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At least 289 records · Page 16

All sources NASA NTRS DOE OSTI

DOE OSTI2022

Kinetics and evolution of solid-state metal dealloying in thin films with multimodal analysis

Thin-film solid-state metal dealloying (thin-film SSMD) is an emerging technique that uses self-organization to design nanostructured thin films. The resulting 3D bicontinuous nanostructures are promising for a wide range of applications, such as catalysis and energy storage. In this work, we prepared thin films by SSMD using Ti-Cu as the parent alloy and Mg as the solvent. Using a multimodal approach, we combined synchrotron X-ray spectroscopy, diffraction, and high-resolution electron-based spectroscopy and imaging to study their morphological, structural, and chemical evolution. The processing-structure relationship was analyzed as a function of parent alloy composition and dealloying temperature and time. Morphological transitions from globular, to lamellar, to bicontinuous structures, in conjunction with a ligament size evolution, were identified as functions of the parent alloy composition. The dealloying rate increased with increasing concentration of interdiffusing elements (dissolving component) in the parent alloy. The parting limit, a dealloying compositional threshold, was systematically analyzed and determined to be 30%–40%. The order of crystalline phase formation is CuMg 2 , Cu 2 Mg, and Ti; the Ti phase first shows self-reorganization during dealloying, separate from the crystallization process. The coarsening in thin-film SSMD was identified and not entirely self-similar; in addition to the increase of ligament size over time, the formation of larger globular ligaments were also observed. This work furthers our fundamental understanding of thin-film SSMD and nanostructured thin-film design, where the thermodynamic and kinetic effects differ from the bulk counterparts. The fact that dealloying and diffusion outpaces the crystallization and new phase formation also offers opportunities to utilize thin-film SSMD in certain alloy systems in which deleterious intermetallic phases need to be suppressed, that may not be possible in the bulk geometry.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2020

Charge generation mechanism tuned via film morphology in small molecule bulk-heterojunction photovoltaic materials

Small organic molecules have emerged as promising component materials for organic photovoltaic devices. Compared to most conjugated polymers for the same application, small molecules have unique morphologies that promote electronic processes relevant to organic solar cell (OSC) function that can be significantly different from those of conjugated polymeric materials. Here we investigate constituent loading-dependent effects on OSC morphology and function using the classical fullerene acceptor, PC 61 BM, in a heterojunction blend with the small molecule donor, NDT (thiophene-capped diketopyrrolopyrrole naphthodithiophene). The evolution of active layer morphology as well as exciton speciation and dynamics as a function of the PC 61 BM content are examined in combined structural studies using GIWAXS and spectroscopic studies using transient absorption spectroscopy. We observe evidence for three types of coexisting excitons and details of the interplay between them determines the yield of charge separated states that afford sustained device efficiency.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Decoding Gas Evolution Pathways and Interfacial Chemistry in Layered Oxide Cathodes for Safer Sodium‐Ion Batteries

Sodium-ion batteries (SIBs) are attractive for the low cost and abundance of sodium. Yet, gas evolution—a critical challenge in SIBs—remains underexplored. Here, online electrochemical mass spectrometry is used to probe gas evolution in layered oxide cathodes with various compositions, cutoff voltages, dopants, and particle morphologies. Compared to LiNiO 2 (LNO), NaNiO 2 releases more gas, even at lower states of charge, due to the higher covalency of Ni─O bond caused by the more ionic Na─O bond through the inductive effect. Among Co, Mn, Al, and Mg, Mn and Mg doping suppress gas release most effectively by enhancing the metal-oxygen bond strength. NaNi 1/3 Fe 1/3 Mn 1/3 O 2 (NFM) cathodes synthesized via coprecipitation (CP-NFM) and solid-state routes exhibit distinct particle morphologies; CP-NFM exhibits more gas evolution, yet secondary particle morphology helps reduce it through differential cathode-electrolyte reactivity between inner and outer primary particles. Among Li, Ti, Mg, and Cu doping in NFM, Li has the largest effect, reducing gas levels comparable to LNO. Nuclear magnetic resonance and X-ray photoelectron spectroscopies reveal that electrolyte solvent decomposition mainly produces organic-rich cathode-electrolyte interphase (CEI) rather than soluble species. NaPF 6 salt further exacerbates cathode-electrolyte reactions, forming surface Na 2 O species. The findings provide actionable guidance for designing safer, durable SIBs.

