High performance porous Si@C anodes synthesized by low temperature aluminothermic reaction
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Mishra, Kuber↗
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Electrochemical stability and corrosion behavior of Ni-Cr alloy in molten LiCl-KCl salt
This study investigated the electrochemical properties and potential-dependent stability of Cr(II) and Ni(II) in a eutectic LiCl-KCl molten salt at 500 °C under an argon atmosphere using a three-electrode cell configuration with a glassy carbon working electrode, Ag/Ag + reference electrode, and graphite counter electrode. Cyclic voltammetry was employed to characterize the Cr(0)/Cr(II)/Cr(III) and Ni(0)/Ni(II) redox transitions, yielding diffusion coefficients of 0.50 (±0.01) × 10 −5 cm 2 s −1 for Cr(II) and 0.91 (±0.16) × 10 −5 cm 2 s −1 for Ni(II) at 500 °C. The redox stability domains of these species provided insight into the corrosion mechanisms of a Ni-Cr alloy (80–20 wt %) in LiCl-KCl salt. The measured open circuit potential of the alloy corresponded to the range of potentials where the Ni(0) and Cr(II) species are stable, indicating a preferential dissolution of Cr. Immersion testing of the alloy for 336 h confirmed significant Cr depletion (or Ni-enrichment) at the surface layer, corroborating Cr dealloying as the dominant corrosion reaction under open circuit conditions. Additionally, the application of a small anodic overpotential (0.11 V) resulted in selective Cr dissolution while a large anodic overpotential (0.25 V) resulted in co-dissolution of both Cr and Ni. Furthermore, these results demonstrate that the corrosion mechanisms of a Ni-Cr alloy in LiCl-KCl depend upon the applied potential, and thus the redox conditions of the molten salt should be carefully controlled in the design of a redox buffer to mitigate corrosion in molten salt environments.
22 GENERAL STUDIES OF NUCLEAR REACTORS↗
Stabilizing a low temperature phase change material based on Glaubers salt
The aim of this research is to enhance the performance of Glauber's salt (sodium sulfate decahydrate, SSD) as a phase change material (PCM) for thermal energy storage applications, as well as for shipping of temperature-sensitive materials. The study investigates the effects of modifying SSD with potassium chloride (KCl) and ammonium chloride (NH 4 Cl) to achieve lower phase transition temperatures of between +6 °C and + 13 °C. Sodium polyacrylate (PAAS) is employed as a thickening agent to prevent phase separation, and borax is used as a nucleating agent to suppress supercooling. Various ratios of KCl:NH 4 Cl are tested, and the impact of PAAS concentration on phase segregation is explored. The results show that a 2 wt% concentration of PAAS effectively prevents phase separation. Samples with a KCl:NH 4 Cl ratio of 1:1.83 exhibit stable phase transition behavior and maintain latent heat values within the range of 130–140 J/g after 30 thermal cycles. Maintaining a total KCl and NH 4 Cl proportion of 10 wt% is crucial to achieve the desired lower melting temperature. As a result, the study highlights the significance of thermal cycling in improving the stability of the PCM. The optimized SSD-based eutectic PCM formulations hold promise for applications in the cold chain industry.
25 ENERGY STORAGE↗
Dynamic modeling of heat pipe integrated thermal battery latent heat storage system experiment validation
A heat pipe integrated thermal battery system has been constructed to investigate a high-temperature latent heat thermal energy storage technology that takes advantage of near isothermal operation of latent heat storage and heat pipes to potentially enable high-energy isothermal heat storage. A dynamic model constructed in Modelica has been validated, showing errors between 2.5 °C–39.7 °C across 10-h to 47-h simulations against experiment results, showing good prediction capability of experiment output, especially against phase change time. Model calibrations showing vessel heat-up capability of 3 kW and heat pipes combining to provide 600 W each during experiment operation validate experiment circumstances including reduced material loading and reduced power capability. The experiment configuration uses an Al-Mg-Zn eutectic metal as the storage material, heated via heat tape wrapped around the vessel and guide tubes to bring the system to operation range (>400 °C) and to simulate charging heat exchange, respectively, with heat rejection occurring through the surfaces of the material and facilitated via guide tubes with less insulation wrapping. The model is available in the open-source repository HYBRID on Github.
