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At least 433 records · Page 24
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Supramolecular design principles in pseudohalides for high-performance perovskite solar mini modules

In this work, we reveal the role of non-covalent interactions, which are known to play important roles in supramolecular phenomena, in achieving efficient perovskite surface and grain boundary passivation. By using a series of pseudohalides, we find that trifluoroacetate (TFA - ) provides the strongest binding to iodide vacancies by means of non-covalent hydrogen bonding and dispersion interactions. By exploiting additional non-covalent dispersion and hydrophobic interactions in aromatic 3,3-diphenylpropylammonium (DPA + ), we present a dual-ion passivation strategy that not only minimizes the non-radiative recombination center and local chemical inhomogeneities but also induces preferentially oriented growth of α-FAPbI 3 lattice. Further, this leads to an outstanding power conversion efficiency (PCE) of 25.63% with an exceptional open-circuit voltage of 1.191 V in a perovskite solar cell with a small area, while perovskite solar mini modules with aperture areas of 25 and 64cm 2 achieved PCE of 22.47% (quasi-steady-state [QSS]-certified 20.50%) and 20.88%, respectively, with outstanding stability under high-humidity conditions.

14 SOLAR ENERGY↗
DOE OSTI2021

Comparison of Biotite Elastic Properties Recovered by Spherical Nanoindentations and Atomistic Simulations — Influence of Nano-Scale Defects in Phyllosilicates

Phyllosilicate minerals, due to their sheets structure and morphology, are known to cause anisotropy in bulk rock properties and make the bulk rock more compliant. Accurately characterizing the micromechanical behavior of phyllosilicate minerals from laboratory observations, which eventually translates to the bulk rock behavior, is still challenging due to their fine-grained nature. Recent advances in atomistic simulations open the possibility of theoretically investigating such mineral mechanical behavior. We compare the elastic properties of biotites recovered by spherical nanoindentation with those predicted from density functional theory (DFT) simulations to investigate to what extent theoretical predictions reproduce actual phyllosilicate properties. Spherical nanoindentation was conducted using schist rocks from Poorman Formation, South Dakota, USA, to recover continuous indentation stress-strain curves. Loading in the layer-normal orientation shows an average indentation modulus (M) of about 35 GPa, while loading in the layer-parallel orientation gives a higher average of about 95 GPa. To facilitate comparison, the elastic stiffness constants (cij) determined from DFT were converted to indentation modulus (M) using solutions proposed in this study. The majority of the nanoindentation modulus results are below the values inferred from the simulation results representing ideal defect-free minerals. We suggest that crystal defects present at the nano-scale, potentially ripplocations, are the dominant cause of the lower indentation modulus recovered from nanoindentation compared to those inferred from DFT simulations. Results highlight the importance of acknowledging the defects that exist down to the nano-scale as it modifies the mechanical properties of phyllosilicates compared to its pure defect-free form.

58 GEOSCIENCES↗
DOE OSTI2026

Why Seeding Works When Nucleation Barriers Vanish

Crystallization is a process governed by the interplay between nucleation and growth. While crystalline seeds are known to reduce nucleation barriers and accelerate crystallization under nucleation-limited conditions, their influence when nucleation is not the limiting step remains poorly understood. This creates a mechanistic puzzle in systems where nucleation barriers are already negligible, yet seeding still accelerates crystallization. Here, the synthesis of zeolites is a quintessential example of growth-limited crystallization in which seeds accelerate the process despite negligible homogeneous nucleation barriers. Using coarse-grained molecular dynamics simulations─validated across two zeolites and the unrelated case of ice crystallization─we establish that growth-limited crystallization produces many small, misoriented crystallites whose slow coarsening into larger domains controls the emergence of X-ray-detectable crystallinity. Local crystalline order, structural coherence, and X-ray detectability are therefore kinetically decoupled milestones: the first can be reached rapidly while the latter two lag significantly. Seeds resolve this lag by imposing a common orientational registry on nascent crystallites, enabling their coherent coalescence into large seed-bound domains. This early coherence-building step produces a crystallite-size asymmetry that accelerates subsequent coarsening, advancing the onset of X-ray-detectable crystallinity without necessarily increasing the nucleated fraction. We conclude that under growth-limited conditions, the apparent induction period observed in powder X-ray diffraction reflects the time required to build long-range coherence, not the time to form crystalline material. Accordingly, seeds function not primarily by reducing nucleation barriers but by enforcing spatial coherence, thereby shortening the time required to develop long-range order detectable by X-ray diffraction.

