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All sourcesNASA NTRSDOE OSTI
NASA NTRS2003

Blowing in the Wind: II. Creation and Redistribution of Refractory Inclusions in a Turbulent Protoplanetary Nebula

Ca-A1 rich refractory mineral inclusions (CAIs) found at 1-6% mass fraction in primitive chondrites appear to be 1-3 million years older than the dominant (chondrule) components which were accreted into the same parent bodies. A prevalent concern is that it is difficult to retain CAIs for this long against gas-drag-induced radial drift into the sun. We reassess the situation in terms of a hot inner (turbulent) nebula context for CAI formation, using analytical models of nebula evolution and particle diffusion. We show that outward radial diffusion in a weakly turbulent nebula can overwhelm inward drift, and prevent significant numbers of CAI-size particles from being lost into the sun for times on the order of 10(exp 6) years. CAIs can form early, when the inner nebula was hot, and persist in sufficient abundance to be incorporated into primitive planetesimals at a much later time. Small (less than or approximately 0.1 mm diameter) CAIs persist for longer times than large (greater than or approximately 5mm diameter ones. To obtain a quantitative match to the observed volume fractions of CAIs in chondrites, another process must be allowed for: a substantial enhancement of the inner hot nebula in silicate-forming material, which we suggest was caused by rapid inward drift of meter-sized objects. This early in nebula history, the drifting rubble would have a carbon content probably an order of magnitude larger than even the most primitive (CI) carbonaceous chondrites. Abundant carbon in the evaporating material would help keep the nebula oxygen fugacity low, plausibly solar; as inferred for the formation environment of CAIs. The associated production of a larger than canonical amount of CO2 might also play a role in mass-independent fractionation of oxygen isotopes, leaving the gas rich in O-16 as inferred from CAIs and other high temperature condensates.

Cuzzi, Jeffrey N.↗
NASA NTRS1999

Soot Aerosol Properties in Laminar Soot-Emitting Microgravity Nonpremixed Flames

The spatial distributions and morphological properties of the soot aerosol are examined experimentally in a series of 0-g laminar gas-jet nonpremixed flames. The methodology deploys round jet diffusion flames of nitrogen-diluted acetylene fuel burning in quiescent air at atmospheric pressure. Full-field laser-light extinction is utilized to determine transient soot spatial distributions within the flames. Thermophoretic sampling is employed in conjunction with transmission electron microscopy to define soot microstructure within the soot-emitting 0-g flames. The microgravity tests indicate that the 0-g flames attain a quasi-steady state roughly 0.7 s after ignition, and sustain their annular structure even beyond their luminous flame tip. The measured peak soot volume fractions show a complex dependence on burner exit conditions, and decrease in a nonlinear fashion with decreasing characteristic flow residence times. Fuel preheat by approximately 140 K appears to accelerate the formation of soot near the flame axis via enhanced fuel pyrolysis rates. The increased soot presence caused by the elevated fuel injection temperatures triggers higher flame radiative losses, which may account for the premature suppression of soot growth observed along the annular region of preheated-fuel flames. Electron micrographs of soot aggregates collected in 0-g reveal the presence of soot precursor particles near the symmetry axis at midflame height, The observations also verify that soot primary particle sizes are nearly uniform among aggregates present at the same flame location, but vary considerably with radius at a fixed distance from the burner. The maximum primary size in 0-g is found to be by 40% larger than in 1-g, under the same burner exit conditions. Estimates of the number concentration of primary particles and surface area of soot particulate phase per unit volume of the combustion gases are also made for selected in-flame locations.

Konsur, Bogdan↗
NASA NTRS2003

Blowing in the Wind: II. Creation and Redistribution of Refractory Inclusions in a Turbulent Protoplanetary Nebula

