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Smart Refractory Sensors Development for Corrosion and Erosion Monitoring in High Temperature Systems

To optimize the operation and functioning of high temperature systems such as slagging gasifiers, coal boilers and glass/steel melters, it is important to monitor corrosion and erosion of refractory used in such systems. Corrosion test strategies are generally based on continuous gravimetric and chemical reactivity monitoring at operational temperatures (750°-1500°C). Both thermocouples and failure sensors and arrays would be useful to monitor the health of any refractory or coatings in these systems. Many of such type of sensors are installed into the systems through open access ports within the refractory; however, there are some disadvantages of this approach where corrosive/erosive gas and molten materials can penetrate and compromise the system. The current work presents the development and performance demonstration of smart refractory with embedded high temperature sensors such as thermocouples, thermistors, and various spallation/crack monitoring sensors, which may be used within a variety of refractory brick in different high temperature processes and applications. The main feature of this technology is that electroceramic based sensors are embedded into smart refractory without significantly impact to the intrinsic properties of the refractory. This technology circumvents the need to insert an isolated monolithic, stand-alone sensor into the refractory via an access port. This technological approach guarantees the integrity and the chemical stability of the materials used in the sensor fabrication within the harsh environment and does not introduce molten material (such as slag) penetration pathways within the refractory. One interesting and important aspect of this innovation is that these embedded sensors can be used to in situ monitoring processes such as chemical reactions and at the same time give information and a deeper understanding of the corrosion and erosion process of the refractory within the system. As stated above, the objective of our work is to develop high-temperature sensors composed of electroceramic materials that are chemically stable at high temperatures (750°-1500°C) and high pressures (up to 1000 psi) that can be used in monitoring corrosion and erosion process in refractory used in high energy systems. The high-temperature sensors investigated in this work were composed of various oxide composites directly embedded into the refractory oxides. The composites used for this work were synthesized by a mixed-oxide route. Metal oxides were inserted within a matrix material composed of refractory oxides (Al2O3, ZrO2, etc.). The physical and electrical properties were specifically manipulated by altering the level of percolation of the conductive species (metal oxides) within the refractory constituent (refractory oxide). Prior to the development of the high-temperature sensors, the oxides composites developed in this study were sintered up to 1600°C under oxidizing atmosphere in order to investigate densification, microstructural evolution, phase development, and their thermoelectrical performance as a function of the composition. The 4-point DC conductivity measurements were performed between 100°-1500°C. The sensors were fabricated from the composite materials by 3D-printing or screen-printing methods into the refractory brick during the consolidation process. An example of one of these embedded sensors consisted of an electroceramic-based thermocouple fabricated with two separate oxide composite compositions which were patterned to produce a couple within the interior of a refractory matrix. The thermocouple successfully displayed thermoelectric voltage trend (as a function of temperature), and the voltage was 220.0 mV around 1400 °C. Corrosion tests on the refractory embedded sensors were performed. To evaluate corrosion in the refractory brick an in-house glass composition was prepared and pressed into pellets and delivered into a pre-cut cavity in the brick. Corrosion experiments results showed the glass penetrated the brick over a 90 h period, and the penetration of the glass through the brick could be monitored by both an amperometric and voltametric based sensor. With this experiment, it was demonstrated that the embedded sensor could dynamically monitor the corrosion process.

20 FOSSIL-FUELED POWER PLANTS↗

A Dynamic Testing Approach for Particulate Erosion–Corrosion for Gas Turbine Coatings

