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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 253 records · Page 14

Assessment of Flow-Enhanced Electrochemical Sensor Testing and Deployments

The goal of our activities in FY24 was to enable advanced materials accountancy for molten salt reactors (MSRs) through the development and optimization of robust flow-enhanced electrochemical sensors (FEES) using a safeguards-focused sensor testing platform called the modular flow instrumentation testbed (MFIT). Flow-enhanced electrochemical sensors are a type of electroanalytical sensor that have been developed at Argonne National Laboratory to be installed directly into MSR flow conduits to make measurements of the salt composition. These sensors represent a significant improvement in capabilities compared to earlier electroanalytical sensors that instead can only be operated in quiescent conditions. Previous work has focused on testing of the FEES in flowing conditions provided by the MFIT to assess the accuracy and precision of the sensor measurements. This year, the FEES technical readiness was increased by (1) demonstrating the use of optimized sensor techniques to achieve measurements in very high-concentration MSR-relevant salts, (2) leveraging new multimodal sensors and automation approaches to reduce measurement uncertainties, and (3) fabricating and deploying sensors to industrial partners to improve their ability to make measurements in challenging environments. Additionally, we also ran the sensors during complex system operations involving combined flow and purification activities to demonstrate safeguards-relevant measurements during online processing for MSRs.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Contactless Calorimetry for Levitated Samples

Temperature and specific heat of hot sample measured with pyrometer in proposed experimental technique. Technique intended expecially for contactless calorimetry of such materials as undercooled molten alloys, samples of which must be levitated to prevent contamination and premature crystallization. Contactless calorimetry technique enables data to be taken over entire undercooling temperature range with only one sample. Technique proves valuable in study of undercooling because difference in specific heat between undercooled-liquid and crystalline phases at same temperature provides driving force to convert metastable undercooled phase to stable crystalline phase.

Lee, M. C.↗

Sample levitation and melt in microgravity

A system is described for maintaining a sample material in a molten state and away from the walls of a container in a microgravity environment, as in a space vehicle. A plurality of sources of electromagnetic radiation, such as of an infrared wavelength, are spaced about the object, with the total net electromagnetic radiation applied to the object being sufficient to maintain it in a molten state, and with the vector sum of the applied radiation being in a direction to maintain the sample close to a predetermined location away from the walls of a container surrounding the sample. For a processing system in a space vehicle that orbits the Earth, the net radiation vector is opposite the velocity of the orbiting vehicle.

Moynihan, Philip I.↗

Of drops and bubbles - The technology of space processing

It is possible to manipulate a large, molten mass of material, such as a glass, aboard an orbital platform using acoustic fields. Attention is presently given to the problem of bubble removal from such a melt; it is desirable to make small bubbles coalesce into larger ones through floating melt rotation, to create an artificial convective field in which the bubbles will move centripetally to the axis of rotation. Computer models of bubble migration have been developed in order to define the operational conditions required aboard such experiment platforms as the Space Shuttle Orbiter.

Subramanian, R. Shankar↗

Scaling analysis applied to the NORVEX code development and thermal energy flight experiment

A scaling analysis is used to study the dominant flow processes that occur in molten phase change material (PCM) under 1 g and microgravity conditions. Results of the scaling analysis are applied to the development of the NORVEX (NASA Oak Ridge Void Experiment) computer program and the preparation of the Thermal Energy Storage (TES) flight experiment. The NORVEX computer program which is being developed to predict melting and freezing with void formation in a 1 g or microgravity environment of the PCM is described. NORVEX predictions are compared with the scaling and similarity results. The approach to be used to validate NORVEX with TES flight data is also discussed. Similarity and scaling show that the inertial terms must be included as part of the momentum equation in either the 1 g or microgravity environment (a creeping flow assumption is invalid). A 10(exp -4) environment was found to be a suitable microgravity environment for the proposed PCM.

Skarda, J. Raymond Lee↗

Scaling analysis applied to the NORVEX code development and thermal energy flight experiment

A scaling analysis is used to study the dominant flow processes that occur in molten phase change material (PCM) under 1 g and microgravity conditions. Results of the scaling analysis are applied to the development of the NORVEX (NASA Oak Ridge Void Experiment) computer program and the preparation of the Thermal Energy Storage (TES) flight experiment. The NORVEX computer program which is being developed to predict melting and freezing with void formation in a 1 g or microgravity environment of the PCM is described. NORVEX predictions are compared with the scaling and similarity results. The approach to be used to validate NORVEX with TES flight data is also discussed. Similarity and scaling show that the inertial terms must be included as part of the momentum equation in either the 1 g or microgravity environment (a creeping flow assumption is invalid). A 10(exp -4) environment was found to be a suitable microgravity environment for the proposed PCM.