Ca-Al rich refractory mineral inclusions (CAIs) found at 1-6% mass fraction in primitive chondrites appear to be 1-3 million years older than the dominant (chondrule) components which were accreted into the same parent bodies. A prevalent concern is that it is difficult to retain CAIs for this long against gas-drag-induced radial drift into the sun. We reassess the situation in terms of a hot inner (turbulent) nebula context for CAI formation, using analytical models of nebula evolution and particle diffusion. We show that outward radial diffusion in a weakly turbulent nebula can overwhelm inward drift, and prevent significant numbers of CAI-size particles from being lost into the sun for times on the order of 10(exp 6) years. CAIs can form early, when the inner nebula was hot, and persist in sufficient abundance to be incorporated into primitive planetesimals at a much later time. Small (less than or approx. equal to 0.1 mm diameter) CAIs persist for longer times than large (greater than or approx. equal to 5mm diameter ones). To obtain a quantitative match t o the observed volume fractions of CAIs in chondrites, another process must be allowed for: a substantial enhancement of the inner hot nebula in silicate-forming material, which we suggest was caused by rapid inward drift of meter-sized objects. This early in nebula history, the drifting rubble would have a carbon content probably an order of magnitude larger than even the most primitive (CI) carbonaceous chondrites. Abundant carbon in the evaporating material would help keep the nebula oxygen fugacity low, plausably solar, as inferred for the formation environment of CAIs. The associated production of a larger than canonical amount of CO2 might also play a role in mass-independent fractionation of oxygen isotopes, leaving the gas rich in l60 as inferred from CAIs and other high temperature condensates.

Cuzzi, Jeffrey N.↗
NASA NTRS2001

Soot Optical Property Study

Recent past studies of soot reaction processes in laminar premixed and nonpremixed flames generally have used the intrusive technique of thermophoretic sampling and analysis by transmission electron microscopy (TEM) to observe soot structure and obtain important fundamental information about soot particle properties, such as soot primary particle diameters, the rate of change of soot primary particle diameter as a function of time (or rate of soot surface growth or oxidation), the amount of soot particle reactive surface area per unit volume, the number of primary soot particles per unit volume, and the rate of formation of primary soot particles (or the rate of soot primary particle nucleation). Given the soot volume per unit volume of the flame (or the soot volume fraction), all these properties are readily found from a measurement of the soot primary particle diameter (which usually is nearly a constant for each location within a laminar flame). This approach is not possible within freely propagating flames, however, because soot properties at given positions in such flames vary relatively rapidly as a function of time in the soot formation and oxidation regions compared to the relatively lengthy sampling times needed to accumulate adequate soot samples and to minimize effects of soot collected on the sampling grid as it moves to and from the sampling position through other portions of the flame. Thus, nonintrusive optical methods must be used to find the soot primary particle diameters needed to define the soot surface reaction properties mentioned earlier. Unfortunately, approximate nonintrusive methods used during early studies of soot reaction properties in flames, found from laser scattering and absorption measurements analyzed assuming either Rayleigh scattering or Mie scattering from polydisperse effective soot particles having the same mass of soot as individual soot aggregates, have not been found to be an effective way to estimate the soot surface reaction area per unit volume. Thus, alternative nonintrusive optical methods of finding these properties must be sought, which was the objective of this phase of the investigation. The alternative method used here involves use of the Rayleigh-Debye-Gans-Polydisperse-Fractal-Aggregate (RDG-PFA) scattering approximation for soot aggregates in flames. Thus, the development of this method will be discussed next before describing its evaluation as a means of nonintrusively measuring soot primary particle diameters in soot-containing flames.

Aung, K. T.↗
NASA NTRS1999

Attenuation of Gas Turbulence by a Nearly Stationary Dispersion of Fine Particles

