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Combinations of fluorinated solvents with imide salts or methide salts for electrolytes
Provided are electrochemical cells and electrolytes used to build such cells. The electrolytes include imide salts and/or methide salts as well as fluorinated solvents capable of maintaining single phase solutions at between about -30.degree. C. to about 80.degree. C. The fluorinated solvents, such as fluorinated carbonates, fluorinated esters, and fluorinated esters, are less flammable than their non-fluorinated counterparts and improve safety characteristics of cells containing these solvents. The amount of fluorinated solvents in electrolytes may be between about 30% and 80% by weight not accounting weight of the salts. Linear and cyclic imide salts, such as LiN(SO.sub.2CF.sub.2CF.sub.3).sub.2, and LiN(SO.sub.2CF.sub.3).sub.2, as well as methide salts, such as LiC(SO.sub.2CF.sub.3).sub.3 and LiC(SO.sub.2CF.sub.2CF.sub.3).sub.3, may be used in these electrolytes. Fluorinated alkyl groups enhance solubility of these salts in the fluorinated solvents. In some embodiments, the electrolyte may also include a flame retardant, such as a phosphazene, and/or one or more ionic liquids.
Investigation of a Novel Salt Stress-Responsive Pathway Mediated by Arabidopsis DEAD-Box RNA Helicase Gene AtRH17 Using RNA-Seq Analysis
Previously, we reported that overexpression of AtRH17, an Arabidopsis DEAD-box RNA helicase gene, confers salt stress-tolerance via a pathway other than the well-known salt stress-responsive pathways. To decipher the salt stress-responsive pathway in AtRH17-overexpressing transgenic plants (OXs), we performed RNA-Sequencing and identified 397 differentially expressed genes between wild type (WT) and AtRH17 OXs. Among them, 286 genes were upregulated and 111 genes were downregulated in AtRH17 OXs relative to WT. Gene ontology annotation enrichment and KEGG pathway analysis showed that the 397 upregulated and downregulated genes are involved in various biological functions including secretion, signaling, detoxification, metabolic pathways, catabolic pathways, and biosynthesis of secondary metabolites as well as in stress responses. Genevestigator analysis of the upregulated genes showed that nine genes, namely, LEA4-5, GSTF6, DIN2/BGLU30, TSPO, GSTF7, LEA18, HAI1, ABR, and LTI30, were upregulated in Arabidopsis under salt, osmotic, and drought stress conditions. In particular, the expression levels of LEA4-5, TSPO, and ABR were higher in AtRH17 OXs than in WT under salt stress condition. Taken together, our results suggest that a high AtRH17 expression confers salt stress-tolerance through a novel salt stress-responsive pathway involving nine genes, other than the well-known ABA-dependent and ABA-independent pathways.
Fluoride salt static freezing study
Molten salt reactor designs such as the FHR must consider the safety implications of freezing, requiring the development of thermal hydraulics models that account for freezing behavior. Pipe models that couple heat transfer, fluid dynamics, and phase change physics will require verification and validation. A static freezing study is being conducted to provide an initial set of validation data with LiF-BeF{sub 2} (FLiBe). The study will also be performed with LiF-NaF-KF (FLiNaK) in order to quantify the distortion that arises from using FLiNaK as a non-toxic surrogate salt for thermal-hydraulic studies. In order to develop the numerical model, accurate inputs for the thermal hydraulic properties of the two salts of interest need to be measured near the freezing point. For this reason, a series of three experiments including Differential Scanning Calorimetry (DSC) measurements, the Density Measurement Experiment, and the Static Freezing Experiment are being conducted to determine these thermo-physical properties at temperatures near the freezing point. The Static Freezing Experiment is also designed to determine the degree of supercooling that FLiBe and FLiNaK experience. Supercooling is a temperature depression below the freezing point that the liquid experiences before freezing initiates. Increased supercooling in a liquid flowing through a pipe leads to increased dendritic freezing and an increased likelihood of pipe blockage and freeze-shut. Based on previous research on supercooling in water and non-fluoride salts, supercooling is likely affected most strongly by cooling rate and sample size (as well as salt purity). No data has been generated previously on supercooling in fluoride salts such as FLiBe and FLiNaK. The results of this set of DSC, Density Measurement and Static Freezing experiments will be used in an ongoing fluoride salt freezing study being conducted to develop pipe freezing models for molten salts to be used in safety analysis. The thermal hydraulic properties measured in this study will serve as inputs for all future models. With the supercooling behavior of both salts quantified, it can be assessed whether supercooling must be included in future thermal hydraulic models. The validated Static Freezing Experiment model can then serve as the framework for a pipe freezing model and eventually a 1D system code.
