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NASA NTRS1984

Directional solidification of flake and nodular cast iron during KC-135 low-g maneuvers

Alloys solidified in a low-gravity environment can, due to the elimination of sedimentation and convection, form unique and often desirable microstructures. One method of studying the effects of low-gravity (low-g) on alloy solidification was the use of the NASA KC-135 aircraft flying repetitive low-g maneuvers. Each maneuver gives from 20 to 30 seconds of low-g which is between about 0.1 and 0.001 gravity. A directional solidification furnace was used to study the behavior of off eutectic composition case irons in a low-g environment. The solidification interface of hypereutectic flake and spheroidal graphite case irons was slowly advanced through a rod sample, 5 mm in diameter. Controlled solidification was continued through a number of aircraft parabolas. The known solidification rate of the sample was then correlated with accelerometer data to determine the gravity level during solidification for any location of the sample. The thermal gradient and solidification rate were controlled independently. Samples run on the KC-135 aircraft exhibited bands of coarser graphite or of larger nodules usually corresponding to the regions solidified under low-g. Samples containing high phosphorous (used in order to determine the eutectic cell) exhibited larger eutectic cells in the low-g zone, followed by a band of coarser graphite.

Curreri, P. A.↗

NASA NTRS1986

Dendrite characteristics in directionally solidified Pb-8 pct Au and Pb-3 pct Pd alloys

The dendritic microstructure and solute compression profiles for Pb-8 pct Au and Pb-3 pct Pd alloy samples are examined. Two groups of models, the minimum undercooled dendrite tip model of Burden and Hunt (1974) and Laxmanan (1974, 1984) and marginal stability at the dendrite tip models of Trivedi (1980) and Laxmanan (1974) are used to predict growth behavior of the alloy samples. The experimentally observed dendrite tip radius, primary arm spacing, and liquid composition at the dendrite tip are compared with theoretical predictions. It is observed that the modified minimum undercooling dendrite tip model and both of the marginal stability models accurately predict dendritic behavior. It is concluded that quantitative comparison of the primary arm spacing measurements can not form the basis for distinguishing among the various dendrite growth models in a positive temperature gradient.

Tewari, S. N.↗

NASA NTRS2012

Contribution to "AIAA Aerospace Year in Review" article

The NASA Marshall Space Flight Center Microgravity Science Program is dedicated to promoting our understanding of materials processing by conducting relevant experiments in the microgravity environment and supporting related modeling efforts with the intent of improving ground-based practices. Currently funded investigations include research on dopant distribution and defect formation in semiconductors, microstructural development and transitions in dendritic casting alloys, coarsening phenomena, competition between thermal and kinetic phase formation, and the formation of glassy vs. crystalline material. NASA Microgravity Materials Science Principle Investigators are selected for funding either through a proposal in response to a NASA Research Announcement or by collaborating on a team that has successfully proposed to a foreign space agency research announcement. In the latter case, a US investigator can then apply to NASA for funding through an unsolicited proposal. The International Space Station (ISS) facilities used for the experimental investigations are provided primarily by partnering with foreign agencies and often US investigators are working as a part of a larger team studying a specific area of materials science. Facilities for conducting experiments aboard the ISS include the European Space Agency (ESA) Low Gradient Facility (LGF) and the Solidification and Quench (SQF) modular inserts to the Materials Research Rack/Materials Science Laboratory and are primarily used for controlled solidification studies. The French Space Agency (CNES) provided DECLIC facility allows direct observation of morphological development in transparent materials that solidify analogously to metals. The ESA provided Electro ]Magnetic Levitator (EML) is designed to levitate, melt and then cool samples in order to determine material properties, study nucleation behavior, and document phase transitions. Finally, the Microgravity Science Glovebox (MSG) serves as a onboard facility for supporting the hardware required to conduct a number of smaller, short-term investigations.

