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At least 451 records · Page 25

Interfacial Surgery Determination of Succinonitrile and Succinonitrile-Acetone Alloy Using Surface Light Scattering Spectrometer

The objectives of this ground based research is to measure the liquid/vapor interfacial surface energies of succinonitrile (SCN) and alloys of succinonitrile and acetone using Surface Light Scattering Spectrometer. Liquid/vapor interfacial energy measurements will be made near and above the melting point and are the primary goal of this proposal. A measurement of viscosity also results from the Surface Light Scattering technique employed. Interfacial free energies between the phases enters into many analysis of phase transformation and flow, including nucleation, dendritic growth, interface stability, Ostwald ripening, and Marangoni flow. Succirionitrile (SCN) is useful as a model for the study of metal solidification, although it is an organic material, it has a BCC crystal structure and solidifies dendriticly like a metal. It is also transparent and has a low melting point (58.08 C). Succinonitrile has been and is being used extensively in NASAs Microgravity Materials Science and Fluid Physics programs and as well as in several ground-based and microgravity studies including the Isothermal Dendritic Growth Experiment (IDGE) due to Glicksman and coworkers and subsequently in several theoretical and numerical studies of dendritic growth. Previous measurements of succinonitrile (SCN) and alloys of succinonitrile and acetone surface tensions are extremely limited. We believe the data sought through this proposal have significant basic physical property data value and thus the work proposed will provide needed data in support of NASAs Microgravity program research.

Tin, Padetha↗

A Comparison between Growth Morphology of "Eutectic" Cells/Dendrites and Single-Phase Cells/Dendrites

Directionally solidified (DS) intermetallic and ceramic-based eutectic alloys with an in-situ composite microstructure containing finely distributed, long aspect ratio, fiber, or plate reinforcements are being seriously examined for several advanced aero-propulsion applications. In designing these alloys, additional solutes need to be added to the base eutectic composition in order to improve heir high-temperature strength, and provide for adequate toughness and resistance to environmental degradation. Solute addition, however, promotes instability at the planar liquid-solid interface resulting in the formation of two-phase eutectic "colonies." Because morphology of eutectic colonies is very similar to the single-phase cells and dendrites, the stability analysis of Mullins and Sekerka has been extended to describe their formation. Onset of their formation shows a good agreement with this approach; however, unlike the single-phase cells and dendrites, there is limited examination of their growth speed dependence of spacing, morphology, and spatial distribution. The purpose of this study is to compare the growth speed dependence of the morphology, spacing, and spatial distribution of eutectic cells and dendrites with that for the single-phase cells and dendrites.

Tewari, S. N.↗

Directionally Solidified Aluminum - 7 wt% Silicon Alloys: Comparison of Earth and International Space Station Processed Samples

Primary dendrite arm spacings of Al-7 wt% Si alloy directionally solidified in low gravity environment of space (MICAST-6 and MICAST-7: Thermal gradient approx. 19 to 26 K/cm, Growth speeds varying from 5 to 50 microns/s show good agreement with the Hunt-Lu model. Primary dendrite trunk diameters of the ISS processed samples show a good fit with a simple analytical model based on Kirkwood s approach, proposed here. Natural convection, a) decreases primary dendrite arm spacing. b) appears to increase primary dendrite trunk diameter.

Grugel, Richard N,↗

Microstructure and Macrosegregation Study of Directionally Solidified Al-7Si Samples Processed Terrestrially and Aboard the International Space Station

This talk reports research that has been carried out under the aegis of NASA as part of a collaboration between ESA and NASA for solidification experiments on the International Space Station (ISS). The focus has been on the effect of convection on the microstructural evolution and macrosegregation in hypoeutectic Al‐Si alloys during directional solidification (DS). The DS‐experiments have been carried out under 1‐g at Cleveland State University (CSU) and under low‐g on the International Space Station (ISS). The thermal processing‐history of the experiments is well defined for both the terrestrially‐processed samples and the ISS‐processed samples. We have observed that the primary dendrite arm spacings of two samples grown in the low‐g environment of the ISS show good agreement with a dendrite‐growth model based on diffusion controlled growth. The gravity‐driven convection (i.e., thermosolutal convection) in terrestrially grown samples has the effect of decreasing the primary dendrite arm spacings and causes macrosgregation. In order to process DS‐samples aboard the ISS, dendritic‐seed crystals have to partially remelted in a stationary thermal gradient before the DS is carried out. Microstructural changes and macrosegregation effects during this period are described.