Particle interactions in gas turbine engines can be multicomponent, complex phenomena leading to the degradation of thermal (TBCs) and environmental barrier coatings (EBCs) meant to protect engine components. Ingestion of particles into the engine can lead to recession of coatings due to particle erosion. Similarly, these same particles can become molten, adhere to coatings and result in thermochemical corrosion of coating materials. Particle erosion testing is often carried out where the particles are injected into a gas stream, accelerated within a nozzle, and impinge on sample. Conversely, most molten particle corrosion testing is often done in static laboratory furnaces, which does not capture the dynamic nature of deposition in application. Nevertheless, these damage mechanisms are often tested separately and no single standard exists to test both erosive and corrosive particle interactions with coating materials under relevant operating conditions for gas turbine engines. Understanding the synergies of particle interactions in engines is crucial in determining operating lifetimes of potential coating materials. Such considerations emphasize the need for realistic approaches in standardizing particle interaction testing in combustion environments. The current study outlines initial efforts at NASA Glenn’s Erosion Burner Rig Facility in improving dynamic erosion/corrosion testing methods by assessing the durability of state-of-the-art (SOA) TBC material 7 wt.% yttria stabilized zirconia (7YSZ) as a function of particle deposition rate, burner temperature, and particle size. Calibration data to determine particle deposition rate will be presented, and mass and optical profilometry measurements were utilized to estimate mass/volume loss versus deposition per increment of particulate used over time. Electron microscopy analyses were then carried out to assess coating damage after testing.

TBC↗

A Dynamic Testing Approach for Particulate Erosion–Corrosion for Gas Turbine Coatings

Particle interactions in gas turbine engines can be multicomponent, complex phenomena leading to the degradation of thermal (TBCs) and environmental barrier coatings (EBCs) meant to protect engine components. Ingestion of particles into the engine can lead to recession of coatings due to particle erosion. Similarly, these same particles can become molten, adhere to coatings and result in thermochemical corrosion of coating materials. Particle erosion testing is often carried out where the particles are injected into a gas stream, accelerated within a nozzle, and impinge on sample. Conversely, most molten particle corrosion testing is often done in static laboratory furnaces, which does not capture the dynamic nature of deposition in application. Nevertheless, these damage mechanisms are often tested separately and no single standard exists to test both erosive and corrosive particle interactions with coating materials under relevant operating conditions for gas turbine engines. Understanding the synergies of particle interactions in engines is crucial in determining operating lifetimes of potential coating materials. Such considerations emphasize the need for realistic approaches in standardizing particle interaction testing in combustion environments. The current study outlines initial efforts at NASA Glenn’s Erosion Burner Rig Facility in improving dynamic erosion/corrosion testing methods by assessing the durability of state-of-the-art (SOA) TBC material 7 wt.% yttria stabilized zirconia (7YSZ) as a function of particle deposition rate, burner temperature, and particle size. Calibration data to determine particle deposition rate will be presented, and mass and optical profilometry measurements were utilized to estimate mass/volume loss versus deposition per increment of particulate used over time. Electron microscopy analyses were then carried out to assess coating damage after testing.

TBC↗

A Dynamic Testing Approach for Particulate Erosion–Corrosion for Gas Turbine Coatings

Particle interactions in gas turbine engines can be multicomponent, complex phenomena leading to the degradation of thermal (TBCs) and environmental barrier coatings (EBCs) meant to protect engine components. Ingestion of particles into the engine can lead to recession of coatings due to particle erosion. Similarly, these same particles can become molten, adhere to coatings and result in thermochemical corrosion of coating materials. Particle erosion testing is often carried out where the particles are injected into a gas stream, accelerated within a nozzle, and impinge on sample. Conversely, most molten particle corrosion testing is often done in static laboratory furnaces, which does not capture the dynamic nature of deposition in application. Nevertheless, these damage mechanisms are often tested separately and no single standard exists to test both erosive and corrosive particle interactions with coating materials under relevant operating conditions for gas turbine engines. Understanding the synergies of particle interactions in engines is crucial in determining operating lifetimes of potential coating materials. Such considerations emphasize the need for realistic approaches in standardizing particle interaction testing in combustion environments. The current study outlines initial efforts at NASA Glenn’s Erosion Burner Rig Facility in improving dynamic erosion/corrosion testing methods by assessing the durability of state-of-the-art (SOA) TBC material 7 wt.% yttria stabilized zirconia (7YSZ) as a function of particle deposition rate, burner temperature, and particle size. Calibration data to determine particle deposition rate will be presented, and mass and optical profilometry measurements were utilized to estimate mass/volume loss versus deposition per increment of particulate used over time. Electron microscopy analyses were then carried out to assess coating damage after testing.