25 ENERGY STORAGE↗

DOE OSTI2025

X-Ray Microtomography Measurements of Coevolving Particle Size and Shape

This study measures simultaneous changes in particle size and shape during grain crushing and proposes quantitative metrics to track their coevolving statistical distribution. Idealized granular materials with widely different initial particle shapes (i.e., spheres, quasi-ellipsoids, plates, and rods) are compressed oedometrically at vertical stress levels sufficient to induce particle breakage. X-ray microtomography and digital image analysis are then used to track changes in particle-scale characteristics. The observations indicate that more irregular particles tend to exhibit a higher degree of breakage compared to more spherical grains subjected to an equivalent stress level. Despite these differences, the measurements also indicate that all the tested particle sets approach a common attractor (expressed in terms of aspect ratio, flatness, and elongation), regardless of their initial morphology. A new shape evolution index is proposed to quantify such trends. With this new metric, it is shown that in all the tested materials, the particle shape evolves faster than size, especially for the more regular morphologies, thus implying that the shape tends to reach its attractor point before the grading reaches its ultimate particle size distribution. Furthermore, this finding underpins an ultimate stage of crushing-driven compression that occurs with particle size reduction but minimal shape changes (i.e., self-replicating shapes due to fractures).

Oedometric compression↗

DOE OSTI2025

An experimental and computational study of thin-layer Rayleigh–Taylor instability development during deceleration with and without an externally applied magnetic field

The importance of mitigating the Rayleigh–Taylor instability (RTI) in inertial confinement fusion (ICF) is critical to successfully achieve high gain fusion yield. Consequently, understanding the seed mechanisms of RTI and the potential evolution of RTI in ICF relevant conditions is crucial. Single feature perturbations consistently demonstrate non-linear RTI evolution, for which an experimental platform on OMEGA-EP is developed. Manufacturing defects introduced into the target design require exploration of unanticipated changes to RTI development and an identification of targets that will still render quantifiable physics results. Consequently, it is presented that the inherent 3D nature of experimental targets necessitates 3D modeling for accurate design work and predictive modeling of experimental targets, especially when high resolution imaging diagnostics, like Fresnel Zone Plates, are utilized. A study of the morphology of the RTI evolution due to changing initial conditions and the presence of an externally applied magnetic field are also explored. Experimental data show thin-layer RTI morphology comparable to resistive magneto hydrodynamic 3D results. A discussion on the impacts of an externally applied magnetic field makes the case for continued efforts to observe a magnetic field's impact on RTI morphology.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

NASA NTRS1973

The nature of circular maria based on gravity studies.

Current thinking on the evolution of major lunar morphological features, i.e., large lunar circular basins, and on the nature and origin of surface structures observed in the fill deposits is summarized. The great lunar circular basins must result from high-velocity impact of large bodies with the moon. A hydrostatic mechanism is outlined, and a working hypothesis is presented for the evolution of lunar circular basins subsequent to their origin by impact. In the main appeal is made to Doppler gravity data to support the hypothesis, although photographic and altimetric information is also used. It is considered that all large ringed circular basins follow a common evolutionary path of superisostatic volcanic flooding followed by partial and variable isostatic adjustment. The difference between basins is the amount of flooding, which in turn may be related to the center of figure-center of mass offset of the moon.

