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DOE OSTI2022

A novel flow cell for optical particle analyzers—application to measurements of Malvern Insitec under high pressure and temperature

A flow cell is a necessary measurement interface for some important optical analyzers. In our application of the flow cell, we utilize a state-of-the-art optical analyzer (Malvern Insitec) to measure particle size distribution and concentration in-situ in a sampled flow from a novel pressurized oxygen-fuel combustion process. However, since this sampling flow is a flow of moist flue gas under high temperature and pressure, and the flow contains particles and corrosive acid gases, it is an extreme challenge to obtain a flow cell with a high optical quality that does not perturb the measurement. To address this challenge, we propose a new design for an optical flow cell. By using a unique flow field in the proposed flow cell, the measurement zone can be well defined by the sampling flow, minimizing the influence of purge flow. To demonstrate this flow cell, we have built a test system, and conduct measurements utilizing polydisperse-particle standards (10-100 µm and 1-10 µm). The results reveal that the optical windows are well protected by the purge flow field, without risk of deposition from the sampling flow, and the Malvern Insitec can measure the particle size distribution by using this flow cell, without generating sample bias.

Cheng, Mao↗

DOE OSTI2024

Indirect additive manufacturing process for fabricating bonded soft magnets

A bonded soft magnet object comprising bonded soft magnetic particles of an iron-containing alloy having a soft magnet characteristic, wherein the bonded soft magnetic particles have a particle size of at least 200 nm and up to 100 microns. Also described herein is a method for producing the bonded soft magnet by indirect additive manufacturing (IAM), such as by: (i) producing a soft magnet preform by bonding soft magnetic particles with an organic binder, wherein the magnetic particles have an iron-containing alloy composition with a soft magnet characteristic, and wherein the particles of the soft magnet material have a particle size of at least 200 nm and up to 100 microns; (ii) subjecting the preform to an elevated temperature sufficient to remove the organic binder to produce a binder-free preform; and (iii) sintering the binder-free preform at a further elevated temperature to produce the bonded soft magnet.

Paranthaman, Mariappan Parans↗

DOE OSTI2021

Polarimetric Radar Variables in Snowfall at Ka- and W-Band Frequency Bands: A Comparative Analysis

Dual-frequency millimeter-wavelength radar observations in snowfall are analyzed in order to evaluate differences in conventional polarimetric radar variables such as differential reflectivity (ZDR) specific differential phase shift (K DP ) and linear depolarization ratio (LDR) at traditional cloud radar frequencies at Ka and W bands (~35 and ~94 GHz, correspondingly). Low radar beam elevation (~5°) measurements were performed at Oliktok Point, Alaska, with a scanning fully polarimetric radar operating in the horizontal–vertical polarization basis. This radar has the same gate spacing and very close beam widths at both frequencies, which largely alleviates uncertainties associated with spatial and temporal data matching. It is shown that observed Ka- and W-band Z DR differences are, on average, less than about 0.5 dB and do not have a pronounced trend as a function of snowfall reflectivity. The observed Z DR differences agree well with modeling results obtained using integration over nonspherical ice particle size distributions. For higher signal-to-noise ratios, KDP data derived from differential phase measurements are approximately scaled as reciprocals of corresponding radar frequencies indicating that the influence of non-Rayleigh scattering effects on this variable is rather limited. This result is also in satisfactory agreement with data obtained by modeling using realistic particle size distributions. Observed Ka- and W-band LDR differences are strongly affected by the radar hardware system polarization “leak” and are generally less than 4 dB. Smaller differences are observed for higher depolarizations, where the polarization “leak” is less pronounced. Realistic assumptions about particle canting and the system polarization isolation lead to modeling results that satisfactorily agree with observational dual-frequency LDR data.