Turbulence attenuation by greater than a factor of two has been observed in many practical gas flows carrying volume fractions as small as 0.01% of dispersed particles. Particles which cause such attenuation usually are smaller than the smallest scales of the turbulence and have time constants 5 to 10 times greater than the time scale of a typical turbulent eddy. That is, strongly attenuating particles usually have Stokes numbers in the range of 5 to 10, indicating that they do not respond to the turbulent fluctuations, but instead just fall through the flow responding only to the mean flow. There are two mechanisms by which free falling particles may attenuate turbulence. First, the unresponsive particles act as a drag on the turbulent eddies, passing energy from the turbulent eddies to the small scale wakes of the particles where it is quickly dissipated by viscosity. The second mechanism is more complicated. Particles falling under gravity convert gravitational potential energy to turbulent velocity fluctuations. If the particles are large, this mechanism increases the overall turbulence level. However, with moderate size particles, the small scale turbulence generated apparently distorts the turbulent eddies leading to more rapid dissipation. Unfortunately, this conclusion is supported only by circumstantial evidence to date. The objectives of the experiment are to use microgravity to separate the two mechanisms. A region of nearly-isotropic decaying turbulence with zero mean flow will be formed in a box in the microgravity environment. Different sets of particles with Stokes numbers in the range of 2 to 20 will be dispersed in the flow. With zero gravity and no mean fluid velocity the particles will have zero mean velocity. With the large Stokes numbers, the fluctuating velocities will also be small. Therefore, the only attenuation mechanism will be the direct action of the particles on the turbulence. Control experiments will also be done in which the particles fall through the measurement volume. Measurements will be acquired using a high resolution image velocimetry (PIV) system being developed specifically for work in particle-laden flows. The measurements will include the decay of the turbulence kinetic energy under various particle loadings. The spatial spectra of the turbulence will also be measured. In a second set of experiments, the interaction of a single eddy with a collection of nearly stationary particles will be examined. The eddy will be a vortex ring emitted by a jet pulse through an orifice. The distortion of the vortex under the influence of the particles will be examined to gain a better understanding of how fine particles can cause such large reductions in turbulence levels. This experiment could not be conducted in terrestrial gravity because the high particle velocities would overwhelm the relatively low speed motion of the vortex ring. This experimental program is just getting underway. The initial challenge is to build a closed facility containing reasonably homogeneous and isotropic turbulence with zero mean velocity. Our approach is to use a set of synthetic jets mounted on the periphery of a transparent plexiglass box to create the turbulence. A synthetic jet is a plenum chamber with an orifice open to the volume of interest. The volume of the chamber fluctuates periodically so alternately a jet is ejected from the volume or flow is drawn back in as a sink. The asymmetry of this situation results in a net transport of momentum and kinetic energy into the volume of interest. The present apparatus includes eight synthetic jets each powered independently by a six inch loudspeaker. The synthetic jets discharge through ejector tubes to increase the scale of the turbulence. Construction of the apparatus is now complete and preliminary flow visualization studies have been conducted. The PIV system is also under development. A compact dual-pulse YAG laser has been acquired as the light source and special software is under development to allow simultaneous measurements of both the particle phase and the fluid phase (marked by fine tracers).

