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At least 1,171 records · Page 65

Preliminary Findings from the SHERE ISS Experiment

The Shear History Extensional Rheology Experiment (SHERE) is an International Space Station (ISS) glovebox experiment designed to study the effect of preshear on the transient evolution of the microstructure and viscoelastic tensile stresses for monodisperse dilute polymer solutions. The SHERE experiment hardware was launched on Shuttle Mission STS-120 (ISS Flight 10A) on October 22, 2007, and 20 fluid samples were launched on Shuttle Mission STS-123 (ISS Flight 10/A) on March 11, 2008. Astronaut Gregory Chamitoff performed experiments during Increment 17 on the ISS between June and September 2008. A summary of the ten year history of the hardware development, the experiment's science objectives, and Increment 17's flight operations are discussed in the paper. A brief summary of the preliminary science results is also discussed.

Hall, Nancy R.↗

Characterization of Dendritic Spatially Extended 3D Patterns in Directional Solidification: Microgravity Experiments in DECLIC-DSI onboard ISS and 3D Phase-field Simulations

To clarify and characterize the fundamental physical mechanisms active in the dynamical formation of three-dimensional (3D) arrays of dendrites under diffusive growth conditions, in situ monitoring of series of experiments on transparent model alloy succinonitrile – 0.46 wt% camphor was carried out under low gravity in the DECLIC Directional Solidification Insert onboard the International Space Station. These experiments offer the very unique opportunity to observe in situ and characterize the dynamics of the microstructure formation and evolution in extended 3D patterns under microgravity environment. The analyses of the dendritic patterns for a broad range of growth velocities displaying different levels of sidebranching will be presented. Especially, the time evolution of primary spacing, in case of solidifications at constant pulling rate as well as for experiments with pulling rate jump, will be compared to 3D phase-field simulations, and the results will be discussed in terms of stable spacing range.

Kaihua Ji↗

Experimental Investigation of Solid Rod Cathode Operation

A series of models have been developed to describe the temperature distribution of thermionic cathodes in high current discharges in an effort to evaluate cathode service life. A number of experimental measures have been made to validate these models and provide values of the input parameters. Examination of the surfaces of several cathodes after varying lengths of operation shows the evolution of surface microstructures and reveals the preferential deposition of thorium metal on the cathode tip.

thermionic↗

Characterization of Dendritic Spatially Extended 3D Patterns in Directional Solidification: Microgravity Experiments in DECLIC-DSI Onboard ISS and 3D Phase-field Simulations

To clarify and characterize the fundamental physical mechanisms active in the dynamical formation of three-dimensional (3D) arrays of dendrites under diffusive growth conditions, in situ monitoring of series of experiments on transparent model alloy succinonitrile – 0.46 wt% camphor was carried out under low gravity in the DECLIC Directional Solidification Insert onboard the International Space Station. These experiments offer the very unique opportunity to observe in situ and characterize the dynamics of the microstructure formation and evolution in extended 3D patterns under microgravity environment. The analyses of the dendritic patterns for a broad range of growth velocities displaying different levels of sidebranching will be presented. Especially, the time evolution of primary spacing, in case of solidifications at constant pulling rate as well as for experiments with pulling rate jump, will be compared to 3D phase-field simulations, and the results will be discussed in terms of stable spacing range.

Kaihua Ji↗

Multi-Scale Modelling of the Bound Metal Deposition Manufacturing of Ti6Al4V

Nonlinear shrinkage of the metal part during manufacturing by bound metal deposition, both on the ground and under microgravity, is considered. A multi-scale physics-based approach is developed to address the problem. It spans timescales from atomistic dynamics on the order of nanoseconds to full-part shrinkage on the order of hours. This approach enables estimation of the key parameters of the problem, including the widths of grain boundaries, the coefficient of surface diffusion, the initial redistribution of particles during the debinding stage, the evolution of the microstructure from round particles to densely-packed grains, the corresponding changes in the total and chemical free energies, and the sintering stress. The method has been used to predict shrinkage at the levels of two particles, of the filament cross-section, of the sub-model, and of the whole green, brown, and metal parts.

Nonlinear shrinkage↗

NASA BPS Reduced Gravity Integrated Computational Materials Engineering (ICME) Study

The Biological and Physical Sciences (BPS) Division of NASA’s Science Mission Directorate (SMD), and its predecessors, has sponsored extensive flight and ground experiments yielding benchmark datasets in many materials science research areas including thermophysical properties and solidification microstructure formation and evolution. The subject study sought to motivate and focus BPS’s engagement within the broader Integrated ICME community to understand the phenomena underlying material processing, structure, and properties in the microgravity environment of space and to support future space exploration efforts.