Growth-Limited Crystallization↗
DOE OSTI2022

Austenitic parent grain reconstruction in martensitic steel using deep learning

In this work we develop a deep convolutional architecture to estimate the prior austenite structure from observed martensite electron backscatter diffraction micrographs. A novel data augmentation strategy randomizes the global reference coordinate system which makes it possible to train our model from only four micrographs. The model is much faster than algorithmic approaches and generalizes well when applied to micrographs of a different material. Empirical evidence suggests the efficacy of the model depends on the scale of the microstructure and receptive field of the vision model. Furthermore, this work demonstrates that modern computer vision approaches are well suited for capturing complex spatial-orientation patterns present in orientation imaging micrographs.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Quantitative characterization of gradient microstructures: A study on friction stir spot processing of pure cobalt

Heterogeneous microstructures in polycrystalline metals can enhance the strength and ductility, outperforming homogeneous structures of similar composition. This study investigates deformed cobalt via friction stir spot processing with varying dwell times to uncover the effects of plastic deformation and heat generation on the formation of morphological, phase, and grain boundary character gradients. A new approach to quantify the morphological gradients in materials, which describes grain morphology in terms of density followed by parametric regression, enables direct quantification of processing depth and gradient sharpness. Results show that longer processing times increase the steepness of morphological gradients and reduce the deformation depth for friction stir spot processing with low plunge depths and high tool rotational speeds. The amount of retained FCC is increased in the shorter processing conditions, primarily due to refined grain size, increased defect content, and reduced heat generation. Crystallographic texture analysis of the HCP phase indicated a dominant B-fiber described by (0001) ∥ shear plane normal in the extreme processing conditions and the formation of a P-fiber, shear direction ∥ ⟨11$\bar2$0⟩ for intermediate dwell times. The texture of the FCC phase for low processing times was a C texture {100}⟨011⟩ where longer processing times were dominated by a [001] fiber texture with a main {110}⟨100⟩ orientation and emergence of a slight [111] fiber in the longest processing condition. The approaches outlined in this work give insight into quantifying gradients and improve the understanding of highly deformed cobalt.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Flux Synthesis of A-site Disordered Perovskite La 0.5 M 0.5 TiO 3 (M$=$Li, Na, K) Nanorods Tailored for Solid Composite Electrolytes

Inorganic fillers play an important role in improving the ionic conductivity of solid composite electrolytes (SCEs) for Li-ion batteries. Among inorganic fillers, perovskite-type lithium lanthanum titanate (LLTO) stands out for its high bulk Li + conductivity on the order of 10 -3 S cm -1 at room temperature. According to a literature survey, the optimal LLTO filler should possess the following characteristics: i) a single-crystal structure to minimize grain boundaries; ii) a small particle size to increase the filler/polymer interface area; iii) a 1D morphology for efficient interface channels; and iv) cubic symmetry to facilitate rapid bulk Li + diffusion within the filler. However, the synthesis of single crystal, 1D LLTO nanomaterials with cubic symmetry is challenging. Herein, a flux strategy is developed to synthesize La 0.5 M 0.5 TiO 3 (LMTO, M$=$Li, Na, and K) single-crystal nanorods with an A-site-disordered, cubic perovskite phase. The flux media promotes the oriented growth of nanorods, prevents nanorods from sintering, and provides multiple alkali metal ion doping at M sites to stabilize the cubic phase. SCEs compositing the Li + -conducting LMTO nanorods as fillers and poly[vinylene carbonate- co -lithium sulfonyl(trifluoromethane sulfonyl)imide methacrylate] matrix exhibit more than twice the conductivity of the neat polymer electrolyte (30.6 vs 14.0 µS cm -1 at 303 K).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Global and local texture development during initial plastic deformation of cold-pilgered Zircaloy-4 tubing

