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At least 649 records · Page 36

Hierarchical morphologies in co-sputter deposited thin films

Co-depositions of immiscible alloy films at specific processing conditions have yielded hierarchical microstructures which consist of distinct features at multiple length scales, often agglomerates and concentration modulations on the sub-micrometer-scale and fine nanoprecipitates in a matrix on the nanoscale. The present work examined a series of immiscible alloy systems: Cu-Mo, Cu-Ag, Cu-Fe, Cu-Ta, Mo-Ag, Cu-Mo-Ag, to determine the kinetic conditions favorable for hierarchical organization and the formation mechanism of such structures. Thin films of six immiscible systems were sputter co-deposited over a range of deposition rates from 0.12 to 2 nm/s and various temperatures from 400 to 800°C. The resulting microstructures indicate that hierarchical structures form with sufficient disparity in kinetic energy between the constituent atoms, one species being highly mobile (A) and the other relatively immobile (B). This condition arises typically at elevated deposition temperatures and reduced deposition rates but is also alloy dependent. The hierarchical structures form during deposition via phase separation and self-organization processes across the multiple length scales. The adatoms diffuse on the film surface with the highly mobile species swiftly agglomerating into A-rich domains within which B-rich nanoprecipitates form, often self-organizing into periodic arrays. The smallest B-rich nanoprecipitates in the A-rich domains are found to be coherent and in a metastable crystal structure (B taking the structure of A), but coarser precipitates that exhibit the equilibrium structure of B element. The A-rich domains are surrounded by a B-rich matrix that phase-separates into a concentration modulated structure. In conclusion, the observations are interpreted via a model incorporating material properties and process parameters.

36 MATERIALS SCIENCE↗

Microstructure‐Dependent Sodium Storage Mechanisms in Hard Carbon Anodes

Sustainable energy storage is essential to support the transition to renewables and meet the increasing demand for energy. Sodium‐ion batteries (NIBs) are attractive for grid‐scale energy storage due to the abundance and low cost of sodium, sustainability of other battery components, and electrochemical performance. Hard carbon (HC) is a leading anode material for NIBs, but its complex microstructure complicates the understanding of sodium storage mechanisms. Using X‐ray total scattering and density functional theory calculations, this study clarifies how HC's microstructural variations influence sodium storage across the slope (high potential) and plateau (low potential) regions of the potential capacity curve. In the slope region, sodium initially adsorbs at high‐binding energy defect sites and subsequently intercalates between graphene layers, adsorbing at low‐binding energy defect sites, correlating with different slopes observed during initial sodiation. Initial irreversibility arises from sodium trapping at surface defects and solid electrolyte interface formation. In the plateau region, sodium simultaneously intercalates and fills pores, influenced by pore size, interlayer spacing, and defect concentration. HCs with larger pore sizes form larger sodium clusters. In conclusion, the proposed mechanism underscores the role of microstructure engineering in enhancing HC performance and advancing NIBs for grid‐scale energy storage.

36 MATERIALS SCIENCE↗

Microstructural characterization of the oxidation of nuclear graphite under chronic and accident conditions via XCT and synchrotron XCT

Graphite is a candidate material to moderate fast neutrons and for structural components in the US next-generation graphite-moderated reactors. A graphite core is conceived as a large formation of interconnected bricks that primarily serves as the moderator of fast neutrons, holds instrumentation, fuel elements, control rods, and is a receptacle for molten salts for Molten Salt Reactors (MSRs) designs. During the operation of a graphite-moderated power plant, graphite components might be subjected to chronic oxidation during normal operating conditions or aggressive oxidation as a result of accidental ingress of air that reacts vigorously with the graphite core. Using synchrotron, x-ray computed tomography (XCT), this research systematically characterized microstructural changes that accompanied these two oxidation scenarios. Chronic oxidation was studied by characterizing IG-110, PCEA, and NBG-18 specimens that were gradually oxidized in air at a low temperature (520°C). The accidental ingress of air into the graphite reactor was simulated by subjecting the grades mentioned above to high-temperature oxidation at approximately 750°C. This research is the first, in situ, systematic characterization of nuclear graphite microstructural evolution that can be associated with the two possible oxidation scenarios and provide insight into related repercussions. The results show that the microstructure and pore connectivity influence the rate of oxidation and evolution of the microstructure under the two oxidation regimes. These results are crucial to understanding which grades are more resilient to each type of oxidation and documenting the damage created in the graphite.