Grugel, Richard N.↗

DOE OSTI2024

The 650 °C Tensile Deformation of Graded IN718-René41 Superalloy Fabricated by Laser Blown-Powder Directed Energy Deposition

The microstructure and 650 °C tensile properties of a compositionally graded IN718-René41 (718-R41) superalloy fabricated by laser blown-powder directed energy deposition (DED-LB/M) are investigated to understand structure–property relationships and baseline tensile properties. Digital Image Correlation (DIC), in situ neutron diffraction, and conventional characterization techniques are performed to study the as-built and heat-treated states. The applied heat treatment generates static recrystallization and equiaxed grains in 718-rich compositions, while R41-rich compositions remain partially or un-recrystallized possibly influenced by a higher MC carbide fraction (>0.5%). The yield strengths of the 718 and R41 sections in the heat-treated state are comparable to wrought forms but the graded compositions show weakness due to unoptimized heat treatment. Diffraction elastic constants first decrease and then increase along the 718-R41 composition gradient, while a small difference is observed between the as-built and heat-treated states and γ, γ′ phases. Overall, the compositionally graded region shows a smooth transition in the elastic properties. Grain-level load transfer from the (220) to (200) grains shows compositional dependence, and qualitatively agrees with DIC-measured macroscopic yield strength. Within the (200) grains, the γ/γ′ phases deform elastically until the γ phase yields and afterwards, the γ′ phase takes load from the γ phase.

Huang, Shenyan (ORCID:0000000196528114)↗

DOE OSTI2025

Effects of Internal and External Heat Sources on Cladding Microstructure and Rupture Performance

In the event of a Loss of Coolant Accident (LOCA), the primary supply of cooling water for a nuclear reactor is lost, leading to a significant pressure differential across the cladding wall. Without adequate cooling, the fuel rods continue to heat as a result of fission reactions. Research at Oak Ridge National Laboratory’s (ORNL’s) Severe Accident Test Station (SATS) is currently focused on evaluating fuel cladding performance using an external infrared lamp as a heat source, whereas legacy testing primarily utilized an internal heating approach. While external heating may better simulate the effect of neighboring fuel rods heating a central rod, it may not accurately represent the internal heat absorption from the fuel during accident transients. The heating dynamics depend greatly on the fuel rod's position within the bundle and the reactor. To fully understand the implications of a LOCA event and assess the influence of internal heating on cladding performance, combined internal heating and pressurization capability was developed at ORNL. Tests were conducted to compare cladding segments heated internally (representing heat from the fuel within the rod) and externally (representing heat from adjacent fuel rods). The findings indicate that both internal and external heating result in comparable rupture temperatures during 5°C/s laboratory LOCA tests and also agree with legacy test data. Axial temperature gradients and internal heat source dispersal were found to significantly impact cladding deformation and rupture geometry. Clear modifications were outlined to further improve the capability with heating rates above 5°C/s.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

Effects of Internal and External Heat Sources on Cladding Microstructure and Rupture Performance

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2025

Texture Analysis of Inconel 718 with Different Modes During Single-Track Laser Surface Re-Melting

An in-depth understanding of the texture formation in melt pools allows for the modification of the surface layer microstructure and corresponding material properties, providing an opportunity to integrate laser surface re-melting into metal additive manufacturing. This study investigates crystallographic texture formation at different cooling rates in single melting tracks on the Inconel 718 (IN718) plate produced by laser surface re-melting. The cooling rate varies from 2.31 × 10 5 °C/s to 9.56 × 10 5 °C/s with the increase in scanning rates from 400 mm/s to 1200 mm/s, measured by recently developed real-time temperature monitoring of melt pools. Columnar grains are dominant, with distinct crystallographic textures forming in the melt pools. At a slower scanning speed, the keyhole mode shows three different textures forming at different depths (crystallographically layered structure), while, at a faster scanning speed, the conduction mode shows only random grain orientation. There are no pores/voids detected, and the columnar grain morphology and columnar grain width (8.6 μm to 12.4 μm) follow the analysis framework in terms of thermal gradient and solidification rate analysis. This implies that laser surface re-melting provides the potential to modify the surface structure from a random grain orientation to a crystallographically layered structure.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Transient behavior of oxide fuels with controlled microstructure and Cr2O3 additive