In this work we present a thorough characterization of the texture development during the initial step of a cold pilgering process of a Zircaloy-4 TREX tube, on which the axial cross section is reduced by 80% over a 40cm length with an overall Q-ratio of 2.34, followed by a recrystallization thermal treatment. Texture across a tapered specimen representing this working zone was characterized by neutron diffraction and high energy synchrotron x-ray diffraction at 28 positions (4 locations along its length and 7 locations across its thickness with 0.3 mm spatial resolution), and on the deformed end after the thermal treatment. Results show that the starting material (TREX tube) presents a texture gradient through its wall thickness, with the c poles aligned to the hoop direction at the outer surface (with radial and hoop Kearns factors: f R =0.36, f H = 0.50), and gradually rotating around the axial direction to become a quasi-radial orientation (~35 o out of the radial direction) at the inner surface ( f R =0.43, f H =0.35). The overall texture becomes more radial due to the cold pilgering, but the texture gradient remains during the whole deformation process, being always more radial at the inner surface, ( f R =0.53, f H =0.37 at 80%) than at the outer surface ( f R =0.41, f H =0.50at 80%). The most remarkable changes in texture produced by the rolling process is a 30 o rotation of the grains around their c-axis, producing a marked increase of the <11 2 ¯ 0> // axial fiber texture at expenses of the original <10 1 ¯ 0> // axial fiber texture observed in the TREX tube. The observed changes in texture during deformation were correctly explained by visco-plastic self-consistent (VPSC) modelling. This was achieved after the inclusion of the basal <a> slip system, which plays a central role to explain the 30 o rotation around the c-axis during deformation. The texture evolution was correctly described after the inclusion of a drag effect to grain rotation due to the interaction with neighbouring grains. The through thickness texture differences are greatly reduced by the recrystallization thermal treatment, with similar Kearns factors at the inner surface ( f R =0.50, f H =0.28) and the outer surface ( f R =0.48, f H =0.39). The predominance of the <10 1 ¯ 0> // axial fiber texture is recovered after recrystallization.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Microstructure and strengthening of Al-6Ce-3Ni-0.7Fe (wt%) alloy manufactured by laser powder-bed fusion

In this study, an Al-6Ce-3Ni-0.7Fe (wt%) alloy was fabricated via laser powder-bed fusion and its microstructure, thermal stability, tensile properties, and creep properties are investigated for two rapid-solidification rates with different eutectic spacings. For both faster- and slower-cooled states, the as-fabricated alloy mostly shows elongated grains with very fine eutectic networks (~40 nm lamellar width) comprising a high-volume fraction (~18 %) of intermetallic phases. Faster-cooled samples, however, display a less continuous eutectic network with finer spacing (~100 nm), leading to higher Orowan strengthening and therefore superior microhardness and yield stress up to ~350 °C. Upon aging (300 - 450 °C), micron-size Al 9 (Ni,Fe) 2 needle-like precipitates form within grains, and the Al 11 Ce 3 eutectic network spheroidizes, while retaining a submicron width and spacing, resulting in 33–37 % drop in microhardness after 144 h aging at 400 °C. Limited tensile ductility (~6 %) and creep ductility (~1-2 %) are measured for both faster- and slower-cooled alloys due to an inhomogeneous microstructure, where cavitation preferentially initiates at melt-pool boundaries, precipitate-free zones, and/or denuded zones, eventually leading to local fracture. Denuded zones, induced by stress, form due to diffusional flow with stress-dependent orientations, and are identified as microstructurally weak regions leading to strain localization. The present alloy does not show a significant difference in 300 °C creep resistance between: (i) tensile and compressive loading, (ii) faster- and slower-cooled samples, and (iii) continuous and spheroidized eutectics. Creep resistance at 300 °C is comparable to that of a Ce-richer Al-10.5Ce-3.1Ni-1.2Mn (wt%) alloy, despite the formation of denuded zones and needle-like Al 9 (Ni,Fe) 2 precipitates.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Using Multigrain Crystallography to Explore the Microstructural Evolution of the α-Olivine to γ-Ringwoodite Transformation and ε-Mg2SiO4 at High Pressure and Temperature