burner rig↗

Computational and experimental analysis of structural and Thermophysical properties of LiX-KX (X = chloride, iodide, or bromide) molten salts

Molten salts containing lithium (Li) and potassium (K) halides, including chlorides (Cl), bromides (Br), and iodides (I), are pivotal in advanced technological applications including nuclear reactor technologies, thermal batteries, and industrial pyrochemical processes. Despite their significance, the availability of the temperature-dependent structural and thermophysical properties of these molten salts remain scarce. Here, this study addresses this knowledge gap by predicting and measuring the key properties such as coordination number, radial distribution function, density, heat capacity, and volumetric thermal expansion of molten LiI-KI, LiBr-KBr and LiCl-KCl eutectic mixtures. Utilizing ab initio molecular dynamics (AIMD) simulations, we predict these properties of LiX-KX (X=Br,I, Cl) across various temperatures, with chlorides as a benchmark. Experimental measurements using Archimedes methods and Differential Scanning Calorimetry validate the densities and heat capacities of these molten salts. Our comprehensive analysis of the structural and thermophysical properties provides critical insights into the behavior of these molten salts at various temperatures, enhancing the understanding necessary for their application in advanced technologies.

36 - MATERIALS SCIENCE↗

The molten salt tritium transport experiment: A pumped fluoride salt loop for hydrogen isotope experimentation

Molten salt reactors (MSRs) and fusion reactors propose to use molten salts as coolants and breeder blanket materials, respectively. Tritium, however, poses safety concerns in both reactor types due to its ability to permeate through reactor materials and potential for environmental release. This manuscript addresses the tritium transport phenomena in molten salts and presents the design and analysis of the Molten Salt Tritium Transport Experiment (MSTTE). MSTTE is a forced-convection fluoride salt loop intended to measure hydrogen isotope permeation through structural materials in a flowing salt system. In the first phase, MSTTE will use FLiNaK salt and deuterium as surrogates for FLiBe and tritium, with future plans to utilize tritium and FLiBe. MSTTE couples a Copenhagen Atomics pumped salt loop with an external test section that introduces hydrogen isotopes into the loop and measures transport phenomena. The Hydrogen Injection System (HIS) controls hydrogen isotope introduction into the molten salt loop. Here, the permeation test section measures the permeation rate through stainless steel tubing in contact with flowing salt. Computational fluid dynamics (CFD) analysis ensures fully developed salt flow in the permeation test section. MSTTE is modeled with MELCOR-TMAP to predict the permeation rate as a function of experimental variables such as source term, salt flow rate, and salt temperature. Results indicate that the source term is the only parameter with a significant effect on the permeation rate. Pressure drop analysis suggests that the loop should operate below 200 LPM to maintain a pressure drop below 200 kPa. Additionally, finite-element analysis assesses thermal stress during loop operation to ensure the experiment's safe design. MSTTE will provide semi-integral data on tritium transport phenomena in molten salts and serve as a testbed for advancing molten salt technology.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Hardness Prediction by Incorporating Heat Transfer and Molten Pool Fluid Flow in a Multi-pass, Multi-layer Weld for Onsite Repair of Grade 91 steel