Paris, A. D.↗
NASA NTRS1999

Instrumentation Working Group Summary

The Instrumentation Working Group compiled a summary of measurement techniques applicable to gas turbine engine aerosol precursors and particulates. An assessment was made of the limits, accuracy, applicability, and technology readiness of the various techniques. Despite advances made in emissions characterization of aircraft engines, uncertainties still exist in the mechanisms by which aerosols and particulates are produced in the near-field engine exhaust. To adequately assess current understanding of the formation of sulfuric acid aerosols in the exhaust plumes of gas turbine engines, measurements are required to determine the degree and importance of sulfur oxidation in the turbine and at the engine exit. Ideally, concentrations of all sulfur species would be acquired, with emphasis on SO2 and SO3. Numerous options exist for extractive and non-extractive measurement of SO2 at the engine exit, most of which are well developed. SO2 measurements should be performed first to place an upper bound on the percentage of SO2 oxidation. If extractive and non-extractive techniques indicate that a large amount of the fuel sulfur is not detected as SO2, then efforts are needed to improve techniques for SO3 measurements. Additional work will be required to account for the fuel sulfur in the engine exhaust. Chemical Ionization Mass Spectrometry (CI-MS) measurements need to be pursued, although a careful assessment needs to be made of the sampling line impact on the extracted sample composition. Efforts should also be placed on implementing non-intrusive techniques and extending their capabilities by maximizing exhaust coverage for line-of-sight measurements, as well as development of 2-D techniques, where feasible. Recommendations were made to continue engine exit and combustor measurements of particulates. Particulate measurements should include particle size distribution, mass fraction, hydration properties, and volatile fraction. However, methods to ensure that unaltered samples are obtained need to be developed. Particulate speciation was also assigned a high priority for quantifying the fractions of carbon soot, PAH, refractory materials, metals, sulfates, and nitrates. High priority was also placed on performing a comparison of particle sizing instruments. Concern was expressed by the workshop attendees who routinely make particulate measurements about the variation in number density measured during in-flight tests by different instruments. In some cases, measurements performed by different groups of researchers during the same flight tests showed an order of magnitude variation. Second priority was assigned to measuring concentrations of odd hydrogen and oxidizing species. Since OH, HO2, H2O2, and O are extremely reactive, non-extractive measurements are recommended. A combination of absorption and fluorescence is anticipated to be effective for OH measurements in the combustor and at the engine exit. Extractive measurements of HO2 have been made in the stratosphere, where the ambient level of OH is relatively low. Use of techniques that convert HO2 to OH for combustor and engine exit measurements needs to be evaluated, since the ratio of HO2/OH may be 1% or less at both the combustor and engine exit. CI-MS might be a viable option for H2O2, subject to sampling line conversion issues. However, H2O2 is a low priority oxidizing species in the combustor and at the engine exit. Two candidates for atomic oxygen measurements are Resonance Enhanced Multi-Photon Ionization (REMPI) and Laser-Induced Fluorescence (LIF). Particulate measurement by simultaneous extractive and non-extractive techniques was given equal priority to the oxidizer measurements. Concern was expressed over the ability of typical ground test sampling lines to deliver an unaltered sample to a remotely located instrument. It was suggested that the sampling probe and line losses be checked out by attempting measurements using an optical or non-extractive technique immediately upstream of the sampling probe. This is a possible application for Laser Induced Incandescence (LII) as a check on the volume fraction of soot. Optical measurements of size distribution are not well developed for ultrafine particles less than about 20 nm in diameter, so a non-extractive technique for particulate size distribution cannot be recommended without further development. Carbon dioxide measurements need to be made to complement other extractive measurement techniques. CO2 measurements enable conversion of other species concentrations to emission indices. Carbon monoxide, which acts as a sink for oxidizing species, should be measured using non-extractive techniques. CO can be rapidly converted to CO2 in extractive probes, and a comparison between extractive and non-extractive measurements should be performed. Development of non-extractive techniques would help to assess the degree of CO conversion, and might be needed to improve the concentration measurement accuracy. Measurements of NO(x) will continue to be critical due to the role of NO and NO2 in atmospheric chemistry, and their influence on atmospheric ozone. Time-resolved measurements of temperature, velocity, and species concentrations were included on the list of desired measurement. Thermocouples are typically adequate for engine exit measurements. PIV and LDV are well established for obtaining velocity profiles. The techniques are listed in the accompanying table; are divided into extractive and non-extractive techniques. Efforts were made to include a measurement uncertainty for each technique. An assessment of the technology readiness was included.

Zaller, Michelle↗
DOE OSTI2024

Effect of Heat Treatment on Microstructure and Mechanical Property of 316L Stainless Steel Produced by Laser Powder Bed Fusion

The advanced non-light water reactor designs (Gen IV reactors), including molten salt/ very high temperature/ sodium-cooled and lead-cooled fast reactors, typically operate at higher temperatures and more extreme radiation conditions than light water reactors. An intrinsic part of the deployment and progress of Gen IV reactor designs is selecting the most suitable structural material for a specific application. Additive manufacturing (AM), a fairly new process of making physical, three-dimensional objects from a computer design file, is going to completely change the way of design, build and certify nuclear systems. It offers a range of opportunities to produce complex geometries from existing materials, offers new routes for processing of previously difficult to process materials, allows for design of new high-performance materials, and finally facilitates hybridization of dissimilar materials. This emerging technology has successfully produced cars, wind turbine blade molds and even live cells. It could also open up big opportunities for the nuclear industry to quickly deploy technologies at a fraction of the cost. So far, AM techniques have been preliminarily applied in the field of nuclear reactors, including the classical parts such as the pressure vessel of a small reactor with 508-III steel, the bottom nozzle of a fuel assembly with 304L steel, the fuel cladding with zirconium alloy and the integrated impeller of a pump and the multi-channel valve body with 316L steel [6,7]. The AM applications for operating nuclear reactors started in auxiliary plant components and have slowly migrated to metallic reactors and core components, but many of these are not safety critical components. Although many parts used for nuclear reactors have been fabricated by AM techniques, practical applications in engineering are still a long way off due to the uncertainty factors focused on the processing, material properties, analysis methods and application standards, which feeds the safety and life-cycle of the nuclear reactor. Due to rapid, repeated heating and cooling during production, a high dislocation density was present in the AM material. This microstructure feature is unstable at elevated temperature while high temperature is one of the typical operation environments for nuclear reactors. Thus, it is important to understand the thermal effect on the microstructure of AM material. The objectives of this study are to investigate the effect of heat treatment on the microstructure and mechanical properties of 316L stainless steel produced by laser powder bed fusion additive manufacturing, and to determine an appropriate heat treatment practice that will be applied to the lightweight AM lattice-structured material with the same chemistry. The heat treatment study consisted of annealing the samples at a temperature range of 800 to 1200 oC with a 50 oC increment for different times (1-24 hours), followed by vacuum or air cooling. Microstructural characterization was carried out by Scanning Electron Microscope (SEM). Grain size and crystallographic orientation were investigated by Electron Backscatter Diffraction (EBSD). Vickers hardness tests with a 0.5 kg load were employed to determine the hardness of samples after different heat treatments. After heat treatment, the random crystallographic orientation was preserved, and the volume fraction of high-angle grain boundaries (grain boundary misorientation =15 oC) remained the same. The dislocation density decreased with annealing temperature due to recovery. The fine subgrain structures in the as-printed specimen were quite stable up to 1200 oC. Minimal recrystallization was observed up to 1200 oC. Recrystallization initiated only after 8.5 hours at 1200 oC. The SEM images did not show obvious dependence of microstructure on cooling rate. The hardness of the specimens decreased with increasing annealing temperature as a result of the decrease in dislocation density. It is interesting to note that the AM material showed very similar hardness to the wrought material when annealing at similar temperature, although the microstructures are very different. Annealing at 1050 oC for 1 hour followed by air cooling was selected as the heat treatment procedure for the lattice designed lightweight AM 316L material.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Structural Phase Separation and Enhanced Superconductivity in La 1.875 Ba 0.125 CuO 4 Under Uniaxial Strain