Electrorefiner Speciation and Phase Model for Prediction of Operation Lifetime
The Mk IV electrorefiner (ER) at Idaho National Laboratory has recovered uranium metal from used nuclear fuels for 27 years. Thus, large quantities of fission product chlorides more electropositive than uranium have accumulated in the ER salt, increasing the complexity of phase equilibria and salt speciation. Importantly, the melt temperature of the salt increases with ER operation and will ultimately exceed design limits without intervention. Methods to remove fission products from molten chloride salt are known, but their implementation at scale is not yet demonstrated. In this work, historical ER composition and differential scanning calorimetry (DSC) are utilized to develop coupled speciation and chloride salt solution thermochemistry models, which enable accurate present-day analysis of ER salt as well as forecast its future disposition. The developed thermochemical models are applicable to chloride salts generally and have been made available in the Molten Salt Thermal Properties Database – Thermochemical.
H-2-SALT: Storing Fossil Energy as Hydrogen in Salt Caverns
Hydrogen storage in subsurface caverns is known as perhaps largest and longest-term energy storage system. While few such systems are currently in service (e.g., Texas; Teesside, UK), they are envisioned as being a pillar of the current energy transition that will allow intermittent power production from renewable sources (e.g., wind, solar) to be balanced with demand at grid-scale. In addition, hydrogen energy storage can allow existing fossil power plants to run more economically either by minimizing startups/shutdowns or by allowing them to take advantage of arbitrage. Finally, stored hydrogen can feed a variety of non-power users such as pipeline gas, heating, transportation, and manufacturing. The H-2-SALT paper study assessed the feasibility of a power-to-hydrogen system utilizing salt cavern storage of hydrogen in bedded salt in central Kansas, where over 750 such caverns have been constructed to date, of which approximately 350 are still in service. Legacy well and salt cavern data were collected to develop a regional geological database for two sites in Central Kansas and adjacent areas for use in more detailed geological and geomechanical site characterization efforts. This study found commercial viability and competitiveness of large-scale, electrolytic H 2 production and storage ($1.78 per kg H 2 ) that can be used for both electrical power supply to the grid during high-priced electricity periods (including co-firing with NG and fuel cell power production) and sale of H 2 for various industries, such as petrochemicals or transportation. The commercial potential of the H-2-SALT system is also relatively high because each of its components operate commercially today. It is recommended that a stratigraphic test well be drilled to collect log data and core samples that can reduce uncertainty surrounding geological and geomechanical properties of the salt beds that will be required for further cavern and energy storage system design studies.
Potential vertical movement of large heat-generating waste packages in salt.
With renewed interest in disposal of heat-generating waste in bedded or domal salt formations, scoping analyses were conducted to estimate rates of waste package vertical movement. Vertical movement is found to result from thermal expansion, from upward creep or heave of the near-field salt, and from downward buoyant forces on the waste package. A two-pronged analysis approach was used, with thermal-mechanical creep modeling, and coupled thermal-viscous flow modeling. The thermal-mechanical approach used well-studied salt constitutive models, while the thermal-viscous approach represented the salt as a highly viscous fluid. The Sierra suite of coupled simulation codes was used for both approaches. The waste package in all simulations was a right-circular cylinder with the density of steel, in horizontal orientation. A time-decaying heat generation function was used to represent commercial spent fuel with typical burnup and 50-year age. Results from the thermal-mechanical base case showed approximately 27 cm initial uplift of the package, followed by gradual relaxation closely following the calculated temperature history. A similar displacement history was obtained with the package density set equal to that of salt. The slight difference in these runs is attributable to buoyant displacement (sinking) and is on the order of 1 mm in 2,000 years. Without heat generation the displacement stabilizes at a fraction of millimeter after a few hundred years. Results from thermal-viscous model were similar, except that the rate of sinking was constant after cooldown, at approximately 0.15 mm per 1,000 yr. In summary, all calculations showed vertical movement on the order of 1 mm or less in 2,000 yr, including calculations using well-established constitutive models for temperature-dependent salt deformation. Based on this finding, displacement of waste packages in a salt repository is not a significant repository performance issue.