Introduction: In the current fleet of fossil-fired power plants, creep strength enhanced ferritic steels (CSEF) are used to sustain the harsh service conditions. Enhanced properties of Grade 91 steel result from tempered martensite with a fine distribution of MX and M23C6 carbides. Grade 91 steel is subjected to onsite welding repair to remedy their degradation due to extreme service condition. Knowledge of weld repairability of these steels, such as as-welded hardness distribution, is essential to establishing sound repair procedures. Experimental trial and error tests can consume a lot of time as many welding variables need to be studied. For numerical modelling, most of the multi-pass multi-layer models are based on finite element method, which are limited to solve the heat conduction equation and ignore convective heat transfer due to melt flow. Moreover, the mesh has to be pre-built based on a known or assumed weld cross-section geometry. These finite element based models thus have limited predictive capability as defects are not considered and nugget size are pre-assumed. This research aims at developing a thermal and microstructure evolution model incorporating molten pool dynamics in a multi-pass multi-layer material deposition to predict the as-welded hardness distribution. Technical Approach: All the thermal, physical, and metallurgical properties of Grade 91 as a function of temperature are collected from the literature and inputted into the thermo-fluid model based on Flow-3D, a computational fluid dynamics software. A multi-pass, multi-layer material deposition is simulated where the melting of filler wire into the molten pool is directly considered based on the volume of fluid (VOF) method. The flow behaviour of the molten pool is used to understand the formation of deposition geometry and defects. The temperature profiles during the multi-pass, multi-layer welding are calculated. The results computed using the new model are compared against the experimental data of fusion zone geometry and thermal cycles. Hardness prediction in the heat-affected zone (HAZ) are made using Johnson-Mehl-Avrami (JMA) equation for solid-state phase transformation kinetics. The JMA parameters are extracted from the experimental data available in the literature. For comparison, a standard finite element heat conduction model is also developed to predict the thermal cycles and hardness distribution in the multi-pass, multi-layer weld. Expected Result: Results obtained using the molten pool dynamic simulation versus the finite element heat conduction model are compared. Specifically, the effects of convective heat transfer on the accuracy of the calculated thermal history, bead shape and size, and HAZ hardness distribution are examined.

Modeling, Grade 91 steel, Multi-pass multi-layer d↗

Design Basis Document / Owner’s Technical Specification for Nitrate Salt Systems in CSP Projects: Volume 1 Specifications for Parabolic Trough Projects, Volume 2 - Specifications for Central Receiver Projects, Volume 3 - Narrative

Design Basis Documents / Owner’s Technical Specifications are developed for parabolic trough and central receiver power plants using nitrate salt as the heat transport fluid and the thermal storage medium. The goals were to 1) distill the successful experience with nitrate salt systems from as many commercial projects as possible, 2) provide technical bases for equipment design/selection that an owner can impose on an EPC contractor, 3) compile this information in one location to provide guidance on salt systems that is as broadly applicable to as many projects as possible, and 4) work toward an industry consensus on a Design Basis Document that reflects the lessons learned from earlier commercial projects. The document allows an owner to provide design guidance, and to impose a minimum set of requirements, above and beyond those in the normal Codes and Standards, on an EPC contractor in an effort to avoid a repeat of past mistakes. If successful, this would allow salt systems to achieve the same levels of reliability and availability as commercial parabolic trough plants using diphenyl oxide / biphenyl (i.e., Dowtherm A, Therminol VP-1) as the heat transfer fluid. The report consists of 3 volumes: • Volume 1 - Specifications for Parabolic Trough Projects • Volume 2 - Specifications for Central Receiver Projects • Volume 3 - Narrative Volumes 1 and 2 include discussions of the following topics: • Plant functional requirements for the salt systems • Plant operating states, and transitions between states, for the salt systems • Risk analysis of the principal salt components • Plant requirements for the salt systems to meet the functional and the operating requirements • Type of specification for the principal salt components: functional; or prescriptive • Current state of the art for salt systems. Volume 3 discusses a number of cases in which the salt equipment at commercial parabolic trough and central receiver projects has not met the projected levels of reliability and availability. Possible reasons for the sources of the problems are discussed, as is a range of possible alternate designs that could avoid the known problems.

