser particle sizer, the tests were used to evaluate different instrument parameters, to determine the most appropriate settings for capturing transient events. Data and samples were collected for weeks to months for each test, and the results are presented here. In addition to the preliminary testing, contracts were developed with WSP Analytical Labs for sample preparation and analysis of the cascade impactor samples. The impactor tower from outdoor test was delivered to WSP and used to train the staff there in disassembly, sample extraction, sample analysis, and tower reassembly with new target substrates. These are tasks that WSP will be performing routinely for the CDFD project. The CASTNET system cannot be purchased or tested until an actual site has been selected for the CDFD test. Work for this FY has been restricted to preparation of contracts for purchasing the CASTNET tower, and for sample analysis, once the tower is in operation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS2024

A Multi‐Probe Automated Classification of Ice Crystal Habits During the IMPACTS Campaign

Although all ice crystals are unique, many can be grouped together by shape or habit, with members of a habit class sharing similar representations of properties such as fall velocity and growth rate. A decision tree algorithm designed to be adaptable to any particle imaging probe, thus enabling the creation of habit size distributions over a size range larger than that of any probe on its own, is used to classify ice crystals imaged by three airborne cloud probes in mid-latitude winter cyclones during the Investigation of Microphysics and Precipitation for Atlantic Coast-Threatening Snowstorms (IMPACTS) field campaign. Crystals are sorted into seven habit classes based on their morphological properties: sphere, column/needle, plate, graupel, dendrite, aggregate, and irregular. Although adaptability was its primary goal, the algorithm was found to be moderately skillful for identifying idealized habit images. Quantitative tests of the algorithm’s adaptability displayed mixed results, as Two-Dimensional Stereo Probe (2DS) classifications showed moderate correlation with Particle Habit Imaging and Polar Scattering Probe (PHIPS) classifications, but only weak correlation with High Volume Precipitation Spectrometer (HVPS) classifications. The algorithm was applied to random sets of images from each probe in a case study of a mesoscale snow band sampled on 7 February 2020. In the case study, qualitative analysis of particle images revealed general agreement on classifications among the probes, supporting the algorithm’s applicability to multiple cloud probes. Most classifications appeared correct upon manual inspection, suggesting that in practical use, the algorithm is reasonably able to classify non-idealized images.

Julian Schima↗

DOE OSTI2022

U Metal Oxidation with Steam (U)

The Savannah Rive National Laboratory 9SRNL) is evaluating a method to produce uranium oxide (UO 2 ) from uranium metal using steam. The typical methods for making UO 2 yield powders with particle-size ranges of 1 to 50 micron. The goal of the steam oxidation is to produce a depleted uranium (DU) product with a larger particle size that can be used as a surrogate for testing physical and mechanical process techniques to refine uranium and/or plutonium bearing residues. Several studies in the literature indicated that reactions between uranium metal and steam will yield UO 2 as fine powders in the 160 to 500 °C range, but granular materials form above 500°C. Above 880 °C, a hard compact scale forms on the U metal. Furthermore, sintering of UO 2 occurs at about 1300 °C, but it has been stated that the presence of steam enhances the sintering characteristics of UO 2 . Initial studies into the oxidation of DU metal in an atmosphere of argon and steam have been completed. Oxidation of depleted uranium metal in Ar/steam at 600, 710, 700, and 830 °C yielded at UO 2 product with little or no impurity at each temperature. Although not enough sample was available to perform sieve analysis for particle size distribution, SEM images reveal that a significant volume fraction of the products at 710, 770, and 830 °C exceeds 100 microns. The material produced at 600 °C was too fine for programmatic needs. Questions associated with the UO 2 include morphology of product, mechanical strength of the particles, and performance in milling operations. The size of the samples produced in these tests did not allow for quantitative assessment of particle size of mechanical strength. A qualitative assessment of the particles formed at 710, 770, and 830 °C was that the samples produced at 710 and 770 °C were friable, and the sample produced 830 °C had more mechanical strength. Sintering of the samples in Ar/steam at 970 °C appeared to increase the strength of the particles without changing their general particle size characteristics. Due to the small sample sizes, the increase in strength could not be quantified. If the sintering at 970 °C is inadequate, higher sintering temperatures in Ar/steam can be evaluated. Future work will increase scale of the steam oxidation conditions which yield the most-favorable particle-size distributions with sufficient mechanical strength for programming usage. Further consideration will be given to oxidation temperature, steam addition to the reaction vessel, U metal pretreatment, and sintering conditions after oxidation. The UO 2 production could involve a two-step process where particles are formed in steam at lower temperatures (700-850 °C) and then sintered in Ar/steam at elevated temperatures (950-1200 °C). Larger samples (50-100 g each) will provide sufficient UO 2 product for sieve analysis and assessment of mechanical strength relatives to subsequent milling operations.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1980