Salt Diapir‐Driven Recycling of Gas Hydrate
Abstract By harnessing both hypothetical, synthetic basin and gas hydrate (GH) system models and real‐world models of well‐studied salt diapir‐associated GH sites at Green Canyon (Gulf of Mexico) and Blake Ridge (U.S. Atlantic coast), we propose and demonstrate salt movement (and in particular, diapirism) to be a new mechanism for the recycling of marine GH. At Green Canyon, for example, we show that by considering this newly proposed diapir‐driven recycling mechanism in conjunction with previously proposed lithological control on sandy‐reservoir‐hosted hydrate at the base of the GH stability zone (BGHSZ; ∼bottom‐simulating reflector, BSR), modeled GH saturations match drilling data. Overall, salt diapir movement‐induced GH recycling provides a temperature‐driven mechanism by which GH saturations at the BGHSZ may reach >90 vol. % and by which GH volumes near and free gas volumes beneath the BGHSZ may be increased significantly through time. Interestingly, comparison of salt diapir‐driven recycling and sediment burial‐driven recycling scenarios suggests notably higher rates of recycling via diapir‐driven versus burial‐driven processes. Our results suggest that GH and associated free gas accumulations above salt diapir crests represent particularly attractive targets for unconventional and conventional hydrocarbon resource exploration and for scientific and academic drilling expeditions aimed at exploiting GH systems. Salt basins containing GH systems—including passive margin basins of the Gulf of Mexico, southeastern Brazil, and southwestern Africa—are therefore compelling localities for studying salt‐driven GH recycling and for salt diapir‐associated natural gas exploration.
Chronopotentiometry of refractory metals, actinides and oxyanions in molten salts: A review
The applications of chronopotentiometry to the study of electrochemical behavior of three technologically important areas of refractory metals, actinides, and oxyanions in molten salts are critically reviewed. Chronopotentiometry is a very versatile diagnostic tool to understand the reaction mechanism of the electrode processes for the electrochemical reduction/oxidation of these electroactive species in molten salt solutions. Well adherent, compact, and uniformly thick coatings of refractory metals may be electrodeposited from their solutions in molten salts.
Temperature and anion ligand field dependence of LnCl 3 (Ln = Nd, Dy, Sm) electronic absorption spectra in LiCl–KCl eutectic molten salt
A comprehensive knowledge of the coordination, bonding, and speciation of elements in molten salt mixtures is necessary to understand and predict the chemical and physical properties of the salt. Absorption spectroscopy can yield information about the chemistry of species of interest in alkali halide molten salt mixtures by revealing information about the electronic structure and transitions of those species. In this study, ultraviolet (UV), visible (vis), and near-infrared (NIR) absorption spectroscopy was used to examine changes to the electronic structure of trivalent Nd, Sm, and Dy in LiCl–KCl eutectic molten salt with changes in temperature and the anion composition of the melt. With increasing temperature, changes to spectral features suggest a distortion of the coordination complexes. Changes to lineshape with the substitution of alternative halide anions were examined and analyzed, revealing differences in the coordination for I – versus F – with the lanthanides. Gaussian peak fitting was used to show that the changes in lineshape with the progressive addition of F – anions can be explained by the superposition of a set of absorption bands from complexes with all Cl – anion ligands and a set of blueshifted absorption bands from complexes containing both F – and Cl – anion ligands. Finally, this work yields a new method to analyze and interpret change to electronic absorption spectra for f-block elements dissolved in alkali halide molten salts as well as new observations of the interactions of larger and smaller halide anions with lanthanides in Cl – -based molten salts.
Electrochemical Salt Wasteform Development: A Review of Salt Treatment and Immobilization Options
Electrochemical reprocessing, also referred to as pyroprocessing, is a technique for recycling actinides from used nuclear fuel (UNF) to produce fuel for future reactors. Here, UNF is dissolved in a molten salt (e.g., LiCl-KCl eutectic) within an electrorefiner. After UNF dissolution, fission products are released into the electrolyte salt and converted to chlorides. This paper discusses wasteform options for processing the base electrolyte salt with the fission product salts as well as just the rare-earth fission products (as RECl 3 , REOCl, or REO x ) with the intent of finding optimal methods for reducing total waste salt volumes or partitioning the salt for alternate wasteform options. Furthermore, two of the more detailed partitioning options discussed herein include halide removal from the salt (dehalogenation), which accounts for more than half of the salt on a molar basis, and RE fission product removal for wasteforms with high-RE loadings. Wasteform properties are compared with emphasis on wasteform volume starting from a given amount of (1) total salt cations or (2) RE cations. Comparisons are also made of wasteform chemical durabilities, with the data available from like testing methods. A main conclusion from this work is the justification of subsequent salt processing after electrorefiner operations for achieving significant wasteform volume reduction.