Angart, Samuel↗

A Discussion of the Failure of a Quad Diode Module and Efforts to Assure the Flight Spares

In 2019 the International Space Station (ISS) experienced an on on-orbit failure that affected 1 of 28 Battery Charge Discharge Units (BCDUs). Telemetry pointed to a short circuit failure of a Power Rectifier Quad Diode Module. Astronauts removed the failed unit from service which was then returned to Earth for failure analysis. The failure analysis confirmed that the quad diode module had failed short circuit. The investigation identified silver dendrites had grown on the insulated, sloped edge of the mesa semiconductor die of the failed diode and also a 2nd diode in the same quad diode module. Voids between the diode’s protective encapsulating ring and the die provided space within which dendrites were able to form and cause catastrophic failure. The NASA Engineering & Safety Center (NESC) convened a EEE Parts Sub-Team to investigate root cause and to assist with risk assessment for all of the flight diode modules (4 distinct production lots) and the flight spares (from a 5th lot). Analysis of the original diode manufacturer’s read and record screening test data identified some lots which contained diodes with parametric instabilities that could signal conditions suited for silver dendrite formation. Computed Tomography (CT) X-ray screening inspection was performed on flight spare modules to identify diodes that do not exhibit voids between the edge of die and encapsulating ring as a mitigation against dendrite formation.

Jay Brusse↗

Controlled Parametric Forcing During Directional Solidification of a Bulk Organic Alloy Under Microgravity

The response of dendritic microstructures to step-like pulling velocity conditions is investigated using microgravity directional solidification experiments conducted on DECLIC-DSI combined with phase-field simulations. Under a constant pulling velocity of 1.5 µm/s, the evolution toward steady-state growth is characterized in terms of primary spacing, dendrite drift, and tip dynamics. For the first time, side-view observations enabled direct measurement of tip radius and sidebranching frequency. When step-like oscillations of the pulling velocity are imposed, the dendritic array exhibits a strongly period-dependent response: short periods lead to rapid tip adaptation, whereas longer periods induce a phase lag between tip position and morphology, resulting in progressive tip flattening and, above a critical period, interface destabilization and dendrite splitting. Quantitative phase-field simulations, including a realistic thermal field and stochastic noise, reproduce the experimental observations and provide insight into the governing mechanisms, highlighting the role of characteristic relaxation times, sequence-dependent effects, and the irreversible reorganization of the microstructure following splitting.

Microgravity↗

Electrodes, lithium-ion batteries, and methods of making and using same

Described herein are improved composite anodes and lithium-ion batteries made therefrom. Further described are methods of making and using the improved anodes and batteries. In general, the anodes include a porous composite having a plurality of agglomerated nanocomposites. At least one of the plurality of agglomerated nanocomposites is formed from a dendritic particle, which is a three-dimensional, randomly-ordered assembly of nanoparticles of an electrically conducting material and a plurality of discrete non-porous nanoparticles of a non-carbon Group 4A element or mixture thereof disposed on a surface of the dendritic particle. At least one nanocomposite of the plurality of agglomerated nanocomposites has at least a portion of its dendritic particle in electrical communication with at least a portion of a dendritic particle of an adjacent nanocomposite in the plurality of agglomerated nanocomposites.

Yushin, Gleb↗

Electrodes, lithium-ion batteries, and methods of making and using same

Described herein are improved composite anodes and lithium-ion batteries made therefrom. Further described are methods of making and using the improved anodes and batteries. In general, the anodes include a porous composite having a plurality of agglomerated nanocomposites. At least one of the plurality of agglomerated nanocomposites is formed from a dendritic particle, which is a three-dimensional, randomly-ordered assembly of nanoparticles of an electrically conducting material and a plurality of discrete non-porous nanoparticles of a non-carbon Group 4A element or mixture thereof disposed on a surface of the dendritic particle. At least one nanocomposite of the plurality of agglomerated nanocomposites has at least a portion of its dendritic particle in electrical communication with at least a portion of a dendritic particle of an adjacent nanocomposite in the plurality of agglomerated nanocomposites.

