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DOE OSTI2024

New dynamic diamond anvil cell for time-resolved radial x-ray diffraction

The dynamic diamond anvil cell (dDAC) is a recently developed experimental platform that has shown promise for studying the behavior of materials at strain rates ranging from intermediate to quasi-static and shock compression regimes. Combining dDAC with time-resolved x-ray diffraction (XRD) in the radial geometry (i.e., with incident x-rays perpendicular to the axis of compression) enables the study of material properties such as strength, texture evolution, and deformation mechanisms. This work describes a radial XRD dDAC setup at beamline P02.2 (Extreme Conditions Beamline) at DESY’s PETRA III synchrotron. Time-resolved radial XRD data are collected for titanium, zirconium, and zircon samples, demonstrating the ability to study the strength and texture of materials at compression rates above 300 GPa/s. In addition, the simultaneous optical imaging of the DAC sample chamber is demonstrated. The ability to conduct simultaneous radial XRD and optical imaging provides the opportunity to characterize plastic strain and deviatoric strain rates in the DAC at intermediate rates, exploring the strength and deformation mechanisms of materials in this regime.

47 OTHER INSTRUMENTATION↗

DOE OSTI2025

Location-Specific Microstructures and Properties of Haynes 282 Alloy with Laser-Wire DED Processing

In this work, the location-specific microstructures in terms of grain morphology, texture, γ′ precipitates, carbides, and residual strains were investigated in a series of laser-wire direct energy deposition (LW-DED) Haynes 282 alloys with varied processing parameters. A bimodal grain distribution was found in these as-printed and heat-treated alloys with columnar grains within the layers and fine equiaxed grains at the interlayer regions. Dominant <001> texture along the build direction with more obvious <111> orientation preference exists at the bottom layers, compared to the top layers. The gradient γ′-precipitates size distribution contributes predominantly to the observed gradient hardness distribution in the as-printed samples. The heat-treated 282 exhibit comparable yield strengths to those conventionally-processed counterparts, while the observed small deviation in their yield strengths is attributed to the Hall-Petch effect. This work establishes the correlation between location-specific microstructures and mechanical properties, providing valuable insights into future printing parameters and heat-treatment optimization.

Haynes 282↗

DOE OSTI2025

Implementation of disruptive designs for gas turbine components using direct energy deposition additive manufacturing

This research aims to develop a framework for establishing the correlation between in-situ monitoring data, process parameters, and microstructure evolution in blown-powder laser-directed energy deposition (DED) additive manufacturing (AM). To achieve this, a comprehensive manufacturing framework has been developed, spanning from in-situ data acquisition, melt-pool simulation, microstructure modeling, and statistical microstructure quantification. A machine learning-based surrogate model is constructed to predict melt pool geometry directly from in-situ coaxial camera data. The surrogate model is trained using outputs from a high-fidelity melt pool simulation, which provides accurate melt pool dimension data under varying process conditions. The predicted melt pool geometry is then used as input to a microstructure model to predict microstructural features. To rigorously compare and analyze microstructures, the project introduces statistical metrics that quantify differences based on key features such as morphology and texture. Microstructures are represented using advanced statistical descriptors including angular chord length distribution, two-point spatial statistics, orientation distribution function, and global spherical harmonic. These representations are used to compute four distinct “dissimilarity scores” that quantitatively capture differences in texture and morphology. This framework is demonstrated to enable automated calibration of simulation parameters by minimizing discrepancies between simulated and target microstructures. The technology developed in this project enables direct correlation between in-situ monitoring data and resulting microstructure, paving the way for adaptive microstructure control in metal AM. This capability strengthens the connection between process parameters and final material properties, facilitating more precise and reliable material design.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Deformation of Polycrystalline MgO Up to 8.3 GPa and 1270 K: Microstructures, Dominant Slip-Systems, and Transition to Grain Boundary Sliding