Abstract Microstructure and Cr 2 O 3 doping profoundly impact the thermal-mechanical properties and fracture of oxides fuels. It is a challenge to study the transient behavior of nuclear fuels under loss-of-coolant-event (LOCA). In this study, the crack behavior of UO 2 pellets with controlled grain structure and Cr 2 O 3 doping was tested with rapid power ramping (300−900 °C per min) mimicking a prototypical LOCA heating profile. Dense micron-sized UO 2 pellets display well-maintained integrity without cracking with the ramping up to 1500 °C at a heating rate of 8 °C per second. Fracture occurs in both pure and Cr 2 O 3 -doped dense nano-sized UO 2 pellets. The Cr 2 O 3 doped oxide fuel pellet with a larger grain size (~ 22.2 μm) displays the best performance under LOCA testing due to its highest thermal conductivity under high temperature. FEA calculations suggest a temperature gradient across the fuel pellet during transient testing, resulting in residual stress and cracking, which can be correlated with their thermal-mechanical properties.

Zhao, Dong (ORCID:0000000191377257)↗

NASA NTRS2003

Oxidation of Carbon Fibers in a Cracked Ceramic Matrix Composite Modeled as a Function of Temperature

The oxidation model simulates the oxidation of the reinforcing carbon fibers within a ceramic matrix composite material containing as-fabricated microcracks. The physics-based oxidation model uses theoretically and experimentally determined variables as input for the model. The model simulates the ingress of oxygen through microcracks into a two-dimensional plane within the composite material. Model input includes temperature, oxygen concentration, the reaction rate constant, the diffusion coefficient, and the crack opening width as a function of the mechanical and thermal loads. The model is run in an iterative process for a two-dimensional grid system in which oxygen diffuses through the porous and cracked regions of the material and reacts with carbon in short time steps. The model allows the local oxygen concentrations and carbon volumes from the edge to the interior of the composite to be determined over time. Oxidation damage predicted by the model was compared with that observed from microstructural analysis of experimentally tested composite material to validate the model for two temperatures of interest. When the model is run for low-temperature conditions, the kinetics are reaction controlled. Carbon and oxygen reactions occur relatively slowly. Therefore, oxygen can bypass the carbon near the outer edge and diffuse into the interior so that it saturates the entire composite at relatively high concentrations. The kinetics are limited by the reaction rate between carbon and oxygen. This results in an interior that has high local concentrations of oxygen and a similar amount of consumed carbon throughout the cross section. When the model is run for high-temperature conditions, the kinetics are diffusion controlled. Carbon and oxygen reactions occur very quickly. The carbon consumes oxygen as soon as it is supplied. The kinetics are limited by the relatively slow rate at which oxygen is supplied in comparison to the relatively fast rate at which carbon and oxygen reactions occur. This results in a sharp gradient in oxygen concentration from the edge where it is supplied to the nearest source of carbon, which is where the oxygen is quickly consumed. A moving reaction front is seen in which the outlaying carbon is consumed before the next inner layer of carbon begins to react.

Halbig, Michael C.↗

DOE OSTI2025

The effect of blue and infrared laser melting frequency on oxide morphology in 304L

Continuous Wave Laser Beam (LB) melting offers control over the localised heating and cooling of melt pools for welding, brazing, additive manufacturing and solidification. Research into laserliquid metal interactions has primarily focused on the heat and mass transport under large thermal gradients imposed by the localised melting conditions. Recent commercial availability of blue (450 nm) wavelength lasers has enabled the printing of material with poor IR (1064) nm attenuation like Cu. However, little research has been conducted into varying input laser frequency and scan rate at fixed absorption to understand the effects of laser light on surface oxide formation and the underlying liquid metal thermodynamic response. Here, this article conducts laser melting of 304L under Blue (450 nm) and Infrared (IR, 1064 nm) laser frequencies and examines their impact on laser oxide thickness, chemistry and coloration. We find that laser frequencies induce changes in the oxide layer thickness and chemistry that cannot be explained using conventional thermal absorption shifts and fluid dynamics. We suggest that light coupling may have thermodynamic implications for the chemical potential of the liquid metal, which may drive the observed phase behaviour. Identifying mechanisms for the tuning of the chemical potential via laser frequency control could enable the ability to control solidification microstructure and atomic ordering in laser welding and additive manufacturing processes.

