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At least 37 records · Page 2

Round Robin Measurements of Molten Salt Properties for LiF-NaF-KF (FLiNaK) and NaCl-KCl Mixtures

The development, operation, and regulation of nuclear reactors that utilize molten salts as fuel or as heat transfer media require knowledge of the thermal properties of the salt systems and quantification of the corresponding uncertainties. Knowledge of molten salt properties is also necessary for applications in material synthesis, processing, separations, solar thermal power generation, and energy storage. A round robin was conducted with national laboratory and university participants from twenty-one laboratories in five countries to compare property measurements, to better understand uncertainties, and to identify possible best practices. Two salt mixtures, each from a common batch, were distributed to participants for evaluation: equimolar NaCl-KCl and 45.0LiF-13.7NaF-41.3KF mol % (FLiNaK). Measurements were performed to determine the major constituent composition, oxygen content, density, thermal expansivity, melting point, and thermal conductivity. Error analysis was performed on each measurement for uncertainty quantification for each type of property that was explored. Finally, the resulting discussion of the methodologies used in this work is meant to lay the groundwork for the development of standard methods and reference materials for future high-temperature property measurements on halide melts.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Effect of tellurium concentration on the corrosion and mechanical properties of 304 stainless steel in molten FLiNaK salt

In this study, the effect of Te concentration in molten FLiNaK salt on the corrosion and mechanical properties of 304 stainless steel was investigated. The corrosion depth of samples after the immersion tests for 48 h at 600 °C decreased with increasing Te concentration. Likewise, the sample after the immersion test containing 1.0 wt% of Te (1.0 wt% Te sample) showed less reduction in mechanical properties than the 0.1 wt% Te sample. We hypothesize that the condition for a Cr-oxide layer that has the protective property is fulfilled underneath the Ni-Fe rich layer which is formed by the selective leaching of Cr.

36 MATERIALS SCIENCE↗

An In Situ , multi-electrode electrochemical method to assess the open circuit potential corrosion of Cr in unpurified molten FLiNaK

An in situ electrochemical method to investigate the time-dependent spontaneous corrosion of pure Cr in an unpurified LiF-NaF-KF eutectic salt at 600 °C was developed. A multi-electrode electrochemical cell and a dual-electrode method were utilized to detect Cr(II) and Cr(III) ions on a platinum working electrode using cyclic voltammetry as a function of exposure time and compensating for the distance from the Cr electrode. XRD was performed to characterize the crystalline composition of the exposed FLiNaK and the salt films formed on the working electrodes. The fate of all electro-oxidized Cr must be accounted for to quantify corrosion rates. The concentrations of Cr(II) and Cr(III) species obtained were compared with the gravimetric mass change and ICP-OES analysis of the residual salt. Finally, outcomes, difficulties, and limitations are discussed.

ICP-OES↗

Corrosion of 316H stainless steel in flowing FLiNaK salt

In this report type 316H stainless steel samples were exposed to flowing FLiNaK salt for 1000 h in a monometallic thermal convection loop (TCL) with a maximum temperature of 650 °C and a minimum of 540 °C. Samples in the hottest part of the TCL lost mass, with a maximum mass loss of 1.4 mg/cm 2 , while samples in the coldest parts of the TCL gained mass, with a maximum mass gain of 1.0 mg/cm 2 . Analysis of the samples that gained mass showed an Fe-rich layer on the sample surfaces, indicating that Fe, not Cr, was the primary deposition product in the TCL. Cr loss was apparent to a depth of ~5 µm in the hot leg. Post-exposure analysis of the salt showed major increases in the Cr, Fe, and Mn contents. The TCL was modeled using the TRANSFORM code. Modeled values matched the experimental temperature measurements showing that TRANSFORM is capable of accurately simulating the TCL conditions.

