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DOE OSTI2025

Quantifying dispersity in size and shape of nanoparticles from small-angle scattering data using machine learning based CREASE

Here, we use machine learning (ML) enhanced computational reverse engineering analysis of scattering experiments (CREASE) to interpret small-angle X-ray scattering (SAXS) data obtained from a system of nanoparticles without a priori knowledge of their exact shapes (e.g. spheres or ellipsoids), sizes (0.5–50 nm) and distributions. The SAXS measurements yielded three categories of scattering profiles exhibiting 'strong', 'weak' and 'no' features. Diminishing features (e.g. broadening or disappearing peaks) in scattering profiles have always been attributed to the presence of significant dispersity in the system. Such featureless SAXS data are not suitable for traditional analysis using analytical models. If one were to fit a relevant analytical model (e.g. the lmfit analytical model for polydisperse spheres) to these 'weak' and 'no' SAXS profiles from our nanoparticle systems, one would obtain non-unique interpretations of the data. Relying on electron microscopy to identify the distributions of nanoparticle shapes and sizes is also unfeasible, especially in high-throughput synthesis and characterization loops. In such situations, to identify the distributions of particle sizes and shapes that could be present in the sample, one must rely on methods like ML-CREASE to interpret the data quickly and output all relevant interpretations about the structure present in the system. The ML-CREASE optimization loop takes the experimental scattering profile as input and outputs multiple candidate solutions whose computed scattering profiles match the SAXS profile input. The ML-CREASE method outputs distributions of relevant structural features, such as the volume fraction of the nanoparticles in the system and the mean and standard deviation of the particle size and aspect ratio, assuming a type of distribution (e.g. normal, log-normal) for size and aspect ratio. We find that, for the SAXS profiles analyzed here, accounting for the shape dispersity along with size dispersity of the nanoparticles using ML-CREASE improved the match between the computed scattering profiles and input experimental profiles.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

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 OSTI2026

Development of large-scale, 3D Printed high temperature ceramic material

Through this collaborative effort, a new 3D printing platform for ceramics called laser-induced slip casting (LIS) was explored and developed for improving the processing and manufacture of silicon carbide (SiC), a high temperature ceramic material. This method prints layers of ceramic slips/slurries with subsequent selective-laser heating to dry each layer to build a 3D structure. The completed and dried part is then sintered. This manufacturing process is inherently lower cost than alternative ceramic printing methods such as binder jet technology or stereolithography when it comes to the feedstock material but is more expensive than robocasting or direct ink writing. However, it has the potential to make more controlled parts with less defects compared to robocasting. The largest cost is the heating source for the printer. With this technique, there is potential to make large ceramic parts in a near-net shape. Further, there is no known commercial manufacturing of 3D printed ceramics that creates a large range of different high-density ceramics at large scale. The goals and outcomes for the development of the new printing technology were: 1) assessing the technology with alumina by characterizing coupons, 2) printing and sintering of silicon carbide (SiC), and 3) characterization and properties testing of materials printed and a scale-up of SiC part(s). Through this collaborative project, it was sought to provide the best solution to achieving highly dense and near-net shaped ceramic parts at large scale and reduced cost. The goal was to produce high density sintered materials for applications in defense, energy generating systems, armor, and wear parts using 3D printing methods. Variables including powder particle sizes, dispersant molecular weights (MWs), binders, printing parameters, and post processing were explored as well as the characterization of the physical properties (add specifics here).

36 MATERIALS SCIENCE↗

NASA NTRS2012

Fischer-Tropsch Cobalt Catalyst Improvements with the Presence of TiO2, La2O3, and ZrO2 on an Alumina Support