Phillips, R. J.↗

DOE OSTI2021

The Dynamic of Complex Two-Phase Mixtures During Coarsening: From Dendritic to Bicontinuous Mixtures

Dendrites are tree-like crystals that frequently form during the solidification of castings. In systems with nearly isotropic interfacial energy, these dendrites possess secondary and sometimes even tertiary arms, and lead to morphologically complex two-phase mixtures. Dealloying, in which one component is selectively leached, leads to nanoporous structures that have proven useful for many technological applications. These bicontinuous two-phase mixtures are topologically and morphologically complex with spatially varying mean and Gaussian curvatures. The evolution of these structures during coarsening is of considerable technological importance since the morphology of the dendrites and nanoporous structure sets the properties of the resulting material. During coarsening, the total surface area per volume of the mixture decreases, thus resulting in an increase in the size-scale of the two-phase mixture. The evolution of interfacial morphology of these interconnected two-phase mixtures is being studied using large-scale computer simulations. The simulations are used to develop a theory of coarsening in these systems that will elucidate the impact of the complicated morphology found in dendritic and nanoporous systems on the coarsening process. The experiments employ four-dimensional X-ray microtomography, which enables the morphology of the two-phase mixture to be followed in three dimensions and time (an additional dimension). The experiments also serve as a test of simulations and theory of the coarsening process, as well as to provide initial conditions for the simulations. Through these experiments and theory, we aim to develop a comprehensive description of coarsening in these complex and technologically important two-phase mixtures.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Baseplate Temperature–Dependent Vertical Composition Gradient in Pseudo–Bilayer Films for Printing Non–Fullerene Organic Solar Cells

Numerous previous reports on the sequential deposition (SD) technique have demonstrated that this approach can achieve a p–i–n active layer architecture with an ideal vertical composition gradient, which is one of the critical factors that can influence the physical processes that determine the photovoltaic performance of organic solar cells. Herein, a commonly used photovoltaic system comprised of PM6 as a donor and Y6 as an acceptor is investigated with respect to sequential blade–processing deposition to comprehensively explore the morphology characteristics as a function of baseplate temperature. A systematic study of the temperature–dependent blend morphology elucidates the SD–processed configuration merits and device physics behind temperature–controlled degree of vertical composition gradient, and constructs the temperature–microstructure–property relationship for the corresponding photovoltaic parameters. The result shows, as the temperature increases, the morphology of the active layer has undergone a distinct evolution from the pseudo–bulk heterojunction to a pseudo–planar heterojunction and then to a pseudo–planar bilayer, leading to a non–monotonic correlation between baseplate temperature and device performance. Further, this investigation not only reveals the importance of precisely controlling baseplate temperature for gaining vertical morphology control, but also provides a path toward rational optimization of device performance in the lab–to–fab transition.

14 SOLAR ENERGY↗

DOE OSTI2023

Analyzing the cosmic web environment in the vicinity of grand-design and flocculent spirals with local geometric index

We explore the environment of a combined set of 367 grand-design and 619 flocculent spiral galaxies. We introduce a novel estimator called the local geometric index to quantify the morphology of the local environment of these 986 spirals. The local geometric index allows us to classify the environment of galaxies into voids, sheets, filaments, and clusters. We find that grand-designs are mostly located in dense environments like clusters and filaments (∼ 78%), whereas the fraction of the flocculents lying in sparse environments like voids and sheets is significantly higher (> 10%) than that of the grand-designs. A p-value < 10 -3 from a Kolmogorov-Smirnov test indicates that our results are statistically significant at 99.9% confidence level. Further, we note that dense environments with large tidal flows are dominated by the grand-designs. On the other hand, low-density environments such as sheets and voids favor the growth of flocculents.