Yushin, Gleb↗

Electrodes, lithium-ion batteries, and methods of making and using same

Described herein are improved composite anodes and lithium-ion batteries made therefrom. Further described are methods of making and using the improved anodes and batteries. In general, the anodes include a porous composite having a plurality of agglomerated nanocomposites. At least one of the plurality of agglomerated nanocomposites is formed from a dendritic particle, which is a three-dimensional, randomly-ordered assembly of nanoparticles of an electrically conducting material and a plurality of discrete non-porous nanoparticles of a non-carbon Group 4A element or mixture thereof disposed on a surface of the dendritic particle. At least one nanocomposite of the plurality of agglomerated nanocomposites has at least a portion of its dendritic particle in electrical communication with at least a portion of a dendritic particle of an adjacent nanocomposite in the plurality of agglomerated nanocomposites.

Yushin, Gleb↗

Electrodes, lithium-ion batteries, and methods of making and using same

Described herein are improved composite anodes and lithium-ion batteries made therefrom. Further described are methods of making and using the improved anodes and batteries. In general, the anodes include a porous composite having a plurality of agglomerated nanocomposites. At least one of the plurality of agglomerated nanocomposites is formed from a dendritic particle, which is a three-dimensional, randomly-ordered assembly of nanoparticles of an electrically conducting material and a plurality of discrete non-porous nanoparticles of a non-carbon Group 4A element or mixture thereof disposed on a surface of the dendritic particle. At least one nanocomposite of the plurality of agglomerated nanocomposites has at least a portion of its dendritic particle in electrical communication with at least a portion of a dendritic particle of an adjacent nanocomposite in the plurality of agglomerated nanocomposites.

Yushin, Gleb↗

CHALLENGES IN THE DEVELOPMENT OF THE ELECTROREFINING PROCESS AT Y-12

In order to ensure future capabilities of the Y-12 site as older buildings retire, a new process was developed, the Metal Purification Process. The purpose of this new process is to provide a simpler and more efficient uranium metal purification that the previous multi-staged, complex chemical processes. The basis for this technology currently exists in the US DOE complex, but it has not been utilized on a large scale for uranium at higher enrichments. The system requires larger-geometry vessels and furnaces in order to meet the through-put requirements. The crux of the process is the electrorefining cell, consisting of several concentric liners and an unfavorable geometry cylindrical crucible. Within the crucible, a molten Li-CL-KCL-UCL3 salt electrolyte is present. ‘Dirty’ metal is placed into a loading basket and loaded into an electrorefining cell. Here, the metal reacts into the molten salt within the cell to form UCL3, while ‘clean’ metal simultaneously plates out from the salt electrolyte in the form of metal dendrites. These dendrites are then collected and removed from the cell. After removal from the cell, the dendrites are taken to a furnace to remove adhered salts. Then, the salt-free dendrites are moved to a separate furnace for consolidation into the final product form. The development of the Criticality Safety Evaluation for this complex system brought with it many NCS Challenges and lessons learned. These challenges include: design decisions for ensuring subcriticalty in the electrorefining cell during abnormal conditions, the interface of the main glovebox system with auxiliary systems such as the purification system and designated storage, implementation of mass tracking, and concerns from production and operation regarding the movement of material within the system.

36 MATERIALS SCIENCE↗

Covalent Organic Framework as an Efficient Protection Layer for a Stable Lithium-Metal Anode

We report Lithium (Li) metal shows great potential for achieving high-energy-density rechargeable batteries. However, the practical applications of Li-metal batteries are still challenged by the formation of Li dendrites and unstable solid-electrolyte interphase (SEI) on metallic Li. Herein, a thin covalent organic framework layer is in situ fabricated on Li (COF-Li) to suppress Li dendrite growth and mitigate the side reaction on the Li anode. The COF has a periodic and uniform porosity, allowing for selectively sieving Li ions and guiding a uniform Li deposition. As a result, the COF-Li exhibits a non-dendrite morphology during repeated Li plating/stripping and demonstrates a remarkable cycle life over 13 200 h with an extremely low overpotential of only 16 mV at a high current density of 10 mA cm -2 and a high areal capacity of 10 mAh cm -2 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Effect of Eutectic Characteristics on Hot Tearing of Cast Superalloys