The objective of this study was to evaluate the effect of titanium oxide, lanthanum oxide, and zirconium oxide on alumina supported cobalt catalysts. The hypothesis was that the presence of lanthanum oxide, titanium oxide, and zirconium oxide would reduce the interaction between cobalt and the alumina support. This was of interest because an optimized weakened interaction could lead to the most advantageous cobalt dispersion, particle size, and reducibility. The presence of these oxides on the support were investigated using a wide range of characterization techniques such as SEM, nitrogen adsorption, x-ray diffraction (XRD), temperature programmed reduction (TPR), temperature programmed reduction after reduction (TPR-AR), and hydrogen chemisorptions/pulse reoxidation. Results indicated that both La2O3 and TiO2 doped supports facilitated the reduction of cobalt oxide species in reference to pure alumina supported cobalt catalysts, however further investigation is needed to determine the effect of ZrO2 on the reduction profile. Results showed an increased corrected cluster size for all three doped supported catalysts in comparison to their reference catalysts. The increase in reduction and an increase in the cluster size led to the conclusion that the support-metal interaction weakened by the addition of TiO2 and La2O3. It is also likely that the interaction decreased upon presence of ZrO2 on the alumina, but further research is necessary. Preliminary results have indicated that the alumina-supported catalysts with titanium oxide and lanthanum oxide present are of interest because of the weakened cobalt support interaction. These catalysts showed an increased extent of reduction, therefore more metallic cobalt is present on the support. However, whether or not there is more cobalt available to participate in the Fischer-Tropsch synthesis reaction (cobalt surface atoms) depends also on the cluster size. On one hand, increasing cluster size alone tends to decrease the active site density; on the other hand, by increasing the size of the cobalt clusters, there is less likelihood of forming oxidized cobalt complexes (cobalt aluminate) during Fischer-Tropsch synthesis. Thus, from the standpoint of stability, improving the extent of reduction while increasing the particle size slightly may be beneficial for maintaining the sites, even if there is a slight decrease in overall initial active site density.

Klettlinger, Jennifer Lindsey Suder↗

NASA NTRS2024

On the Role of Friction and Particle Size Distribution in Granular Packings

Packing of particles in a disordered arrangement has tremendous significance in both condensed matter physics and engineering applications. The last three decades have seen remarkable progress in our understanding of the physics of granular packings that has been largely facilitated by a rapid growth in the power of modern computers. Although granular packings are ubiquitous in diverse natural settings, from clogging of powders in hoppers to the crowding of living cells, a significant motivation for modeling granular packings has emerged from a proposal that the transition from a fluid-like state to a solid-like state of a granular material upon increasing volume fraction, called jamming, is intimately related to the origins of glass transition in thermal systems. As such, a majority of modeling efforts have focused on the jamming behavior of an idealized granular material: frictionless, monodisperse sphere. While such studies have illuminated the rich physics of jamming, granular materials in nature and engineering practice are rarely frictionless or monodisperse. The analogous research on the packing of these ‘real-world’ granular materials is still not fully developed. Besides requiring the exploration of a huge parameter space, three key computational considerations have inhibited their modeling: (i) traditional computational methods are not adept at simulating mechanically-stable packings of frictional particles near the jamming transition; (ii) standard algorithms of contact detection in discrete element methods are impractical to simulate granular packings with a wide distribution of particle sizes; (iii) a lack of well-established contact mechanics models of friction that can accurately reproduce experimental data. This chapter will review the latest computational advances to simulate the jamming of size-dispersed frictional particles, and describe the rich microstructural diversity that emerges in their packings.

granular↗

NASA NTRS1981

Ionic conductivity and thermoelectric power of pure and Al2O3-dispersed AgI

Ionic and electronic conductivities, and thermoelectric power have been measured for AgI and AgI containing a dispersion of submicron size Al2O3 particles. While the dispersion of Al2O3 enhances the ionic conductivity significantly, it does not affect the electronic properties of the matrix. The enhancement is a strong function of the size and concentration of the dispersoid. Various models have been tested to account for the enhanced conduction. However, the complex behavior of the present results points out the need for more sophisticated theoretical models. Ionic conduction and thermoelectric power data suggest that the dispersed Al2O3 generates an excess of cation vacancies and thereby enhances the conductivity and suppresses the thermoelectric power of the matrix. The individual heats of transport of cation interstitials and vacancies have been estimated and compared to their respective migration energies.

Shahi, K.↗

NASA NTRS1994

Flocculation and aggregation in a microgravity environment (FAME)

An experiment to study flocculation phenomena in the constrained microgravity environment of a space shuttle or space station is described. The small size and light weight experiment easily fits in a Spacelab Glovebox. Using an integrated fiber optic dynamic light scattering (DLS) system we obtain high precision particle size measurements from dispersions of colloidal particles within seconds, needs no onboard optical alignment, no index matching fluid, and offers sample mixing and shear melting capabilities to study aggregation (flocculation and coagulation) phenomena under both quiescent and controlled agitation conditions. The experimental system can easily be adapted for other microgravity experiments requiring the use of DLS. Preliminary results of ground-based study are reported.