42 ENGINEERING↗

DOE OSTI2021

Instance Segmentation for Direct Measurements of Satellites in Metal Powders and Automated Microstructural Characterization from Image Data

In this work, we propose instance segmentation as a useful tool for image analysis in materials science. Instance segmentation is an advanced technique in computer vision which generates individual segmentation masks for every object of interest that is recognized in an image. Using an out-of-the-box implementation of Mask R-CNN, instance segmentation is applied to images of metal powder particles produced through gas atomization. Leveraging transfer learning allows for the analysis to be conducted with a very small training set of labeled images. As well as providing another method for measuring the particle size distribution, we demonstrate the first direct measurements of the satellite content in powder samples. After analyzing the results for the labeled data dataset, the trained model was used to generate measurements for a much larger set of unlabeled images. The resulting particle size measurements showed reasonable agreement with laser scattering measurements. The satellite measurements were self-consistent and showed good agreement with the expected trends for different samples. Finally, we present a small case study showing how instance segmentation can be used to measure spheroidite content in the UltraHigh Carbon Steel DataBase, demonstrating the flexibility of the technique.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Physical Properties of Moist, Fermented Corn Grain after Processing by Grinding or Milling

A novel biomass production system, integrating the co-harvesting and co-storage of moist corn grain and stover, promises a reduction in delivered feedstock costs. In this innovative method, the dry grain traditionally utilized for feed or biofuel production will now be processed at a considerably greater moisture content. The adoption of this approach may necessitate a substantial redesign of existing material handling infrastructure to effectively accommodate the handling and storage of moist grain after processing by milling or grinding. A comprehensive study was conducted to quantify the physical properties of this grain after processing with a knife processor or a hammermill. The geometric mean particle size, bulk and tapped density, sliding angle, material coefficient of friction, and discharged angle of repose were quantified. Five grain treatments, either fermented or unfermented, and having different moisture contents, were used. After processing, the moist, fermented ground grain exhibited a significantly smaller particle size compared to the dry grain. Additionally, both moist processed grains resulted in a decreased bulk density and increased material sliding angle, friction coefficient, and angle of repose. The examined metrics collectively suggest that handling, mixing, and storing moist ground grain will pose significant challenges compared to conventional dry ground grain. This increased difficulty may lead to substantially higher costs, a crucial factor that must be carefully considered when evaluating the overall economics of implementing this new biomass production system using combined harvesting and storage of corn grain and stover.

Blazer, Keagan J.↗

NASA NTRS1987

Automated Reduction of Data from Images and Holograms

Laser techniques are widely used for the diagnostics of aerodynamic flow and particle fields. The storage capability of holograms has made this technique an even more powerful. Over 60 researchers in the field of holography, particle sizing and image processing convened to discuss these topics. The research program of ten government laboratories, several universities, industry and foreign countries were presented. A number of papers on holographic interferometry with applications to fluid mechanics were given. Several papers on combustion and particle sizing, speckle velocimetry and speckle interferometry were given. A session on image processing and automated fringe data reduction techniques and the type of facilities for fringe reduction was held.

Lee, G.↗

NASA NTRS1988

Soil mechanics on the Moon, Mars, and Mulberry

From a soil mechanics point of view, the Moon is a relatively simple place. Without any water, organics, or clay minerals, the geotechnical properties of the lunar soil are confined to a fairly limited range. Furthermore, the major soil-forming agent is meteorite impact, which breaks the big particles into little particles; and simultaneously, cements the little particles back together again with molten glass. After about a hundred million years of exposure to meteorite impact, the distribution of particle sizes in the soil achieves a sort of steady state. The majority of the returned lunar soil samples have been found to be well-graded silty-sand to sandy-silt (SM in the Unified Soil Classification System). Each of the particle size distributions plots within a relatively narrow band, which appears to be uniform over the entire lunar surface. This further restricts the range of physical properties of the lunar surface. In contrast, Martian soils should exhibit an extremely wide range of properties. We already know that there is a small amount of water in the soil, greater than in the Martian atmosphere. Furthermore, the soil is suspected to be smectitic clay. That makes two out of the three factors that greatly affect the properties of terrestrial soils.