The occurrence of hot cracks in the blades of Ni-based superalloy turbocharger wheels is thought to be closely related to eutectic characteristics. Different alloys that are susceptible to hot tearing, namely K418, K419 and K424, were studied. SEM was used to obtain the microstructure of the alloys. DSC, isothermal solidification quenching process and EPMA were conducted to determine the relationship between the eutectic characteristics and solidification process, segregation behavior and dendrite coalescence. The results show that a large volume fraction of γ/γ′ eutectic indicates a wide-temperature solidification range and severe segregation. A large γ/γ′ eutectic size is a result of element segregation and poor dendrite coalescence. Ti is thought to promote the formation of a large isolated residual liquid pool and lead to a large eutectic size, leading to the poor coalescence behavior of the dendrites. The volume fraction and size of the γ/γ′ eutectic were considered, and a eutectic influence factor (E) was defined to evaluate the effect of eutectic characteristics on hot tearing in cast superalloys. It was found that a high E corresponds to high hot-tearing susceptibility.

36 MATERIALS SCIENCE↗

Evaluation of the Microstructure and Performance of Fe-21Cr-15Ni-6Mn-Nb Nonmagnetic Stainless Steel Welded Joints

In the present study, double-sided gas shield welding (GSW), in a single pass, was applied to Fe-21Cr-15Ni-6Mn-Nb nonmagnetic stainless steel plate. The microstructure and performance of the welded joint were investigated via microstructural and phase analysis, mechanical testing and magnetic analysis. The results showed a satisfactory micrographic appearance with full penetration, and no solidification defects observed in the welded joint, which showed typical epitaxial growth characteristics in the welding solidification. Slight grain growth, with an average size of ~ 18.9 μm, occurred in the heat-affected zone (HAZ). The primary dendrite arms, on both sides of welding joint, grew along the direction of the temperature gradient and met at the centerline of the weld with no parting microstructure in evidence. The secondary dendrite arm spacing was stable in all parts of the weld zone (WZ). The hardness of the weld zone was higher than that of the HAZ and the base metal (BM), with the lowest hardness occurring in the HAZ. The results of tensile testing showed a higher strength of the welded metal (WM) compared to the BM, and a good strength-ductility balance of the welded joint. The impact energy of the HAZ was higher than that of the WZ, corresponding to 60.5 J at room temperature and 52.7 J at − 196 °C. Microvoid coalescence, concurrent with crack propagation along the direction of the long axis of the dendritic sub-grains, was observed during plastic deformation in the WZ. Additionally, the excellent paramagnetic characteristics of the welded specimens were revealed.

36 MATERIALS SCIENCE↗

Microstructure and Mechanical Properties of Ni-based Superalloy K418 Produced by the Continuous Unidirectional Solidification Process

Adopting effective strategies to control the solidification structure of Ni-based superalloys is a very interesting subject for metallurgists. Despite the achievement of developing and applying the continuous unidirectional solidification process in simple alloys, the utilization of this process for K418 alloys has been ignored. The microstructure and mechanical properties of a K418 alloy ingot produced by the continuous unidirectional solidification process were investigated. We found that the γ dendrites were typically cross-shaped in the transverse section. The orientation of surviving grains along the casting direction was <001> during competitive growth. The secondary dendrite arm spacing was 32.3 ± 2.5 μm at a cooling rate of 1.75 ± 0.35 °C/s from the surface to the center of the K418 alloy ingot. Due to the higher cooling rate than that of the conventional casting process, a more uniform microstructure and finer γ′ precipitation were obtained in the ingot. Thus, compared with the conventional casting, the tensile strength and the elongation are increased by 8.4 and 21.3%, respectively, at 25 °C. The tensile strength and elongation increased by 15.2 and 49.3%, respectively, at 800 °C. In addition, the fracture surfaces exhibited numerous typical dimples and dendritic fracture characteristics.