Louise Littles↗

Additive Manufactured Composite Phase-Change Material for Thermal Energy Storage Applications

Phase-change materials play a critical role in industrial energy storage applications to drive efficiency improvements, thermal energy management, and carbon emissions reductions. Recently, it has been shown that rapid solidification of alloys with metastable immiscibility in the liquid phase has the potential to form unique microstructures in which a low-melting phase is uniformly distributed in a high-melting matrix. This feature can be exploited using additive manufacturing to produce components with complex geometries containing such unique phase-change microstructures. Phase-field simulations utilizing high-performance computing were used to provide a detailed description of the evolution of the active phase during service in terms of their morphology and composition in different polycrystalline matrix grain morphologies that are typically produced during additive manufacturing. Phase field simulations were performed using, MEUMAPPS-SL (Microstructure Evolution Using Massively Parallel Phase-field Simulations – Solid Liquid) code that was developed in-house by the Oak Ridge National Laboratory. The simulations utilized the capabilities of the Kestrel supercomputer at the National Renewable Energy Laboratory. The simulation results were compared with experimental results generated at Siemens Energy, Inc. The results indicate that the kinetics of liquid spreading along grain boundaries is largely determined by the mobility of the triple line along the intersection of the grain boundary liquid and the grain boundary plane.

25 ENERGY STORAGE↗

Effects of Thermal Exposure on the Microstructure and Mechanical Properties of Al-Si-Cu-Ni-Mg-Gd Alloy

The present study focused on the effect of thermal exposure on the phase evolution and properties of the cast-T6 Al-12Si-4Cu-2Ni-0.8Mg-xGd (x = 0, 0.1, and 0.2) alloy used for cast piston.The thermal stability of the alloys was studied in the temperature range of 200-300 °C for exposure duration up to 500 h, thus obtaining the relationship between the microstructural evolution and its impact on the mechanical properties. The fine Al{sub 2}Cu phase grew into the coarse θ-Al{sub 2}Cu phases during the thermal exposure, resulting in a decrease in the mechanical strength of the alloy. The thermal stability and stiffness of the Al-Si-Cu-Ni-Mg alloys were improved with the increase in Gd content from 0 to 0.2%.

36 MATERIALS SCIENCE↗

Synchrotron Tomography of SiC/SiC Minicomposites to Observe and Quantify Damage Evolution

Composite performance is dictated by its microstructure – property relationships. For example, the characteristic response of ceramic matrix composites (CMCs) depends on the distribution of its constituents (i.e. fibers, matrix, fiber coatings, matrix cracks, and voids). Micro x-ray computed tomography (micro-CT) provides an opportunity to characterize the distribution of these constituents and to quantify the CMC microstructure in three-dimensions. To this end, In-situ micro-CT was performed at the Advanced Light Source (ALS) in combination with uniaxial tensile testing on SiC/SiC minicomposites. This work will describe the tensile load-dependent damage evolution within the microstructure of the SiC/SiC CMC specimens. The results from the micro-CT datasets can be used to develop micromechanical models that effectively capture damage initiation and progression in CMCs. In addition, details regarding the segmentation tools and techniques employed to understand and quantify these large tomography datasets will be presented.

Ashley Hilmas↗

Material Failure Mechanisms of Alkaline Zn Rechargeable Conversion Electrodes

Zinc (Zn) alkaline electrodes hold great importance and promise in the battery technology community, yet their behavior in real-world applications is still poorly understood. Here, we report a study of failure mechanisms and material evolution during cycling of 27 zinc–manganese dioxide (Zn–MnO 2 ) cells wherein the percent utilization of the Zn electroactive material is systematically varied between 1 and 16%. Cell fabrication is kept typical of the prevailing industrial cell design. The cycle life ranges from 2800 to 60, depending inversely on the Zn utilization. In all cases, the Zn material microstructure sheds the polytetrafluoroethylene (PTFE) binder and forms zinc oxide (ZnO) rods, with longer rods formed by lower current per Zn mass. Irreversible side reactions such as the hydrogen evolution reaction (HER), short circuits, or gas crossover cause the Zn anode’s charging efficiency to average 92% (as low as 86%), which in turn causes the baseload of metallic Zn to gradually disappear. Cell failure occurs after the baseload of metallic Zn is exhausted. The total lifetime discharge capacity remains constant near 12 ± 5 Ah/g Zn invariant of Zn utilization, which suggests that the aforementioned processes of Zn microstructural evolution and side-reaction destruction of baseload metallic zinc both progress linearly with cell capacity throughput. Manual reproduction of individual Zn failure mechanisms is performed in 22 fresh cells. Tight packing of the microstructure can lead to poor mass transfer, which causes supersaturation of soluble Zn and finally produces a high overvoltage during discharge. Here, the low charging current density yields poor coulombic efficiency due either to the competitive HER or soft short circuits.