14 SOLAR ENERGY↗

Real-time tracking of protein unfolding with time-resolved x-ray solution scattering

The correct folding of proteins is of paramount importance for their function, and protein misfolding is believed to be the primary cause of a wide range of diseases. Protein folding has been investigated with time-averaged methods and time-resolved spectroscopy, but observing the structural dynamics of the unfolding process in real-time is challenging. Here, we demonstrate an approach to directly reveal the structural changes in the unfolding reaction. We use nano- to millisecond time-resolved x-ray solution scattering to probe the unfolding of apomyoglobin. The unfolding reaction was triggered using a temperature jump, which was induced by a nanosecond laser pulse. We demonstrate a new strategy to interpret time-resolved x-ray solution scattering data, which evaluates ensembles of structures obtained from molecular dynamics simulations. We find that apomyoglobin passes three states when unfolding, which we characterize as native, molten globule, and unfolded. The molten globule dominates the population under the conditions investigated herein, whereas native and unfolded structures primarily contribute before the laser jump and 30 μs after it, respectively. The molten globule retains much of the native structure but shows a dynamic pattern of inter-residue contacts. Our study demonstrates a new strategy to directly observe structural changes over the cause of the unfolding reaction, providing time- and spatially resolved atomic details of the folding mechanism of globular proteins.

59 BASIC BIOLOGICAL SCIENCES↗

Small- and Wide-Angle X-ray Scattering Studies of Liquid–Liquid Phase Separation in Silicate Melts

Incongruent liquid-liquid phase separation is a common phenomenon in molten oxides, but there are few structural studies due to the high temperatures involved ca. >1600oC. In this work, we present a high-energy x-ray combined small/wide angle scattering (SAXS/WAXS) method that can directly probe non-equilibrium phase diagrams. The Porod exponent in the SAXS signal is extracted, which measures the roughness of the interface formed between different phases. Problematic volatilization of silica in Al 2 O 3 -, CaO-, and MgO-bearing silica-rich liquids were minimized using levitation, laser heating and rapid time-resolved measurements (lasting tens of seconds), to probe the kinetics of the phase separation process. The WAXS measurement simultaneously probes the local atomic structure of the liquid state and shows that the primary structural changes are associated with the SiO 2 network. Cation coordination numbers extracted from pair distribution functions support the model that the origin of phase separation in binary silicate systems is due to Coulombic repulsions between poorly screened cations. For CaO-SiO 2 , the liquid-liquid phase separation is found to correlate with a pause in the temperature dependent atomic disorder associated with SiO4 tetrahedra.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Pyrolysis in Molten Salts Converts Plastics into a Mesoporous Electrocatalyst with a High Density of Atomic Fe–N–C Active Site

Upcycling plastic waste into value-added products is a promising strategy for both economic and environmental sustainability. However, achieving control over structure–property correlations during the upcycling process remains challenging. Here, in this study, we investigate the modulation of active site formation during pyrolytic conversion of plastics to carbon by composition-controlled molten salts. Using melamine formaldehyde (MF) foams as a precursor, we demonstrate that their pyrolysis in eutectic chloride molten salts with Fe 2+ , Na + , and K + ions directs the carbonization process toward the formation of mesoporous functional carbon enriched with atomically dispersed Fe–N–C sites, which are well-known for their catalytic activity in oxygen reduction reaction (ORR). Compared to pyrolysis in the FeCl 2 -only salt, the incorporation of alkali metal ions (Na + , K + ) in the eutectic mixture facilitates nitrogen retention in the carbon matrix and modulates iron speciation. This synergistic environment promotes a higher density and more uniform dispersion of Fe–N–C moieties within the carbon matrix. Consequently, the resulting catalyst exhibits a high surface area, hierarchical porosity, and improved electrochemical properties. When tested as an ORR catalyst, the Fe–N–C-enriched catalyst delivers a high half-wave potential (E 1/2 = 0.875 V vs RHE) with nearly exclusive 4e – pathway. These properties are comparable to those of commercial Pt/C catalysts, along with improved stability.