36 MATERIALS SCIENCE↗

Tribocorrosion of stainless steel sliding against graphite in FLiNaK molten salt

The molten salt reactor (MSR) concept recently gained renewed interest in developing Generation IV nuclear reactors. One MSR design uses fluoride molten salts to cool tri-structural isotropic particle fuel encapsulated by a carbon matrix into spherical pebbles, which would inevitably contact the reactor's stainless steel container wall during salt circulation. Characterizing this interaction is crucial for reactor safety. Here, in this work, we report the tribocorrosion behavior of graphite sliding against Type 316H stainless steel lubricated by a FLiNaK (LiF:NaF:KF; 46.5:11.5:42 mol %) molten salt in an argon environment. Accelerated wear loss was observed at a higher temperature because of a lower molten salt viscosity and a higher corrosion rate. The graphite had a more rapid material loss at a higher sliding speed than stainless steel because of its higher vulnerability to vibration-induced microfracture. The salt-starved condition caused more material loss than either the no-salt or the salt-flooded condition because neither a graphite transfer film nor stable boundary lubrication could be established at salt starvation. An interesting dual-layer surface film was discovered on the stainless steel worn surface: a chromium-rich top film and a nickel-accumulated but chromium-depleted interlayer. The film composition and structure provide fundamental insights to the mechanochemical interactions between stainless steel and graphite in a molten salt environment.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Comparative Studies of the Structural and Transport Properties of Molten Salt FLiNaK Using the Machine-Learned Neural Network and Reparametrized Classical Forcefields

Despite surging interest in molten salt reactors and thermal storage systems, knowledge of the physicochemical properties of molten salts are still inadequate due to demanding experiments that require high temperature, impurity control, and corrosion mitigation. Therefore, the ability to predict these properties for molten salts from first-principles computations is urgently needed. Herein, we developed and compared a machine-learned neural network force field (NNFF) and a reparametrized rigid ion model (RIM) for a prototypical molten salt LiF–NaF–KF (FLiNaK). We found that NNFF was able to reproduce both the structural and transport properties of the molten salt with first-principles accuracy and classical-MD computational efficiency. Furthermore, the correlation between the local atomic structures and the dynamics was identified by comparing with RIMs, suggesting the significance of polarization of anions implicitly embedded in the NNFF. Furthermore, this work demonstrated a computational framework that can facilitate the screening of molten salts with different chemical compositions, impurities, and additives, and at different thermodynamic conditions suitable for the next-generation nuclear reactors and thermal energy storage facilities.

36 MATERIALS SCIENCE↗

Morphological Evolution and Dealloying During Corrosion of Ni20Cr (wt.%) in Molten FLiNaK Salts

The dealloying corrosion behavior of the FCC Ni20Cr (wt%) in molten LiF-NaF-KF (FLiNaK) salts at 600 °C under varying applied potentials was investigated. Using in-operando electrochemical techniques and a multi-modal suite of characterization methods, we connect electrochemical potential, thermodynamic stability, and electro-dissolution kinetics to the corrosion morphologies. Notably, under certain potential regimes, a micron-scale bicontinuous structure, characterized by a network of interconnected pores and ligaments riched with the composition of the more noble (MN) element, becomes prominent. At other potentials both MN and less noble (LN) elements dealloy but at different rates. The dealloying process consists of lattice and grain boundary diffusion of Cr to the metal/salt interface, interphase Cr oxidation, accompanied by surface diffusion of Ni to form interconnected ligaments. At higher potentials, the bicontinuous porous structure undergoes further surface coarsening. Concurrently, Cr(II), Cr(III), and Ni(II) begin to dissolve, with the dissolution of Ni occurring at a significantly slower rate. When solid-state transport of Cr is exceeded by the interfacial rates, dealloying depths are limited.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Thermochemical Property Measurements of FLiNaK and FLiBe in FY 2020

The technical bases and methods developed at Argonne to measure thermochemical properties of molten salt mixtures are summarized and results provided to show the precision achieved. These methods include measurements of phase transition temperatures and heat capacity at temperatures to approximately 700 °C for eutectic mixture of 46.5-11.5-42.0 mol% LiF-NaF-KF (FLiNAK) and 67-33 mol% LiF-BeF 2 (FLiBe). Details of procedures, calibrations and operation of instruments are discussed and results are compared with values available in the literature. Additional discussions address the sources of error and estimated uncertainties in the reported values.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Thermochemical Property Measurements of FLiNaK and FLiBe in FY 2020