25 - ENERGY STORAGE↗
Tritium permeability measurement in hydrogen-tritium system
Fusion power promises to provide electricity generation with outstanding safety and environmental performance. Safety plays a crucial role in fusion material selection since tritium behavior in materials determines two key safety evaluation source terms: in-vessel inventory source term and ex-vessel release term, which are used in reactor safety assessments for licensing fusion facilities. Tritium permeation through materials at elevated temperature during long pulse operation expected in a burning plasma environment will become a major safety issue and development of tritium permeation barrier materials is required to minimize ex-vessel release to the environment [1]. Extensive work on hydrogen and deuterium behavior in fusion materials has been conducted, but very little database is available for tritium, the radioactive fuel for future reactors, due to the cost and difficulty associated with handling tritium [2]. A majority of the experiments were carried out at high hydrogen/deuterium partial pressure (> 100 Pa), but the expected tritium partial pressure in the blanket system is at low tritium partial pressure (< 100 Pa), where the tritium behavior deviates from diffusion-limited to surface-limited permeation. At these pressures the behavior of tritium is suspected to deviate from diffusion-limited to surface-limited permeation or isotope-limited [3]. The use of tritium enables us to investigate hydrogen isotope behavior in low partial pressure range with beta radiation detection. The physics of two-component hydrogen (H+T) permeation through metal in the surface-limited regime and through liquid breeding material are still too poorly understood to confidently design environmentally benign and safe fusion systems. In this paper, we discuss development of tritium permeation system for low tritium partial pressure [4], and discuss the results from two-component hydrogen (H+T) permeation in 20 mm disc samples of pure alpha-iron at H2 partial pressure of 100 Pa, wide T2 partial pressure range from 10-12 to 10 Pa, and sample temperature up to 600 °C to uncover the basic scientific understanding of tritium permeation behavior at realistic blanket conditions for DEMO. [1] FESAC report on “Opportunities for Fusion Materials Science and Technology Research Now and During the ITER Era” (2012) DOE/SC-0149 [2] R.A. Causey, R.A. Karnesky, and C. San Marchi, “4.16 Tritium Barriers and Tritium Diffusion in Fusion Reactors”, Comprehensive Nuclear Materials (2012) Chapter 4.16. [3] P. Humrickhouse “Permeation of Tritium and Hydrogen in the Diffusion-Limited and Surface–Limited Regimes”, submitted to Journal of Nuclear Materials. [4] R.J. Pawelko, M. Shimada, K. Katayama, S. Fukada, P.W. Humrickhouse, and T. Terai, “Low tritium partial pressure permeation system for mass transport measurement in lead lithium eutectic”, Fusion Engineering and Design 102 (2016) 8
70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
Compatibility of SiC with ODS FeCrAl in flowing Pb-Li at 600° - 700°C
To establish the maximum operating temperature for the dual coolant lead lithium (DCLL) blanket concept, thermal convection loop (TCL) experiments were conducted for 1000 h with a peak temperature of 700 °C to determine compatibility with commercial eutectic Pb~17at.%Li. Two TCLs were fabricated from alloy APMT (FeCrAlMo) and the baseline TCL experiment contained only APMT specimens. The second TCL experiment exposed more fusion relevant CVD SiC and ODS Fe-10Cr-6Al specimens in the hot and cold legs. In the second experiment, the mass losses were much larger for the ODS FeCrAl specimens and most of the CVD SiC specimens experienced a mass gain as SiC reacted to form an Fe- and Cr-rich carbide reaction product. Dissolved Fe and Cr reacted with the SiC and removing Fe and Cr from the liquid appeared to increase ODS FeCrAl dissolution. Such a dissimilar material interaction appears consistent with thermodynamic calculations. Significant attack at the top of the hot leg in both experiments suggests that the Pb-Li compatibility of FeCrAl alloys is inadequate at 700 °C in a flowing environment and the maximum PbLi temperature is < 675 °C.