Fe−N−C active sites↗

Thermophysical Properties of NaCl–UCl 3 –PuCl 3 Molten Salts: A Combined Computational and Experimental Study

Actinide-bearing molten salts for use as fuels are an essential part of next generation molten salt reactors. Yet, numerous multicomponent salt mixtures are underdeveloped or have not been investigated. Here, this study, based on a combination of experimental and modeling techniques, is dedicated to determining and understanding a variety of properties of the ternary system of NaCl–UCl 3 –PuCl 3 , which represents a scenario for burnup of NaCl–UCl 3 fuel, at two compositions (∼10 and 5 mol % PuCl 3 in eutectic NaCl–UCl 3 pseudobinary) and a range of temperatures. Evaluation of the heat flow and mass loss data showed the 0.61NaCl–0.30UCl 3 –0.09PuCl 3 salt had a melting temperature of 551 ± 5 °C. Two additional thermal effects were observed occurring at approximately 410 and 494 °C. The transition occurring at 410 °C may be due to the presence of oxide in the salt. Extrapolation of thermodynamic data indicates the transition occurring at 494 °C is due to the formation of a liquid phase. Experimental testing determined the density of this system is a linear function of temperature and can be represented by the equation ρ = 4.014–0.0010T(°C), R 2 = 0.992. Additionally, by using atomistic modeling, we found that increasing the PuCl 3 content from 5 to 10 mol % led to the formation of larger Pu 3+ clusters and slower transport of ions.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Microreactor Automated Control System - Digital Twin Models and Advanced Control Systems Updates

Automation of control systems is expected to be important in the economic and safe operation of microreactors. Therefore, there is a need to develop and demonstrate automated control for microreactors, along with the development of testbeds for this purpose. This report provides updates on the status of a nonnuclear microreactor automated control system (MACS)—a real-time, hardware-in-the-loop testbed for non-nuclear testing of microreactor control system automation. A real-time hardware-in-the-loop testbed incorporates the realistic dynamics of physical systems into control system development and testing. The collaborative effort between Oak Ridge National Laboratory (ORNL) and Idaho National Laboratory (INL) resulted in the development of a prototypic microreactor plant-level digital twin that includes the reactor and a balance of plant system. Advanced control strategies were incorporated to demonstrate testing of control automation solutions. The gRPC communication protocol, which was implemented in the hardware-in-the-loop testbed by INL, was coupled to a digital twin model developed using the TRANsient Simulation Framework of Reconfigurable Models (TRANSFORM) library in Modelica. This digital twin simulation was tested with the ViBRANT hardware for realistic feedback and visual representation of control action in real time. A modular Python client structure was developed to manage functional mock-up unit-based simulation and real-time gRPC communication. Hardware-in-the-loop testing indicated that the modeled reactor—a natural-convection, molten-salt coolant loop configuration—responds well to control of drum positioning for modulation of reactor core power, as well as system-level control and downstream demand changes. Ongoing research is focused on integrating additional control algorithms that utilize data from newly included sensors within the MACS hardware testbed, as well as demonstrating and assessing the performance of the different automated control algorithms on multiple additional operational scenarios.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Effect of iodides on thermal behavior and phase partitioning in LiCl-KCl

Liquid-fueled molten salt reactors (MSRs) are designed to operate with fissile materials and, ultimately, fission products dissolved in the primary molten salt coolant. Understanding the speciation and transport of iodine—a high-yield fission product—is essential because this element’s accidental release poses significant environmental concerns due to its capacity to be readily absorbed by the human thyroid gland. Here, we report the impact of iodide species (LiI and KI) on phase transitions, phase distribution, and phase stability in LiCl–KCl-eutectic salt mixtures. The study employed a combination of computational and experimental techniques, including thermodynamic FactSage calculations, differential scanning calorimetry, and high-temperature X-ray diffraction. The results indicate that the presence of iodide (10–25 wt%) significantly alters the melting behavior of the LiCl–KCleutectic system. Adding 10 wt% LiI has a more-pronounced effect than 10 wt% KI, as LiI converts to KI, leading to formation of LiCl, thereby, altering the LiCl-KCl ratio which significantly affects the melting temperature of the mixture. Furthermore, the evolution of crystalline structure, solid-fraction composition, and the dynamics of mixed-halide solid–liquid partitioning as a function of temperature indicate the potential for selective iodide separation from chloride-salt mixtures via solid–liquid separation techniques. Overall, the presented findings provide valuable insights that are beneficial for the design and operation of MSRs, as well as for the safe handling and effective processing of used nuclear fuel using advanced pyrochemical techniques.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Rotating Molten Metallic Drops and Related Phenomena: A New Approach to the Surface Tension Measurement