Arregui Mena, Jose'↗

Effects of varying gelatin coating concentrations on RANKL induced osteoclastogenesis

Here, we assessed the effects of varying concentrations of gelatin coating on Receptor Activator of Nuclear Factor κ-B Ligand (RANKL)-induced RAW264.7 murine macrophage differentiation into osteoclast (OC) via osteoclastogenesis. The microstructures of coating surfaces with different concentrations of gelatin were examined by scanning electron microscopy and atomic force microscopy. Increased gelatin coating concentrations led to decreased gel rigidity but increased surface adhesion force attenuated OC differentiation and the decreased actin ring formation in RANKL-induced osteoclastogenesis. The decreased actin ring formation is associated with decreased lysosomal-associated membrane protein 1 (LAMP1) activity and bone resorption in the differentiated OCs with different gelatin coating concentrations as compared to the cells differentiated without gelatin coatings. In addition, increasing concentrations of gelatin coating attenuated the medium TGF-β1 protein levels and the expression levels of TGF-β and type-I (R1) and type-II (R2) TGF-β receptors in OCs, suggesting the gelatin-induced suppression of TGF-β signaling for the regulation of RNAKL-induced OC differentiation. Taken together, these findings showed that changes in gelatin coating concentrations, which were associated with altered gel thickness and substrate rigidity, might attenuate TGF-β signaling events to modulate OC differentiation and concomitant actin ring formation and bone matrix resorption in RANKL-induced osteoclastogenesis.

60 APPLIED LIFE SCIENCES↗

Interfacial Void Formation and Self-Healing in Oxide Scales on Al-containing High-Entropy Alloy

The exceptional high-temperature oxidation resistance of Al-containing high-entropy alloys (HEAs) is often attributed to the formation of a protective α-Al 2 O 3 scale. However, the dynamic, atomic-scale mechanisms governing the stability of this scale—including interfacial void formation and the often-postulated but rarely visualized “self-healing” capacity—remain poorly understood. Herein, we reveal the complex evolution of the triple-layer oxide scale on an Al 10 CoCrFeNi HEA through combined electron microscopy and diffraction study. We show that interfacial voids are an inherent consequence of the scaling process, originating from two distinct mechanisms: the Kirkendall effect at the interface between the γ-Al 2 O 3 /α-Al 2 O 3 and alloy driven by cationic diffusion imbalance and volumetric contraction due to phase transformations at the spinel/Cr 2 O 3 interface. Crucially, we provide microstructural evidence consistent with an intrinsic self-healing response. This process is driven by coupled inward diffusion of oxygen and outward diffusion of metal cations, leading to the in-situ formation of transient θ-Al 2 O 3 and spinel phases that partially fill and seal the voids. Here, these results provide atomic-scale insights into the phase evolution, defect formation, and self-repair of oxide scales in HEAs—highlighting pathways to enhance their oxidation resistance in extreme environments.

High-entropy alloy↗

First-principles calculations for understanding microstructures and mechanical properties of co-sputtered Al alloys

Recent experimental studies show that co-sputtering solutes with Al, together, can refine columnar grain size around few tens of nanometers and promote the formation and enhance the stability of planar defects such as stacking faults (SFs) and grain boundaries (GBs) in Al alloys. These crystal defects and fine columnar grains result in high strength, enhanced strain hardening and thermal stability of Al alloys. Using first-principles density-functional theory (DFT) calculations, we studied the role of eleven solutes in tailoring kinetics and energetics of adatoms and clusters on Al {111} surface, stable and unstable stacking fault energies, and kinetic energy barriers for the migration of defects. The calculations show that most solutes can effectively refine columnar grain size by decreasing the diffusivity of adatoms and surface clusters. These solutes do not necessarily decrease the stacking fault energy of Al alloys, but reduce the formation energy of faulted surface clusters and increase the energy barriers for the recovery of faulted surface clusters. Correspondingly, the formation of SFs is kinetically promoted during sputtering. Furthermore, solutes are segregated into the core of Shockley partial dislocations and play a pinning effect on SFs, SF arrays and twin boundaries, enhancing the thermal stability of these crystal defects. These findings provide insights into the design of high-strength Al alloys for high-temperature applications.