Skarda, J. R. L.↗

Was Martian mantle wet? A possible consequence of rapid core formation

Degassing of H2O in the planetary interior possibly plays an important role in the evolution of surface environment as well as geologic activity on the terrestrial planets. Mars may be such a planet that well preserves the materials and the geologic features directly related to early evolution of H2O. H2O content in the interior of proto-Mars during accretion and also core formation were investigated. Geodetic data shows that Mars has a dense core. The existence of iron-rich core on Mars may be also supported by the depletion of siderophile elements in SNC meteorites assuming that these samples came from Mars. Isotope systematics of these meteorites indicate that the core formation occurred very early, probably concurrently with Mars formation. Considering the kinetics of metal segregation from silicate, the melting of silicate is likely to precede the core formation. Once the core formation occurs, substantial amount of gravitational energy is released and thus the planetary interior is heated. This energy may be large enough to keep the silicate material in partially molten state along with the accretional heating. Under such circumstances, the silicate melt probably migrates to the surface. Early crustal formation, therefore, is also likely to be associated with the core formation.

Kuramoto, Kiyoshi↗

A thermodynamic approach to obtain materials properties for engineering applications

With the ever increases in the capabilities of computers for numerical computations, we are on the verge of using these tools to model manufacturing processes for improving the efficiency of these processes as well as the quality of the products. One such process is casting for the production of metals. However, in order to model metal casting processes in a meaningful way it is essential to have the basic properties of these materials in their molten state, solid state as well as in the mixed state of solid and liquid. Some of the properties needed may be considered as intrinsic such as the density, heat capacity or enthalpy of freezing of a pure metal, while others are not. For instance, the enthalpy of solidification of an alloy is not a defined thermodynamic quantity. Its value depends on the micro-segregation of the phases during the course of solidification. The objective of the present study is to present a thermodynamic approach to obtain some of the intrinsic properties and combining thermodynamics with kinetic models to estimate such quantities as the enthalpy of solidification of an alloy.

Chang, Y. Austin↗

A Noncontact Measurement Technique for the Density and Thermal Expansion Coefficient of Solid and Liquid Materials

A noncontact measurement technique for the density and the thermal expansion refractory materials in their molten as well as solid phases is presented. This technique is based on the video image processing of a levitated sample. Experiments were performed using the high-temperature electrostatic levitator (HTESL) at the Jet Propulsion Laboratory in which 2-3 mm diameter samples can be levitated, melted, and radiatively cooled in a vacuum. Due to the axisymmetric nature of the molten samples when levitated in the HTESL, a rather simple digital image analysis can be employed to accurately measure the volumetric change as a function of temperature. Density and the thermal expansion coefficient measurements were made on a pure nickel sample to test the accuracy of the technique in the temperature range of 1045-1565 C. The result for the liquid phase density can be expressed by p = 8.848 + (6.730 x 10(exp -4)) x T (degC) g/cu cm within 0.8% accuracy, and the corresponding thermal expansion coefficient can be expressed by Beta=(9.419 x 10(exp -5)) - (7.165 x 10(exp -9) x T (degC)/K within 0.2% accuracy.

Chung, Sang K.↗

Sample levitation and melt in microgravity

A system is described for maintaining a sample material in a molten state and away from the walls of a container in a microgravity environment, as in a space vehicle. A plurality of sources of electromagnetic radiation, such as an infrared wavelength, are spaced about the object, with the total net electromagnetic radiation applied to the object being sufficient to maintain it in a molten state, and with the vector sum of the applied radiation being in a direction to maintain the sample close to a predetermined location away from the walls of a container surrounding the sample. For a processing system in a space vehicle that orbits the Earth, the net radiation vector is opposite the velocity of the orbiting vehicle.

Moynihan, Philip I.↗

Accelerating effects of galvanic corrosion and dissimilar materials on the corrosion of 316H in NaCl-MgCl2 salt

Corrosion of materials presents a significant challenge for the long-term operation of molten salt reactors. This study aims to identify the most effective techniques for evaluating the corrosion performance of materials in molten salts, with a focus on the effects of galvanic corrosion and dissimilar materials. A reliable testing methodology for assessing material corrosion in molten chloride salts has been successfully developed. The corrosion of Alloy 316H in molten NaCl-MgCl2 salt was found to be significantly accelerated by galvanic corrosion. Additionally, the presence of dissimilar materials resulted in a slight increase in the corrosion rate of Alloy 316H in NaCl-MgCl2 salt. Microstructural characterization was utilized to understand the corrosion behavior of test samples under different conditions. Common trends observed across samples include chromium depletion and iron enrichment near corroded surfaces. Molybdenum enrichment along grain boundaries and corrosion surfaces was also frequently noted.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Low-Temperature Molten Salt Electrochemical CO 2 Upcycling for Advanced Energy Materials