Carrier, W. D., III↗

DOE OSTI2022

Symmetry-Breaking and Self-Sorting in Block Copolymer-Based Multicomponent Nanocomposites

Co-assembly of inorganic nanoparticles (NPs) and nanostructured polymer matrix represents an intricate interplay of enthalpic or entropic forces. Particle size largely affects the phase behavior of the nanocomposite. Theoretical studies indicate that new morphologies would emerge when the particles become comparable to the soft matrix's size, but this has rarely been supported experimentally. By designing a multicomponent blend composed of NPs, block copolymer-based supramolecules, and small molecules, a 3-D ordered lattice beyond the native BCP's morphology was recently reported when the particle is larger than the microdomain of BCP. The blend can accommodate various formulation variables. In this work, when the particle size equals the microdomain size, a symmetry-broken phase appears in a narrow range of particle sizes and compositions, which we named the "train track" structure. In this phase, the NPs aligned into a 3-D hexagonal lattice and packed asymmetrically along the c axis, making the projection of the ac and the bc plane resemble train tracks. Computational studies show that the broken symmetry reduces the polymer chain deformation and stabilizes the metastable hexagonally perforated lamellar morphology. Given the mobility of the multicomponent blend, the system shows a self-sorting behavior: segregating into two macroscopic phases with different nanostructures based on only a few nanometers NP size differences. Smaller NPs form "train track" morphology, while larger NPs form a "simple hexagon" structure, where the NPs take a symmetric hexagonal arrangement. Detailed structural evolution and simulation studies confirm the systematic-wide cooperativity across different components, indicating the strong self-regulation of the multicomponent system.

"train track" morphology↗

NASA NTRS1979

Fuel spray data with LDV

Droplet size and two component velocities in the severe environment of an operating gas turbine combustor system can be measured simultaneously using the solar laser morphokinetomer (SLM) which incorporates the following capabilities: (1) measurement of a true two-dimensional velocity vector with a range of + or - (0.01-200 m/sec); (2) measurement of particle size (range 5 to 300 micron m) simultaneously with the measurement of velocity; (3) specification of probe volume position coordinates with a high degree of accuracy (+ or - 0.5 mm); (4) immediate on-line data checks; and (5) rapid computer storage of acquired data. The optical system of the SLM incorporates an ultrasonic beam splitter to allow the measurement of a two-dimensional velocity vector simultaneously with particle size. A microprocessor with a limited storage capability permits immediate analysis of test data in the test cell.

Rohy, D. A.↗

NASA NTRS1978

Saturn's rings: Particle composition and size distribution as constrained by microwave observations. I - Radar observations

The radar backscattering characteristics of compositional and structural models of Saturn's rings are calculated and compared with observations of the absolute value, wavelength dependence, and degree of depolarization of the rings' radar cross section (reflectivity). The doubling method is used to calculate reflectivities for systems that are many particles thick using optical depths derived from observations at visible wavelengths. If the rings are many particles thick, irregular centimeter- to meter-sized particles composed primarily of water ice attain sufficiently high albedos and scattering efficiencies to explain the radar observations. In that case, the wavelength independence of radar reflectivity implies the existence of a broad particle size distribution; a narrower size distribution is also a possibility. Particles of primarily silicate composition are ruled out by the radar observations. Purely metallic particles may not be ruled out on the basis of existing radar observations. A monolayer of very large ice 'particles' that exhibit multiple internal scattering may not yet be ruled out.

Cuzzi, J. N.↗

NASA NTRS1985

Measurements in the flow field of a cylinder with a laser transit anemometer and a drag rake in the Langley 0.3 m transonic cryogenic tunnel

An experiment was conducted at the 0.3 m Transonic Cryogenic Tunnel using a Laser Transit Anemometer (LTA) to probe the flow field around a 3.05 centimeter-diameter circular cylinder. Measurements were made along the stagnation line and determination of particle size was evaluated by their ability to follow the flow field. The LTA system was also used to scan into the boundary layer near the 45 degree point on the model. Results of these scans are presented in graphic and tabular form. Flow field particle seeding was accomplished by inbleeding dry service air. The residual moisture (5-10 ppm) condensed and formed ice particles which served as Mie scattering centers for the LTA detection system. Comparison of data taken along the stagnation streamline with theory indicated that these particles tracked the velocity gradient of the flow. Tunnel operating conditions for the tests were a Mach number of 0.3, a pressure of 1.93 x 100000 n/m squared, and a temperature of 225 degrees K. Free stream Mach number and pressure were varied for the particle size determination.