Strain engineering has attracted significant attention in recent years due to its capability in tuning lattice and electronic structures of quantum materials. Using moderate uniaxial compressive strain, structural phase separation is induced in the low-temperature phase of x = 1/8 La 2-x Ba x CuO 4 (LBCO) single crystals. These structures are low temperature tetragonal (LTT), low temperature less orthorhombic (LTLO), and a plastically deformed nano-domain structure (PDNS), comprised of few-nanometer-sized orthorhombic domains within an amorphous matrix. These three structures exhibit distinct superconducting behaviors. The volume fraction of the LTT structure is suppressed with increasing strain, while its superconducting transition temperature increases and broadens. The LTLO structure exhibits a sharp superconducting transition above 32 K, which increases up to ≈ 36 K at maximum strain. The PDNS phase exhibits a very broad superconducting transition and persists even after removing the strain. This study illustrates the sensitivity of superconductivity to the structure of the LBCO sample near its stripe instability.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2025

Reactive Carbide‐Based Synthesis and Microstructure of NASICON Sodium Metal All Solid‐State Electrolyte

Reactive carbide precursor-based synthesis of NASICON-type NZSP (Na 1+x Zr 2 Si x P 3-x O 12 ) solid-state electrolyte (SSE) is demonstrated, in contrast to the established oxide-based approach. Exothermic decomposition of ZrC and SiC in air homogenizes microstructure, yielding 98% compact density after conventional sintering at 1200 °C. Quantitative stereology demonstrates that significant microstructural differences are present. Compacts of carbide-derived Carb-NZSP are 98% dense with a secondary zirconium oxide (ZrO 2 ) volume fraction of 0.2% ± 0.3%, versus 93% dense and 3% ± 1% for oxide-derived baseline. For Carb-NZSP, the secondary glassy phosphate phase is agglomerated, while for baseline, it is dispersed and percolated. Electrochemical testing combined with post-mortem analysis demonstrates how microstructural control of secondary phases is critical for dendrite suppression: Carb-NZSP critical current density (CCD) is 3.1 ± 0.8 mA cm −2 at 0.1 mAh cm −2 , versus 1.0 ± 0.7 mA cm −2 at 0.1 mAh cm −2 . Cryogenic focused ion beam (cryo-FIB) analysis demonstrates that in both materials, the porous 2D sheet-like sodium metal dendrites propagate around and subsume NZSP grains, likely following a path enriched with glassy phase and with porosity. Dendrites also flow around isolated zirconia particles. Phase field simulation reveals deflection of dendrites by mechanically tough zirconia, while brittle glassy phase accelerates dendrite growth, especially when finely distributed.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Deciphering the Dynamic Balance Between Solvation Strength and Polysulfides Reaction Heterogeneity in Practical Lithium‐Sulfur Batteries