79 ASTRONOMY AND ASTROPHYSICS↗

DOE OSTI2022

Unveiling the Emergent Traits of Chiral Spin Textures in Magnetic Multilayers

Abstract Magnetic skyrmions are topologically wound nanoscale textures of spins whose ambient stability and electrical manipulation in multilayer films have led to an explosion of research activities. While past efforts focused predominantly on isolated skyrmions, recently ensembles of chiral spin textures, consisting of skyrmions and magnetic stripes, are shown to possess rich interactions with potential for device applications. However, several fundamental aspects of chiral spin texture phenomenology remain to be elucidated, including their domain wall (DW) structure, thermodynamic stability, and morphological transitions. Here the evolution of these textural characteristics are unveiled on a tunable multilayer platform—wherein chiral interactions governing spin texture energetics can be widely varied—using a combination of full‐field electron and soft X‐ray microscopies with numerical simulations. With increasing chiral interactions, the emergence of Néel helicity, followed by a marked reduction in domain compressibility, and finally a transformation in the skyrmion formation mechanism are demonstrated. Together with an analytical model, these experiments establish a comprehensive microscopic framework for investigating and tailoring chiral spin texture character in multilayer films.

36 MATERIALS SCIENCE↗

DOE OSTI2024

A Gaussian process autoregressive model capturing microstructure evolution paths in a Ni–Mo–Nb alloy

Additive manufacturing is increasingly being employed to produce components of complex geometries in structural alloys because of the expected energy savings associated with the near-net-shape capability and the ability to build in novel internal features that are not possible with many conventional manufacturing approaches. However, because of the extreme thermal conditions encountered, the non-equilibrium microstructures produced during powder bed-based additive manufacturing processes must be subjected to custom post-heat treatment processes to recover the target mechanical properties. Phase-field models and simulation techniques have matured to a state where the microstructure evolution paths, and the morphologies of the resulting precipitate phases can be predicted reasonably accurately, considering alloy-specific thermodynamic and kinetic aspects of the nucleation and growth processes. However, phase-field simulations are computationally intensive, which precludes the ability to apply the simulations directly to the length scale of the entire component. Therefore, it is highly desirable to develop low-computational-cost surrogate models that effectively capture the physics at the microstructural length scale, while facilitating the design of optimized processing conditions resulting in location-specific targeted microstructures at the component scale. The work presented here demonstrates the application of the materials knowledge system framework to develop a surrogate model that effectively captures the microstructural path during annealing of a Ni–Mo–Nb alloy containing different Mo and Nb compositions known to segregate during solidification under additive manufacturing conditions. Specifically, the surrogate model built in this work is based on a Gaussian process autoregressive model informed by statistical representation of simulated microstructures using two-point correlations and dimensionality reduction through principal component analysis. In conclusion, this surrogate model is shown to capture the bifurcation of the microstructural path during precipitation, which yields a microstructure dominated by the $\gamma^{\prime\prime}$ phase at high Nb concentrations and the $\delta$ phase at low Nb concentrations.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Inkless, dry printing nanographene via in-Situ Coordinated laser ablation and sintering processes

Printing carbon, such as graphene and other carbon structures, for flexible and printed electronics currently relies on either ink-based printing, laser-induced forward transfer (LIFT), or laser-induced graphitization (LIG) to convert carbon-rich precursor materials, such as polymers, to graphene-like carbon structures. Liquid inks contain toxic solvents, surfactants, and stabilizing additives that degrade electrical conductivity and require high-temperature post-processing. On the other hand, LIG is limited by the substrate. Here, this study introduces an additive manufacturing method for dry-printing carbon nanomaterials, ranging from amorphous carbon to crystalline graphene-like structures, on various substrates. The system utilizes laser ablation of a solid graphite target to create pure carbon nanoparticles in situ and on demand. An inert gas carries the nanoparticles onto the substrate, where they can be deposited either as amorphous structures or laser-sintered in real time to form various graphitic structures. The study of laser processing parameters, specifically fluence and pulse repetition frequency, revealed three unique regimes of nanostructure evolution that influence the morphological and electrical properties of these printed structures. Raman spectroscopy confirmed graphitization with a resistivity slightly higher than that of the bulk graphite target. The conductivity/resistivity could be tuned as a function of sintering laser power. Scanning transmission electron microscopy (STEM) revealed that turbostratic nanographene formed with an interlayer spacing of 0.40 nm. Despite ink-based printing methods, such as screen printing, inkjet printing (IJP), and aerosol jet printing (AJP), this eco-friendly and green manufacturing technique could eliminate toxic chemicals, reduce environmental impact, and enable single-step fabrication of carbon-based devices for applications in wearable sensors, energy storage, flexible electronics, and Internet of Things (IoT) devices.