36 MATERIALS SCIENCE↗

In Situ and Operando Observation of Zinc Moss Growth and Dissolution in Alkaline Electrolyte for Zinc–Air Batteries

As a promising battery technology, zinc–air batteries still face significant challenges, including the formation of a mossy structure on the zinc metal anode in alkaline electrolyte. Because a similar phenomenon also plagues lithium and sodium metal batteries, elucidating its mechanism has important implications for progress in energy storage. Herein, operando X-ray nanotomography was employed to visualize zinc moss growth and dissolution at the individual colony level. By tracking its microstructure evolution, zinc moss was found to display irreversible plating/stripping behavior. While zinc moss exhibits self-limiting growth and zinc deposition occurs mainly in its outer region, zinc dissolution is more uniformly distributed inside the moss colony upon stripping, leading to the formation of “dead” zinc and capacity loss. A direct correlation is established between the moss amount and zinc plating/stripping efficiency. Finally, results from this study offer new insights into mitigating the unstable zinc plating morphology and improving the cycle life of aqueous zinc–air batteries.

36 MATERIALS SCIENCE↗

Microstructural evolution of diamond growth during HFCVD

High resolution transmission electron microscopy (HRTEM) was used to study the nucleation and growth mechanism of diamond by hot filament chemical vapor deposition (HFCVD) process. A novel technique has shown a direct evidence for the formation of the diamond-like carbon layer 8-14 nm thick in which small diamond micro-crystallites were embedded. These diamond micro-crystallites were formed as a result of transformation of diamond-like carbon into diamond. The diamond micro-crystallites present in the amorphous diamond-like carbon layer provided nucleation sites for diamond growth. Large diamond crystallites were observed to grow from these micro-crystallites. The mechanism of diamond growth will be presented based on experimental findings.

TRT-EXPERIMENTAL↗

Visualizing diverse lithium growth and stripping behaviors in anode-free solid-state batteries with operando X-ray tomography

Anode-free solid-state batteries (SSBs), which eliminate the need for lithium metal use during cell assembly, have the potential to enable high energy densities and simplified manufacturing. However, the factors that control lithium growth/stripping at the anode current collector are not well understood. Here, we use operando X-ray microcomputed tomography to comprehensively image and quantify lithium deposition and stripping under various conditions in three different Li|Li 6 PS 5 Cl|current collector cells, revealing diverse behavior that depends on interface morphology, cell resistance, and solid-state electrolyte (SSE) microstructure. A cell with high resistance exhibits extensive lithium filament growth across the entire current collector interface, with filaments that grow around pre-existing pores in the SSE rather than lithium filling these pores. Lithium filament formation is partially reversible, with the cracks shrinking as lithium metal is stripped. Uniform lithium deposition is achievable at low current densities in low-resistance cells, whereas higher current densities in these cells cause an increase in interfacial roughness, which is correlated with subsequent filamentary growth at the edges of the cell. These results provide insight into filamentary vs. planar lithium growth and highlight that the evolution of lithium is sensitively dependent on SSE microstructure and electrochemical processes.

25 ENERGY STORAGE↗

The subsurface structure of abraded Al–Zn–Mg–Cu alloy

Surface abrasion has been shown to introduce heavy shear stress and produce a few hundred nanometers thick altered surface layer (ASL) on Al alloys. Such ASLs exhibit microstructural changes at room temperature and different corrosion resistance than the underlying substrate. Here, we report how sample dimensions and temperature affect the deformed subsurface microstructure evolution on an abraded Al–Zn–Mg–Cu alloy using transmission electron microscopy (TEM) and atom probe tomography. The ASL microstructure evolves differently in the bulk sample than in the thin TEM specimen. In the freshly abraded ASL, the original η'/η precipitates and grain boundaries were deformed toward the abrasion direction. After 7-day natural aging of the freshly abraded bulk sample, well-defined subgrains formed locally in the ASL, and unusual Al 2 Cu (θ) and Mg x Zn y phases precipitated at the subgrain boundaries. However, during natural aging of this TEM specimen taken from the abraded and aged bulk samples, much faster changes occurred, including the continued formation of subgrains and θ particles in the entire ASL, and the diffusion of Zn atoms out of Mg x Zn y particles to form a Zn particle. On the other hand, no obvious microstructural changes occurred in the ASL during 3-month natural aging of the TEM specimen immediately taken from the freshly abraded sample. Finally, this work advances the understanding of how Al alloy microstructures respond during and following any shear deformation, and complex and unexpected effects of sample dimensions on the behavior.

36 MATERIALS SCIENCE↗

Creep properties of advanced austenitic steel 709 determined through short experiments under in-situ neutron diffraction followed by TEM characterization

Here in this study, the creep mechanisms at play in Alloy 709 (Fe-20Cr-25Ni) are investigated by performing short-term creep-type tests under in-situ neutron diffraction experiments. Short tests are performed in the temperature range of 500 to 900 °C under constant load with a load ranging from 50 to 150 MPa. The creep exponent and activation energy are determined using the Bird-Mukherjee-Dorn relation and compared to that obtained from conventional longer creep tests from the literature. Scanning transmission electron microscopy (S/TEM) of the post-creep microstructure indicates that interaction of dislocations with precipitates are a dominant mechanism at play. Furthermore, local elemental mapping indicated chemical segregation at grain boundaries and formation of complex precipitates.

