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At least 73 records · Page 4

Studies of Model Immiscible Systems

The objectives are to use model transparent monotectics to obtain fundamental information applicable to two-phase systems in general, to apply this understanding to materials of interest in the Microgravity Science and Applications program, and to interpret results of flight experimental involving monotectic alloys. A number of model immiscible systems are in use to study various aspects of two-phase behavior within the miscibility gap and during solidification. Particle growth, coalescence and particle motions are under investigation using a holographic microscopy system. The system is capable of working with particle densities up to 10 to the 7th power particles/cubic centimeters through a 100 micron depth and can resolve particles of the order of 2 to 3 micron in diameter throughout the entire cell volume. Particle size, distribution changes with respect to time and temperature are observable from sequential holograms. Initial experiments using diethylene glycol/ethyl salicylate (DEG/ES) have demonstrated the usefulness of the technique. The thermal system controls temperature to at least plus or minus 0.001 K over the course of an experiment. A time-lapse film, made from holograms, of a succinonitrile/water solution shows particle size and number distribution changes with time under isothermal conditions. The observations are consistent with Ostwald ripening theory.

Frazier, D. O.↗

Intern Designed Modules for Conducting Potential Microgravity Solidification Experiments Aboard the International Space Station

MMaJIC (Microgravity Materials Joining Investigation Chamber) is a modular experiment chamber for performing materials science investigations. MMaJIC was initially designed to provide a controlled and sealed test environment to accommodate a wide variety of soldering and brazing experiments. However, its modular cartridge design is well suited to easily conduct any number and variety of science experiments. SoLIDD (Solid Liquid Interface Directional Device) is an apparatus for conducting directional solidification experiments with low melting temperature alloys. It has capability for varying the sample’s temperature gradient and growth velocity thus ensuring microstructural development under controlled conditions. ICED-T (Interface Control Experiment with Directional Translation) is an apparatus that conducts directional solidification experiments of transparent materials such that direct observation/recording of the advancing solid/liquid interface can be made. Currently, it is a functional breadboard that consists of the components mounted to a surface that allows the sample to be placed in an upright position. Orientation of the experiment (solid on the bottom, liquid on top) is important during testing ground samples to maintain stability. Ultimately, the goal of MMaJIC, SoLIDD and ICED-T is to conduct successful ground tests and then be re-configured for eventual use by aboard the ISS.

McElderry, Justin↗

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↗

The Effect of Growth Rate on Interface Morphology

Since significantly different solidification structures of a given alloy can be obtained by varying experimental growth rates, it is desirable to understand the basic factors which control the formation and stability of these microstructures when conditions are altered. Directional solidification experiments are described and the results obtained in metallic and transparent organic systems are presented. Emphasis is on the characteristics of dendritic structures obtained under different solidification conditions. Specifically, the effect of the growth rate on the primary dendritic spacing, the secondary dendrite spacing, and the dendrite tip radius is discussed. It is shown that significant changes in the primary spacing are observed when a dendrite to cellular transition takes place at lower velocities. It is found that the primary cellular spacing is much smaller than the primary dendrite spacing so that a maximum in the primary spacing occurs as a function of velocity at the dendrite-cellular transition. A theoretical model is also described which quantitatively explains various microstructural features of dendritic and cellular structures.

Trivedi, R.↗

Characterization of High-Entropy Alloys for Accelerator Beam Window Applications

Particle production targets and accelerator beam windows receive millions of high-energy/intensity beam pulses throughout their service lifetime. For next-generation multi-MW accelerators, it is necessary for beam windows to be able to withstand higher levels of thermal shock and radiation damage, while also having good high-temperature mechanical properties. Novel High-Entropy Alloys (HEAs) that form a single-phase microstructure, have nanoscale precipitates, and are made from low-Z elements are good candidates for beam window materials. This is due to their high-temperature strength and high resistance to radiation-induced swelling and hardening, as well as their beam transparency, allowing for maximized particle production and a longer service lifetime.