Achieving stable interfacial chemistry in lithium–sulfur batteries under practical conditions remains a key barrier to commercialization. Here, we demonstrate that interfacial dynamics can be effectively regulated by coupling solvation-power control with intrinsic heterogeneity of sulfur redox chemistry through the introduction of a weakly solvating fluorinated cosolvent, LIB 1200ET (1200ET). Compared with conventional fluorinated ethers, 1200ET efficiently shifts Li + solvation environment toward a more non-coordinated configuration at low volume fractions, enabling substantial solvation modulation without significantly impairing sulfur redox kinetics. This solvation transition weakens Li + –solvent interactions while strengthening Li + –anion and Li + –lithium polysulfide (LPS) coordination, suppressing LPS solubility and promoting reconstruction of solid–electrolyte interphase (SEI). Regulated LPS chemistry, together with 1200ET, leads to formation of a S 4+ -rich, LiF-reinforced SEI with enhanced ionic conductivity and mechanical robustness. Spatially resolved sulfur K-edge X-ray absorption spectroscopy on pouch cells reveals pronounced current-density-dependent chemical heterogeneity, distinguishing kinetically dominated and solvation-controlled regions. Under practical conditions (3.7 mg cm −2 sulfur loading, E/S = 6 µL mg −1 ), a single-layer pouch cell delivers 527 mAh g −1 over 200 cycles at C/3, while an Ah-level multilayer pouch cell achieves an energy density of 358 Wh kg −1 . These results establish non-coordinating cosolvent-driven solvation engineering as a scalable strategy for practical Li–S batteries.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Additive manufacturing of sandwich panels with continuous fiber reinforced high modulus composite facings

Abstract An improved approach consisting of a combination of fiber placement and fused filament fabrication is introduced for the additive manufacture (AM) of structural grade sandwich beams. Here, sandwich beams are additively manufactured using in‐situ deposition and consolidation of continuous fiber unidirectional facings made from a commingled yarn system of e‐glass fiber (~50% vol.) and amorphous PET, and a hexagonal honeycomb core structure made from PETG. Both facings and the sandwich core are manufactured on a single machine, in one sequence (skin‐core‐skin), employing the benefit of matrix compatibility to create autohesion at the interfaces. Flexural and transverse shear rigidity are determined experimentally and compared with analytical predictions and show correlation to within 3%. Flexural strength and core shear strength are also measured. Post‐mortem examinations show that core fracture and core facing debond were the dominant failure mode in flexure. Single cantilever beam tests were performed to evaluate core facing debond toughness. Subsequently, surface preheat using infrared heaters was utilized to increase autohesion between core and facing. The results show debond toughness was increased 4 times using infrared heating. This research effort presents a manufacturing approach that has the potential for the AM of stiff, well bonded, structural grade sandwich beams, in an integrated sequence, employing in‐situ consolidation to the facings, without the need for the use of intermediate adhesives for skin‐to‐core bonding. Highlights An improved additive manufacturing technique for making sandwich panels is developed. Sandwich panel facings have fiber volume fractions of approximately 50%. Surface preheat improves core‐to‐facing debond toughness by a factor of 4. Top and bottom facings are consolidated during manufacture leading to better properties. Experimental results are compared to analytical predictions and show good correlation.

17 WIND ENERGY↗
DOE OSTI2025

Automated Scoring of Morphological Changes in Images of Pentaerythritol Tetranitrate

Recent advances in characterization techniques that generate large datasets of material microstructure images require robust, automated image-processing. We applied an unsupervised anomaly detection method called feature anomaly detection system (FADS) to automatically detect and quantify microstructure changes in images of the explosive pentaerythritol tetranitrate (PETN) aged at various temperatures. We demonstrated the FADS approach on two-dimensional images extracted from computed tomography scans, but the same technique can be readily applied to other imaging modalities. FADS calculates anomaly scores on the basis of differences in filter activations of nominal and test data in pretrained convolutional neural networks. The FADS scores successfully differentiated between pristine PETN and PETN aged at a temperature where material coarsening occurred. Morphological metric analysis of segmented images verified observed trends in FADS scores as a function of aging temperature and aging time, specifically by calculating volume fractions, specific boundary lengths, two-point correlation functions, and local thicknesses. Here, the FADS technique has two important advantages compared to traditional morphological analysis: First, it uses grayscale images as input, rather than images that are segmented to separate the appropriate phases; and second, FADS scores capture any type of changes among image sets, rather than requiring prior knowledge or selection of a relevant set of metrics.