Ferropericlase is the second most abundant mineral in the Earth’s lower mantle and its mechanical properties have a strong influence on the rheology of this region. Here, we deform polycrystalline MgO, the magnesium end-member of ferropericlase, at conditions ranging from 1.6 to 8.3 GPa and 875–1,270 K. We analyse the flow laws and microstructures of the recovered samples using electron microscopy and compare our observations with predictions from the literature. We identify a first mechanism for samples deformed at 1,270 K, attributed to a regime controlled by grain boundary sliding accommodated by diffusion, and characterized by a small grain size, an absence of texture, and no intracrystalline deformation. At 1,070 K and below, the deformation regime is controlled by dislocations. The samples show a more homogeneous grain size distribution, significant texture, and intracrystalline strains. In this regime, deformation is controlled by the ⟨110⟩{110} slip system and a combined ⟨110⟩{110} and ⟨110⟩{100} slip, depending on pressure and temperature. Based on these results, we propose an updated deformation map for polycrystalline MgO at mantle conditions. The implications for ferropericlase and seismic observations in the Earth’s lower mantle are discussed.

Ledoux, Estelle Elisa↗

DOE OSTI2019

Long-Term Studies Reveal Differential Responses to Climate Change for Trees Under Soil- or Herbivore-Related Stress

Worldwide, trees are confronting increased temperature and aridity, exacerbating susceptibility to herbivory. Long-term studies comparing patterns of plant performance through drought can help identify variation among and within populations in vulnerability to climate change and herbivory. We use long-term monitoring data to examine our overarching hypothesis that the negative impacts of poor soil and herbivore susceptibility would be compounded by severe drought. We studied pinyon pine, Pinus edulis, a widespread southwestern tree species that has suffered extensive climate-change related mortality. We analyzed data on mortality, growth, male reproduction, and herbivory collected for 14–32 years in three areas with distinct soil-types. We used standardized precipitation-evapotranspiration index (SPEI) as a climate proxy that summarizes the impacts of drought due to precipitation and temperature variation on semi-arid forests. Several key findings emerged: (1) Plant performance measurements did not support our hypothesis that trees growing in stressful, coarse-textured soils would suffer more than trees growing in finer-textured soils. Stem growth at the area with coarse, young cinder soils (area one) responded only weakly to drought, while stem growth on more developed soils with sedimentary (area two) and volcanic (area three) substrates, was strongly negatively affected by drought. Male reproduction declined less with drought at area one and more at areas two and three. Overall mortality was 30% on coarse cinder soils (area one) and averaged 55% on finer soil types (areas two and three). (2) Although moth herbivore susceptible trees were hypothesized to suffer more with drought than moth resistant trees, the opposite occurred. Annual stem growth was negatively affected by drought for moth resistant trees, but much less strongly for moth susceptible trees. (3) In contrast to our hypothesis, moths declined with drought. Overall, chronically water-stressed and herbivore-susceptible trees had smaller declines in performance relative to less-stressed trees during drought years. These long-term findings support the idea that stressed trees might be more resistant to drought since they may have adapted or acclimated to resist drought-related mortality.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2022

Pore-Scale Modeling of Mineral Growth and Nucleation in Reactive Flow

A fundamental understanding of mineral precipitation kinetics relies largely on microscopic observations of the dynamics of mineral surfaces exposed to supersaturated solutions. Deconvolution of tightly bound transport, surface reaction, and crystal nucleation phenomena still remains one of the main challenges. Particularly, the influence of these processes on texture and morphology of mineral precipitate remains unclear. This study presents a coupling of pore-scale reactive transport modeling with the Arbitrary Lagrangian-Eulerian approach for tracking evolution of explicit solid interface during mineral precipitation. It incorporates a heterogeneous nucleation mechanism according to Classical Nucleation Theory which can be turned “on” or “off.” This approach allows us to demonstrate the role of nucleation on precipitate texture with a focus at micrometer scale. In this work precipitate formation is modeled on a 10 micrometer radius particle in reactive flow. The evolution of explicit interface accounts for the surface curvature which is crucial at this scale in the regime of emerging instabilities. The results illustrate how the surface reaction and reactive fluid flow affect the shape of precipitate on a solid particle. It is shown that nucleation promotes the formation of irregularly shaped precipitate and diminishes the effect of the flow on the asymmetry of precipitation around the particle. The observed differences in precipitate structure are expected to be an important benchmark for reaction-driven precipitation in natural environments.