304L↗

NASA NTRS1999

Gravitational Effects on the Morphology and Kinetics of Photodeposition of Polydiacetylene Thin Films From Monomer Solutions

The goal of this proposed work is to study gravitational effects on the photodeposition of polydiacetylene thin films from monomer solutions onto transparent substrates. Polydiacetylenes have been an extensively studied class of organic polymers because they exhibit many unusual and interesting properties, including electrical conductivity and optical nonlinearity. Their long polymeric chains render polydiacetylenes readily conducive to thin film formation, which is necessary for many applications. These applications require thin polydiacetylene films possessing uniform thicknesses, high purity, minimal inhomogeneities and defects (such as scattering centers), etc. Also, understanding and controlling the microstructure and morphology of the films is important for optimizing their electronic and optical properties. The lack of techniques for processing polydiacetylenes into such films has been the primary limitation to their commercial use. We have recently discovered a novel method for the formation of polydiacetylene thin films using photo-deposition from monomer solutions onto transparent substrates with UV light. This technique is very simple to carry out, and can yield films with superior quality to those produced by conventional methods. Furthermore, these films exhibit good third-order properties and are capable of waveguiding. We have been actively studying the chemistry of diacetylene polymerization in solution and the photo-deposition of polydiacetylene thin films from solution. It is well-known that gravitational factors such as buoyancy-driven convection and sedimentation can affect chemical and mass transport processes in solution. One important aspect of polydiacetylene thin film photodeposition in solution, relevant to microgravity science, is that heat generated by absorption of UV radiation induces thermal density gradients that under the influence of gravity, can cause fluid flows (buoyancy-driven convection). Additionally, changes in the chemical composition of the solution during polymerization may cause solutal convection. These fluid flows affect transport of material to and from the film surface and thereby affect the kinetics of the growth process. This manifests itself in the morphology of the resulting films; films grown under the influence of convection tend to have less uniform thicknesses, and can possess greater inhomogeneities and defects. Specifically, polydiacetylene films photodeposited from solution, when viewed under a microscope, exhibit very small particles of solid polymer which get transported by convection from the bulk solution to the surface of the growing film and become embedded. Even when carried out under conditions designed to minimize unstable density gradients (i.e., irradiating the solution from the top), some fluid flow still takes place (particles remain present in the films). It is also possible that defect nucleation may be occurring within the films or on the surface of the substrate; this, too, can be affected by convection (as is the case with crystal growth). Hence films grown in 1-g will, at best, still possess some defects. The objective of this proposal is to investigate, both in 1-g and in low-g, the effects of gravitational factors (primarily convection) on the dynamics of these processes, and on the quality, morphology, and properties of the films obtained.

Paley, Mark S.↗

DOE OSTI2025

Investigation of residual stress distribution in wire-arc directed energy deposited refractory molybdenum alloy utilizing numerical thermo-mechanical analysis and neutron diffraction method

Directed energy deposition (DED), a metal additive manufacturing (AM) technique, offers higher deposition rates and energy efficiency, making it suitable for fabricating components from refractory molybdenum alloys, such as molybdenum-titanium-zirconium (TZM). However, large thermal gradients and non-equilibrium thermal cycles in DED could generate high residual stress in the component, potentially deteriorating quality and performance. Thus, this study aims to investigate residual stress generation and its distribution in wire-arc DED of TZM thin-wall, utilizing thermo-mechanical analysis and high-fidelity neutron diffraction (ND) method. Two interpass temperatures (50°C and 200°C) have been considered to investigate their impact on residual stress formation. During experiments, in-situ thermal data has been recorded using thermocouples, which have been utilized for calibrating the thermal model. Thermocouple data shows a good agreement with the simulation results, having a difference of less than 10 %. Post-deposition part deformation has been observed, which is measured using a coordinate measuring machine, showing maximum values of 0.93 mm and 0.78 mm for interpass temperatures of 50°C and 200°C, respectively. Numerical predictions of distortion deviated by less than 15% from the experimental results. ND measurement and simulation results indicate that residual stress magnitude and evolution vary across the TZM deposits, revealing microstructural anisotropy in both conditions. Notably, lower interpass temperatures resulted in higher residual stresses, confirmed by experimental and simulation data. Further, this study demonstrated that an integrated experimental and thermo-mechanical analysis can potentially reveal the temperature history, part deformation, and residual stress formation in wire-arc DED TZM alloy.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Boride-based Ceramic Super-high Temperature Thermocouples in Harsh Environments (Final Scientific/Technical Report)