25 ENERGY STORAGE↗

Imaging transient solidification behavior

Solidification processing offers the first opportunity to control microstructure, properties, and performance in metallic alloy components. Until recently, microstructural evaluations were limited to post-solidification characterization by destructive methods. We review the development of time-resolved, in situimaging techniques capable of capturing solid-liquid interfacial evolution in metallic alloys with high spatial and temporal resolution underdiverse solidification conditions relevant for applications ranging from conventional directional solidification, crystal growth, and casting,to welding and additive manufacturing. These experiments enable direct visualization of transient behaviors that would otherwise remain unknown, uniquely providinginsights into the physics that impact microstructure and defect development and strategies for microstructuralcontrol and defect mitigation. Understanding microstructural evolution and the characteristics that form under various solidification conditions is essential for the development of multiscale, experimentallyinformed predictive modeling. This is highlightedby solidification simulations that utilize in situmeasurements of solidification dynamics from state-of-the-art experimental techniques.

36 MATERIALS SCIENCE↗

Nanoscale selective growth and microstructural control of indium nitride (InN)

Selective area growth (SAG) is a phenomenon in thin film deposition where the sample surface is masked by a dielectric or refractory layer such that growth takes place only in the exposed window regions. As the opening window is pushed to nano-scale, it becomes possible to confine and control epitaxial evolution with lithographically engineered geometry with a feature size comparable to that ofa single nucleus. Two fundamental questions in nano-scale SAG are studied. The first one is how does nano-scale constriction in one direction impact the microstructure evolution in the other orthogonal directions. The other question is how does the presence of nano-scale geometric boundaries affect the crystallographic orientation in selective area epitaxy? InN is chosen as a case study to demonstrate the efficacy and unveil the science in nano-scale SAG. For the first time, we achieve uniform InN nanowires in the large scale with nano-trenches. The engineering of InN nuclei with interfacial energy and the possibility of orientation filtering are also studied.

36 MATERIALS SCIENCE↗

Effect of Mg-Bearing Oxide(+TiN) Inclusion on Microstructure of Fe-16 Mass Pct Cr Ferritic Alloy and Its Evolution During Heating at 1573 K (1300 °C)

Both the effects of Mg-bearing oxide and Mg-bearing oxide +TiN inclusions on the microstructures of Fe-16 mass pct Cr alloy should be clarified. In this paper, the effects of Mg-bearing oxide(+TiN) inclusions on the microstructures of Fe-16 mass pct Cr ferritic alloy and changes due to the inclusions during heating at 1573 K (1300 °C) were studied by manual and automatic SEM-EDS analyses. Three alloys were used as specimens. The inclusions were Al{sub 2}TiO{sub 4} +TiN with a small amount of TiN in alloy #1, Al{sub 2}(Mg, Ti)O{sub 4} in alloy #2 and Al{sub 2}(Mg, Ti)O{sub 4} +TiN in alloy #3. The average grain size was smaller, and the ratio of columnar grains was lower in the as-cast alloy #2 and as-cast alloy #3 than that in the as-cast alloy #1. This is attributed to the heterogeneous nucleation of delta ferrite on Al{sub 2}(Mg, Ti)O{sub 4} during solidification. Refinement of the microstructures of ferritic steel by Mg-bearing oxide + multi-TiN inclusions is proposed. Changes in composition, aspect ratio, and size distribution of inclusions in each alloy during heating were investigated systematically. Mg-bearing oxide(+TiN) was dispersed in both the as-cast alloys and heated alloys, which contributed to microstructural refinement of the heated alloys through the pinning effect.

36 MATERIALS SCIENCE↗

In situ high-energy X-ray diffraction mapping of Lüders band propagation in medium-Mn transformation-induced plasticity steels

Two-dimensional distributions of microstructural characteristics of austenite (γ) around the Lüders band in medium-Mn transformation-induced plasticity (TRIP) steel were revealed by in situ high-energy X-ray diffraction. Lüders band propagation leads to significant changes in the volume fraction and lattice strains of austenite. The evolution of the lattice strain of γ-311 accords well with the true yield behavior model and is used to estimate the angle of the Lüders band front with respect to the tensile axis. The modified Williamson-Hall analysis shows that the dislocation density in austenite increased from 7 × 10 14 m -2 to 1.5 × 10 15 m -2 after Lüders band propagation. This in situ high-energy X-ray diffraction study unravels two-dimensional distribution of microstructural evolution during Lüders band propagation in medium-Mn TRIP steels.