Ansari, Rafat R.↗

NASA NTRS1981

Material response from Mach 0.3 burner rig combustion of a coal-oil mixture

Wedge shaped specimens were exposed to the combustion gases of a Mach 0.3 burner rig fueled with a mixture of 40 weight percent micron size coal particles dispersed in No. 2 fuel oil. Exposure temperature was about 900 C and the test duration was about 44 one hour cycles. The alloys tested were the nickel base superalloys, IN-100, U-700 and IN-792, and the cobalt base superalloy, Mar-M509. The deposits on the specimens were analyzed and the extent of corrosion/erosion was measured. The chemical compositions of the deposits were compared with the predictions from an equilibrium thermodynamic analysis. The experimental results were in very good agreement with the predictions.

Santoro, G. J.↗

NASA NTRS1984

Unsolved problems in planetary ring dynamics

Voyager photographic data are used for microscopic and macroscopic analyses of the dynamics of the Saturn rings. Attention is given to particle collisions, local velocity dispersion, the particle size distribution, mechanisms governing the ring structure and interactive effects with Saturn satellite orbits. The mechanical properties and collision dynamics of the particles are discussed, along with models for perturbed and unperturbed disks. The forces involved and true scale of particle erosion are considered, as are instabilities in the rings, satellite torques, resonances, and the time scale for the evolution of the satellite orbits. Finally, the possibility that angular momentum exchanges are occurring between individual rings and satellite orbits is examined.

Borderies, N.↗

DOE OSTI2025

Production of Creep-Resistant FeCrAl-ODS

Four ODS FeCrAl alloys with base alloy composition Fe-16Cr-4Al-2Mo-0.2Y (wt.%) were mechanically alloyed with minor additions of CeO 2 and Y 2 O 3 additions and were successfully extruded into rectangular-shaped bars. Two oxide compositions were explored, which were designated NC with oxide addition of 0.5CeO 2 plus 0.2Yin solution of the base alloy powder and PC with additions of 0.5CeO 2 and 0.7Y 2 O 3 to elevate the O level. The microstructure of both alloys revealed by SEM and EBSD to consist of very small grains with sizes of ~450-520 nm and weak texture components. Sub-size tensile specimens fabricated from both alloys were tensile tested from room temperature to 800ºC. The results for both alloys from room temperature to 400ºC showed very high strengths, but low ductilities, especially uniform strain. From 500ºC to 800ºC, the strengths decreased rapidly, and the ductilities increased significantly. The reason for the rapid decreases in tensile strengths above 500ºC for both alloys is not clear, but will require advanced characterization techniques including atom probe tomography, to determine the size and number density of the nano-size oxide particles, and TEM/EFTEM, for investigating the dispersion of nano-size oxide particles on grain boundaries to assess the Zener grain boundary pinning effect, which will hinder grain coarsening at high temperatures that may enhance the Hall Petch strengthening mechanism.

36 MATERIALS SCIENCE↗

NASA NTRS1999

Dispersion of 0.5- to 2-micron aerosol in microG and hypergravity as a probe of convective inhomogeneity in the lung

We used aerosol boluses to study convective gas mixing in the lung of four healthy subjects on the ground (1 G) and during short periods of microgravity (microG) and hypergravity ( approximately 1. 6 G). Boluses of 0.5-, 1-, and 2-micron-diameter particles were inhaled at different points in an inspiration from residual volume to 1 liter above functional residual capacity. The volume of air inhaled after the bolus [the penetration volume (Vp)] ranged from 150 to 1,500 ml. Aerosol concentration and flow rate were continuously measured at the mouth. The dispersion, deposition, and position of the bolus in the expired gas were calculated from these data. For each particle size, both bolus dispersion and deposition increased with Vp and were gravity dependent, with the largest dispersion and deposition occurring for the largest G level. Whereas intrinsic particle motions (diffusion, sedimentation, inertia) did not influence dispersion at shallow depths, we found that sedimentation significantly affected dispersion in the distal part of the lung (Vp >500 ml). For 0.5-micron-diameter particles for which sedimentation velocity is low, the differences between dispersion in microG and 1 G likely reflect the differences in gravitational convective inhomogeneity of ventilation between microG and 1 G.

