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Mixed Element Microparticle Characterization by Electron Probe Microanalysis
Abstract Microparticle compositional characterization for nuclear forensics has traditionally been achieved by “gold-standard” destructive analytical techniques such as large geometry-secondary ion mass spectrometry and fission track-thermal ionization mass spectrometry, but long processing times and total sample consumption eliminate the option of subsequent analysis by other methods. Electron probe microanalysis has long been widely employed for rapid, nondestructive, micrometer-scale compositional measurements and imaging in fields such as material science and geology and may therefore need to be reevaluated as an alternative tool for microparticle analysis for the nuclear forensics community. This study presents the use of electron probe microanalysis for imaging and quantitative characterization of homogeneous microparticles utilizing a calibration curve based on high-precision quadrupole-inductively coupled plasma-mass spectrometry analyses. Samples of opportunity synthesized at Savannah River National Laboratory, nickel-doped cerium oxide microparticles, were selected as analogs for plutonium-doped uranium oxide microparticles. Positive detection and accurate quantification of variable amounts of nickel dopant down to trace levels (10s of parts per million) suggest applicability of this technique to other mixed element systems (e.g., actinides). Quantitative single-particle characterization via electron probe microanalyzer may thus provide a high fidelity, nondestructive complement to techniques currently in use.
Metal alloy microparticle tagging of UO 2 fuel pellets for nuclear forensics
A tagging strategy for UO 2 fuel pellets will be discussed which involves the creation of alloyed metal microparticles that can be tuned to create a unique identification (“barcode”) indicating provenance of the pellets. These specialized markers would contain high temperature resistant materials, such as Ti, Mo, and Cr, in small quantities such that they do not interfere with the performance of the pellets but are recoverable by standard analytical techniques. The Amazemet rePowder ultrasonic atomization system was used to manufacture the microparticles, and sample pellets were fabricated and sintered containing these dopants. Various techniques, such as Scanning Electron Microscopy (SEM) and Electron Probe Microanalysis (EPMA), were used to evaluate these sample pellets to determine if particles (and their alloy compositions) were recoverable. Details on how the particles were manufactured and characterized will be detailed, as well as results from their incorporation into test pellets. Next steps will involve the scale of this technique using more conventional mass production methods, as well as the implementation of other alloys.
Heterogeneous microstructural evolution during hydrodynamic penetration of a high-velocity copper microparticle impacting copper
Microparticle hydrodynamic penetration (HDP) may be associated with the erosion regime in cold spray processing and other high-velocity impact events. Here, in an experimental approach where we can individually launch particles and study the impact sites, we explore copper microparticles impacted on copper substrates at velocities above 900 m/s where HDP begins. We lift cross-sectional lamellae from the impact sites with a focused-ion beam for further microstructural characterization using electron backscatter diffraction and scanning transmission electron microscopy. Due to the gradients of strain, strain rate, and temperature associated with HDP, heterogeneous microstructures result. The structural evolution processes observed include deformation twinning and multiple dislocation-mediated grain recrystallization mechanisms—geometric dynamic recrystallization (gDRX), discontinuous DRX (dDRX), and meta DRX (mDRX). The higher strains at the interface lead to the most significant structural changes and complex mechanisms. In contrast, there is a gradient to more conventional dislocation plasticity away from the interface (on either the particle or substrate side). Here, these microstructural observations are consistent with the deformation map for copper and extend the observations of impact-induced recrystallization across new regimes of behavior.
Particle dynamics of nanoplastics suspended in water with soil microparticles: insights from small angle neutron scattering (SANS) and ultra-SANS
Small-angle neutron scattering (SANS) and ultra-SANS (USANS) were employed to understand the aggregation behavior and observe the size reduction for nanoplastics (NPs) formed from a biodegradable mulch film, and microparticles of vermiculite (V), an artificial soil, suspended in water in the presence of low convective shear (ex situ stirring) prior to measurements. Neutron contrast matching was employed to minimize the signal of V (by 100-fold) and thereby isolate the signal due to NPs in the neutron beam, as the contrast match point (CMP) for V (67 vol% deuteration of water) differed from that of NPs by more than 20%. The original NPs' size distribution was bimodal: <200 nm and 500–1200 nm, referred to as small and large NPs, i.e., SNPs and LNPs, respectively. In the absence of V, SNPs formed homoaggregates at higher concentrations that decreased with stirring time, while the size of LNPs remained unchanged. The presence of V at 2-fold lower concentration than NPs did not change the size of SNPs but reduced the size of LNPs by nearly 2-fold as stirring time increased. Because the size of SNPs and LNPs did not differ substantially between CMP and 100% D 2 O solvents, it is evident that SNPs and LNPs are mainly composed of NPs and not V. In conclusion, the results suggest that LNPs are susceptible to size reduction through collisions with soil microparticles via convection, yielding SNPs near soil–water interfaces within vadose zones.