58 GEOSCIENCES↗

DOE OSTI2025

What regulates decomposition in agroecosystems? Insights from reading the tea leaves

Litter decomposition is a critical Earth process, recycling nutrients and setting a portion of plant tissue on a path toward soil organic matter. Despite this importance, we still lack a good understanding of local factors that regulate decomposition, especially in agroecosystems where management plays an outsized role. Using a narrow range of climate and soils, we buried 1,308 pre-manufactured “litter bags” of differing residue quality (i.e., green and rooibos tea leaves) in 109 plots across several management practices to (1) explore the local controls on decomposition in agroecosystems and (2) test the robustness of the Tea Bag Index (TBI). We found that management practices intended to increase soil ecosystem services, that is, soil health, altered the decomposition of both teas. For example, adding nitrogen fertilizer and implementing perennial cropping decreased the extent of green tea decomposition (carbon-to-nitrogen ratio, or C:N = 12.8). No-tillage increased, but perennial cropping decreased, the rate of rooibos tea decomposition (C:N = 50.1). Cropped prairie accelerated green tea decomposition and increased the extent of red tea decomposition. A random forest regression model showed that soil temperature was the strongest predictor of green tea decomposition, but a soil health score also played a significant role in predicting the mass remaining. Soil texture and nutrient availability best predicted rooibos tea decomposition. Finer textured soils seemed to decelerate rooibos decomposition but increased the extent of decomposition. Furthermore, we demonstrated that the TBI metrics correlated somewhat well with empirically derived decomposition constants and were similarly sensitive to the effects of management. Still, the green tea stabilization factor had a substantial prediction bias. Our study increased our basic understanding of what regulates decomposition in agroecosystems. It also showed that the TBI can be a scientifically rigorous citizen science approach to monitoring changes in soil health.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2026

Unlocking the Future of Aircraft Manufacturing: The Environmental Benefits of Laser Patterning for Surface Enhancement of Aircraft-Certified Alloys

Surface protection and functional modification of aircraft-certified aluminum alloys are essential for corrosion resistance, durability, and long-term airworthiness. At the same time, increasingly restrictive environmental regulations motivate the development of alternatives to legacy wet-chemical surface treatments. This study presents an integrated assessment of ultrafast femtosecond laser surface texturing as a surface functionalization approach for Aluminum 6061 alloys within an aerospace manufacturing and sustainability context. Ultrashort-pulse laser processing enables controlled micro- and nano-scale surface topographical modification with limited thermal impact, allowing adjustment of wettability and surface functionality while preserving bulk material integrity. As a dry and contactless process, femtosecond laser treatment eliminates the use of hazardous chemicals, reduces consumable inputs, and generates minimal secondary waste. A streamlined cradle-to-gate life cycle assessment conducted in accordance with ISO 14040/14044 indicates a lower global-warming potential per functional unit compared with conventional surface treatments, including anodization, plasma-assisted coatings, and organic coating systems. Complementary qualitative analyses addressing environmental health and safety, supply-chain risk, and ESG alignment indicate potential advantages related to occupational safety, regulatory compliance, waste management, and end-of-life recyclability. The investigation is performed on planar Aluminum 6061 reference surfaces with a treated area of 25 mm 2 , providing a controlled laboratory-scale basis for analyzing process behavior, functional surface modification, and associated environmental metrics. Within this defined scope, the results support further evaluation of femtosecond laser surface texturing as a surface engineering option for future aerospace manufacturing.

corrosion resistance↗

DOE OSTI2018

Trade-off between Photon Management Efficacy and Material Quality in Thin-Film Solar Cells on Nanostructured Substrates of High Aspect Ratio Structures

Although texturing of the transparent electrode of thin-film solar cells has long been used to enhance light absorption via light trapping, such texturing has involved low aspect ratio features. With the recent development of nanotechnology, nanostructured substrates enable improved light trapping and enhanced optical absorption via resonances, a process known as photon management, in thin-film solar cells. Despite the progress made in the development of photon management in thin-film solar cells using nanostructures substrates, the structural integrity of the thin-film solar cells deposited onto such nanostructured substrates is rarely considered. Here, we report the observation of the reduction in the open circuit voltage of amorphous silicon solar cells deposited onto a nanostructured substrate with increasing areal number density of high aspect ratio structures. For a nanostructured substrate with the areal number density of such nanostructures increasing in correlation with the distance from one edge of the substrate, a correlation between the open circuit voltage reduction and the increase of the areal number density of high aspect ratio nanostructures of the front electrode of the small-size amorphous silicon solar cells deposited onto different regions of the substrate with graded nanostructure density indicates the effect of the surface morphology on the material quality, i.e., a trade-off between photon management efficacy and material quality. Lastly, this observed trade-off highlights the importance of optimizing the morphology of the nanostructured substrate to ensure conformal deposition of the thin-film solar cell.