An electromotive force (emf) can be generated along a temperature gradient between the cold end and hot end of a thermoelectric material, termed the Seebeck effect. Based on the Seebeck effect, metallic alloys have been extensively employed to detect temperatures for centuries, named thermocouples. However, commercially available thermocouple alloys suffer from limitations, such as oxidation, chemical degradation, and poor long-term stability under high-temperature harsh environments. This DOE-funded project aimed to develop high-temperature, chemically tolerant thermocouples suitable for operation in extreme environments relevant to semiconducting thermoelectric materials. The research focused on boride-based semiconducting thermoelectric compounds as candidates for next-generation thermocouples with enhanced oxidation resistance, chemical stability, and thermal robustness under conditions representative of charcoal-fired electricity facilities. During the funded years, boride materials were synthesized using an arc-plasma technique under ambient air and argon atmospheres, enabling scalable and cost-effective production compared with conventional boride fabrication methods. The synthesized borides were processed into nanostructured powders, followed by consolidation into dense bulk materials using a spark plasma sintering (SPS) bottom-up approach. Comprehensive characterization was performed, including microstructural analysis, electrical transport measurements, and optical and thermal property evaluation. Both p-type and n-type boride electric legs were fabricated and integrated into boride-based thermocouples. The thermal and irradiation stabilities of the boride nanomaterials and bulk thermoelectric materials were systematically evaluated to assess suitability for long-term operation in harsh environments. Additionally, 12 students were broadly hands-on trained spanning the full research workflow, including word processing and technical editing (e.g., LATEX for manuscript and poster preparation), data collection and analysis (using Python and related libraries and hardware interfaces), sample preparation (including arc-plasma synthesis and spark plasma sintering), and advanced characterization techniques (such as X-ray diffraction, UV–vis spectroscopy, electron microscopy, differential thermal analysis (DTA), and Seebeck coefficient measurements, etc). Overall, this project demonstrated the feasibility of boride-based thermoelectric materials as durable high-temperature thermocouples, providing a promising pathway toward robust temperature sensing technologies aligned with DOE energy infrastructure and extreme-environment monitoring needs.

20 FOSSIL-FUELED POWER PLANTS↗

DOE OSTI2026

Structural uniformity and compositional homogeneity of solid-phase alloyed rod

Solid-phase processes have emerged as an alternative to fusion-based alloying to avoid coarse microstructures, undesirable phase formation, and high energy consumption. However, achieving uniform distribution of alloying elements during friction-based processing remains challenging due to highly heterogeneous thermomechanical conditions. This work evaluates the structural uniformity and compositional homogeneity of Al–Cu–Zn alloyed rods produced by friction extrusion (FE) and establishes the role of the rotational speed to feed rate ratio (N/V) on alloying effectiveness. A systematic matrix of FE experiments was conducted at constant extrusion ratio with N/V values ranging from 3.7 to 300. Compositional uniformity was assessed along the rod length (ICP-OES), in three dimensions (X-ray computed tomography), and at the microscale (SEM–EDS), supported by a gray-level co-occurrence matrix (GLCM)–based homogeneity metric. Smoothed particle hydrodynamics (SPH) simulations were used to reveal material flow and thermomechanical fields. Results show that N/V = 100 produces a high-shear mixing zone that eliminates the unmixed core and enables near-full dissolution and dispersion of Cu and Zn. At lower N/V, a laminar flow region persists at the rod center, causing segregation and large composition gradients. The combined experimental–computational analysis provides mechanistic insight into the transition from fragmented particle dispersion to thermomechanically assisted metallurgical mixing. This study establishes processing–structure relationships for solid-phase alloying and provides guidance for achieving homogenized compositions comparable to wrought alloys via rapid, scalable FE processing.