Kidwell, Tristan [U. Chicago (main)] (ORCID:000900↗

Novel Directional Solidification of Hypermonotectic Alloys

There are many metal alloy systems that separate into two different liquids upon cooling from a higher temperature. Uniform microstructural development during solidification of these immiscible liquids on Earth is hampered by inherent density differences between the phases. Microgravity processing minimizes settling but segregation still occurs due to gravity independent wetting and coalescence phenomena. Experiments with the transparent organic, metal analogue, succinonitrile-glycerol system were conducted in conjunction with applied ultrasonic energy. The processing parameters associated with this technique have been evaluated in view of optimizing dispersion uniformity. Characterization of the experimental results in terms of an initial modeling effort will also be presented.

Grugel, Richard N.↗

Novel Directional Solidification of Hypermonotectic Alloys

There are many metal alloy systems that separate into two different liquids upon cooling from a higher temperature. Uniform microstructural development during solidification of these immiscible liquids on Earth is hampered by inherent density differences between the phases. Microgravity processing minimizes settling but segregation still occurs due to gravity independent wetting and coalescence phenomena. Experiments with the transparent organic, metal analogue, succinonitrile-glycerol system were conducted in conjunction with applied ultrasonic energy. The processing parameters associated with this technique have been evaluated in view of optimizing dispersion uniformity. Characterization of the experimental results in terms of an initial modeling effort will also be presented.

Grugel, R. N.↗

Particle Engulfment and Pushing By Solidifying Interfaces

The phenomenon of interaction of particles with solid-liquid interfaces (SLI) has been studied since the mid 1960's. While the original interest stemmed from geology applications (frost heaving in soil), researchers soon realized that fundamental understanding of particles behavior at solidifying interfaces might yield practical benefits in other fields, including metallurgy. In materials engineering the main issue is the location of particles with respect to grain boundaries at the end of solidification. Considerable experimental and theoretical research was lately focused on applications to metal matrix composites produced by casting or spray forming techniques, and on inclusion management in steel. Another application of particle SLI interaction is in the growing of Y1Ba2Cu3O(7-delta) (123) superconductor crystals from an undercooled liquid. The oxide melt contains Y2Ba1Cu1O5 (211) precipitates, which act as flux pinning sites. The experimental evidence on transparent organic materials, as well as the recent in situ observations on steel demonstrates that there exist a critical velocity of the planar SLI below which particles are pushed ahead of the interface, and above which particles are engulfment. The engulfment of a SiC particle in succinonitrile is exemplified. However, in most commercial alloys dendritic interfaces must be considered. Indeed, most data available on metallic alloys are on dendritic structures. The term engulfment is used to describe incorporation of a particle by a planar or cellular interface as a result of local interface perturbation, as opposed to entrapment that implies particle incorporation at cells or dendrites boundaries. During entrapment the particles are pushed in the intercellular or interdendritic regions and then captured when local solidification occurs. The physics of these two phenomena is fundamentally different.

Stefanescu, Doru M.↗

Binary Colloidal Alloy Test Conducted on Mir

Colloids are tiny (submicron) particles suspended in fluid. Paint, ink, and milk are examples of colloids found in everyday life. The Binary Colloidal Alloy Test (BCAT) is part of an extensive series of experiments planned to investigate the fundamental properties of colloids so that scientists can make colloids more useful for technological applications. Some of the colloids studied in BCAT are made of two different sized particles (binary colloidal alloys) that are very tiny, uniform plastic spheres. Under the proper conditions, these colloids can arrange themselves in a pattern to form crystals. These crystals may form the basis of new classes of light switches, displays, and optical devices. Windows made of liquid crystals are already in the marketplace. These windows change their appearance from transparent to opaque when a weak electric current is applied. In the future, if the colloidal crystals can be made to control the passage of light through them, such products could be made much more cheaply. These experiments require the microgravity environment of space because good quality crystals are difficult to produce on Earth because of sedimentation and convection in the fluid. The BCAT experiment hardware included two separate modules for two different experiments. The "Slow Growth" hardware consisted of a 35-mm camera with a 250- exposure photo film cartridge. The camera was aimed toward the sample module, which contained 10 separate colloid samples. A rack of small lights provided backlighting for the photographs. The BCAT hardware was launched on the shuttle and was operated aboard the Russian space station Mir by American astronauts John Blaha and David Wolf (launched September 1996 and returned January 1997; reflown September 1997 and returned January 1998). To begin the experiment, one of these astronauts would mix the samples to disperse the colloidal particles and break up any crystals that might have already formed. Once the samples were mixed and the experiment was powered on, the hardware operated autonomously, taking photos of the colloidal samples over a 90-day period.