14 SOLAR ENERGY↗

DOE OSTI2019

Processing of Alnico Magnets by Additive Manufacturing

Permanent magnets without rare earth (RE) elements, such as alnico, will improve supply stability and potentially decrease permanent magnet cost, especially for traction drive motors and other increased temperature applications. Commercial alnico magnets with the highest energy product are produced by directional solidification (DS) to achieve a < 001 > columnar grain orientation followed by significant final machining, adding to the high cost. Additive manufacturing (AM) is an effective method to process near net-shape parts with minimal final machining of complex geometries. AM also, has potential for texture/grain orientation control and compositionally graded structures. This report describes fabrication of alnico magnets by AM using both laser engineered net shaping (LENS)/directed energy deposition (DED) and electron beam melting powder bed fusion (EBM/PBF). High pressure gas atomized (HPGA) pre-alloyed alnico powders, with high purity and sphericity, were built into cylindrical and rectangular samples, followed by magnetic annealing (MA) and a full heat treatment (FHT). The magnetic properties of these AM processed specimens were different from their cast and sintered counterparts of the same composition and show a great sensitivity to heat treatment. The AM process parameters used in this developmental study did not yet result in any preferred texture within the alnico AM builds. These findings demonstrate feasibility for near net-shape processing of alnico permanent magnets for use in next generation traction drive motors and other applications requiring increased operating temperatures and/or complex engineered part geometries, especially with further AM process development for texture control.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Microstructural and Hall–Petch Analysis of Additively Manufactured Ferritic Alloy Using 2507 Duplex Stainless Steel Powder

The powder bed fusion–laser beam (PBF-LB) process, a method of additive manufacturing (AM), was used to print duplex stainless steel (DSS) using commercial-grade 2507 powders. While conventionally processed DSS has a two-phase microstructure consisting of 50% austenite and 50% ferrite, the PBF-LB-printed 2507 alloy was nearly 100% ferrite. Optimal processing conditions that minimized porosity were determined to be 290 W laser power and 1000 mm/s scan speed, and grain size, texture, and phases were characterized as a function of laser power and scan speed. Grain size increased with increasing laser power but decreased with increasing scan speed. A <100> texture diminished with increasing scan speed from 1000 mm/s to 1400 mm/s. No austenite phase was detected. Transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) characterization revealed nanoscale chromium nitride precipitates in the ferritic matrix (incoherent hexagonal close-packed (HCP) precipitates at grain boundaries and coherent body-centered cubic (BCC) precipitates within the grains) and a high density of tangled dislocations. Tensile tests of as-printed alloys showed a yield strength of 570 MPa, an ultimate tensile strength of 756 MPa, and an elongation to failure of 10%. The tensile properties were analyzed based on the observed microstructure considering grain size, nanoscale precipitates, and the high density of dislocations.

Crystallography↗

DOE OSTI2024

Anisotropic Tensile Properties of a 14YWT Nanostructured Ferritic Alloy: On the Role of Cleavage Fracture

