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Lithium Nucleation of Anode-Free Solid-State Batteries with a Dry Compressible Interlayer

Anode-free lithium batteries offer promising advantages, including increased energy density and the ability to address common mechanistic failures within the cell, thus increasing safety. One way that can make this possible is to control lithium nucleation. This could be achieved by reducing the overpotential required and implanting lithophilic nucleation sites in an anodic interlayer to aid in lithium ion transport and plating. The concept has been utilized in solid-state battery systems where electrolytes are solids with further improved safety and structural longevity. In this presentation, we discuss the use of a silver-holey graphene-based anodic interlayer that can be fabricated via direct dry compression without the use of solvent or binder. The addition of silver to the holey graphene matrix creates a route to lithium plating via a lower-energy intermediate. This idea is supported by the presence of a lithium-silver alloy that forms during the activation step. It is understood that the embedded silver acts as a nucleation site for lithium ions, thereby assisting in even plating. This control, combined with the added cushion of the holey graphene itself, can help reduce dendrite formation, ultimately increasing the safety and lifetime of the solid-state batteries.

Solid state batteries↗

NASA NTRS1984

Changes in solidified microstructures

The properties and casting behavior of metals are significantly affected by their cast structure. This structure is optimized by producing columnar versus equiaxed grains and coarse versus fine grains by controlling solidification conditions. The transition from columnar to equiaxed grains is favored by: constitutional supercooling with effective nucleation of free dendrites; melting off and transport of dendrite tips and arms; mechanical vibration; falling down of free dendrites from a chilled top surface; and induced flow in the solidifying structure by oscillation of rotation.

Wallace, J. F.↗

NASA NTRS1985

Structure-property characterization of rheocast and VADER processed IN-100 superalloy

Two recent solidification processes have been applied in the production of IN-100 nickel-base superalloy: rheocasting and vacuum arc double electrode remelting (VADER). A detailed microstructural examination has been made of the products of these two processes; associated tensile strength and fatigue crack propagation (FCP) rate at an elevated temperature were evaluated. In rheocasting, processing variables that have been evaluated include stirring speed, isothermal stirring time and volume fraction solid during isothermal stirring. VADER processed IN-100 was purchased from Special Metals Corp., New Hartford, NY. As-cast ingots were subjected to hot isostatic pressing (HIP) and heat treatment. Both rheocasting and VADER processed materials yield fine and equiaxed spherical structures, with reduced macrosegregation in comparison to ingot materials. The rheocast structures are discussed on the basis of the Vogel-Doherty-Cantor model of dendrite arm fragmentation. The rheocast ingots evaluated were superior in yield strength to both VADER and commercially cast IN-100 alloy. Rheocast and VADER ingots may have higher crack propagation resistance than P/M processed material.

Cheng, J. J. A.↗

NASA NTRS2015

Study of Stable Cathodes and Electrolytes for High Specific Density Lithium-Air Battery

Future NASA missions require high specific energy battery technologies, greater than 400 Wh/kg. Current NASA missions are using "state-of-the-art" (SOA) Li-ion batteries (LIB), which consist of a metal oxide cathode, a graphite anode and an organic electrolyte. NASA Glenn Research Center is currently studying the physical and electrochemical properties of the anode-electrolyte interface for ionic liquid based Li-air batteries. The voltage-time profiles for Pyr13FSI and Pyr14TFSI ionic liquids electrolytes studies on symmetric cells show low over-potentials and no dendritic lithium morphology. Cyclic voltammetry measurements indicate that these ionic liquids have a wide electrochemical window. As a continuation of this work, sp2 carbon cathode and these low flammability electrolytes were paired and the physical and electrochemical properties were studied in a Li-air battery system under an oxygen environment.

cathodes↗

NASA NTRS2003

Basic and Applied Materials Science Research Efforts at MSFC Germane to NASA Goals