36 MATERIALS SCIENCE↗
Demonstration of RELAP5-3D for transient analysis of a dual coolant lead lithium fusion blanket concept
Our research aims to build a multiphysics framework for transient analysis of the Dual- Coolant Lead-Lithium (DCLL) blanket design of the proposed Fusion Nuclear Science Facility (FNSF) for all Onticipated Operational Occurrences (AOOs) using Reduced Order Models (ROMs). This paper presents an assessment of using RELAP5-3D for transient thermal-hydraulic blanket analysis of the DCLL design. Preliminary validation studies for the RELAP5-3D properties were conducted using a representative vertical flow loop model and a comparison study using experimental data from the thermal convection corrosion loops at ORNL. These studies inspected the thermal hydraulic response of Lead-Lithium Eutectic (PbLi) systems within the RELAP5-3D code; mainly pressure drop and heat transfer, as compared to analytical calculations and experimental data. The Magnetohydrodynamic (MHD) pressure drop effect for liquid metal under the effects of a uniform magnetic field was implemented into our models using an equivalent forms loss coefficient based on the phasic momentum equations. We verified our implementation of MHD pressure drop within RELAP5-3D using a systematic approach consisting of two studies. Models were developed to perform comparison studies based on experimental data from the Argonne Liquid metal EXperiment (ALEX) facility and the Magnetohydrodynamic PbLi Experiment (MaPLE) facility. Using the developed validation basis, we built a simplified DCLL channel model within RELAP5-3D, inspected MHD pressure drop and performed transient temperature analysis. The DCLL channel model used radial heating data from the International Thermonuclear Experimental Reactor (ITER) which was normalized to the FNSF design. Here, a representative startup transient was performed using a relative power curve from the initial ramp up of a long-term power pulse of the Tore Supra reactor. This study demonstrated that RELAP5-3D ROMs are capable of accurate transient analysis of the DCLL blanket. We have since utilized MCNP to develop heating profiles based on the FNSF design and are working toward implementing them into our DCLL model.
70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
Prediction of PbLi fluid flow and temperature field in a thermal convection loop for qualification of fusion materials
Two modeling tools, a thermohydraulics code and a computational model in COMSOL Multiphysics, have been developed, tested and then applied to the analysis of fluid flow and heat transfer in a thermal convection loop (TCL). Such a device has recently been used to experimentally evaluate corrosion compatibility of APMT (Fe–21Cr–5Al–3Mo) steel with high-temperature molten eutectic lead-lithium (PbLi) alloy at Oak Ridge National Lab, TN, USA. Here, the 1-D thermohydraulics code allows for rapid calculations of the loop parameters as a function of the applied heat flux. The supplemental COMSOL finite-element computations provide detailed 3-D velocity and temperature field data but are much more time consuming. Both modelling tools demonstrate an excellent agreement in the computed circulation velocity as well as maximum and minimum temperatures. The performed TCL analysis focuses on flow development in the “hot” and “cold” legs, formation of Dean vortices in corner regions, blocking effect of the immersed samples, and radiative and convective cooling effects under the experiment-relevant conditions for Prandtl number Pr = 0.015, Grashof numbers Gr ~10 7 , and Reynolds numbers Re ~10 4 .