36 MATERIALS SCIENCE↗

Lithiophilic V 2 O 5 nanobelt arrays decorated 3D framework hosts for highly stable composite lithium metal anodes

The lithium metal anode has been considered to be an optimal anode material for high-energy-density battery system due to its ultrahigh specific capacity. However, the sharp dendrite growth and infinite volume expansion have significantly impeded its commercial application. In this paper, we propose that V 2 O 5 as the lithiophilic substance can be decorated onto 3D stable frameworks to fabricate dendrite-suppressed composite Li metal anodes via a molten Li infusion method. It is demonstrated that the energetic chemical reaction between V 2 O 5 and molten Li together with the capillary effect based on the nanostructure of interconnected V 2 O 5 nanobelt arrays contributes synergistically to the great Li affinity of the V 2 O 5 -Ni foam (V 2 O 5 -NF) host and facilitate the efficient and uniform intake of molten Li into the 3D framework. Benefitting from the homogeneous Li distribution in the framework, the decreased local current density of the electrode and the stable property of the host, dendrite-free Li stripping/plating behavior and alleviated volume fluctuation have been achieved for the Li-V 2 O 5 -NF composite anode. Compared with the bare Li anode, the as-obtained Li-V 2 O 5 -NF composite anode exhibits much stable stripping/plating profiles with low overpotential (~18 mV) for ultralong lifespan (1600 h) at a current density of 1 mA cm -2 in symmetric Li/Li cell. Furthermore, outstanding rate capability and long-term cycling performance (78.8% capacity retention after 500 cycles under 2 C) are obtained in full cells when coupled with Li 4 Ti 5 O 12 (LTO) cathodes, indicating a promising potential for practical application. Moreover, this work demonstrates that using a new lithiophilic material, V 2 O 5 , should be an effective method to construct high stable 3D Li metal anode for Li metal battery.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Enhancing microsegregation during rapid directional solidification through ternary microalloying

The nano-cellular dendritic microstructure formed during rapid directional solidification in powder bed fusion additive manufacturing creates unique properties such as simultaneous improvement in strength and ductility. However, process control of microsegregation features remains challenging due to low sensitivity of critical solidification mechanisms to process parameters. This study leverages microalloying to achieve large changes in dendrite composition, microstructure, and interdendritic zone width during laser powder bed fusion without modifying process parameters. CALPHAD simulations predict that the addition of Zr significantly steepens the solidus line of the dilute Cu-Cr alloy system, leading to enhanced Cr rejection into the melt and greater than 95% reduction in solubility of Cr in the solidified Cu matrix. Experimental validation using time-of-flight secondary ion mass spectrometry and Kelvin probe force microscopy reveals that the ternary alloy containing 0.01 wt% Zr exhibited wider interdendritic regions compared to the binary, a significantly higher number of Cr-rich particles within interdendritic regions, near-complete ejection of oxygen impurities from the matrix, and greater nanoscale work function contrast. These features indicate more aggressive Cr segregation in the presence of Zr and a purer Cu matrix and provide a potentially robust method for engineering the nano-cellular dendritic solidification microstructure.

CALPHAD↗

Understanding the Influence of Li 7 La 3 Zr 2 O 12 Nanofibers on Critical Current Density and Coulombic Efficiency in Composite Polymer Electrolytes

Composite polymer electrolytes (CPEs)are attractive materials for solid-state lithium metal batteries, owing to their high ionic conductivity from ceramic ionic conductors and flexibility from polymer components. As with all lithium metal batteries, however, CPEs face the challenge of dendrite formation and propagation. Not only does this lower the critical current density (CCD) before cell shorting, but the uncontrolled growth of lithium deposits may limit Coulombic efficiency (CE) by creating dead lithium. Here, we present a fundamental study on how the ceramic components of CPEs influence these characteristics. CPE membranes based on poly-(ethylene oxide) and lithium bis-(trifluoro methane sulfonyl)-imide(PEO-LiTFSI) with Li 7 La 3 Zr 2 O 12 (LLZO) nanofibers were fabricated with industrially relevant roll-to-roll manufacturing techniques. Galvanostatic cycling with lithium symmetric cells shows that the CCD can be tripled by including 50 wt % LLZO, but half-cell cycling reveals that this comes at the cost of CE. Varying the LLZO loading shows that even a small amount of LLZO drastically lowers the CE, from 88% at 0 wt % LLZO to 77% at just 2 wt % LLZO. Mesoscale modeling reveals that the increase in CCD cannot be explained by an increase in the macroscopic or microscopic stiffness of the electrolyte; only the microstructure of the LLZO nanofibers in the PEO-LiTFSI matrix slows dendrite growth by presenting physical barriers that the dendrites must push or grow around. This tortuous lithium growth mechanism around the LLZO is corroborated with mass spectrometry imaging. In conclusion, this work highlights important elements to consider in the design of CPEs for high-efficiency lithium metal batteries.

36 MATERIALS SCIENCE↗