Aluminum↗

DOE OSTI2024

Evaluation of DED and LPBF Fe-based Alloys Process Application Envelopes based on Performance, Process Economics, Supply Chain Risks, and Reactor-specific Targeted Components

The U.S. Department of Energy (DOE), Office of Nuclear Energy (NE), Advanced Materials and Manufacturing Technologies (AMMT) program aims to develop extreme-environment materials solutions for use in the deployment of advanced nuclear reactors and the sustainment of the current fleet. To achieve this objective, a combination of experiment, a computational tool, and machine learning (ML) for the design of materials is adopted for the maturation of materials for nuclear technology. Through advanced manufacturing techniques such as laser powder bed fusion (LPBF) and laser powder direct energy deposition (LP-DED), components with complex geometries can be fabricated with reduced time and effort. Such advanced manufacturing methods can also provide the opportunity to improve materials performance through optimized microstructures and mechanical properties. However, existing engineering alloys are not always well suited for fabrication with additive manufacturing (AM), as their compositions have been tuned to optimize fabrication via conventional methods. Thus, similar alloys with modified compositions that are better suited for AM can be studied for improved performance. Over the past three years, the AMMT teams from Argonne National Laboratory (ANL) and Pacific Northwest National Laboratory (PNNL) studied various known Fe-based alloys by evaluating their initial printability using LPBF, and an AMMT-developed down-selection and decision matrix reduced the number of alloys to be studied from six to three in fiscal year (FY) 2024. Additionally, in FY 2024, for parallel evaluation, these three alloys were studied using LPDED. While LPBF is better for small- to medium-sized components with high detail and internal features, LP-DED combines a material feed system to place the powder onto the exact spot where the laser will melt the material. This AM method can be easily scaled to extremely large components and provides high build rate speeds compared to those of conventional LPBF systems. Additionally, DED is a better choice for complex geometries and compositional gradients.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

NASA NTRS1999

Containerless, Low-Gravity Undercooling of Ti-Ce Alloys in the MSFC Drop Tube

Previous tests of the classical nucleation theory as applied to liquid-liquid gap miscibility systems found a discrepancy between experiment and theory in the ability to undercool one of the liquids before the L1-L2 separation occurs. To model the initial separation process in a two-phase liquid mixture, different theoretical approaches, such as free-energy gradient and density gradient theories, have been put forth. If there is a large enough interaction between the critical liquid and the crucible, both models predict a wetting temperature (T(sub w)) above which the minority liquid perfectly wets and layers the crucible interface, but only on one side of the immiscibility dome. Materials with compositions on the other side of the dome will have simple surface adsorption by the minority liquid before bulk separation occurs when the coexistence (i.e., binoidal) line in reached. If the interaction between the critical liquid and the crucible were to decrease, T(sub w) would increase, eventually approaching the critical consolute temperature (T(sub cc)). If this situation occurs, then there could be large regions of the miscibility gap where non-perfect wetting conditions prevail resulting in droplets of L1 liquid at the surface having a non-zero contact angle. The resulting bulk structure will then depend on what happens on the surface and the subsequent processing conditions. In the past several decades, many experiments in space have been performed on liquid metal binary immiscible systems for the purpose of determining the effects that different crucibles may have on the wetting and separation process of the liquids. Potard performed experiments that showed different crucible materials could cause the majority phase to preferentially wet the container and thus produce a dispersed microstructure of the minority phase. Several other studies have been performed on immiscibles in a semi-container environment using an emulsion technique. Only one previous study was performed using completely containerless processing of immiscible metals and the results of that investigation are similar to some of the emulsion studies. In all the studies, surface wetting was attributed as the cause for the similar microstructures or the asymmetry in the ability to undercool the liquid below the binoidal on one side of the immiscibility dome. By removing the container completely from the separation process, it was proposed that the loss of the crucible/liquid interaction would produce a large shift in T(sub w) and thus change the wetting characteristics at the surface. By investigating various compositions across the miscibility gap, a change in the type and amount of liquid wetting at the surface of a containerless droplet should change the surface nucleating behavior of the droplet - whether it be the liquid-liquid wetting or the liquid-to-solid transition. Undercooling of the liquid into the metastable region should produce significant differences in the separation process and the microstructure upon solidification. In this study, we attempt to measure these transitions by monitoring the temperature of the sample by optical pyrometry. Microstructural analysis will be made to correlate with the degree of undercooling and the separation mechanisms involved.