Presently, a number of investigations are ongoing that blend basic research with engineering applications in support of NASA goals. These include (1) "Pore Formation and Mobility (PFMI) " An ISS Glovebox Investigation" NASA Selected Project - 400-34-3D; (2) "Interactions Between Rotating Bodies" Center Director's Discretionary Fund (CDDF) Project - 279-62-00-16; (3) "Molybdenum - Rhenium (Mo-Re) Alloys for Nuclear Fuel Containment" TD Collaboration - 800-11-02; (4) "Fabrication of Alumina - Metal Composites for Propulsion Components" ED Collaboration - 090-50-10; (5) "Radiation Shielding for Deep-Space Missions" SD Effort; (6) "Other Research". In brief, "Pore Formation and Mobility" is an experiment to be conducted in the ISS Microgravity Science Glovebox that will systematically investigate the development, movement, and interactions of bubbles (porosity) during the controlled directional solidification of a transparent material. In addition to promoting our general knowledge of porosity physics, this work will serve as a guide to future ISS experiments utilizing metal alloys. "Interactions Between Rotating Bodies" is a CDDF sponsored project that is critically examining, through theory and experiment, claims of "new" physics relating to gravity modification and electric field effects. "Molybdenum - Rhenium Alloys for Nuclear Fuel Containment" is a TD collaboration in support of nuclear propulsion. Mo-Re alloys are being evaluated and developed for nuclear fuel containment. "Fabrication of Alumina - Metal Composites for Propulsion Components" is an ED collaboration with the intent of increasing strength and decreasing weight of metal engine components through the incorporation of nanometer-sized alumina fibers. "Radiation Shielding for Deep-Space Missions" is an SD effort aimed at minimizing the health risk from radiation to human space voyagers; work to date has been primarily programmatic but experiments to develop hydrogen-rich materials for shielding are planned. "Other Research" includes: BUNDLE (Bridgman Unidirectional Dendrite in a Liquid Experiment) activities (primarily crucible development), vibrational float-zone processing (with Vanderbilt University), use of ultrasonics in materials processing (with UAH), rotational effects on microstructural development, and application of magnetic fields for mixing.

Source record↗

NASA NTRS1991

Buoyancy effects of a growing, isolated dendrite

The buoyancy effect of a growing isolated dendrite on the solidification process in the undercooling liquid material was investigated by developing an analytic solution to the growth/convection problem in powers of a buoyancy parameter G. The solution depends on the Prandtl number P and the Stefan number S (undercooling) for the local velocity and thermal fields and also the buoyant alteration of the interface shape. Results suggest that buoyancy effect for metals (low P) may be qualitatively different from that for organics (high P).

Canright, D.↗

NASA NTRS1996

Development and Processing of Nickel Aluminide-Carbide Alloys

With the upper temperature limit of the Ni-based superalloys attained, a new class of materials is required. Intermetallics appear as likely candidates because of their attractive physical properties. With a relatively low density, high thermal conductivity, excellent oxidation resistance, high melting point, and simple crystal structure, nickel aluminide (NiAl) appears to be a potential candidate. However, NiAl is limited in structural applications due to its low room temperature fracture toughness and poor elevated temperature strength. One approach to improving these properties has been through the application of eutectic composites. Researchers have shown that containerless directional solidification of NiAl-based eutectic alloys can provide improvement in both the creep strength and fracture toughness. Although these systems have shown improvements in the mechanical properties, the presence of refractory metals increases the density significantly in some alloys. Lower density systems, such as the carbides, nitrides, and borides, may provide NiAl-based eutectic structure. With little or no information available on these systems, experimental investigation is required. The objective of this research was to locate and develop NiAl-carbide eutectic alloys. Exploratory arc-melts were performed in NiAl-refractory metal-C systems. Refractory metal systems investigated included Co, Cr, Fe, Hf, Mo, Nb, Ta, Ti, W, and Zr. Systems containing carbides with excellent stability (i.e.,HfC, NbC, TaC, TiC, and ZrC) produced large blocky cubic carbides in an NiAl matrix. The carbides appeared to have formed in the liquid state and were randomly distributed throughout the polycrystalline NiAl. The Co, Cr, Fe, Mo, and W systems contained NiAl dendrites with a two-phase interdendritic microconstituent present. Of these systems, the NiAl-Mo-C system had the most promising microstructure for in-situ composites. Three processing techniques were used to evaluate the NiAl-Mo-C system: arc-melting, slow cooling, and containerless directional solidification. Arc-melting provided a wide range of compositions in an economical and simple fashion. The slow cooled ingots provided larger ingots and slower cooling rates than arc-melting. Directional solidification was used to produce in-situ composites consisting of NiAl reinforced with molybdenum carbides.