The introduction of multigrain crystallography (MGC) applied in a laser-heated diamond anvil cell (LH-DAC) using synchrotron X-rays has provided a new path to investigate the microstructural evolution of materials at extreme conditions, allowing for simultaneous investigations of phase identification, strain state determination, and orientation relations across phase transitions in a single experiment. Here, we applied this method to a sample of San Carlos olivine beginning at ambient conditions and through the α-olivine → γ-ringwoodite phase transition. At ambient temperatures, by measuring the evolution of individual Bragg reflections, olivine shows profuse angular streaking consistent with the onset of yielding at a measured stress of ~1.5 GPa, considerably lower than previously reported, which may have implications for mantle evolution. Furthermore, γ-ringwoodite phase was found to nucleate as micron to sub-micron grains imbedded with small amounts of a secondary phase at 15 GPa and 1000 °C. Using MGC, we were able to extract and refine individual crystallites of the secondary unknown phase where it was found to have a structure consistent with the ε-phase previously described in chondritic meteorites.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Strength, deformation, and equation of state of tungsten carbide to 66 GPa

Here, strength, texture, and equation of state of hexagonal tungsten monocarbide (WC) have been determined under quasi-hydrostatic and non-hydrostatic compression to 66 GPa using angle-dispersive X-ray diffraction in the diamond anvil cell. Quasi-hydrostatic compression in a Ne pressure medium demonstrates that nanocrystalline WC is slightly less incompressible than bulk-scale WC, with respective bulk moduli of K 0 = 377 ± 7 and 397 ± 7 GPa and pressure derivatives K 0 ’ = 3.8 ± 0.3 and 3.7 ±0.3. This decrease in incompressibility with grain size is similar to behavior observed in other ceramics. Under nonhydrostatic compression, WC supports a mean differential stress of ~12-15 GPa at plastic yielding, which occurs at ~30 GPa. Strength in WC is anisotropic, with the (001) plane supporting 29-42% higher stress than stresses calculated from mean strain. Simulations using an Elasto-ViscoPlastic Self-Consistent model indicate that strength inferred from lattice strain theory may be overestimated due to effects of plastic deformation. Plastic deformation generates a texture maximum near $\langle\bar{2}110\rangle$ in the compression orientation, initially through prismatic slip on the {$10\bar{1}0$}$\langle\bar{1}2\bar{1}0\rangle$ and {$10\bar{1}0$}$\langle0001\rangle$ slip systems, followed by activation of pyramidal slip on {$10\bar{1}1$}$\langle\bar{2}113\rangle$ at ~40-50 GPa.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Automated extraction of interfacial dislocations and disconnections from atomistic data

Here we introduce Interfacial Line Defect Analysis (ILDA), a method for identifying and extracting interfacial dislocations and disconnections with little-to-no input from the user on the nature of the interface. By simply providing the orientations and coherency strains for the crystals in a coherent reference state of the interface, ILDA provides exact Burgers vectors. Alternatively, these orientations and strains can be estimated using local atomic deformation gradients, making ILDA fully automated and providing estimated Burgers vectors. ILDA also determines the step height associated with each defect line segment, in case the associated defect is a disconnection. The heart of the method is the identification of atoms residing at co-incidence sites between the two crystals and the construction of a surface mesh connecting these sites that is used to compose Burgers circuits and insert defect line segments. We demonstrate the performance of ILDA in two test cases: a twist grain boundary and a phase boundary.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Toughening of interface networks through the introduction of weak links