The technical bases and methods developed at Argonne to measure thermochemical properties of molten salt mixtures are summarized and results provided to show the precision achieved. These methods include measurements of phase transition temperatures and heat capacity at temperatures to approximately 700°C for eutectic mixture of 46.5-11.5-42.0 mol% LiF-NaF-KF (FLiNaK) and 67-33 mol% LiF-BeF 2 (FLiBe). Details of procedures, calibrations and operation of instruments are discussed, and results are compared with values available in the literature. Additional discussions address the sources of error and estimated uncertainties in the reported values.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Measuring the Dissolution of Cr and Fe at 550°-750°C in FLiNaK and FLiBe

Assessing the compatibility of 316H stainless steel with molten fluoride salts has been identified as a key research topic for molten salt reactor development. Current developers are interested in 316H stainless steel due to its ready availability and ASME code qualification. Previous studies of 316H stainless steel compatibility in molten fluoride salts have shown general agreement that Cr is selectively removed from the alloy during the exposures in molten salts. However, the extent of Cr dissolution depends on the initial purity of the salt and Fe also readily dissolves in the salt. In order to model dissolution, it is necessary to understand how time and temperature affect the dissolution rates of the alloying elements which may lead to saturation of these elements in the salt. To study the dissolution of 316H, Cr and Fe specimens were exposed in FLiNaK and LiFBeF2 (FLiBe) salt at three different temperatures (550°-750°C) and three different durations (100-2000 h) in isothermal capsule experiments.

36 MATERIALS SCIENCE↗

Friction and wear of nuclear graphite exposed to molten FLiNaK salt environment

This report formally documents the completion of the Advanced Reactor Technologies Level 3 Milestone (M3TG-25OR0501104), “Initiate graphite wear studies of graphite samples exposed to molten salt environment,” due August 1, 2025. The report summarizes the ongoing activities aimed at characterizing the friction and wear behavior of graphite in molten LiF–NaF–KF (FLiNaK) salt environment. The wear and friction behavior of self-mated ET-10 nuclear graphite were tested at varying temperatures (550°C and 650°C), contact loads (40 and 80 N) and sliding speeds (1 and 10 mm/s) in a controlled argon environment. The results were compared to the wear and friction behavior of the same graphite material in a dry argon environment. This report presents initial studies on the friction and wear behavior of graphite in sliding contact mode, with future work focused on investigating the graphite matrix materials, as well as rolling and impact contact modes. The outcomes of this report could provide insights into assessing the integrity of the graphitic components of pebble-bed fluoride salt–cooled high-temperature reactors (PB-FHRs) to enhance their safe operation.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Elucidating the role of Cr migration in Ni-Cr exposed to molten FLiNaK via multiscale characterization

Structural materials used in nuclear reactor environments are subjected to coupled extremes such as high temperature, irradiation, and corrosion which act in concert to degrade their functional performance. Connecting alloy microstructure such as grain boundaries, and accumulating point defects with corrosion attack and pore morphology is critical to understanding underlying mechanisms. We uncover the compositional variations and morphology at multiple length scales in corrosion-damaged Ni-Cr alloy after exposure to oxidants in molten fluoride salts. A complex network of dense corrosion pores is detected by surface-level SEM observations. The corrosion pores take on a 1-dimensional morphology and are enriched with Ni and depleted of Cr 1–5 µm from the pore surface. STEM-EDS and 4D-STEM strain maps acquired simultaneously highlight the local variations in composition and structure of a ≤ 200 nm Cr-rich layer identified from a cross-section taken at the bottom of an isolated corrosion pore between the Ni-Cr alloy matrix and the embedded salt. However, the absence of an observed interface between the Ni-Cr alloy matrix and the FCC-structured Cr-rich layer suggests that Cr plating from the salt did not transpire. These findings support a proposed Cr lattice diffusion mechanism rather than Cr-precipitation from the salt to accommodate temperature transient conditions during sample cooling. Through the development of a 1D phase field model, these results are rationalized by formation energies for the Ni- and Cr-oxidation into the molten salt. This study reveals the locally altered microstructure caused by high temperature corrosion in non-steady-state molten salt nuclear reactor environments.

36 MATERIALS SCIENCE↗