Newport, Timothy Scott↗

NASA NTRS2019

In Situ Observation of Growth Dynamics in DECLIC Directional Solidification Insert Onboard ISS: DSI-R Flight Campaign

The study of solidification microstructure formation is of utmost importance for materials design and processing, as solid-liquid interface patterns largely govern mechanical and physical properties. Pattern selection occurs under dynamic conditions of growth in which the initial morphological instability evolves nonlinearly and undergoes a reorganization process. The dynamic and nonlinear nature of this instability renders in situ observation of the interface an invaluable tool to gain knowledge on the time-evolution of the interface pattern. Transparent organic analogs, which solidify like metallic alloys, allow direct visualization of interface dynamics. Extensive ground-based studies of both metallic and organic bulk samples have established the presence of significant convection during solidification processes that alters the formation of interfacial microstructures. A reduced-gravity environment is therefore mandatory for fluid flow elimination in bulk samples. In the framework of the CNES project MISOL3D (MIcrostrutures de SOLidification 3D) and the NASA projects DSIP (Dynamical Selection of 3D Interface Patterns), SPADES (SPAtiotemporal Evolution of three-dimensional DEndritic array Structures) and CAMUS (ComputAtional Studies of MicrostrUcture Formation During Alloy Solidification in Microgravity), we participated in the development of the Directional Solidification Insert (DSI) of the DEvice for the study of Critical Liquids and Crystallization (DECLIC). The DECLIC-DSI is dedicated to in situ and real-time characterization of solid-liquid interface patterns during directional solidification of transparent alloys in diffusive transport regime. Between April 2010 and March 2011, the first ISS campaign (DSI) explored the entire range of microstructures resulting in unprecedented observations. A second campaign (DSI-R), performed between October 2017 and December 2018, in which the insert contained an alloy of higher solute concentration, allowed to complete the benchmark database. The increase of solute concentration resulted in well-developed dendritic patterns at lower velocities (lower interface curvature and larger tip radius). The microstructure resulting from dendritic growth is dominant in metallurgy so that it is fundamental to understand the mechanisms of its formation. The main aims of this experimental campaign are to understand: the mechanisms of the cell to dendrite transition, the fundamental mechanisms of sidebranching formation, the dependence of dendrite tip shapes on growth conditions, the interaction of primary array and secondary sidebranches, and the influence of subgrain boundaries on the spatiotemporal organization of the array structure. Preparation, analysis and interpretation of the experiments performed onboard ISS are considerably enhanced by experiments performed on ground using thin-samples (Pr. Trivedi’s group) and phase-field simulations of microstructure formation in a diffuse growth regime (Pr. Karma’s group). In this summary, we will present an initial assessment of the results obtained during the DSI-R campaign. Nomenclature Vp: pulling velocity G: thermal gradient L: solidified length rtip: tip curvature radius Acronyms/Abbreviations CADMOS: Centre d'Aide au Développement des activités en Micro-pesanteur et des Opérations Spatiales CNES: Centre National d’Études Spatiales DECLIC: Device for the study of Critical LIquids and Crystallization DSI: Directional Solidification Insert DSI-R: Directional Solidification Insert - Refurbish ISS: International Space Station NASA: National Aeronautics and Space Administration PF: phase-field SCN: Succinonitrile 3D: three-dimensional

Mota, F.L.↗

NASA NTRS1984

The potential for bulk undercooling as an industrial process

The main focus is on solidification occurring in highly supercooled melts. Solidification rates in such melts are extremely high, an attractive feature from a commercial standpoint. Thus, the reported growth velocities for pure Ni and Co dendrites at a supercooling of 175 K are in excess of 180 km/hr. Rapidly quenched crystalline alloys produced by various atomization processes (e.g., centrifugal atomization or inert gas atomization) or melt spinning are examples of solidification processes, currently being intensively explored commercially, wherein extremely high solidification rates are achieved. Estimated dendrite tip growth rates are about 2 km/hr in a binary Al-4.5 wt % alloy, with a heat transfer coefficient of 6.4x10 sub 5 w/sq cm K or 15 cal/cu cm sK. In the limit, when the solidification rate exceeds a critical value, a glassy microstructure is obtained even in highly alloyed melts, which under normal conditions would solidity to form one or more crystalline phases. Glassy metals, also called metallic glasses, are candidate materials for distribution transformers because of their very low energy losses and are also being used in brazing and soldering applications.

Laxmanan, V.↗

NASA NTRS2000

Particle Engulfment and Pushing Micro-Gravity Experiments and Mathematical Modeling