Additive nanomanufacturing↗

DOE OSTI2020

Degradation mechanism of lead-vanado-iodoapatite in NaCl solution

Degradation mechanism of lead-vanado-iodoapatite (IAPT) in NaCl solution at 90 °C was investigated through systematic characterization of surface morphology, microstructure and microchemistry evolution of the alteration layer. Nano-scale characterization indicated that IAPT crystals degraded from grain boundaries toward inner grains, forming ultrafine Cl-bearing crystallites. A coupled interface dissolution-reprecipitation replacement mechanism and the ion exchange between Cl - and I - across the degradation zone may together play roles in determining the nano-scale degradation behavior of IAPT. This work highlights the degradation through multiple reactions and elemental transport across the liquid-solid and solid-solid interfaces at length scales from sub-millimeter to nanoscale.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2020

Illuminating White Dwarf Spectra through Laboratory Experiments at Cosmic Conditions

We establish the work on white dwarf stars in the larger context of the experiments of the Wootton Center for Astrophysical Plasma Properties (WCAPP); these experiments are conducted at the plasma conditions found in the cosmos, without the need for scaling. We briefly summarize the results of these experiments to-date and their astrophysical and physical import, before focusing on the white dwarf experiments. Over 97% of stars either are, or will become, white dwarf stars, giving them broad relevance. We describe the astrophysical and physical problems associated with white dwarf photospheres, the plasma where the observed light arises. Here, the astrophysical questions include the age of the universe, the age and history of star formation in our Galaxy's varied morphological components and the evolution of stars. The compact nature of these ubiquitous stars means that the atomic physics is not well constrained even in the outermost layers. Further, it suggests that many important processes, including crystallization in dense Coulomb plasma, occur and have a significant effect on the evolution and structure of these stars and thus all their many applications.

79 ASTRONOMY AND ASTROPHYSICS↗

DOE OSTI2026

Solid state 59 Co NMR study of a Np(VII) compound

Np(VII) compounds with [Co(NH 3 ) 6 ] 3+ cations were synthesized and structurally examined using powder X-ray diffraction. Multiple phases were observed, consisting of octahedral [Co(NH 3 ) 6 ] 3+ cations, discrete tetragonal bipyramidal [NpO 4 (OH) 2 ] 3− anions, and waters of hydration. Electric field gradient tensors at Co sites were measured by solid state 59 Co nuclear magnetic resonance (NMR) spectroscopy and compared with theoretical calculations. The relative contributions of the chemical shift and electric field tensors to the NMR lineshape were determined by recording spectra at field strengths of 7.04 and 11.74 Tesla. Further, the evolution of structure and morphology as a function of sample age and the effects on NMR spectral parameters has also been investigated. These results demonstrate the use of NMR at multiple fields to expand understanding of the stability and electronic structure of high valent neptunium compounds.

heptavalent neptunium↗

DOE OSTI2020

Structural stability of mechanically alloyed amorphous (FeCoNi) 70 Ti 10 B 20 under high-temperature and high-pressure