Continuous flow photochemical synthesis of metal–ceramic composite microparticles
We developed a UV-assisted microfluidic system to synthesize FeCrAl–Al 2 O 3 composite microparticles for additive manufacturing. Here, the system ensures precise particle size, morphology, and elemental distribution control. Increasing the dispensing pressure while keeping the oil flow rate constant resulted in larger microparticles. Laser fusing revealed FeCrAl and Al 2 O 3 phases, showing their potential as feedstocks for 3D printed heterogeneous materials such as FeCrAl/Al 2 O 3 bi-phase materials.
Quantifying platinum binding on protein-functionalized magnetic microparticles using single particle-ICP-TOF-MS
This work describes an analytical procedure, single particle-inductively coupled plasma-time-of-flight-mass spectrometry (SP-ICP-TOF-MS), that was developed to determine the platinum binding efficiency of protein-coated magnetic microparticles.
Microstructure effects on high velocity microparticle impacts of copper
Constitutive models can fail to predict high-rate deformation behavior due to their inability to account for microstructural effects. In part, this is because of a dearth of experimental benchmarking data in the high strain-rate, low pressure regime, since many high-rate experiments also probe a region of strong shockwaves, at which point microstructure effects no longer play a primary role. This work uses laser-induced particle impact testing to quantitatively study high velocity impacts of small, rigid alumina microspheres on flat copper substrates with varying amounts of initial cold work in the weak shock regime, but at very high strain rates up to ~10 7 s –1 . Through paired experiments and numerical simulations, this work shows that the initial microstructure condition can have significant influence on dynamical mechanical properties in this range. Specifically, prior work hardening of the copper substrate leads to increased rebounding of the microparticles (i.e., less plastic dissipation in the impact) as well as smaller craters. Each of these experimental measurables can be converted into a strength measure, i.e., the dynamic yield strength or dynamic hardness, respectively, neither of which is well predicted consistently by existing constitutive laws. The general trend of hardening can be captured by such models by incorporating an existing “pre-strain,” suggesting that future calibration of the materials parameters may yield a good fit over a broader range of conditions. Our results emphasize the importance of reporting the microstructural condition in dynamic studies, as well as the necessity of accounting for these factors when formulating and optimizing constitutive models.
Eutectic melting of alloy microparticles upon low velocity impact
Although impact melting has been quantified in a number of pure metals, alloyed microparticles have access to low melting-point eutectics that can promote earlier melting. Through real-time monitoring of single particle impacts resolved at the nanosecond- and micron-scales, we explore the impact melting of AA7075 from high velocities, where it is abundant and clear, to velocities as low as ∼269 m/s. Here, by using a hard substrate to isolate the deformation largely to the particle, we show that the adiabatic heat produced by the plasticity of the impact can explain the onset of melting at low velocity.
Rapid isotopic analysis of uranium microparticles via SP-ICP-TOF-MS
Inductively coupled plasma – time-of-flight – mass spectrometry (ICP-TOF-MS) was employed for the isotopic analysis of uranium particles of varying 235 U enrichment levels. Here, a single particle (SP)-based introduction scheme was employed such that individual particles, in a suspension, were analyzed. The uranium oxide microparticles were comprised of depleted uranium (DU, 235 U/ 238 U of 0.0017316(14)), natural uranium (NU, 235 U/ 238 U of 0.0072614(39)), and low enriched uranium (LEU, 235 U/ 238 U of 0.051025(15)). The percent relative difference of the SP-ICP-TOF-MS measured isotopic ratios compared to the expected values for the DU, NU, and LEU particle populations were 8.75, 0.12, and 1.23 %, respectively. After characterization, the DU and NU particles were doped within a complex sample matrix (Arizona Test Dust) containing Fe, Ti, Al, and Si particles, among others. Then, the suspension was analyzed via SP-ICP-TOF-MS and the detected particles were classified as DU or NU based on their measured 235 U/ 238 U ratio. In the same analysis, the matrix particles (i.e., Al, Fe, and Ti) were detected, demonstrating the simultaneous nuclide detection provided by the measurement platform. The presented SP-ICP-TOF-MS methodology for uranium particle characterization proved to be a high throughput method for detecting and isotopically discerning uranium particles with varying enrichment levels, in a complex matrix.
Upconversion of Infrared Light by Graphitic Microparticles Due to Photoinduced Structural Modification
Recent reports of upconversion and white light emission from graphitic particles warrant an explanation of the physics behind the process. A model is offered, wherein the upconversion is facilitated by photoinduced electronic structure modification allowing for multiphoton processes. As per the prediction of the model, it is experimentally shown that graphite upconverts infrared light centered around 1.31 μm (0.95 eV) to broadband white light centered around 0.85 μm (1.46 eV). The results suggest that upconversion from shortwave infrared (≈3 μm, 0.45 eV) to visible region may be possible. The experiments show that the population dynamics of the electronic states involved in this upconversion process occur in the timescale of milliseconds.