Accelerated aging↗
DOE OSTI2025

Megahertz Rate Optical Diagnostics of Explosively Generated Soot

Detonation of a solid explosive produces a turbulent and luminous post‐detonation fireball containing condensed carbon soot. Diagnostics of soot dynamics are needed for model validation and to interpret emission signals. Diffuse back‐illumination extinction imaging (DBI‐EI) and laser‐induced incandescence (LII) are two common optical diagnostics for flame soot. This work extends both to measure time‐resolved soot dynamics from a 12 mm HMX hemisphere. DBI‐EI measured line‐of‐sight optical extinction exceeds 99% in some regions. Results are tomographically inverted to obtain a signal proportional to the soot volume fraction. Pulse‐burst LII measures are presented at 1 MHz. For the first time, LII results are combined with DBI‐EI extinction measurements to quantify and correct for signal trapping. Following this, spatially and temporally resolved DBI‐EI and LII measures are shown to be in reasonable agreement. Finally, experimental results are compared against recently developed simulations. Quantitative differences in the soot mixing dynamics are resolved. These findings motivate future model improvements and demonstrate ongoing needs for diagnostic advancements for heavily sooting environments.

diffuse back-illumination extinction imaging↗
DOE OSTI2024

Level-set topology optimization with PDE generated conformal meshes

This paper presents a level-set topology optimization approach that uses conformal meshes for the analysis of the displacement field. The structure’s boundary is represented by the iso-contour of a level-set field discretized on a fixed background design mesh. The conformal mesh is updated for each design iteration via a PDE based mesh morphing process that identifies the set of facets in the background mesh that are homeomorphic to the boundary and relaxes the homeomorphic mesh to conform to the structure’s boundary and ensure high element quality. The conformal mesh allows for a more accurate computation of the response versus density and some level-set based methods which interpolate material properties using the volume fraction. Numerical examples illustrate the proposed approach by optimizing linear-elastic two- and three-dimensional structures, wherein insight into the performance of the mesh morphing process is provided. The examples also highlight the scalability of the approach.

42 ENGINEERING↗
DOE OSTI2024

Microstructural evolution in a precipitate-hardened (Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 ) 94 Ti 2 Al 4 multi-principal element alloy during high-pressure torsion

Multi-principal element alloys demonstrate high strength, thermal stability, and irradiation resistance, making them excellent candidate materials for applications in nuclear reactors and other harsh environments. Some studies have examined the use of high-pressure torsion to strengthen MPEAs through grain size reduction and strain hardening. However, no studies have investigated the effect of HPT on secondary phases (precipitates) within an MPEA. Two alloys, (Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 ) 94 Ti 2 Al 4 containing Ni(Ti, Al) B2 phase, and CrFe σ phase, and single-phase Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 , were fabricated by casting and heat treatment. Both alloys were then processed with HPT to study microstructural evolution. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to characterize the alloys before and after HPT processing. HPT processing produced a nanocrystalline structure in both alloys, but (Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 ) 94 Ti 2 Al 4 exhibited a significantly smaller grain size and higher dislocation density than Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 , with corresponding higher hardness. Before HPT, the (Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 ) 94 Ti 2 Al 4 alloy consisted of large grain (~ 400 μm) and precipitates, including B2 of ~ 38 μm average size, B2 of ~ 0.7 μm average size, and small amounts of σ of ~ 1.5 μm average size. After HPT, the larger B2 precipitates were decreased in size and volume fraction, while the smaller B2 precipitates were completely dissolved; the σ precipitates appeared unaffected by HPT, likely due to their much higher hardness. Finally, observation of the B2 precipitate distribution along radial distance indicates that the strain caused the precipitates to fracture at intermediate strain (γ = 125) and dissolve at high strain (γ = 280).