Two plates of nanostructured ferritic alloy NFA-1 were processed by ball milling atomized Fe-14Cr-3W-0.4Ti-0.2Y (wt.%) with FeO powders, canning, and hot-extrusion at 850 °C, followed by annealing and multipass cross-rolling at 1000 °C. This produces a severe (001) brittle cleavage texture on planes running parallel to the plate faces. In the first plate (P1), pre-existing microcracks (MCs) formed on the cleavage planes during cross-rolling. The second plate (P2) contained far fewer, if any, MCs. Here, we compare the tensile data for out-of-plane (S) and in-plane (L) tensile axis orientations, at temperatures from −196 °C to 800 °C. We also assess the tensile property differences between P1 and P2, and the effect of specimen size. The L-orientation strength and ductility were excellent; for example, the room temperature (RT) yield stress, σy ≈ 1042 ± 102 MPa, and the total elongation, εt ≈ 12.9 ± 1.5%. In contrast, the S-orientation RT σy ≈ 708 ± 57 MPa, and εt ≤ 0.2%. These differences were due to cleavage on the brittle (001) planes. Cleavage leads to beneficial delamination toughening, but is deleterious to deformation processing and through-wall heat transfer. Therefore, it is important to quantitatively characterize the pronounced NFA-1 strength anisotropy due to severe crystallographic texturing and cleavage fracture.

Crystallography↗

DOE OSTI2023

Effect of Melt-Spinning Parameters on the Structure and Properties of Ni 55.5 Mn 18.8 Ga 24 Si 1.7 Heusler Alloy Ribbons

Ni–Mn-based Heusler alloys are known to demonstrate magnetic shape memory and giant magnetocaloric effect (MCE). These effects depend on the phases, crystallographic and magnetic phase transitions, and the crystallographic texture characteristics. These structural characteristics, in turn, are a function of the processing parameters. In the current work, Ni 55.5 Mn 18.8 Ga 24 Si 1.7 Heusler alloy was processed by melt-spinning under a helium atmosphere. This process results in a fine microstructure. The ribbon that was produced with a narrower nozzle width, faster wheel speed, and higher cast temperature, indicating a faster cooling rate, had double the magnetic entropy change close to room temperature. However, the other ribbon demonstrated a large entropy change over a broader temperature range, extending its usability. The effect of the melt-spinning process parameters on the developing microstructure, crystallographic structure and texture, transformation temperatures, and the magnetic entropy change were studied to explain the difference in magnetocaloric behavior.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Crystal Plasticity Modeling and Experimental Validation with an Orientation Distribution Function for Ti-7Al Alloy

An orientation distribution function based model is used for micromechanical modeling of the titanium-aluminum alloys, Ti-0 wt % Al and Ti-7 wt % Al, which are in demand for many aerospace applications. This probability descriptor based modeling approach is different than crystal plasticity finite element techniques since it computes the averaged material properties using upper bound averaging. A rate-independent single-crystal plasticity model is implemented to compute the effect of macroscopic strain on the polycrystal. An optimization problem is defined for calibrating the basal, prismatic, pyramidal slip system and twin parameters using the available tension and compression experimental data. The crystal plasticity parameters of Ti-7 wt % Al are not studied extensively in literature, and therefore the optimization results for the crystal plasticity model realization produce unique data, which will be beneficial to future studies in the field. The sensitivities of the slip and twin parameters to the design objectives are also investigated to identify the most critical slip system parameters. Using the optimum design parameters, the microstructural textures, during the tension test, are predicted by the crystal plasticity finite element simulations, and compared to the available experimental texture and scanning electron microscope—digital image correlation data.

36 MATERIALS SCIENCE↗

DOE OSTI2022

High-Temperature Ferroelectric Behavior of Al 0.7 Sc 0.3 N

Currently, there is a lack of nonvolatile memory (NVM) technology that can operate continuously at temperatures > 200 °C. While ferroelectric NVM has previously demonstrated long polarization retention and >10 13 read/write cycles at room temperature, the largest hurdle comes at higher temperatures for conventional perovskite ferroelectrics. Here, we demonstrate how AlScN can enable high-temperature (>200 °C) nonvolatile memory. The c-axis textured thin films were prepared via reactive radiofrequency magnetron sputtering onto a highly textured Pt (111) surface. Photolithographically defined Pt top electrodes completed the capacitor stack, which was tested in a high temperature vacuum probe station up to 400 °C. Polarization–electric field hysteresis loops between 23 and 400 °C reveal minimal changes in the remanent polarization values, while the coercive field decreased from 4.3 MV/cm to 2.6 MV/cm. Even at 400 °C, the polarization retention exhibited negligible loss for up to 1000 s, demonstrating promise for potential nonvolatile memory capable of high–temperature operation. Fatigue behavior also showed a moderate dependence on operating temperature, but the mechanisms of degradation require additional study.