The resistance of polycrystalline materials to intergranular fracture depends on the toughness of the interfaces between neighboring grains. Using finite element simulations on model, two-dimensional microstructures, we demonstrate that the steady-state crack growth resistance of a polycrystal that contains exclusively high toughness interfaces is suboptimal: its crack growth resistance may be increased by introducing a minority fraction of weak interfaces at random locations within the interface network. Furthermore, the weaker are these interfaces, the greater is their toughening effect. These weak interfaces toughen the material through crack deflection and branching, nucleation of secondary cracks, and inelastic dissipation within intact interfaces. Furthermore, our findings suggest that fracture resistance-oriented material development should not aim to eliminate all weak interfaces, but rather judiciously incorporate a low fraction of them.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Microstructure effects on fatigue crack growth in additively manufactured Ti–6Al–4V

In this article we investigate the relationship between the different microstructural features in additively-manufactured (AM) Direct Metal Laser Deposited Ti–6Al–4V alloys and the observed fatigue and fracture behaviors, using high resolution Digital Image Correlation experiments and microstructural imaging. Fatigue cracks in the AM specimens were observed to periodically propagate parallel to the α' laths and deflect at prior β grain boundaries. Corresponding plastic strain distributions show needle-like regions of high strain that correlated to the α' laths, suggesting significant influence of the microstructure on the plastic zone. In many cases, the fatigue cracks also propagated towards voids from unsintered powder or gas entrapment in the vicinity. In several experiments, premature failure of the AM specimens occurred under monotonic fracture or cyclic fatigue loading, which we attribute to the presence of void clusters located near the crack-tip. These fatigue and fracture characteristics were similar for AM specimens of different build-orientations.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Ultra-Fast Vertical Ordering of Lamellar Block Copolymer Films on Unmodified Substrates

To utilize the full potential of block copolymer (BCP) thin films for use in technological devices ranging from ion conduction membranes, transistors to nanowire array antennas, rapid self- assembly of lamellar block copolymers (l-BCPs) with vertically oriented lamellar domains on a variety of unmodified substrates is needed. l-BCPs have an inherently larger interfacial area for transport compared to their cylindrical counterpart. Our observations demonstrate that the as-cast weakly ordered vertically oriented state of l-BCP films of polystyrene-block-poly(methyl methacrylate) (PS-b-PMMA) from directional evaporation of select solvents, act as “seed templates” for their ultra-fast evolution (~30 s) into well-ordered vertically oriented nanostructures, using a thermal gradient-based Cold Zone Annealing (CZA) technique. Furthermore, vertical lamellae are obtained on unmodified substrates, Quartz and Kapton, and the kinetics of l-BCP ordering is much faster by CZA as compared to the isotropic oven annealing. The rapid ordering kinetics of vertical l-BCPs is tested and found applicable to different molecular weights and film thicknesses ranging from 20 nm to 480 nm, which ultimately flip over to their equilibrium parallel morphology at upper limits of annealing times. This rapid ordering strategy for vertical orientation of l-BCPs using roll-to-roll compatible CZA would be highly relevant for fundamental studies of interfacial transport as well as for industrial applications from membranes to nanowires.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Characterization of the Interfacial Orientation and Molecular Conformation in a Glass-Forming Organic Semiconductor

The ability to control structure in molecular glasses has enabled them to play a key role in modern technology; in particular, they are ubiquitous in organic light-emitting diodes. While the interplay between bulk structure and optoelectronic properties has been extensively investigated, few studies have examined molecular orientation near buried interfaces despite its critical role in emergent functionality. Direct, quantitative measurements of buried molecular orientation are inherently challenging, and many methods are insensitive to orientation in amorphous soft matter or lack the necessary spatial resolution. To overcome these challenges, we use polarized resonant soft X-ray reflectivity (pRSoXR) to measure nanometer-resolved, molecular orientation depth profiles of vapor-deposited thin films of an organic semiconductor Tris(4-carbazoyl-9-ylphenyl)amine (TCTA). Our depth profiling approach characterizes the vertical distribution of molecular orientation and reveals that molecules near the inorganic substrate and free surface have a different, nearly isotropic orientation compared to those of the anisotropic bulk. Comparison of pRSoXR results with near-edge X-ray absorption fine structure spectroscopy and optical spectroscopies reveals that TCTA molecules away from the interfaces are predominantly planar, which may contribute to their attractive charge transport qualities. Buried interfaces are further investigated in a TCTA bilayer (each layer deposited under separate conditions resulting in different orientations) in which we find a narrow interface between orientationally distinct layers extending across ≈1 nm. Coupling this result with molecular dynamics simulations provides additional insight into the formation of interfacial structure. This study characterizes the local molecular orientation at various types of buried interfaces in vapor-deposited glasses and provides a foundation for future studies to develop critical structure–function relationships.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Self-Organized Stress Distributions in Polycrystalline Materials [Dissertation]