Hoffmann, Monica I.↗

Zinc Alloys for the Fabrication of Semiconductor Devices

ZnBeO and ZnCdSeO alloys have been disclosed as materials for the improvement in performance, function, and capability of semiconductor devices. The alloys can be used alone or in combination to form active photonic layers that can emit over a range of wavelength values. Materials with both larger and smaller band gaps would allow for the fabrication of semiconductor heterostructures that have increased function in the ultraviolet (UV) region of the spectrum. ZnO is a wide band-gap material possessing good radiation-resistance properties. It is desirable to modify the energy band gap of ZnO to smaller values than that for ZnO and to larger values than that for ZnO for use in semiconductor devices. A material with band gap energy larger than that of ZnO would allow for the emission at shorter wavelengths for LED (light emitting diode) and LD (laser diode) devices, while a material with band gap energy smaller than that of ZnO would allow for emission at longer wavelengths for LED and LD devices. The amount of Be in the ZnBeO alloy system can be varied to increase the energy bandgap of ZnO to values larger than that of ZnO. The amount of Cd and Se in the ZnCdSeO alloy system can be varied to decrease the energy band gap of ZnO to values smaller than that of ZnO. Each alloy formed can be undoped or can be p-type doped using selected dopant elements, or can be n-type doped using selected dopant elements. The layers and structures formed with both the ZnBeO and ZnCdSeO semiconductor alloys - including undoped, p-type-doped, and n-type-doped types - can be used for fabricating photonic and electronic semiconductor devices for use in photonic and electronic applications. These devices can be used in LEDs, LDs, FETs (field effect transistors), PN junctions, PIN junctions, Schottky barrier diodes, UV detectors and transmitters, and transistors and transparent transistors. They also can be used in applications for lightemitting display, backlighting for displays, UV and visible transmitters and detectors, high-frequency radar, biomedical imaging, chemical compound identification, molecular identification and structure, gas sensors, imaging systems, and for the fundamental studies of atoms, molecules, gases, vapors, and solids.

Ryu, Yungryel↗

Development of composite structures in hypermonotectic alloys through the use of in-situ fibers

This study demonstrates how the otherwise detrimental surface wetting and coarsening in a metallic system can be put to advantage through the inclusion of aligned fibers which accrue the excess liquid II phase while passing through the range of the miscibility gap and, some lower temperature, uniformly incorporate it into the solid I plus liquid II matrix. This is initially shown through the utilization of a hypermonotectic succinonitrile-glycerol mixture, a transparent organic system which exhibits solidification behavior in a manner analogous to metals. Results are compared with the analogue study and both are reviewed in terms of relevant wetting theory and surface area considerations.

Grugel, R. N.↗

Novel Directional Solidification Processing of Hypermonotectic Alloys

Gravity driven separation precludes uniform microstructural development during controlled directional solidification (DS) processing of hypermonotectic alloys. It is well established that liquid/liquid suspensions, in which the respective components are immiscible and have significant density differences, can be established and maintained by utilizing ultrasound. A historical introduction to this work is presented with the intent of establishing the basis for applying the phenomena to promote microstructural uniformity during controlled directional solidification processing of immiscible mixtures. Experimental work based on transparent organics, as well as salt systems, will be presented in view of the processing parameters.