The phenomenon of interaction of particles with solid-liquid interfaces that results in particle engulfment or pushing (PEP) has been Studied since mid 1960's. While the original interest stemmed from geology applications (frost heaving in soil), it was recognized early that understanding particle behavior at solidifying interfaces mi ht yield 9 practical benefits in other fields. In metallurgical applications the issue is the location of particles with respect to grain boundaries at the end of solidification. Considerable amount of experimental and theoretical research was lately focused on applications to metal matrix composites produced by casting; or spray forming techniques. Another application of PEP is in the growing of Y1Ba2CU3O7-delta(123) superconductor crystals from an undercooled liquid. The oxide melt contains Y2Ba1CU1O5 (211) precipitates, which act as flux pinning sites. The paper presents results of PEP micro-gravity research performed by the authors on two shuttle missions using metallic and polymeric materials. In addition. a discussion on the theoretical aspects of the physics of PEP is offered. Analytical and numerical models for planar solidification interfaces developed by the authors are used to explain the experimental results. Shortcomings of steady-state models are emphasized. A numerical model that includes the effect of the solutal field and of natural convection is introduced. A discussion of phenomena associated with dendritic solidification based on experimental observations is also offered. A mechanism of engulfment is proposed.

Stefanescu, Doru M.↗

NASA NTRS2002

Biosensors for Real-Time Monitoring of Radiation-Induced Biologic Effects in Space

This proposal seeks to develop cellular biosensors based on dendritic polymers. Nanoscale polymer structures less than 20 nm in diameter will be used as the basis of the sensor/actuators. The structures will be designed to target into specific cells of an astronaut and be able to monitor health issues such as the exposure to radiation or infectious agents. Multiple components can be assembled on the polymers including target directors, analytical devices (such as molecular probes), magnetic particles and metals, and imaging agents. The design and assembly of these devices has been pioneered at the Center for Biologic Nanotechnology in the University of Michigan. These molecules would also be able to administer therapeutics in response to the needs of the astronaut, and act as actuators to remotely manipulate an astronaut as necessary to ensure their safety. The reporting will be accomplished either through fluorescence signal monitoring, with the use of multispectral analysis for signal interpretation, or through functional MRI. These nanosensors coupled to NEMS devices could facilitate the success and increase the safety of extended space flight.

Baker, James R., Jr.↗

NASA NTRS1974

Metallographic study of metallic fragment of lunar surface material

A high precision investigation of a metallic fragment from the lunar material returned by the Soviet Luna 16 automatic station revealed three characteristic temperature intervals with different kinetics of solid solution decomposition. The following were found in the structure of the iron-nickel-cobalt alloy: (1) delta-phase and alpha-ferrite of diffusional, displacement origin in the grain boundary and acicular forms; and (2) martensite of isothermal and athermal nature, acicular, lamellar, massive, and dendritic. The diversity of the shapes of structural constituents is associated with the effect on their formation of elastic distortions and various mechanisms of deformation relaxation processes.

Mints, R. I.↗

NASA NTRS1979

Phase 2 of the array automated assembly task for the low cost solar array project

The process sequence for the fabrication of dendritic web silicon into solar panels was modified to include aluminum back surface field formation. Plasma etching was found to be a feasible technique for pre-diffusion cleaning of the web. Several contacting systems were studied. The total plated Pd-Ni system was not compatible with the process sequence; however, the evaporated TiPd-electroplated Cu system was shown stable under life testing. Ultrasonic bonding parameters were determined for various interconnect and contact metals but the yield of the process was not sufficiently high to use for module fabrication at this time. Over 400 solar cells were fabricated according to the modified sequence. No sub-process incompatibility was seen. These cells were used to fabricate four demonstration modules. A cost analysis of the modified process sequence resulted in a selling price of $0.75/peak watt.

Campbell, R. B.↗

NASA NTRS2013

Castable Amorphous Metal Mirrors and Mirror Assemblies

A revolutionary way to produce a mirror and mirror assembly is to cast the entire part at once from a metal alloy that combines all of the desired features into the final part: optical smoothness, curvature, flexures, tabs, isogrids, low CTE, and toughness. In this work, it has been demonstrated that castable mirrors are possible using bulk metallic glasses (BMGs, also called amorphous metals) and BMG matrix composites (BMGMCs). These novel alloys have all of the desired mechanical and thermal properties to fabricate an entire mirror assembly without machining, bonding, brazing, welding, or epoxy. BMGs are multi-component metal alloys that have been cooled in such a manner as to avoid crystallization leading to an amorphous (non-crystalline) microstructure. This lack of crystal structure and the fact that these alloys are glasses, leads to a wide assortment of mechanical and thermal properties that are unlike those observed in crystalline metals. Among these are high yield strength, carbide-like hardness, low melting temperatures (making them castable like aluminum), a thermoplastic processing region (for improving smoothness), low stiffness, high strength-to-weight ratios, relatively low CTE, density similar to titanium alloys, high elasticity and ultra-smooth cast parts (as low as 0.2-nm surface roughness has been demonstrated in cast BMGs). BMGMCs are composite alloys that consist of a BMG matrix with crystalline dendrites embedded throughout. BMGMCs are used to overcome the typically brittle failure observed in monolithic BMGs by adding a soft phase that arrests the formation of cracks in the BMG matrix. In some cases, BMGMCs offer superior castability, toughness, and fatigue resistance, if not as good a surface finish as BMGs. This work has demonstrated that BMGs and BMGMCs can be cast into prototype mirrors and mirror assemblies without difficulty.