36 MATERIALS SCIENCE↗

Direct observations and characterization of crack closure during microstructurally small fatigue crack growth via in-situ high-energy X-ray characterization

This study provides direct observation of the crack closure mechanism of a naturally occurring, tortuous, 3D microstructurally small fatigue crack (SFC) in additively manufactured Inconel 718. In-situ non-destructive characterization is performed using high-energy X-ray diffraction techniques to capture the evolution of the 3D microstructure and micromechanical response in the vicinity of the crack front. Based on the stress state of twelve grains analyzed at the crack tip, the crack closure events of the SFC front was found to be spatially heterogeneous with respect to loading progression governed by the local stress state of the grains (specifically the stress reversal from compression to tension). From this analysis, three grains that displayed different degrees of crack closure were further investigated, based on the orientation of the crack relative to the grains and the associated modality of crack growth. The stress normal to the crack plane and the associated degree of Mode I crack behavior were correlated with events of the crack opening earlier during the loading cycle. This was further corroborated by diffraction spot spreading analysis that quantified the crystallographic lattice distortion caused by the opening crack. Additionally, the detailed characterization of the opening behavior of the grains located at the crack tip and their associated states of stress elucidates the mechanism governing crack closure and will inform future modeling efforts of this phenomenon.

36 MATERIALS SCIENCE↗

Microstructurally Strained Pyrochlore–Perovskite Biphasic Electrocatalysts for the Oxygen Evolution Reaction

Efficiency of water splitting for hydrogen production is often limited by the sluggish kinetics of multiple electronic transfers required in the heterogeneous oxygen evolution reaction (OER). Catalyst design for reducing the high OER overpotential remains a major scientific challenge. Lattice-strain engineering, a method for tuning the electronic structure and surface geometric configuration of active sites, may greatly affect the interaction between adsorbates and catalytic surfaces for high activity and stability. Here, in this study, we present the synthesis of biphasic oxides of YPrSrRuMnO x , which consists of distinct phases of Y 2 Ru 2 O 7 pyrochlore and (Pr 0.7 Sr 0.3 )MnO 3 perovskite, and the development of a suitable analytical approach to study the strain–catalytic property relationship. Linear sweep voltammetry results reveal that the biphasic oxide exhibits approximately 3.1 times greater mass activity and 2.4 times larger turnover frequency (TOF) than single-phase Y 2 Ru 2 O 7 in the 0.1 M HClO 4 electrolyte. The biphasic catalyst is also about 3 times more stable than the single-phase oxide under acidic conditions. X-ray photoelectron spectroscopy, nitrogen isotherm, and electrochemical surface area analyses indicate that the oxidation state, specific surface area, and electrochemical surface area do not cause enough difference in the observed enhancement of OER performance. We examined the effects of microstrain on electrocatalysis, originating from lattice mismatch between different phases, using three different structural models. Specifically, we compared the Williamson–Hall method, standard stress–strain analysis, and Rietveld refinement in analyzing the structure–property relationship. Strain mapping using geometric phase analysis (GPA) further revealed significant microstrain and lattice dislocations localized near phase boundaries in the biphasic oxide, in contrast to the uniform strain in single-phase materials. The results reveal that the increased microstrain correlates well with the improved OER performance, as the biphasic oxide catalyst exhibits 2–3 times greater microstrain than Y 2 Ru 2 O 7 pyrochlore.

electrocatalysts↗

Influence of Mo Content on the Precipitation Behavior of 13Ni Maraging Ultra-High Strength Steels

This study offers valuable insights into the precipitation behavior of 13Ni maraging steels, emphasizing the role of molybdenum content in their microstructure, strengthening, and precipitate evolution. Precipitate morphology and crystallography were examined using a combination of high-resolution transmission electron microscopy and selected area electron diffraction. Strengthening mechanisms were assessed through Vickers hardness measurements. All the examined samples exhibited a lath martensite microstructure and displayed an increasing hardness over the aging time. The molybdenum content not only influenced the presence of retained austenite in the initial microstructure but also affected the type of precipitates formed during the early aging stages. Initially, Ni 3 Mo precipitates were formed, succeeded by the formation of more stable Fe 2 (Mo,Ti) Laves precipitates. The ultra-high strength of 13Ni maraging steels arises from the combination of the precipitate type and size distribution. The base composition of 13Ni maraging steels achieved a peak hardness of 798 HV1 through the precipitation of Laves Fe 2 (Mo,Ti) phases ranging from 3 to 14 nm in diameter.

13Ni maraging steels↗