Nanostructured (FeCoNi) 70 Ti 10 B 20 (at%) alloy was synthesized by mechanical alloying from elemental powder mixture of Fe, Co, Ni, Ti and B using ball milling. The effect of ball milling time on the evolution of structure and morphology was investigated by X-ray diffraction, scanning and transmission electron microscopy and differential thermal analysis. It was observed that the formation of solid solution of (FeCoNi) 70 Ti 10 B 20 started from the very onset of the milling process. Crystallite size and lattice strains seemed to be leveled off after 20 h of milling with no further major changes. The milling process for longer periods introduced severe plastic deformations causing formation of amorphous phase of (FeCoNi) 70 Ti 10 B 20 . The amorphous alloy composition was confirmed by energy dispersive X-ray spectroscopy analysis that showed an excellent homogeneity of the alloying elements. The phase stability of the mechanically alloyed amorphous sample was further verified by employing high-temperature and high-pressure studies. The alloy samples heat-treated at 700 °C revealed crystallization of the amorphous phase. However, synchrotron-based high-pressure ambient temperature X-ray diffraction studies confirmed that the amorphous phase of the alloy remained stable up to the pressure of 30 GPa. Here, the 50 h milled sample after being annealed at 350 °C showed improvement in the soft magnetic properties of the alloy, which was due to the probable elimination of the residual stress in the amorphous phase of the alloy powders.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Transformation of a ceramic precursor to a biomedical (metallic) alloy: Part I – sinterability of Ta 2 O 5 and TiO 2 mixed oxides

Mixed Ta 2 O 5 – TiO 2 binary system was studied by a combination of differential thermal analysis (DTA), scanning electron microscopy-energy dispersive spectrometry (SEM-EDS), X-ray diffraction (XRD) and in situ high temperature X-ray diffraction (HT-XRD) techniques. Different compositions of the mixed oxide powders were fabricated by ball–milling the powdered compositions, pelletizing the homogenized composite powders, and heating the green pellets in air at different temperatures for fixed time intervals. The sintered pellets were evaluated and characterized with respect to porosity, morphology, and phase distribution. DTA runs of the un-sintered powders indicated the onset temperatures for both exothermic and endothermic changes in the binary system. Significant amount of sintering was observed to take place at temperatures higher than 900 °C. Both room and high temperature X-ray diffraction patterns exhibited consistency in phase formation. A ternary compound (TaTiO 4 ) and a ternary solid solution (Ti 0.33 Ta 0.67 O 2 ) were observed to form in both room and high temperatures in addition to the respective binary phases (Ta 2 O 5 and TiO 2 ). A sintering temperature in the range 900–1000 °C was observed to be adequate to achieve the requisite mechanical strength and optimum internal porosity (40–48%) for subsequent electrochemical polarization experiments.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Tunable Growth of Layered Double Hydroxide Nanosheets through Hydrothermal Conversion of Atomic Layer Deposition Seed Layers

To enable the design and manufacturing of hierarchical nanomaterial architectures, there is a need for synthesis and processing methods that can enable tunable geometric control at the nanoscale while maintaining conformality on complex 3-D templates. Here, in this study, we explore the programmable control of vertically oriented Zn-Al layered double hydroxide (LDH) nanosheet arrays using atomic layer deposition (ALD) to deposit a seed layer of Al 2 O 3 , which is subsequently consumed and converted into the LDH phase under hydrothermal growth conditions. We demonstrate tunable control over the spacing and length of the nanosheets by varying the thickness of the initial ALD seed layer with subnanometer precision. This can be viewed as a nanoscale titration reaction, where Al acts as the limiting reagent during the hydrothermal synthesis of the nanosheets. Elemental mapping demonstrates the dynamic evolution of the resulting morphology, which is driven by surface diffusion and nucleation processes. The conformal nature of ALD allows for hierarchical growth of nanosheets on the surface of a variety of nonplanar substrate geometries, including microposts, paper fibers, and porous ceramic supports. This illustrates the power of ALD to enable bottom-up growth of 3-D nanoarchitectures with tunable geometries by controlling nucleation and growth in subsequent solution reactions.

36 MATERIALS SCIENCE↗