Honaker, W. C.↗

DOE OSTI2022

Pre-combustion mercury removal with co-production of hydrogen via coal electrolysis

Here, pre-combustion mercury removal via coal electrolysis was performed and investigated on a bench-scale coal electrolytic cell (CEC) systemically, and factorial design was used to determine the effect of different operating conditions (coal particle size, operating temperature, operating cell voltage, and flow rate of slurry) on the percentage of mercury removal, percentage of ash removal, and dry heating value change. The results showed that the operating cell voltage, as well as the interaction between operating cell voltage and coal particle size, are significant factors in the percentage of mercury removal. There is no significant factor in the percentage of ash removal and the dry heating value change, but the coal could be purified while keeping the dry heating value almost constant after electrolysis. A co-product of hydrogen could be produced during coal electrolysis with 50% lower energy consumption compared with water electrolysis. Meanwhile, a mechanism for mercury removal in coal was proposed. The facts indicate that coal electrolysis is a promising method for pre-combustion mercury removal.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS1994

The viability of photovoltaics on the Martian surface

The viability of photovoltaics (PV) on the Martian surface may be determined by their ability to withstand significant degradation in the Martian environment. Probably the greatest threat is posed by fine dust particles which are continually blown about the surface of the planet. In an effort to determine the extent of the threat, and to investigate some abatement strategies, a series of experiments were conducted in the Martian Surface Wind Tunnel (MARSWIT) at NASA Ames Research Center. The effects of dust composition, particle size, wind velocity, angle of attack, and protective coatings on the transmittance of light through PV coverglass were determined. Both initially clear and initially dusted samples were subjected both to clear winds and simulated dust storms in the MARSWIT. It was found that wind velocity, particle size, and angle of attack are important parameters affecting occlusion of PV surfaces, while dust composition and protective coatings were not. Neither induced turbulence nor direct current biasing up to 200 volts were effective abatement techniques. Abrasion diffused the light impinging on the PV cells, but did not reduce total coverglass transmittance by more than a few percent.

Gaier, James R.↗

DOE OSTI2021

Experimental study on rheological and settling properties of shape memory polymer for fracture sealing in geothermal formations

This article studies the rheology and annular flow of a smart lost circulation material (LCM) at 160 °C, using a high-temperature flow loop. The smart LCM is a shape memory polymer (SMP) that activates at high temperatures, and its particle size increases to seal fractures in geothermal formations. SMP was mixed with the base fluid in two different concentrations, 1.0 and 3.0 wt%, to study rheology, wellbore hydraulics, activation process, and settling behavior under different testing conditions. The results of this study showed that the SMP could be activated at high temperatures. An increase of 80–100% in the particle size was observed at 160 °C. The mud samples showed a high shear-thinning behavior at the two concentrations with a Power-law flow index (n) ranging between 0.025 and 0.101. No additional frictional pressure losses were observed when SMP was added to the base fluid. SMP particles showed an excellent suspension at 1.0 wt% while, at 3.0 wt%, a bed was formed at a low flow rate and without pipe rotation. Increasing the drill pipe rotational speed or flow rate effectively removed the bed and homogeneously dispersed the SMP particles, ensuring a better sealing efficiency. SMP particle dispersion in inclined wells was better than in horizontal wells. Moreover, the findings of this study help optimize the lost circulation treatment by considering a wide range of operating parameters that can further be extended to different systems and geometries.