36 MATERIALS SCIENCE↗

Microstructure and texture evolution of friction stir lap welded dissimilar multi-aluminum stack

Here this work investigates the microstructural evolution of a dissimilar multiple-aluminum alloy stack (AA7055, AA7055, AA6022) produced by friction stir lap welding (FSLW). A through-thickness analyses of grain orientation map, grain size and distribution, strain distribution, and texture evolution by electron backscattered diffraction-based characterization technique were performed. Two different welding parameters (combination of tool rotation and traverse speed) were used to study the effects of the welding parameters on these microstructural characteristics. The study shows that higher welding speed and higher rotation speed of the FSLW tool yield finer grains. FSLW resulted in shear texture formation in the weld regions due to high welding speeds. This texture development in the nugget zone is consistent with shear deformation, and (111) pole figures show ideal shear texture components. The Stir Zone (SZ) exhibits shear texture (A/A ̅ and B/B ̅ components), consistent with other shear-assisted processes. Recrystallization mechanisms observed are CDRX in SZ and DDRX in TMAZ (Thermo-Mechanically Affected Zone). Interface analysis reveals the presence of oxide layers between different aluminum sheets, affecting joint mechanical performance. The mechanical property of the lap welded joints was presented in terms of microhardness distribution across the weld cross section. Slightly higher hardness in higher speed welding setup was observed throughout the SZ and AA6022 layer, indicating greater grain refinement and uniform grain structure distribution.

36 MATERIALS SCIENCE↗

Diversification in the Archean Biosphere: Insight from NanoSIMS of Microstructures in the Farrel Quartzite of Australia

The nature of early life on Earth is difficult to assess because potential Early Archean biosignatures are commonly poorly preserved. Interpretations of such materials have been contested, and abiotic or epigenetic derivations have been proposed (summarized in [1]). Yet, an understanding of Archean life is of astrobiological importance, as knowledge of early evolutionary processes on Earth could provide insight to development of life on other planets. A recently-discovered assemblage of organic microstructures in approx.3 Ga charts of the Farrel Quartzite (FQ) of Australia [2-4] includes unusual spindle-like forms and a variety of spheroids. If biogenicity and syngeneity of these forms could be substantiated, the FQ assemblage would provide a new view of Archean life. Our work uses NanoSIMS to further assess the biogenicity and syngeneity of FQ microstructures. In prior NanoSIMS studies [5-6], we gained an understanding of nano-scale elemental distributions in undisputed microfossils from the Neoproterozoic Bitter Springs Formation of Australia. Those results provide a new tool with which to evaluate poorly preserved materials that we might find in Archean sediments and possibly in extraterrestrial materials. We have applied this tool to the FQ forms.

Oehler, D. Z.↗

Development of Large Bandgap Materials Using Reactive Growth in Al-SI Eutectic for Optical and RF Applications

Carbon was utilized as reactive element to modify the microstructure using forced mixing during crystallization of the Al-Si alloy by rotation and stirring. We nucleated the material on SiC substrates while the Al-Si melt was rotated with a speed of 30rpm in a graphite crucible. Several experiments were performed and parameters such as time of mixing, soaking temperature, rotation rate of the substrate and rate of cooling during the solidification was changed. We observed dendrite and cell morphologies during the solidification of rotating melt. The microstructure was characterized by optical microscopy and SEM-EDX and compositional spectroscopy. The effect of carbon impurities was studied on the solidifying microstructure. When we used the longer soak time of the melt in presence of carbon impurities we observed the destruction of dendritic morphology and the formation of cellular and colony structures. Similar approach has been used for Ga2O3, a novel large bandgap material also.

Singh, N. B.↗

Chapter 21. Atomic-Level Dislocation Dynamics in Irradiated Metals

Primary damage and microstructure evolution in structural nuclear materials operating under conditions of a high flux of energetic atomic particles and high temperature and stress lead to the formation of a high concentration, non-homogeneous distribution of defect clusters in the form of dislocation loops, voids, gas-filled bubbles and radiation-induced precipitates of nanometer scale. They cause changes in many material properties. Being obstacles to dislocation glide, they strongly affect the mechanical properties, with an increase in yield and flow stresses and a reduction in ductility. Atomic-scale computer simulations can provide details of how these effects are influenced by the obstacle structure, applied stress, strain rate and temperature. Processes such as obstacle cutting, transformation, absorption and drag are observed. Some recent results for body-centered and face-centered cubic metals are described in this review and, where appropriate, comparisons are drawn with predictions based on the elasticity theory of crystal defects. Perspectives on how to use this information at higher scales and in particular in mesoscale, dislocation dynamics simulations are also discussed.