Magnetospheric multiprobes: Investigations and instrumentation

The multiprobe scientific objectives are to: (1) determine the spatial structure of plasma phenomena such as the aurora, convection reversals, and ion troughs; (2) separate spatial and temporal variations in these phenomena; (3) determine field aligned current densities; (4) perform multiple point analysis of particle beams, wave fields, and plasma clouds that are injected into the ionosphere and magnetosphere by Spacelab active experiment facilities. Trade studies described include: instrument accommodations, power, attitude determination, electric field antennas, storage and ejection, thermal control, tracking communications, command and data management, payload and mission specialist support, functional objectives, and orbital analysis.

Burch, J. L.↗

NASA NTRS2016

The Orion Exploration Flight Test Post Flight Solid Particle Flight Environment Inspection and Analysis

Orbital debris in the millimeter size range can pose a hazard to current and planned spacecraft due to the high relative impact speeds in Earth orbit. Fortunately, orbital debris has a relatively short life at lower altitudes due to atmospheric effects; however, at higher altitudes orbital debris can survive much longer and has resulted in a band of high flux around 700 to 1,500 km above the surface of the Earth. While large orbital debris objects are tracked via ground based observation, little information can be gathered about small particles except by returned surfaces, which until the Orion Exploration Flight Test number one (EFT-1), has only been possible for lower altitudes (400 to 500 km). The EFT-1 crew module backshell, which used a porous, ceramic tile system with surface coatings, has been inspected post-flight for potential micrometeoroid and orbital debris (MMOD) damage. This paper describes the pre- and post-flight activities of inspection, identification and analysis of six candidate MMOD impact craters from the EFT-1 mission.

Miller, Joshua E.↗

DOE OSTI2023

Computational fluid dynamic analysis of a novel particle-to-air fluidized-bed heat exchanger for particle-based thermal energy storage applications

Long-duration energy storage technologies are being targeted to enable cost-effective, decarbonized energy systems. Particle-based thermal energy storage systems are one promising technology by storing excess electricity or heat as sensible thermal energy in inexpensive, solid, inert particles. These systems are only possible if an effective and economical particle-to-working fluid heat exchanger exists. This study predicts the performance of a proposed, direct-contact, particle-to-air, pressurized fluidized-bed heat exchanger using computational fluid dynamics. The common Eulerian-Eulerian framework for modeling fluidized beds is first benchmarked to experimental results at a previously untested operating condition and application. Then, the benchmarked model evaluates the performance of a proposed design for a commercial-scale version of the novel particle-to-air heat exchanger. The results show pressure drop and gas-phase approach temperatures are advantageous compared to other proposed designs for particle-to-air heat exchangers in the literature; approach temperatures were less than 5 °C and gas-phase pressure drop across the fluidized bed was 32 kPa. The model also highlights the importance of gas distributor design and representation in the Eulerian-Eulerian framework to control fluidization behavior. In conclusion, the model built and benchmarked in this study can be leveraged to advance the design and analysis of these heat exchangers critical to the deployment of a promising long-duration energy storage technology.

25 ENERGY STORAGE↗

DOE OSTI2022

Quasilinear theory of general electromagnetic fluctuations including discrete particle effects for magnetized plasmas: General analysis

The general quasilinear Fokker–Planck kinetic equation for the gyrophase-averaged plasma particle distribution functions in magnetized plasmas is derived, making no restrictions on the energy of the particles and on the frequency of the electromagnetic fluctuations and avoiding the often made Coulomb approximation of the electromagnetic interactions. Here, the inclusion of discrete particle effects breaks the dichotomy of nonlinear kinetic plasma theory divided into the test particle and the test fluctuation approximation because it provides expression of both the non-collective and collective electromagnetic fluctuation spectra in terms of the plasma particle distribution functions. Within the validity of the quasilinear approach, the resulting full quasilinear transport equation can be regarded as a determining nonlinear equation for the time evolution of the plasma particle distribution functions.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

NASA NTRS1997

Soft Particle Spectrometer, Langmuir Probe, and Data Analysis for Aerospace Magnetospheric/Thermospheric Coupling Rocket Program

Under this grant two instruments, a soft particle spectrometer and a Langmuir probe, were refurbished and calibrated, and flown on three instrumented rocket payloads as part of the Magnetosphere/Thermosphere Coupling program. The flights took place at the Poker Flat Research Range on February 12, 1994 (T(sub o) = 1316:00 UT), February 2, 1995 (T(sub o) = 1527:20 UT), and November 27, 1995 (T(sub o) = 0807:24 UT). In this report the observations of the particle instrumentation flown on all three of the flights are described, and brief descriptions of relevant geophysical activity for each flight are provided. Calibrations of the particle instrumentation for all ARIA flights are also provided.