02 PETROLEUM↗

DOE OSTI2023

The impact of feedstock size and composition on the hydrothermal growth of (U,Th)O 2

Bulk crystal growth of refractory oxides requires unique approaches, and the U x Th 1-x O 2 solid solution is no exception. Hydrothermal transport reactions of U 0.1 Th 0.9 O 2 onto ThO 2 seeds with feedstocks comprised of U 0.1 Th 0.9 O 2 or mixtures of UO 2 and ThO 2 with a nominal composition of U 0.1 Th 0.9 O 2 are investigated with µ-Raman spectroscopy and X-ray fluorescence. In each case, the trends in stoichiometry as a function of distance from the seed are analyzed and the deviations from the nominal stoichiometry discussed. When the feedstock is composed of mixed oxides, the particle surface area’s influence on the feedstock dissolution rate is the dominant factor and can produce U-rich stoichiometries as high as U 0.75 Th 0.25 O 2 . When composed solely of U 0.1 Th 0.9 O 2 , the total growth amount depends on the particle size, but the obtained stoichiometry is the product of differing solubilities. Although the U0.1Th0.9O 2 feedstock produces the most homogeneous growth, the ending growth of the smallest particle UO 2 /ThO 2 mixture yields the stoichiometry closest to U 0.1 Th 0.9 O 2 . How to obtain desired stoichiometries from mixtures by matching the particle size and solubilities is briefly discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Size-resolved particle and black carbon deposition over the cryosphere (Final Report)

Our project focused on providing observational constraints and investigation of aerosol deposition by performing the first unambiguous direct eddy flux covariance measurements of aerosol dry deposition over the cryosphere. The project aimed to make eddy covariance flux measurements of dry deposition and off-line wet deposition measurements of black carbon containing aerosol plus eddy covariance measurements of size-resolved accumulation mode scattering aerosol over the DOE ARM AMF3 Oliktok Point site in Fall 2020. We aimed to compare our measurements to model parameterizations to constrain uncertainties and systematic bias, and improve deposition parameterizations in models. Due to disruptions in field work from COVID-19, our work was delayed and moved to an alternate site on the North Slope of Alaska. This report summarizes the key findings from the project, including data analysis from previous field projects and from the North Slope of Alaska.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2019

Can Single-Walled Carbon Nanotube Diameter Be Defined by Catalyst Particle Diameter?

The need of designing and controlling single-walled carbon nanotube (SWCNT) properties is a challenge in a growing nanomaterials-related industry. Recently, great progress has been made experimentally to selectively control SWCNT diameter and chirality. However, there is not yet a complete understanding of the synthesis process, and there is a lack of mathematical models that explain nucleation and diameter selectivity of stable carbon allotropes. Here, in situ analysis of chemical vapor deposition SWCNT synthesis confirms that the nanoparticle-to-nanotube diameter ratio varies with the catalyst particle size. It is found that the tube diameter is larger than that of the particle below a specific size (dc ≈ 2 nm) and above this value is smaller than particle diameters. Additionally, to explain these observations, we develop a statistical mechanics based model that correlates possible energy states of a nascent tube with the catalyst particle size. This model incorporates the equilibrium distance between the nucleating SWCNT layer and the metal catalyst (e.g., Fe, Co, and Ni) evaluated with density functional theory (DFT) calculations. The theoretical analysis explains and predicts the observed correlation between tube and solid particle diameters during growth of supported SWCNTs. This work also brings together previous observations related to the stability condition for SWCNT nucleation. Tests of the model against various published data sets and our own experimental results show good agreement, making it a promising tool for evaluating SWCNT synthesis processes.

36 MATERIALS SCIENCE↗

NASA NTRS1980

Theoretical and experimental studies of microwave radiation from a natural snow field

The brightness temperature of a natural snow field in northern Europe was studied theortically and experimentally at 5, 12, and 37 GHz for satellite remote sensing applications. A snow model consisting of ice spheres covered by a water shell was used in calculation, taking into account scattering and absorption. The brightness temperature of a natural snow field as a function of view angle was measured from a tower in 1978 and 1979. The measured brightness temperature curves can be fitted with calculated ones by assuming reasonable values for the wetness and the particle size of snow. Experimental results also show that relatively small changes in the snow conditions cause large changes in the brightness temperature. In order to obtain a more controlled situation, experiments were continued in 1980 using a measuring site covered with aluminum sheets and determining the wetness and the particle size in addition to the density and physical temperature.

Tiuri, M.↗