36 MATERIALS SCIENCE↗
Galinstan liquid metal breakup and droplet formation in a shock-induced cross-flow
Liquid metal breakup processes are important for understanding a variety of physical phenomena including metal powder formation, thermal spray coatings, fragmentation in explosive detonations and metalized propellant combustion. Since the breakup behaviors of liquid metals are not well studied, we experimentally investigate the roles of higher density and fast elastic surface oxide formation on breakup morphology and droplet characteristics. This work compares the column breakup of water with Galinstan, a room-temperature eutectic liquid metal alloy of gallium, indium and tin. A shock tube is used to generate a step change in convective velocity and back-lit imaging is used to classify morphologies for Weber numbers up to 250. Digital in-line holography (DIH) is then used to quantitatively capture droplet size, velocity and three-dimensional position information. Differences in geometry between canonical spherical drops and the liquid columns utilized in this paper are likely responsible for observations of earlier transition Weber numbers and uni-modal droplet volume distributions. Scaling laws indicate that Galinstan and water share similar droplet size-velocity trends and root-normal volume probability distributions. Furthermore, measurements indicate that Galinstan breakup occurs earlier in non-dimensional time and produces more non-spherical droplets due to fast oxide formation.
36 MATERIALS SCIENCE↗
Thermodynamic properties and phase stability of the Ba-Bi system: A combined computational and experimental study
The thermodynamic properties and phase stability of the Ba-Bi system are investigated computationally and experimentally in the present work. The enthalpies of formation and the finite temperature thermodynamic properties of seven compounds are predicted by first-principles calculations based on density functional theory (DFT), indicating five compounds (BaBi 3 , Ba 11 Bi 10 , Ba 4 Bi 3 , Ba 5 Bi 3 , and Ba 2 Bi) to be stable. Phase relations at 773 K and 858 K with composition x Ba = 0.90 are established by isothermal annealing and powder X-ray diffraction (XRD) to clarify the previously observed phase transition at 796 K. The extremely low chemical activity of Ba in liquid for a wide range of temperatures and compositions indicates very strong short-range ordering in the liquid phase which is modeled in the present work by introducing the Ba 4 Bi 3 and BaBi 3 associates in the liquid phase. Both thermodynamic and phase equilibrium data are then used to evaluate the model parameters in Gibbs energy functions of the five stable compounds and three solution phases of liquid, bcc, and rhombohedral phases by the CALPHAD (CALculation of PHAse Diagram) technique. Here the present work shows that the Ba-Bi system consists of three eutectic reactions, two peritectic reactions, one peritectoid reaction, and two congruent reactions, as well as that the concentrations of associates are very high in the liquid phase with very low concentration of atomic Ba, which provides the fundamental understanding as to why Bi can be used to remove Ba ions from molten salt solutions.
36 MATERIALS SCIENCE↗
Effect of Sb substitution on crystal structure, texture and hard magnetic properties of melt-spun MnBi alloys
Melt-spun Mn 50 Bi 50-x Sb x alloys with x ≤ 5 were prepared at different solidification rates and characterized both in the as-spun state and after annealing. In the as-spun alloys, the Sb substitution leads to the formation of a metastable phase, similar to the binary "quenched high-temperature phase" but without the superstructure of the latter and exhibiting a different – increasing – temperature dependence of coercivity. The new nanocrystalline metastable phase is not only itself characterized by a high room-temperature coercivity (in excess of 20 kOe), but upon annealing it transforms into a high-coercivity (up to 13.5 kOe) "low-temperature" α phase. However, the advantage of obtaining a high coercivity without the otherwise required milling made possible by the Sb substitution is undermined by the absence of a local crystallographic texture in the melt-spun alloys. The best combination of the isotropic hard magnetic properties realized for the Mn 55 Bi 43.5 Sb 1.5 composition is a remanence of 35.5 emu/g and a coercivity of 8.1 kOe. The annealed Sb-free Mn 50 Bi 50 alloys did possess a local crystallographic alignment and, for high solidification rates, a moderate coercivity up to 5.6 kOe; however, they had an inadequate "rectangularity" in the demagnetization curve. The orthorhombic compound known as MnBi 0.9 Sb 0.1 and described earlier as antiferromagnetic was obtained in the annealed ribbons with x ≈ 5. The compound was found to order ferromagnetically between 200 K and ≈250 K and to exhibit a significant coercivity, 14.3 kOe at 50 K. Here, it is suggested that the MnBi 0.9 Sb 0.1 may actually be a Sb-stabilized "new phase" observed earlier as metastable in the Bi–MnBi eutectic alloys.