Molten aluminum and tin drops were levitated in a high vacuum by controlled electric fields, and they were systematically rotated by applying by a rotating magnetic field. When the evolution of the drop shape was measured as a function of rotation frequency, it agreed quantitatively well with the Brown and Scriven's theoretical prediction. The normalized rotation frequencies at the bifurcation point agreed with the predicted value 0.559, within 2%. An anomalous phenomenon which totally deviated from the prediction was observed in rotating molten tin drops when they were kept in a high rotation rate for several hours. No anomaly was observed in aluminum drops when they underwent similar condition. It was speculated that under the strong centrifugal force in the drop the tin isotopes must be separating. Since Al-27 is essentially the only naturally abundant isotope in the aluminum drops, the same anomaly is not expected. Based on the shape deformation of a rotating drop, an alternate approach to the surface tension measurement was verified. This new surface tension measurement technique was applied to a glassforming alloy, Zr(41.2)Ti(13.8)Cu(12.5)Ni(10.0)Be(22.5) in its highly viscous states. Also demonstrated in the paper was a use of a molten aluminum drop to verify the Busse's prediction of the influence of the drop rotation on the drop oscillation frequency.

Rhim, Won-Kyu↗

Implementation of an Experimental Setup Based on the Three-Omega Method for Thermal Conductivity Measurements of Molten Salts

Molten salt reactors (MSRs) are one of the most promising next-generation nuclear reactor designs which use molten salts as the fuel and coolant. To design, model, predict, license, and operate MSRs, the behavior of the fuel and coolant must be understood as a function of temperature and irradiation, i.e., burnup. Of particular importance and complexity is the reliable and reproducible measurement of thermal conductivity of molten salts at high temperatures (> 500 °C). Thermal conductivity provides information on the rate at which heat passes through a specified material and is dependent on chemical composition. Currently, in the national laboratory complex, several methods for measuring thermal conductivity on molten salt systems are under development, however, to date, consistent data have not been produced. Typically, thermal conductivity measurements of high-temperature melts have been conducted by using the Transient Hot Wire (THW) method where thermal conductivity is determined by the change in temperature over time at a certain distance from a heating wire. Another time-dependent technique is the laser flash method, commonly used for solid samples. Laser flash requires prior measurements of density and heat capacity to calculate the thermal conductivity of the sample, introducing additional measurement errors. Steady state and time-dependent measurements such as THW and laser flash have errors from convection and ambient temperature fluctuations (heat radiation). In order to produce high fidelity thermal conductivity data, a measurement technique needs to be developed that will reduce the effect of convection at high temperatures by measuring in a very fast time window. In addition, to measure on actinide and irradiated salts the sample size should be small. Therefore, this project aims to develop a frequency-domain technique based on the three-omega (3?) method, previously proven to work on solids, nanofluids and low temperature solar salts (25 to 250 °C). If the 3?-device can be designed with materials that can withstand high temperatures (>500 °C) and can be configured to reduce errors due to convection, then it would prove to be a valuable technique for ensuring thermal conductivity on molten salt systems needed for MSR development. For this proposal, the 3? instrument will be designed, assembled, and tested on non-radioactive salts before being used on actinide bearing salts. In addition, a thermal model will be developed to determine the thermal conductivity of the sample from the measured thermal oscillation of the sensor. Because 3? is a direct method that requires a small volume of sample and works in a very fast time window, it will aid in suppressing the interference due to convection which is ideal when working with high temperature liquid samples.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Neutron Characterization for Additive Manufacturing