Understanding stress distributions in solid materials is complicated by the fact that most materials are polycrystalline in nature, with each crystal having an elastically anisotropic reaction to force. This study is to gain a better understanding on how external forces placed on a polycrystal are related to internal reactions within and between the grains. The hypothesis is that the stress distribution in porous to fully dense materials are self-organized based on strong contacts between and within the individual grains created by force chains. Force chains, commonly known in loaded granular materials, and could be the phenomenon that connect micro to macro deformation. Scale bridging measurements conducted through Raman spectroscopy, Atomic Force Microscopy, and Digital Image Correlation will be used to create stress maps, modulus maps, and elastic strain maps across a variety of geological and pharmaceutical polycrystals. When possible, the resulting maps will be compared to current homogenization schemes and a full field models. Finite element modeling will be used to assess whether the patterning seen in the experimental map is a reasonable approximation based on the orientation data of the samples used. A minimum of three publications is projected to be accomplished focusing each on a different method to experimentally test and analyze stress distributions.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Response to the comments on creep-induced elemental redistribution at grain boundaries of 304L stainless steel – An experimental evidence for diffusional creep mechanisms

Sandström and He reanalyzed our 304L creep data (Acta Materialia 121137, 2025) at 10 MPa/750 °C and proposed that: (i) primary dislocation creep dominates based on the ϕ -model; (ii) measured creep rates deviate from published 304H data and Coble creep predictions using literature grain boundary (GB) diffusivity; and (iii) creep-induced elemental redistribution (CIER) could be explained by dislocation emission/absorption (DEAA) and GB creep (GBC), as opposed to diffusional creep. Here, in this response, we propose that: (i) the creep behavior at 15 MPa/750 °C—for which we demonstrated CIER—is only partially captured by the ϕ -model; (ii) direct comparison between 304L and 304H creep data is inappropriate due to carbides in 304H, and Coble creep predictions estimated from CALPHAD-based bulk diffusivity span experimental rates; and (iii) CIER exhibits distinct fingerprint for diffusional creep characterized by anisotropy and stress orientation dependence whereas neither DEAA nor GBC have been mechanistically substantiated.

36 - MATERIALS SCIENCE↗
DOE OSTI2024

Multiscale in-situ characterization of static recrystallization using dark-field X-ray microscopy and high-resolution X-ray diffraction

Abstract Dark-field X-ray microscopy (DFXM) is a high-resolution, X-ray-based diffraction microstructure imaging technique that uses an objective lens aligned with the diffracted beam to magnify a single Bragg reflection. DFXM can be used to spatially resolve local variations in elastic strain and orientation inside embedded crystals with high spatial (~ 60 nm) and angular (~ 0.001°) resolution. However, as with many high-resolution imaging techniques, there is a trade-off between resolution and field of view, and it is often desirable to enrich DFXM observations by combining it with a larger field-of-view technique. Here, we combine DFXM with high-resolution X-ray diffraction (HR-XRD) applied to an in-situ investigation of static recrystallization in an 80% hot-compressed Mg–3.2Zn–0.1Ca wt.% (ZX30) alloy. Using HR-XRD, we track the relative grain volume of > 8000 sub-surface grains during annealing in situ. Then, at several points during the annealing process, we “zoom in” to individual grains using DFXM. This combination of HR-XRD and DFXM enables multiscale characterization, used here to study why particular grains grow to consume a large volume fraction of the annealed microstructure. This technique pairing is particularly useful for small and/or highly deformed grains that are often difficult to resolve using more standard diffraction microstructure imaging techniques.

36 MATERIALS SCIENCE↗