NASA Discipline Cardiopulmonary↗

NASA NTRS2003

Effect of gravitational sedimentation on simulated aerosol dispersion in the human acinus

We studied the effect of gravitational sedimentation on the dispersion of 0.5 and 1 micrometer-diameter particle boluses within a two-dimensional symmetric six-generation model of the human acinus. Boluses were introduced at the beginning of a 2-s inspiration immediately followed by a 4-s expiration, in normal gravity (1 G) and in the absence of gravity (0 G). The flow corresponded to a flow rate at the mouth of 500 ml/s. In 0 G, simulated dispersion (Hsim) was 16 ml for both particle sizes. In 1 G, Hsim was 71 and 242 ml for 0.5 and 1 micrometer-diameter particles, respectively, showing the effect of gravitational sedimentation. The difference between experimental data (J. Appl. Physiol. 86 (1999) 1402) and simulations was independent of particle size. This suggests that the residual dispersion was independent of the intrinsic properties of the particles and was more likely due to other mechanisms such as ventilation inhomogeneities, cardiogenic oscillations and alveolar wall motion. c2003 Elsevier Science Ltd. All rights reserved.

short duration↗

DOE OSTI2025

Effect of particle shape on stratification in drying films of binary colloidal mixtures

The role of particle shape in evaporation-induced auto-stratification in polydisperse colloidal suspensions is explored with molecular dynamics simulations of mixtures of spheres and aspherical particles. A unified framework based on the competition between diffusion and diffusiophoresis is proposed to understand the effects of shape and size dispersity. In general, particles diffusing more slowly (e.g., larger particles) tend to accumulate more strongly at the evaporation front. However, larger particles have larger surface areas and therefore greater diffusiophoretic mobility. Hence, they are more likely to be driven away from the evaporation front via diffusiophoresis. For a rapidly dried bidisperse suspension containing small and large spheres, the competition leads to “small-on-top” stratification. Here, we employ a computational model in which the diffusion coefficient is inversely proportional to particle mass. For a mixture of spheres and aspherical particles with similar mass, the diffusion contrast is reduced, and the spheres are always enriched at the evaporation front as they have the smallest surface area for a given mass and, therefore, the lowest diffusiophoretic mobility. Furthermore, for a mixture of solid and hollow spheres that have the same outer radius and thus the same surface area, the diffusiophoretic contrast is suppressed, and the system is dominated by diffusion. Consequently, the solid spheres, which have a larger mass and diffuse more slowly, accumulate on top of the hollow spheres. Finally, for a mixture of thin disks and long rods that differ significantly in shape but have similar mass and surface area, both diffusion and diffusiophoresis contrasts are suppressed, and the mixture does not stratify.

Classical molecular dynamic simulations↗

NASA NTRS1974

Generation of a monodispersed aerosol

The identity and laboratory test methods for the generation of a monodispersed aerosol are reported on, and are subjected to the following constraints and parameters; (1) size distribution; (2) specific gravity; (3) scattering properties; (4) costs; (5) production. The procedure called for the collection of information from the literature, commercial available products, and experts working in the field. The following topics were investigated: (1) aerosols; (2) air pollution -- analysis; (3) atomizers; (4) dispersion; (5) particles -- optics, size analysis; (6) smoke -- generators, density measurements; (7) sprays; (8) wind tunnels -- visualization.

Schenck, H.↗

NASA NTRS2000

Apse-Alignment of the Uranian Rings

An explanation of the dynamical mechanism for apse-alignment of the eccentric Uranian rings is necessary before observations can be used to determine properties such as ring masses, particle sizes, and elasticities. The leading model relies on the ring self-gravity to accomplish this task, yet it yields equilibrium masses which are not in accord with Voyager radio measurements. We explore possible solutions such that the self-gravity and the collisional terms are both involved in the process of apse-alignment. We consider limits that correspond to a hot and a cold ring, and show that pressure terms may play a significant role in the equilibrium conditions for the narrow Uranian rings. In the cold ring case, where the scale height of the ring near periapse is comparable to the ring particle size, we introduce a new pressure correction pertaining to a region of the ring where the particles are locked in their relative positions and jammed against their neighbors, and the velocity dispersion is so low that the collisions are nearly elastic. In this case, we find a solution such that the ring self-gravity maintains apse-alignment against both differential precession (m = 1 mode) and the fluid pressure. We apply this model to the Uranian alpha ring, and show that, compared to the previous self-gravity model, the mass estimate for this ring increases by an order of magnitude. In the case of a hot ring, where the scale height can reach a value as much as fifty times larger than a particle size, we find velocity dispersion profiles that result in pressure forces which act in such a way as to alter the ring equilibrium conditions, again leading to a ring mass increase of an order of magnitude; however, such a velocity dispersion profile would require a different mechanism than is currently envisioned for establishing heating/cooling balance in a finite-sized, inelastic particle ring. Finally, we introduce an important correction to the model of Chiang and Goldreich.