Hofmann, Douglas C.↗

NASA NTRS1983

Supercooling and structure of levitation melted Fe-Ni alloys

A study has been made of the effect of supercooling, quenching rate, growth inhibitors, and grain refiners on the structure of levitation-melted Fe- 25 pct Ni alloys. A combination of three morphologies, dendritic, spherical, and mixed dendritic and spherical, is observed in samples superheated or supercooled by less than 175 K. At larger supercooling, however, only the spherical morphology is observed. The grain size and the grain boundary shape are found to be strongly dependent on the subgrain morphology but not on the quenching temperature. Considerable grain growth is evident in samples with spherical and mixed morphologies but not in the dendriitic samples. The average cooling rates during solidification and the heat transfer coefficients at the metal-quenching medium boundary are calculated. For samples solidified in water, molten lead, and ceramic molds, the heat transfer coefficients are 0.41, 0.52, and 0.15 w/sq cm, respectively.

Abbaschian, G. J.↗

NASA NTRS1984

Characterization of macrosegregation in ESR IN-718

Aspects of macrosegregation theory, such as dendrite arm spacing, pool profile and mushy zone depth are beneficial to developing consumable melting process for Ion Nickel IN-718, Electro-Slag Refining, especially ESR. Aspects of microsegregation theory, such as correlation of dendrite arm spacing with heat transfer mechanisms and local solidification time, are used to minimize remnant dendritism in both ESR and Vacuum Arc Remelting VAR IN-718. Specifically, ESR IN-718 must be optimized by developing practices which maximize ingot cooling rate and minimize the steepness of the solidus and liquidus isotherms. The knowledge concerning macrosegregation in consumable melted IN-718 is in the form of correlations. Since the isotherm steepness is undoubtedly involved, investigations which include a microgravity environment might separate microsegregation effects from macrosegregation effects. Accounting for the effects of gravity and density differences between the metal pool and the interdendritic fluid, in combination with the pool and mushy zone profiles, can lead to improved melting solidification practices for IN-718, and allow prediction of macrosegregation tendency to be incorporated into high temperature alloy design.

Domingue, J. A.↗

NASA NTRS1985

Metals Electroprocessing in Molten Salts

The present study seeks to explain the poor quality of solid electrodeposits in molten salts through a consideration of the effects of fluid flow of the electrolyte. Transparent cells allow observation of electrolyte circulation by a laser schlieren optical technique during the electrodeposition of solid zinc from the molten salt electrolyte, ZnCl2 - LiCl-KCl. Experimental variables are current, density, electrolyte composition, and cell geometry. Based on the results of earlier electrodeposition studies as well as reports in the literature, these parameters are identified as having the primary influence on cell performance and deposit quality. Experiments are conducted to measure the fluid flow patterns and the electrochemical cell characteristics, and to correlate this information with the morphology of the solid electrodeposit produced. Specifically, cell voltage, cell current, characteristic time for dendrite evolution, and dendrite growth directions are noted. Their relationship to electrolyte flow patterns and the morphology of the resulting electrodeposit are derived. Results to date indicate that laser schlieren imaging is capable of revealing fluid flow patterns in a molten salt electrolyte.

Sadoway, D. R.↗

NASA NTRS2002

Triggered Nucleation in Ni60Nb40 Using an Electrostatic Levitator

External triggering of nucleation in an undercooled liquid metal has been performed for the first time in an electrostatically levitated sample of undercooled eutectic Ni60Nb40. With the Electrostatic Levitator (ESL) facility at NASA/MSFC, NiNb alloys were externally nucleated at various undercooling increments. Observation of the resulting microstructure indicates that only one nucleation site is initiated with a trigger if the undercooling is sufficiently high. Well-defined transition zones exist in all the samples. An "anomalous" fine structured eutectic is initially grown from the nucleation point into the undercooled liquid followed by an unexpected variable width transition zone leading to a coarse structured region of dendrites. Our study tends to corroborate the findings of other studies on highly undercooled eutectics regarding a coupled growth zone within which the lamellar structure is formed and outside of which the anomalous is found.

Rathz, T.↗