Sharber, J. R.↗

NASA NTRS2021

High Energy Particle Excitations as a Measure of Electronic Crosstalk in MODIS and VIIRS VIS/NIR Bands

The MODIS instruments aboard the Terra and Aqua satellites and the VIIRS instruments aboard the SNPP and NOAA-20 satellites each contain several arrays of Si detectors that measure Earth-reflected radiance in the visible and near-infrared spectral range. Even in the absence of incident light, the Si detectors are occasionally excited by high energy charged particles that pass through the spacecraft. These particle radiation events are, fortunately, infrequent enough that they do not lead to significant degradation of the detectors and they do not have a significant impact on the Earth scene radiance images. On the other hand, they are frequent enough that the cumulative data from many years on orbit may provide valuable diagnostic information about the sensors. In this paper, we provide some basic statistics on the frequency and magnitude of the particle excitation events for MODIS and VIIRS and explore the usefulness of this data as a measure of electronic crosstalk. Large amounts of crosstalk can degrade the quality of the Earth images, so it is crucial to have methods to characterize and correct for it on-orbit, which has previously been done for MODIS using lunar image analysis. The particle excitations can manifest as single-pixel spikes in the otherwise dark space view background, which may be an ideal source for evaluating crosstalk. We derive crosstalk coefficients between the NIR band detectors of Terra MODIS, and compare them to coefficients previously derived from lunar observations. The same approach is applied to SNPP VIIRS, which does not show any significant electronic crosstalk. While the HgCdTe detectors used in the MODIS and VIIRS infrared bands can also be excited by particle radiation, the magnitudes of the excitations are much smaller compared to the Si detectors and in general are not large enough to be useful for examining crosstalk.

MODIS↗

NASA NTRS1991

Particle size distributions in polar mesospheric clouds derived from solar mesosphere explorer measurements

Data from the visible and UV spectrometers on the Solar Mesosphere Explorer are used to derive the color ratios of the reflectance at 265, 296, and 393 nm of light scattered from polar mesospheric cloud particles. This analysis extends the spectral coverage into the visible region of the spectrum. The data reduction technique compared the cloud brightness to the brightness scattered from the background atmosphere at the same wavelength. The ratios determined in this way are independent of systematic errors in instrument radiometric calibration. The data are analyzed using theoretical determinations of the color ratios from the Mie theory of small particle scattering, assuming a lognormal distribution for the particle size dispersion. Here 'size' means the average radius of the sphere having the same ice volume. The present results confirm earlier findings that the effective sizes of polar mesospheric cloud particles are less than 70 nm. Still, there exists a small number of measurements which result in particle sizes of the order of 80 nm. Even for these large particle sizes the required vertical column content of water vapor does not exceed limits imposed by the available atmospheric water vapor concentrations.

Rusch, D. W.↗

DOE OSTI2025

Particle balance of deuterium during deuterium shattered pellet injection shutdown in DIII-D

A particle balance analysis was conducted during a deuterium (D 2 ) shattered pellet injection-induced plasma shutdown on the DIII-D tokamak to determine why less than 20% of the pellet material is assimilated into the core plasma by the mid-current quench (CQ). Initially, most of the D 2 is injected as frozen shards and ionized upon entering the vessel. During the thermal quench, ionized particles move to the divertors and subsequently to the center post (CP) walls, where they rapidly recycle and partially accumulate as neutrals without assimilating into the core plasma. In contrast, the particle flux to the outer midplane walls is negligible, despite being accompanied by hot plasma with electron temperatures exceeding 100 eV. During mid-CQ, volume recombination effects, although not large enough to impact overall particle balance, were significant enough to require accounting for accurate interpretation of fast-framing camera D-alpha signals and the estimation of the CP wall particle flux. In addition, toroidal asymmetries, observed in measurements of toroidal electron density perturbations and the phase of magnetohydrodynamic modes, are present throughout the shutdown and can account for a discrepancy in the assimilation rate for up to 50% of the observed D 2 particle inventory. These sources and sinks of particles and fluxes were identified using absolutely calibrated D-alpha brightness and Langmuir probes.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