Oak Ridge National Laboratory (ORNL) is leveraging decades of experience in neutron characterization of advanced materials together with resources such as the Spallation Neutron Source (SNS) and the High Flux Isotope Reactor (HFIR) shown in Fig. 1 to solve challenging problems in additive manufacturing (AM). Additive manufacturing, or three-dimensional (3-D) printing, is a rapidly maturing technology wherein components are built by selectively adding feedstock material at locations specified by a computer model. The majority of these technologies use thermally driven phase change mechanisms to convert the feedstock into functioning material. As the molten material cools and solidifies, the component is subjected to significant thermal gradients, generating significant internal stresses throughout the part (Fig. 2). As layers are added, inherent residual stresses cause warping and distortions that lead to geometrical differences between the final part and the original computer generated design. This effect also limits geometries that can be fabricated using AM, such as thin-walled, high-aspect- ratio, and overhanging structures. Distortion may be minimized by intelligent toolpath planning or strategic placement of support structures, but these approaches are not well understood and often "Edisonian" in nature. Residual stresses can also impact component performance during operation. For example, in a thermally cycled environment such as a high-pressure turbine engine, residual stresses can cause components to distort unpredictably. Different thermal treatments on as-fabricated AM components have been used to minimize residual stress, but components still retain a nonhomogeneous stress state and/or demonstrate a relaxation-derived geometric distortion. Industry, federal laboratory, and university collaboration is needed to address these challenges and enable the U.S. to compete in the global market. Work is currently being conducted on AM technologies at the ORNL Manufacturing Demonstration Facility (MDF) sponsored by the DOE's Advanced Manufacturing Office. The MDF is focusing on R&D of both metal and polymer AM pertaining to in-situ process monitoring and closed-loop controls; implementation of advanced materials in AM technologies; and demonstration, characterization, and optimization of next-generation technologies. ORNL is working directly with industry partners to leverage world-leading facilities in fields such as high performance computing, advanced materials characterization, and neutron sciences to solve fundamental challenges in advanced manufacturing. Specifically, MDF is leveraging two of the world's most advanced neutron facilities, the HFIR and SNS, to characterize additive manufactured components.

Watkins, Thomas↗

Grail Refinements to Lunar Seismic Structure

To probe a planet's interior, seismology provides the most direct constraints on the variables that govern the dynamic properties of the body. However, the GRAIL (Gravity Recovery and Interior Laboratory) mission's high-resolution measurements of the lunar gravity field provide constraints on crustal thickness, mantle structure, core radius and stratification, and core state (solid vs. molten). These data complement seismic investigations, and joint interpretation permits improved constraints on the Moon's internal structure. Joint interpretation of disparate geophysical datasets helps reduce drawbacks that can result from analyzing them individually. The Apollo seismic network was situated on the lunar nearside surface in a roughly equilateral triangle having sides approximately 1000 km long, with stations 12/14 nearly co-located at one corner. Due to this limited geographical extent, near-surface ray coverage from moonquakes is low, but increase with depth. In comparison, gravity surveys and their resulting gravity anomaly maps have traditionally offered optimal resolution at crustal depths. Gravimetric maps and seismic data sets are therefor well suited to joint inversion, since the complementary information reduces inherent model ambiguity. We will perform a joint inversion of Apollo seismic delay times and gravity data collected by GRAIL lunar gravity mission, in order to recover seismic velocity and density as a function of latitude, longitude and depth within the Moon. We will relate density (rho) to seismic velocity (v) using a linear relationship that is allowed to be depth-dependent. The corresponding coefficient (B) can reflect a variety of material properties that vary with depth, including temperature and composition. The inversion seeks to recover the set of rho, v, and B perturbations that minimize (in a least-squares sense) the difference between the observed and calculated data.

Weber, Renee C.↗