One strategy for addressing the climate crisis caused by CO 2 emissions is to efficiently convert CO 2 to advanced materials suited for green and clean energy technology applications. Porous carbon is widely used as an advanced energy storage material because of its enhanced energy storage capabilities as an anode. Herein, we report electrochemical CO 2 upcycling to solid carbon with a controlled microstructure and porosity in a ternary molten carbonate melt at 450 °C. Controlling the electrochemical parameters (voltage, temperature, cathode material) enabled the conversion of CO 2 to porous carbon with a tunable morphology and porosity for the first time at such a low temperature. Additionally, a well-controlled morphology and porosity are beneficial for reversible energy storage. In fact, these carbon materials delivered high specific capacity, stable cycling performances, and exceptional rate capability even under extremely fast charging conditions when integrated as an anode in lithium-ion batteries (LIBs). In conclusion, the present approach not only demonstrated efficient upcycling of CO 2 into porous carbon suitable for enhanced energy storage but can also contribute to a clean and green energy technology that can reduce carbon emissions to achieve sustainable energy goals.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Tuning the Morphology and Electronic Properties of Single-Crystal LiNi 0.5 Mn 1.5 O 4-δ : Exploring the Influence of LiCl–KCl Molten Salt Flux Composition and Synthesis Temperature

Single-crystal materials have played a unique role in the development of high-performance cathode materials for Li batteries due to their favorable chemomechanical stability. The molten salt synthesis method has become one of the most prominent techniques used to synthesize single-crystal layered and spinel materials. In this work, the molten salt synthesis method is used as a technique to tune both the morphology and Mn 3+ content of high-voltage LiNi 0.5 Mn 1.5 O 4 (LNMO) cathodes. The resulting materials are thoroughly characterized by a suite of analytical techniques, including synchrotron X-ray core-level spectroscopy, which are sensitive to the material properties on multiple length scales. Furthermore, the multidimensional characterization allows us to build a materials library according to the molten salt phase diagram as well as to establish the relationship among synthesis, material properties, and battery performance. The results of this work show that the Mn 3+ content is primarily dependent on the synthesis temperature and increases as the temperature is increased. Additionally, the particle morphology is mostly dependent on the composition of the molten salt flux, which can be tailored to obtain well-defined octahedrons enclosed by (111) facets, plates with predominant ($11\tilde{2}$) facets, irregularly shaped particles, or mixtures of these. The electrochemical measurements indicate that the Mn 3+ content has a larger contribution to the battery performance of LNMO than do morphological characteristics and that a significant amount of Mn 3+ could become detrimental to the battery performance. However, with similar Mn 3+ contents, morphology still plays a role in influencing the battery cycle life and rate performance. The insights of molten salt synthesis parameters on the formation of LNMO, with deconvolution of the roles of Mn 3+ and morphology, are crucial to continuing studies in the rational design of LNMO cathode materials for high-energy Li batteries.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Rapid Screening of Liquid Metal Wetting for a Materials Compatibility Library

Wetting behavior of molten metals on solid substrates is a critical phenomenon influencing numerous industrial applications, including welding, anti-corrosion coatings, and metal additive manufacturing (AM). In particular, molten metal jetting (MMJ), an emerging AM technology, requires that the molten metal remain pinned at the nozzle exit. Thus, each new metal requires a specific nozzle material to ensure consistent droplet ejection and deposition, making it important to rapidly identify the appropriate wetting combinations. However, traditional measurements of wetting angles require expensive equipment and only allow one combination of materials to be investigated at a time which can be time consuming. This work introduces a rapid screening method based on sessile droplet experiments to evaluate wetting profiles across multiple metal–substrate combinations simultaneously. This study investigates the wetting interactions of molten Al alloy (Al4008), Cu, and Sn on various ceramic and metal substrates to identify optimal material combinations for MMJ nozzle designs. Results demonstrate that Al4008 achieves wetting on ceramic substrates such as AlN, TiO 2 , and SiC, with varying mechanisms including chemical reactions and weak surface interactions. Additionally, theoretical predictions regarding miscibility gaps and melting point differences were verified for Cu and Sn on refractory metals like Mo and W. Findings from this study contribute to the establishment of a materials compatibility library, enabling the selection of wetting/non-wetting combinations for stable MMJ operation. This resource not only advances MMJ technologies but also provides valuable insights for broader applications such as welding, coating, and printed electronics.