Grugel, Richard N.↗

Block Copolymer-Templated Synthesis of Fe–Ni–Co-Modified Nanoporous Alumina Films

Despite intense interest in the catalytic potential of transition metal oxide heterostructures, originating from their large surface area and tunable chemistry, the fabrication of well-defined multicomponent oxide coatings with controlled architectures remains challenging. Here, we demonstrate a simple and effective swelling-assisted sequential infiltration synthesis (SIS) strategy to fabricate hierarchically porous multicomponent metal-oxide electrocatalysts with tunable bimetallic composition. A combination of solution-based infiltration (SBI) of transition metals, iron (Fe), nickel (Ni), and cobalt (Co), into a block copolymer (PS73-b-P4VP28) template, followed by vapor-phase infiltration of alumina using sequential infiltration synthesis (SIS), was employed to synthesize porous, robust, conformal and transparent multicomponent metal-oxide coatings like Fe/AlO x , Fe+Ni/AlO x , and Fe+Co/AlO x . Electrochemical assessments for the oxygen evolution reaction (OER) in a 0.1 M KOH electrolyte demonstrated that the Fe+Ni/AlO x composite exhibited markedly superior catalytic activity, achieving an impressive onset potential of 1.41 V and a peak current density of 3.29 mA/cm 2 . This superior activity reflects the well-known synergistic effect of alloying transition metals with a trace of Fe, which facilitates OER kinetics. Overall, our approach offers a versatile and scalable path towards the design of stable and efficient catalysts with tunable nanostructures, opening new possibilities for a wide range of electrochemical energy applications.

conformal films↗

Crystal Growth in the SUBSA furnace in MSG: 2002 to 2022

In 2002, the investigation “Solidification Using a Baffle In Sealed Ampoules (SUBSA)” was the first investigation to utilize the Microgravity Science Glovebox (MSG) Facility on the International Space Station (ISS). The SUBSA furnace was designed for growth of indium antimonide. It features a transparent section, which allows a side view of the melt, the solid-liquid (SL) interface and the growing crystal. In 2002, four Te-doped and three Zn-doped InSb crystals were grown in microgravity. Subsequently, the SUBSA furnace was used in several materials science investigations, including growing the radiation detector materials, InI and Cs2LiYCl6:Ce from the melt and vapor phase (2017 to 2019) and “Brazing of Aluminum alloys in Space (BRAINS)”. A review of the SUBSA furnace features and parameters will be presented, including the design of the growth ampoules, charge preparation, and the procedures used to grow InSb (in 2002) and InI (in 2019).

Aleksandar Ostrogorsky↗

Crystal Growth in the SUBSA furnace at the International Space Station (ISS)

In 2002, our investigation Solidification Using a Baffle In Sealed Ampoules (SUBSA) was the first investigation to utilize the Microgravity Science Glovebox (MSG) Facility on the International Space Station (ISS). The SUBSA furnace was designed for growth of indium antimonide. It features a transparent section, which allows a side view of the melt, the solid-liquid (SL) interface and the growing crystal. In 2002, four Te- doped and three Zn-doped InSb crystals were grown in microgravity. Subsequently, the SUBSA furnace was used in several other materials science investigations, including growing the radiation detector materials InI and Cs2LiYCl6:Ce from the melt and vapor phase (2017 to 2019) and Brazing of Aluminum alloys in Space (BRAINS). A review of the SUBSA furnace features and parameters will be presented, including the design of the growth ampoules, charge preparation, and the procedures used to grow InSb (in 2002) and InI (in 2019).

A.G. Ostrogorsk↗

An Experimental and Mathematical Study to Evaluate the Role of Ultrasonic Energy in Promoting Microstructural Uniformity During Controlled Directional Solidification Processing

There are many commercially relevant metal and non-metal "alloy" systems that separate into two different liquids upon cooling from a higher temperature. Consequently during solidification processing the inherent density differences between the two liquid phases leads to rapid, gravity driven, separation and severe segregation, a factor that significantly compromises the desired material properties. Processing in a microgravity environment minimizes settling but segregation still occurs due to gravity independent wetting and coalescence phenomena. This presentation reports on experiments that utilized succinonitrile-glycerol mixtures, a transparent system that 1) separates into two liquids upon cooling and 2) is also well established as an analogue to solidification phenomena observed in metals. Segregation was significantly reduced when the mixtures were subjected to ultrasonic energy during directional solidification processing. The processing parameters introduced by this application have been evaluated in view of optimizing dispersion uniformity. The improvement is in good agreement with a novel model that 1) predicts the achievable size of the droplets as a function of applied ultrasonic energy and then 2) calculates their relative sinking velocity through the bulk liquid.