36 MATERIALS SCIENCE↗

DOE OSTI2016

FADING CORONAL STRUCTURE AND THE ONSET OF TURBULENCE IN THE YOUNG SOLAR WIND

Above the top of the solar corona, the young, slow solar wind transitions from low- β , magnetically structured flow dominated by radial structures to high- β , less structured flow dominated by hydrodynamics. This transition, long inferred via theory, is readily apparent in the sky region close to 10° from the Sun in processed, background-subtracted solar wind images. We present image sequences collected by the inner Heliospheric Imager instrument on board the Solar-Terrestrial Relations Observatory ( STEREO /HI1) in 2008 December, covering apparent distances from approximately 4° to 24° from the center of the Sun and spanning this transition in the large-scale morphology of the wind. We describe the observation and novel techniques to extract evolving image structure from the images, and we use those data and techniques to present and quantify the clear textural shift in the apparent structure of the corona and solar wind in this altitude range. We demonstrate that the change in apparent texture is due both to anomalous fading of the radial striae that characterize the corona and to anomalous relative brightening of locally dense puffs of solar wind that we term “flocculae.” We show that these phenomena are inconsistent with smooth radial flow, but consistent with the onset of hydrodynamic or magnetohydrodynamic instabilities leading to a turbulent cascade in the young solar wind.

79 ASTRONOMY AND ASTROPHYSICS↗

DOE OSTI2013

Image segmentation by hierarchial agglomeration of polygons using ecological statistics

A method for rapid hierarchical image segmentation based on perceptually driven contour completion and scene statistics is disclosed. The method begins with an initial fine-scale segmentation of an image, such as obtained by perceptual completion of partial contours into polygonal regions using region-contour correspondences established by Delaunay triangulation of edge pixels as implemented in VISTA. The resulting polygons are analyzed with respect to their size and color/intensity distributions and the structural properties of their boundaries. Statistical estimates of granularity of size, similarity of color, texture, and saliency of intervening boundaries are computed and formulated into logical (Boolean) predicates. The combined satisfiability of these Boolean predicates by a pair of adjacent polygons at a given segmentation level qualifies them for merging into a larger polygon representing a coarser, larger-scale feature of the pixel image and collectively obtains the next level of polygonal segments in a hierarchy of fine-to-coarse segmentations. The iterative application of this process precipitates textured regions as polygons with highly convolved boundaries and helps distinguish them from objects which typically have more regular boundaries. The method yields a multiscale decomposition of an image into constituent features that enjoy a hierarchical relationship with features at finer and coarser scales. This provides a traversable graph structure from which feature content and context in terms of other features can be derived, aiding in automated image understanding tasks. The method disclosed is highly efficient and can be used to decompose and analyze large images.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Multi-Objective Optimization of a Wrought Magnesium Alloy for High Strength and Ductility

An optimization technique is coupled with crystal plasticity based finite element (CPFE) computations to aid the microstructural design of a wrought magnesium alloy for improved strength and ductility. The initial microstructure consists of a collection of sub-micron sized grains containing deformation twins. The variables used in the simulations are crystallographic texture, and twin spacing within the grains. It is assumed that plastic deformation occurs mainly by dislocation slip on two sets of slip systems classified as hard and soft modes. The hard modes are those slip systems that are inclined to the twin planes and the soft mode consists of dislocation glide along the twin plane. The CPFE code calculates the stress-strain response of the microstructure as a function of the microstructural parameters and the length-scale of the features. A failure criterion based on a critical shear strain and a critical hydrostatic stress is used to define ductility. The optimization is based on the sequential generation of an initial population defined by the texture and twin spacing variables. The CPFE code and the optimizer are coupled in parallel so that new generations are created and analyzed dynamically. In each successive generation, microstructures that satisfy at least 90% of the mean strength and mean ductility in the current generation are retained. Multiple generation runs based on the above procedure are carried out in order to obtain maximum strength-ductility combinations. The implications of the computations for the design of a wrought magnesium alloy are discussed. Research sponsored by the Laboratory Directed Research and Development Program of Oak Ridge National Laboratory, managed by UT-Battelle, LLC, for the U. S. Department of Energy.

Radhakrishnan, Balasubramaniam↗