36 MATERIALS SCIENCE↗
Thermodynamic properties of Gd-Bi alloys determined by emf measurements in LiCl-KCl-GdCl 3 electrolyte
Thermodynamic properties of binary Gd-Bi alloys (mole fraction, x Gd = 0.02–0.35) were determined using electromotive force (emf) measurements in molten LiCl-KCl-GdCl 3 electrolyte in complement with structural, microstructural, and thermal characterization. X-ray diffractometry (XRD) and scanning electron microscopy (SEM) identified the phase constituents of Gd-Bi alloys (x Gd = 0.02–0.35) as Bi matrix and GdBi compound. According to differential scanning calorimetry (DSC) measurements up to 1250 K, a eutectic transition [L = Bi + GdBi] was observed at 543 K but the reported peritectic transition [L + GdBi = GdBi 2 ] was not detected, suggesting the absence of the GdBi 2 compound. Based on structural, microstructural, and thermal characterization of Gd-Bi alloys (x Gd = 0.02–0.35), the GdBi 2 compound was not detected, and its thermodynamic stability is questionable. The emf of Gd-Bi alloy (x Gd = 0.16) at 700–1048 K relative to Gd(s) was measured by electrodepositing pure Gd metal at 25 K increments. Further, the emf values of Gd-Bi alloys were determined via coulometric titration of Gd into liquid Bi using a two-phase [L + GdBi] alloy as a reference electrode at 773–973 K. The solubility of Gd in liquid Bi was also estimated to be 0.50 mol% (773 K), 0.99 mol% (873 K), and 2.21 mol% (973 K) and the excess partial molar Gibbs energy (Δ$\mathrm{\bar{G}^{ex}_{Gd}}$) of liquid Gd-Bi alloys was as low as 65 kJ mol –1 , indicating strong chemical interactions between Gd and Bi.
36 MATERIALS SCIENCE↗
Microstructure-refinement–driven enhanced tensile properties of high-pressure die-cast A380 alloy through friction stir processing
This work employs friction stir processing (FSP), a well-known severe plastic deformation technique, to selectively modify the microstructure of thin-walled, high-pressure die-cast (HPDC) aluminum alloy A380, a major HPDC alloy fabricated in the die casting sector. FSP effectively breaks down Al dendrites and acicular Si particles, creating a homogenized distribution of equiaxed Si particles in the aluminum matrix. After FSP, the refined Si particles (~1.5 µm) are smaller than the eutectic Si particles (3–8 µm) in HPDC condition. In addition, interparticle distance has decreased almost 50% compared to dendritic arm spacing, and FSP has reduced the aspect ratio of Si particles to ~2. Furthermore, FSP eliminates porosity, and breaks down needle-like second-phase Fe-Mn and Cu-rich particles, yielding a refined, homogeneous distribution. The FSP-induced microstructural refinement and porosity reduction improve bulk yield strength and ductility by 23% and 66%. Tensile properties are enhanced beyond those of the die skin of the HPDC plate, and the alloy possesses lower defect density and a highly refined microstructure. This study establishes the viability of FSP as a tool for microstructure modification and mechanical property improvement for HPDC Al alloys for the light-weighting goal of the automotive industries.
36 MATERIALS SCIENCE↗
Microstructure analysis and machinability of additively manufactured A205 aluminum with heat treatments
A205 aluminum is one of the few high-strength aluminum alloys discovered for additive manufacturing (AM). The microstructure and heat treatment effects of AM A205 vary from those of its cast form, indicating possible differences in machinability during post-processing. Here, the objective of this research is to determine these variations of AM A205 and their effects on machinability using the cast condition as the baseline. As built and two heat-treated conditions (solution treatment and age hardening) were applied and compared in terms of their microstructures, micro-hardness, and machinability including vibration, specific cutting energy, chip morphology, and surface finish. The effects of print orientations on machinability were tested as well and found to be insignificant. AM as built had a higher hardness and slightly better machinability than its cast as built cast counterpart due to a smaller grain size (1 µm vs. 15 µm), eutectic θ-Al 2 Cu lattice and a fine, homogeneous TiB 2 distribution. The solution treatment dissolved this θ-Al 2 Cu lattice and increased the grain size (3 µm) which decreased the hardness, increased the ductility seen in the chips, and reduced the overall machinability. The presence of θ’-Al 2 Cu precipitates improved the machinability of aged AM A205. In addition, it was found that A205 exhibited both ductile and brittle behavior depending on the cutting speed, thus producing different machinability. The speed dependency is related to the material condition and heat treatment.