Mosqueira, I.↗

NASA NTRS2019

Further Characterization of Aerosols Sampled on the International Space Station

Spacecraft cabin air quality is of fundamental importance to crew health, with concerns encompassing both gaseous contaminants and airborne particles. Quantification of spacecraft indoor aerosols will increase our understanding of crew exposure and cabin cleanliness. Aerosols on the International Space Station (ISS) have been sampled and brought back to Earth for analysis to characterize the airborne particulate matter in the cabin. Microscopic analyses have been performed to determine morphology and particle size information, and Energy Dispersive X-ray Spectroscopy (EDS) provides information on the chemical elements present in the particles. With the use of IntelliSEM software for computer-controlled scanning electron microscopy (CCSEM), this data provides particle size distribution information and statistics on particle materials. Many of the particles collected were made up of multiple elements and had uncommon morphologies compared to typical indoor aerosols on Earth. These characteristics are thought to be from unique formation mechanisms in the microgravity environment. Several notable particle types are examined further in this work. Bromine-containing particles and cadmium-containing particles are discussed as they constitute a health hazard to crew members. Humans in indoor living and working spaces are typically the single largest particle emission source, and this was observed in the sampled aerosols in ISS as well.

Sampling↗

NASA NTRS1990

Reexamination of data from the asteroid/meteoroid detector

A reexamination of the results of the Pioneer 10 and 11 Asteroid Meteoroid Detector, or Sisyphus, was carried out in the light of a recently derived theory characterizing interplanetary matter and the Zodiacal Light (ZL). Sisyphus measured individual meteoroids from reflected sunlight and ZL between meteoroid events. The results were questioned because meteoroid orbits could not be calculated as intended and the ZL as computed from individual meteoroids did not agree with values determined from the ZL mode and from the other ZL sensor on the spacecraft. It is first shown that, independent of any explanation, the measurements are, with high probability, valid and strongly correlated with the ZL. The model which explains the strange behavior of the Sisyphus instrument also resolves the enigma why the three dust experiments on the Pioneer 10 and 11 spacecraft produced extreme disparate results for the distribution and orbits of meteoric particles and the ZL. The theory based primarily on these measurements requires a population in the inner solar system of cold meteoroid material composed mainly of volatile molecules. These meteoroids in orbits of high eccentricity are called cosmoids. They are impulsively disrupted from solar heating, resulting in order of magnitude increases in optical cross section. The dispersed particles, predominantly micron sized, scatter most of the ZL and supply the polarization. The sublimation time in sunlight for micron sized particles of volatile composition opposes the gravitational flux increase expected in approaching the sun. The other two Pioneer 10/11 dust experiments were: the Imaging Photopolarimeter for the ZL, and the Meteoroid Detection Experiment that measured penetration of 25 micron (Pioneer 10) and 50 micron (Pioneer 11) thick walls of pressurized gas cells.

Soberman, Robert K.↗

NASA NTRS2000

Fiber-Optic Imaging Probe Developed for Space Used to Detect Diabetes Through the Eye

Approximately 16 million Americans have diabetes mellitus, which can severely impair eyesight by causing cataracts, diabetic retinopathy, and glaucoma. Cataracts are 1.6 times more common in people with diabetes than in those without diabetes, and cataract extraction is the only surgical treatment. In many cases, diabetes-related ocular pathologies go undiagnosed until visual function is compromised. This ongoing pilot project seeks to study the progression of diabetes in a unique animal model by monitoring changes in the lens with a safe, sensitive, dynamic light-scattering probe. Dynamic light scattering (DLS), has the potential to diagnose cataracts at the molecular level. Recently, a new DLS fiber-optic probe was developed at the NASA Glenn Research Center at Lewis Field for noncontact, accurate, and extremely sensitive particle-sizing measurements in fluid dispersions and suspensions (ref. 1). This compact, portable, and rugged probe is free of optical alignment, offers point-and-shoot operation for various online field applications and challenging environments, and yet is extremely flexible in regards to sample container sizes, materials, and shapes. No external vibration isolation and no index matching are required. It can measure particles as small as 1 nm and as large as few micrometers in a wide concentration range from very dilute (waterlike) dispersions to very turbid (milklike) suspensions. It is safe and fast to use, since it only requires very low laser power (10 nW to 3 mW) with very short data acquisition times (2 to 10 sec).

Ansari, Rafat R.↗