36 MATERIALS SCIENCE↗
DOE OSTI2025

Phase equilibria and microstructure evolution in the Ni-rich region of binary Ni-Ce and ternary Ni-Ce-X (X=Al, Nb, Cr, Ti) systems at 900 °C

The equilibrium compositions of all phases in the Ni-rich region of binary Ni-Ce and ternary Ni-Ce-X (X=Al, Nb, Cr, Ti) systems at 900 °C were determined experimentally through isothermal annealing for up to 500 h and compared with currently available computational thermodynamic descriptions. Additionally, the study examined how adding a third element to the binary system affects the microstructure by analyzing changes in the volume fraction of the intermetallic phase in the eutectic region. It was observed that Nb and Ti addition lowered the intermetallic fraction in the eutectic region while Al and Cr addition did the opposite. The fraction of intermetallic phase in the eutectic region is very important because it contributes to extreme brittleness of these alloys. Also, Al, Nb and Ti addition promoted different precipitates upon annealing when added in sufficient amounts. The collected data on composition and phase equilibria provides crucial information for improving the thermodynamic assessments of the binary and ternary alloy systems.

energy dispersive spectrometry↗
DOE OSTI2025

Creep Deformation and Damage Mechanisms in an Advanced High-Temperature Additively Manufactured Nickel-Base Superalloy

Abstract This research investigates the processing–structure–properties–performance relationship in a novel nickel-base superalloy, ABD ® -900AM, designed for extreme environments. Specifically tailored for additive manufacturing (AM), ABD ® -900AM maintains mechanical integrity at high temperatures and is comparable to other nickel-based superalloys with a 30–40% gamma-prime volume fraction. A comprehensive study was conducted using laser-beam powder bed fusion and electron-beam powder bed fusion methods. Factors such as heat treatment, porosity, build orientation, and hot isostatic pressing were evaluated to understand their effects on microstructure and mechanical performance. Microstructural characterization revealed significant differences in grain size and orientation across build processes and heat treatments. High-temperature mechanical testing indicated that grain size, heat treatment, and orientation significantly influence creep behavior. A super-solvus heat treatment led to recrystallization and grain growth, significantly improving creep properties compared to a near-solvus heat treatment. Various creep mechanisms were identified across different conditions, and creep rupture models were developed for each build process. Post-test microstructural analysis showed grain boundary damage, with differences in creep cavitation morphology under varying stress conditions. It was shown that MC carbides grow at the expense of gamma-prime near grain boundaries, leading to precipitate-free zones in specimens tested at higher temperatures. This study fills a significant gap in fundamental research by offering a deeper insight into the high-temperature mechanical behavior of additively manufactured nickel-base superalloys. It also explores critical research questions regarding the role of carbides and the significance of heat treatment. The insights gained enhance confidence in the industry adoption of ABD ® -900AM and similar alloys for high-temperature applications, bridging the knowledge gap and supporting the development of reliable AM processes for extreme environments.

Bridges, Alex (ORCID:000000030338759X)↗
DOE OSTI2025

Rules for the crystallite size and dislocation density evolution in phases during α-ω transformation in Zr under high-pressure and severe plastic flow

The first in-situ X-ray diffraction (XRD) study of the evolution of the crystallite size and dislocation density in phases during plastic strain-induced phase transformation (PT) is performed utilizing α-ω PT in strongly pre-deformed commercially pure Zr as an important example. Rough diamond anvils (rough-DA) are introduced to intensify all occurring processes during heterogeneous compression of Zr in a diamond anvil cell (DAC). The main rule is found that during α-ω PT the crystallite size and dislocation density in ω-Zr depend solely on the volume fraction of ω-Zr and are independent of pressure, plastic strain tensor, its path, and initial nanostructure. Crystallite size in ω-Zr increases from 10 to 60 nm during the PT, while dislocation density reduces from 1.83×10 15 /m 2 to 0.6×10 15 /m 2 . Rough-DA produce a steady nanostructure in α-Zr before PT with smaller crystallite size and larger dislocation density than smooth-DA, leading to a reduction of the minimum pressure for α-ω PT to a record value 0.67 GPa, 9 times smaller than under hydrostatic loading and 5.1 times lower than the phase equilibrium pressure. In addition to strain, the kinetics of strain-induced PT unexpectedly depends on time. Also, strain-controlled part of kinetics is zero order, in contrast to the first-order kinetics with smooth-DA. The obtained results open a new window for understanding the mutual effects of nanostructure evolution and PT during severe plastic flow in various technological and natural processes. In conclusion, they may bring up economic strategies of producing nanocomposites and single-phase nanostructured materials with optimal properties.

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