36 MATERIALS SCIENCE↗
A novel method combining additive manufacturing and alloy infiltration for NdFeB bonded magnet fabrication
In this paper, binder jetting additive manufacturing technique is employed to fabricate NdFeB isotropic bonded magnets, followed by an infiltration process with low-melting point eutectic alloys [i.e., Nd 3 Cu 0.25 Co 0.75 (NdCuCo) and Pr 3 Cu 0.25 Co 0.75 (PrCuCo)]. Densification and mechanical strength improvement are achieved for the as-printed porous part. Meanwhile, the intrinsic coercivity H ci is enhanced from 732 to 1345 kA/m and 1233 kA/m after diffusion of NdCuCo and PrCuCo, respectively. This study presents a novel method for fabricating complex-shaped bonded magnets with promising mechanical and magnetic properties.
36 MATERIALS SCIENCE↗
Irradiation stability and thermo-mechanical properties of NITE-SiC irradiated to 10 dpa
In this study, five variants of nano-infiltration transient eutectic (NITE) SiC were prepared using nanopowder feedstock and sintering additive contents of <10 wt%. The dense monolithic materials were subsequently irradiated to 2 and 10 dpa in a mixed spectrum fission reactor at nominally 400 and 700°C. The evolution in swelling, strength, and thermal conductivity of these materials were examined after irradiation, where in all cases properties saturated at < 2dpa, without appreciable change for further irradiation to 10 dpa. Swelling behavior appeared similar to high-purity chemical vapor deposition (CVD) SiC within measurement uncertainty. The strength roughly doubled after irradiation. Finally, thermal resistivity increase as a result of irradiation was ~20% higher when compared to CVD-SiC.
36 MATERIALS SCIENCE↗
Analysis and modeling of the equilibrium behaviors of U and Pu in molten LiCl-KCl/Cd system at 500 °C
In the field of pyroprocessing of used nuclear fuels, liquid cadmium is applied in different ways to recover transuranics from molten salt, while effecting some degree of separations between transuranics and lanthanides. In this work, a model of the separation performance between uranium and plutonium across the phase boundary between molten salt and liquid cadmium is presented. The salt is the LiCl-KCl eutectic with solute concentrations of UCl 3 and PuCl 3 . The cadmium is the liquid cadmium phase field from the Cd-U-Pu ternary alloy system. Lastly, the model used to describe the behavior of uranium and plutonium in the salt/cadmium system is applied to describe the behavior of plutonium and lanthanide in the salt/cadmium system.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
Uranium exchange kinetics in a molten LiCl-KCl/Cd system at 500 °C
A dissolution experiment is performed in order to examine the kinetics of uranium isotope equilibration in a molten salt and cadmium system. The salt contains a solute concentration of UCl 3 in LiCl-KCl eutectic and the cadmium contained dissolved uranium at 500 °C. A small piece of high enriched uranium is introduced to the cadmium, which perturbs the equilibrium with respect to the uranium enrichment of the salt and cadmium phases. The series of salt and cadmium samples trace how the enrichment of the two phases reach equilibrium (in the absence of a chemical driving force) over the course of approximately 24 h. Here, a model linking dissolution and isotope exchange kinetics is developed to track the evolution of uranium isotope composition. With the assumption of unaccounted salt mass incurred from the dated sample reporting practice, the model explains the trend of the measured uranium isotope composition well.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