Robinson, M. B.↗

NASA NTRS1999

In Situ Monitoring of Crystal Growth Using MEPHISTO, Mission STS 87-Program USMP-4: Experimental Analysis

This report summarizes the results of the In situ Monitoring of Crystal Growth Using MEPHISTO (Material por l'Etude des Phenomenes Interessant de la Solidification sur Terre et en Orbite) experiment on USMP-4. The report includes microstructural and compositional data obtained during the first year of the post flight analysis, as well as numerical simulation of the flight experiment. Additional analyses are being continued and will be reported in the near future. The experiments utilized MEPHISTO hardware to study the solidification and melting behavior of bismuth alloyed with 1 at% tin. The experiments involved repeated melting and solidification of three samples, each approximately 90 cm long and 6mm in diameter. Half of each sample also included a 2 mm. diameter growth capillary, to assist in the formation of single grain inside. One sample provided the Seebeck voltage generated during melting and freezing processes. Another one provided temperature data and Peltier pulsed demarcation of the interface shape for post flight analysis. The third sample provided resistance and velocity measurements, as well as additional thermal data. The third sample was also quenched at the end of the mission to preserve the interface composition for post flight determination. A total of more than 45cm of directionally solidified alloy were directionally solidified at the end of the flight for post mission structural and compositional characterization. Metallurgical analysis of the samples has shown that the interfacial kinetics play a key role in controlling the morphological stability of faceted alloys. Substantial differences were observed in the Seebeck signal between the ground-based experiments and the space-based experiments. The temperature gradient in the liquid for the ground-based experiments was also significantly lower than the temperature gradient in the liquid for the space-based experiments. Both of these observations indicate significant influence of liquid convection for the ground-based experiments.

Abbaschian, Reza↗

NASA NTRS2000

A New High Efficiency Segmented Thermoelectric Unicouple

To achieve high thermal-to-electric energy conversion efficiency, it is desirable to operate thermoelectric generator devices over large temperature gradients and also to maximize the thermoelectric performance of the materials used to build the devices. However, no single thermoelectric material is suitable for use over a very wide range of temperatures (approx. 300 - 1000 K). It is therefore necessary to use different materials in each temperature range where they possess optimum performance. This can be achieved in two ways: 1) multistage thermoelectric generators where each stage operates over a fixed temperature difference and is electrically insulated but thermally in contact with the other stages and 2) segmented generators where the p- and n-legs are formed of different segments joined in series. The concept of integrating new thermoelectric materials developed at the Jet Propulsion Laboratory (JPL) into a segmented thermoelectric generator has been presented in detail in earlier publications . This new generator is expected to operate over a 300-973 K temperature difference and will use novel segmented legs based on a combination of state-of-the-art thermoelectric materials and novel p-type Zn4Sb3, p-type CeFe4Sb12-based alloys and n-type CoSb3-based alloys. An increase in the conversion efficiency of about 60% is expected compared to conventional Bi2Te3- and PbTe-based generators. We present in this paper the latest experimental results from the bonding studies between the different segments of the p-legs, n-legs, and p-leg to n-leg interconnect. Evaluation of the bond quality was done by measuring the contact resistance across the joints as well as by detailed microstructure investigations to reveal any potential interdiffusion. Among the materials investigated as inter-layers between the different segments of the legs, Pd-Ag joining alloys have been found to provide mechanically stable and low electrical resistance bonds.

Caillat, T.↗