Grugel, R. N.↗

Molten Salt Corrosion Tests of Additively Manufactured Stainless Steel 316H

Molten salt reactors (MSRs) have drawn considerable interest due to their favorable safety features, high thermal efficiency, and compatibility with different fuel cycles. Yet, the success of MSRs hinges critically on the performance of structural materials to be used in these aggressive molten salt environments, where corrosion and material compatibility remain primary challenges to long-term reliability. Additively manufactured (AM) nuclear structural materials prompt the use of novel geometries and compositions to enhance material performance and reduce costs of constructing MSRs. The rapid solidification conditions inherent to AM processing impart distinctive microstructural features, including cellular sub-structures, dislocation densities, residual stress, and oxide inclusions, which can influence material performance in MSR components. While the mechanical properties of AM stainless steels have been widely studied, their corrosion behavior, particularly in molten salt environments, has received far less attention. Addressing these needs, the Advanced Materials and Manufacturing Technologies (AMMT) program provides a framework for systematically evaluating how unique microstructures produced by AM processes influence the performance of these materials in these demanding environments and for developing reproducible testing workflows that can support future code qualification efforts and standards development. Bridging this knowledge gap is essential for assessing the viability of AM alloys in MSRs and informing qualification strategies. A further challenge is the absence of standardized protocols for molten salt corrosion testing. Accordingly, this report provides an account of the corrosion evaluation of AM 316H stainless steel in NaCl 2 -MgCl 2 molten salt at 550 °C, with exposure times of 100 and 500 hours. It documents the experimental procedures implemented under the AMMT program, including salt preparation, exposure protocols, and post-test characterization methods, to establish reproducibility and transparency. Importantly, the study examines AM 316H samples in the as-fabricated condition, directly reflecting the surface state most relevant to engineering applications, and compares their behavior to machine-cut surfaces. Overall, preliminary evaluations have noted that surface conditions (e.g. morphology, contamination, etc.) have a noticeable impact on the corrosion resiliency. The impact of the corrosion is difficult to detect at 100h, unless, in the case of AM 316H, the specimen surface is decontaminated. After 500 h, as-fabricated surfaces of AM and wrought 316H display evidence of general versus preferential corrosion attack, respectively. Both AM and wrought 316H machine-cut surfaces exhibit a continuous Cr depletion zone, evident of general corrosion. While the estimated extent of corrosion appears within the same order of magnitude regardless of the surface condition, it is apparent that more predictable behavior is observed on machine-cut surfaces. Nonetheless, further investigation is necessary to fully elucidate the corrosion mechanism under these conditions.

36 - MATERIALS SCIENCE↗

Separation processes during binary monotectic alloy production

Observation of microgravity solidification processes indicates that outside of sedimentation, at least two other important effects can separate the phases: critical-point wetting and spreading; and thermal migration of second-phase droplets due to interfacial tension gradients. It is difficult to study these surface tension effects while in a unit gravity field. In order to investigate the processes occurring over a temperature range, i.e., between a consolute point and the monotectic temperature, it is necessary to use a low-gravity environment. The MSFC drop tube (and tower), the ballistic trajectory KC-135 airplane, and the Space Shuttle are ideal facilities to aid formation and testing of hypotheses. Much of the early work in this area focuses on transparent materials so that process dynamics may be studied by optical techniques such as photography for viewing macro-processes; holography for studying diffusional growth; spinodal decomposition and coalescence; ellipsometry for surface wetting and spreading effects; and interferometry and spectroscopy for small-scale spatial resolution of concentration profiles.

Frazier, D. O.↗