Materials science↗

Fatigue and Creep-Fatigue Evaluation of Alloy 709 at 760 and 816°C

A significant research and development effort is underway to support the qualification of Alloy 709 as a Class A construction material in the American Society of Mechanical Engineers (ASME) Boiler and Pressure Vessel Code, Section III, Division 5, High Temperature Reactors. This initiative includes a comprehensive Alloy 709 code qualification plan aimed at generating extensive material testing data crucial for compiling the code case data package. The data package is essential in establishing material-specific design parameters for Alloy 709 to be used as Section III, Division 5 Class A construction material for fast reactors, molten salt reactors and gas-cooled reactors. An ASME Section III, Division 5 material code case requires the evaluation of mechanical properties from a minimum of three commercial heats, covering anticipated compositional ranges. A key part of the data package involves fatigue and creep-fatigue testing at elevated temperatures, needed for developing the fatigue design curves and the damage envelope of the creep-fatigue interaction diagram (D-diagram). This paper summarizes the strain-controlled fatigue testing on three commercial heats of Alloy 709 at 760 and 816°C with strain ranges between 0.25% and 3%. The fatigue failure data are used to generate a preliminary fatigue design curve. Additionally, the creep-fatigue testing results at 816°C with tensile hold times of 10, 30, and 60 minutes are presented in support of developing the D-diagram for Alloy 709.

Wang, Yanli↗

In-Situ TEM Molten Salt Corrosion

Molten salt reactors (MSRs) offer a compelling pathway for next-generation nuclear energy, with advantages in thermal efficiency, inherent safety, and flexible fuel management. Yet, halide-based molten salts introduce significant materials challenges, particularly alloy corrosion. Alloy performance in these environments ultimately depends on understanding how corrosion initiates and progresses at the nanoscale, however most existing models rely on post-exposure characterization, leaving degradation mechanisms largely inferred rather than directly observed. NiCr alloys have garnered interest in MSRs applications as the Ni-based matrix provides strength and creep resistance, while Cr content offers oxidation resistance in air. However, NiCr corrosion resistance in chloride salts has proven poor due to preferential chromium dissolution, the formation of Cr-depleted pathways, and grain-boundary attack. This work aims to directly visualize corrosion of Ni-20Cr exposed to LiCl-KCl using in-situ Transmission Electron Microscopy (TEM) to capture real-time microstructural evolution during corrosion. Experiments will be performed at ~800 °C under controlled pressure conditions while utilizing Energy-Dispersive X-ray Spectroscopy (EDS) to analyze elemental redistribution. Observation of chromium depletion fronts, associated surface restructuring, and localized chloride enrichment are expected. Ultimately, this study is expected to provide a link between microscale processes and the macroscopic degradation behaviors relevant to MSR operation in advanced reactor environments. Simultaneously, this approach enables future in-situ investigations regarding alloy composition, salt chemistry, and their influence on corrosion pathways and long-term stability.?

36 - MATERIALS SCIENCE↗

Corrosion Testing Of Additively Manufactured Stainless Steel 316H In Molten Salt Environments

The development of a new ASTM standard for evaluating the corrosion resistance of additive manufactured (AM) stainless steel (SS) 316H in chloride molten salts is critical for the use of these materials in extreme environments such as molten salt reactors (MSRs). This report pertains to a work package of the Advaned Materials and Manufacturing Technologies (AMMT) developing a systematic methodology to link changes in AM fabrication parameters, namely surface finishing, porosity, microstructure, and chemical heterogeneity, to corrosion performance in NaCl-MgCl2 salt, a proposed secondary coolant for MSRs. During Fiscal Year 2024, Idaho National Laboratory investigators in the AMMT program, utilized SS316H bars, fabricated with laser bed powder fusion at Los Alamos National Laboratory, to establish and optimize the workflow for evaluating these process-to-performance relationships. Standard practices for specimen preparation were established using these specimens, with particular focus on descaling and sectioning methods that align with ASTM guidelines. A comprehensive experimental design for static corrosion testing was developed, with pre- and post-exposure analysis utilizing optical microscopy and scanning electron microscopy. So far standard descaling techniques were optimized, one static corrosion test was conducted on the LANL AM SS316H specimens, and pre- and post-corrosion practices were established. In addition, the work package yielded a review paper on corrosion testing gaps for AM materials in nuclear applications and submitted a proposal for a rapid-turnaround experiment to the Nuclear Science User Facilities Program to investigate the combined effects of proton irradiation and corrosion on AM SS316H. This work package establishes a foundation for evaluating processing-to-performance relationships for AM SS316H in harsh conditions, contributing to the safe and efficient design of components for next-generation nuclear reactors. The creation of a standardized methodology and the generation of relevant publications and future research pathways represent significant strides towards integrating AM materials into critical applications where corrosion resistance is paramount.

36 MATERIALS SCIENCE↗