NASA NTRS2008

Analysis of Thermal and Reaction Times for Hydrogen Reduction of Lunar Regolith

System analysis of oxygen production by hydrogen reduction of lunar regolith has shown the importance of the relative time scales for regolith heating and chemical reaction to overall performance. These values determine the sizing and power requirements of the system and also impact the number and operational phasing of reaction chambers. In this paper, a Nusselt number correlation analysis is performed to determine the heat transfer rates and regolith heat up times in a fluidized bed reactor heated by a central heating element (e.g., a resistively heated rod, or a solar concentrator heat pipe). A coupled chemical and transport model has also been developed for the chemical reduction of regolith by a continuous flow of hydrogen. The regolith conversion occurs on the surfaces of and within the regolith particles. Several important quantities are identified as a result of the above analyses. Reactor scale parameters include the void fraction (i.e., the fraction of the reactor volume not occupied by the regolith particles) and the residence time of hydrogen in the reactor. Particle scale quantities include the particle Reynolds number, the Archimedes number, and the time needed for hydrogen to diffuse into the pores of the regolith particles. The analysis is used to determine the heat up and reaction times and its application to NASA s oxygen production system modeling tool is noted.

Hegde, U.↗

NASA NTRS2009

Analysis of Thermal and Reaction Times for Hydrogen Reduction of Lunar Regolith

Hegde, U.↗

DOE OSTI2020

Real-time biomass feedstock particle quality detection using image analysis and machine vision

Abstract A common and costly challenge in the nascent biorefinery industry is the consistent handling and conveyance of biomass feedstock materials, which can vary widely in their chemical, physical, and mechanical properties. Solutions to cope with varying feedstock qualities will be required, including advanced process controls to adjust equipment and reject feedstocks that do not meet a quality standard. In this work, we present and evaluate methods to autonomously assess corn stover feedstock quality in real time and provide data to process controls with low-cost camera hardware. We explore the use of neural networks to classify feedstocks based on actual processing behavior and pixel matrix feature parameterization to further assess particle attributes that may explain the variable processing behavior. We used the pretrained ResNet neural network coupled with a gated recurrent unit (GRU) time-series classifier trained on our image data, resulting in binary classification of feedstock anomalies with favorable performance. The textural aspects of the image data were statistically analyzed to determine if the textural features were predictive of operational disruptions. The significant textural features were angular second moment, prominence, mean height of surface profile, mean resultant vector, shade, skewness, variation of the polar facet orientation, and direction of azimuthal facets. Expansion of these models is recommended across a wider variety of labeled feedstock images of different qualities and species to develop a more robust tool that may be deployed using low-cost cameras within biorefineries.

09 BIOMASS FUELS↗

NASA NTRS1971

Nature of the Martian surface as inferred from the particle-size distribution of lunar-surface material.

Analysis of lunar particle size distribution data indicates that the surface material is composed of two populations. One population is caused by comminution from the impact of the larger-sized meteorites, while the other population is caused by the melting of fine material by the impact of smaller-sized meteorites. The results are referred to Mars, and it is shown that the Martian atmosphere would vaporize the smaller incoming meteorites and retard the incoming meteorites of intermediate and large size, causing comminution and stirring of the particulate layer. The combination of comminution and stirring would result in fine material being sorted out by the prevailing circulation of the Martian atmosphere and the material being transported to regions where it could be deposited. As a result, the Martian surface in regions of prevailing upward circulation is probably covered by either a rubble layer or by desert pavement; regions of prevailing downward circulation are probably covered by sand dunes.

Mason, C. C.↗

DOE OSTI2025

A novel closed-form inversion of the convection–diffusion equation for rapid convection, diffusion, and source profile estimation

To simplify and routinize particle transport analysis in fusion devices, a novel closed form linear inversion of the 1-D convection diffusion equation to estimate diffusion and convection profiles D(r ⃗ ), v(r ⃗ ) and source distribution s(r ⃗ ), of a single species from measured data is derived and demonstrated on synthetic data. Profile estimates of D(r ⃗ ), v(r ⃗ ), s(r ⃗ ) and their uncertainties are given as a matrix expression constructed directly from the incoming density data of the transported species in space and time, as well as physics assumptions such as particle conservation and experimental geometry. The derived matrix expression can be applied to a pumped or non-pumped recycling species, or a non-recycling species that is effectively “pumped” by plasma-facing surfaces.

Hinson, Edward [ORNL] (ORCID:000000019713140X)↗