Osetskiy, Yury N.↗

Multimodal Characterization of Crystal Structure and Formation in Rubrene Thin Films Reveals Erasure of Orientational Discontinuities

Abstract Multimodal multiscale characterization provide opportunities to study organic semiconducting thin films with multiple length scales, across multiple platforms, to elucidate crystallization mechanisms of the various microstructures that impact functionality. With polarized scanning transmission X‐ray and 4D‐scanning transmission electron microscopy, hybrid crystalline structures in rubrene thin films in which large crystalline domains surround a common nucleus and transition to a spherulite morphology at larger radii is observed. These high‐resolution techniques reveal how azimuthal orientational discontinuities at smaller radii are erased as spherulite morphology takes hold. In situ crystallization in the films with optical microscopy is also captured, discovering the importance of considering the initial temperature increase of a film during thermal annealing over the crystallization timescale. This kinetic information of the radial crystallization rate and of corresponding film heating kinetics is used to estimate the temperature at which the larger crystalline regions transition into a spherulite. By combining the results obtained from the different characterization modes, it is learned that thermal conditions can sensitively affect the crystallization of rubrene and other organic thin films. The observations suggest opportunities for more complex temperature‐dependent processing to maximize hybrid structures’ functionality in organic thin films and demonstrate that multimodal studies deepen the understanding of structure‐function dynamics.

Tan, Jenna A.↗

Flash Formation of I-Rich Clusters during Multistage Halide Segregation Studied in MAPbI 1.5 Br 1.5

Wide band gap mixed halide perovskites such as MAPb(I 1–x Br x ) 3 sparked great research interest because of their outstanding optoelectronic properties, ease of fabrication, and band gap tunability. Their application thus far is however limited by light-induced halide segregation in which microscopic clusters with a high iodide content are formed and act as recombination centers. The key mechanism(s) underlying this halide segregation process are still debated. Here, we present a study on the photoluminescence evolution in MAPb(I 1.5 Br 1.5 ) perovskites with varying microstructures under constant illumination at room temperature and at elevated temperature. Our findings reveal a more complicated picture of the segregation mechanism occurring in three stages instead of two as commonly reported. The process starts with a flash formation of I-rich domains. Following is a rapid blue shift before the gradual and typically observed red shift occurs. The evolution of the three stages is fully reversible in the dark and is also present at elevated temperatures (50 °C). We explain the existence of multiple stages during light-induced halide segregation by natural compositional fluctuations of the halides and the formation of halide clusters with a dynamically changing distribution in I–Br content. The variation in the I–Br ratio depends on the grain size and film heterogeneity. Overall, these findings add further details in the quest of unraveling the underlying segregation mechanism(s), which need to be identified to stabilize halides in wide band gap perovskites.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Ultra-grain refinement creates FCC pure cobalt with high strength and high ductility

Although pure cobalt is generally known to have a hexagonal close-packed (HCP) structure at room temperature, we show that its high-temperature face-centered cubic (FCC) phase can be strongly stabilized through grain refinement, resulting in FCC pure cobalt at room temperature. Ultrafine-grained (UFG) FCC cobalt exhibits a hierarchical microstructure consisting of dense stacking fault (SF) networks in the dominant FCC grains and numerous SFs and thin FCC layers within a few HCP plates. This unique microstructure leads to a high tensile strength exceeding 1 GPa, together with a tensile elongation of over 35%, thereby surpassing the well-known strength–ductility trade-off of pure metals. In-situ synchrotron X-ray diffraction revealed that the UFG FCC cobalt exhibited a markedly enhanced deformation-induced FCC→HCP martensitic transformation, which provided sustained strain hardening through the transformation-induced plasticity (TRIP) effect. Furthermore, ultra-grain refinement dramatically suppressed premature void and crack formation, causing a transition in the fracture mode from brittle to ductile. These findings advance the fundamental understanding of the phase stability and TRIP-assisted deformation in elemental cobalt and offer new guidelines for the microstructure-driven design of high-performance cobalt-based structural alloys.

Metastability↗