Modeling of melting and erosion in high velocity microparticle impacts
High velocity collisions can cause melting, a situation involving elasticity, plasticity, and phase transformations in tandem, which is very challenging for mechanical modeling. Here, this paper advances the use of smoothed particle hydrodynamics (SPH) simulations for this complex situation, investigating stainless steel microspheres impacting a tin substrate. After extensive validation against a range of mechanical and geometrical measurements of experimental impacts, the model provides a detailed, quantitative view of melt volume production over a broad range of impact velocities. It also enables direct decomposition of the impact energy partitioning, including analysis of the energy absorbed by plasticity in the impactor, the system kinetic energy, and the adiabatic heating of the substrate in addition to the melting itself. Since these quantities are not available experimentally, SPH modeling substantially enhances the quantitative understanding of such impacts. Finally, the model speaks to the phase characteristics of the ejecta formed during impact, confirming the experimental inference that the ejected material likely contains a significant fraction of solid material.
Nanoscale interfacial melting enables bonding during high velocity microparticle impacts
Melting during high-velocity particle impact has been understood to be typically detrimental to bonding by lowering the strength at the interface and promoting rebound before solidification can occur. Here we establish a possible remedy to this challenge: by dramatically restricting the volume of molten material, its resolidification is accelerated, effectively forming a nanoscale, braze-type joint during impact. In-situ single particle impact imaging is combined with post-mortem structural and chemical analyses to reveal a regime where adhesion is governed not by extensive plastic deformation, but by the kinetics of melt layer resolidification. Furthermore, these findings redefine the role of melting in impact-based processes, establishing transient melting and rapid solidification as a viable strategy for engineering successful adhesion events.
Understanding the impact of formulation design on microstructure and drug release from porous microparticle-based tretinoin topical gels
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Fission gas trapped in Chornobyl fuel microparticles reveals details of reactor operations
The isotopic ratios of fission gas would provide important source information of a nuclear fuel sample found in the environment. However, it is believed that during a reactor accident like Chornobyl all fission gas is lost and that the radioactive particles found in the Chornobyl Exclusion Zone today are depleted in gases by the initial explosion and subsequent fire. We disprove this hypothesis by detection and analysis of trapped krypton and xenon in these particles. Our analysis of krypton and xenon isotopes by noble gas mass spectroscopy in combination with resonance ionization mass spectrometry establishes that important information about reactor operations like age, neutron flux and plutonium fission fraction can still be reconstructed from individual micrometer-sized particles even after decades of weathering in the environment.
Measuring the strength of ductile microparticles at extreme strain rates
Not Available
Optimizing ensemble NV − spin properties of fluorescent diamond microparticles by systematic low pressure high temperature annealing
Low pressure high temperature annealing is a means for driving nitrogen and defect diffusion in diamond to reduce internal lattice damage without the need for technically complicated high-pressure cells. Herein, we perform a systematic time (5, 15, and 30 min) and temperature (1200 °C–1800 °C) study of effects of low-pressure high temperature annealing on photoluminescence, spin concentrations, and spin relaxation properties of NV centers in ca. 3 μm synthetic type 1b diamond particles. Annealing in the temperature range of ca. 1400 °C–1700 °C for even 5 min leads to a higher optically detected magnetic resonance contrast as compared to standard annealing at 900 °C for 2 h. Particles annealed at 1700 °C for 5 min exhibit a contrast close to about 13% as compared to about 9% for those annealed at 900 °C for 2 h. A reduction in the zero-field splitting strain parameter from E ≈ 4.5 MHz to ≈ 2.5 MHz and spectral linewidth from Δν ≈ 7 MHz to ≈ 4 MHz are observed even after 5 min annealing at 1700 °C. Improvements in these spectral parameters resulted in a roughly 2-fold reduction in the noise level of temperature monitoring experiment utilizing an ensemble of NV centers in the particles. Annealing in the temperature range of 1600 °C for 15 or 30 min or 1700 °C for 5 min resulted in NV T 1 relaxation times approaching ca. 5 ms typically observed for bulk diamond. Quantitative electron paramagnetic resonance (EPR) allowed for estimations of thermal activation energies of paramagnetic center annihilation. Monitoring the primary defect concentration (P1 and other defects with half integer spins) and utilizing second order kinetic modeling, an activation energy of 3.63 ± 0.28 eV was estimated. Alternatively, using the NV half field EPR signal and first order kinetic modeling, a similar activation energy 3.89 ± 0.29 eV was estimated.