Techno-Economic Optimization of Advanced Energy Plants with Integrated Thermal, Mechanical, and Electro-Chemical Storage (Final Report)
The increasing use of renewable energy sources is leading to increased cycling of fossil-fueled power plants (FFPP) that are designed to operate at base-loaded conditions. Integrating energy storage facilities with the FFPPs can be helpful in reducing load-following operation of FFPPs. Decentralized deployment of energy storage facilities at the FFPP level has considerable advantages due to possibilities of smaller storage capacities, immediate benefits realized by the host power plant due to the increase in the efficiency, cleaner emission and higher plant life to name a few. Most importantly, deployment at the FFPP level can exploit the existing equipment items and facilities at the host power plant, thus reducing the CAPEX and reducing the storage capacity. However, realization of these benefits will critically depend on novel configuration/integration strategies with the least impact on the power plant operation and its configuration. Furthermore, dynamics of the entire integrated system including both the FFPP and the storage technologies must be taken into account to obtain the cost-optimal solution. With these motivations, the objective of this project was to complete a focused evaluation of decentralized deployments of energy storage facilities at the FFPP level. Promising thermal, chemical, mechanical, and electro-chemical storage technologies were evaluated with due consideration of their transient response to obtain various optimal system concepts that can minimize the levelized cost of storage. For thermal storage, cryogenic energy storage along with high temperature heat storage in molten salt as well as phase change material were evaluated. For mechanical storage, cryogenic air storage and pumped hydro storages were evaluated. For chemical storage, hydrogen storage was evaluated. For electrochemical storage, the team evaluated sodium sulfur, vanadium redox flow battery as well as Li-ion batteries. Integration of these storage technologies with the natural gas combined cycle (NGCC) and supercritical pulverized coal (SCPC) plants was considered. Six technologies, namely molten salt, cryogenics, compressed air, pumped hydro, H2 storage and Li-ion battery storage, were downselected based on their levelized cost of storage. It was observed that the ranking of the optimal storage technology can differ based on the host power plant technology even when same demand/supply/price profile for electricity are considered. It was also observed that as the variability in power demand varies, the ranking of the optimal storage technologies vary. However, for the same demand and LMP profile, top six optimal storage technologies for NGCC vs SCPC plants did not differ much even though LCOS for the same technology and optimal size of a given storage technology did differ. Detailed techno-economic assessment of these six technologies was undertaken.
Magnetic coupling at perovskite and rock-salt structured interfaces
We study magnetic coupling between hole-doped manganite layers separated by either a perovskite or a rock-salt barrier of variable thickness. Both the type and the quality of the interface have a strong impact on the minimum critical barrier thickness where the manganite layers become magnetically decoupled. A rock-salt barrier layer only 1 unit cell (0.5 nm) thick remains insulating and is able to magnetically de-couple the electrode layers. The technique can therefore be used for developing high-performance planar oxide electronic devices such as magnetic tunnel junctions and quantum well structures that depend on magnetically and electronically sharp heterointerfaces.
A Triple Bubbler System to Measure Density, Surface Tension, and Depth of Electrorefiner Molten Salt
In pyroprocessing of used nuclear fuel (UNF), uranium from the fuel is electrochemically dissolved at the anode and transported through a molten salt electrolyte to the cathode—where it is later recovered for reuse. As part of this process, special nuclear materials (SNM) dissolve into the molten salt electrolyte. Monitoring the mass of these materials, particularly plutonium, is important for material accountability and safeguards of the electrorefiner (ER) used in pyroprocessing. The mass of plutonium in the ER vessel is a function of the volume and density of the salt as well as the plutonium concentration. Measuring these parameters presents challenges due to the high temperature, radiation, and accessibility of the ER within a hotcell. Here, the main motivation for this work was to develop a method capable of measuring the density and depth (volume) of salt under the extreme operating conditions within the ER to enhance the SNM accountability and safeguards of pyroprocessing. In addition, these online measurements would be useful for monitoring level changes associated with removal of electrolyte from the ER and different unit operations associated with electrochemical reprocessing of used nuclear fuel.
Experimental Technetium Release from Simulated Salt-stone Cementitious Waste Form - 18419
Experiments are being conducted to evaluate the early release of technetium (Tc) from fresh salt-stone waste forms using dynamic flow-through tests. Salt-stone is a chemically reducing, grout-based waste form used by the U.S. Department of Energy (DOE) to dispose of low-activity salt solutions arising from high-level radioactive waste tank closure activities at the Savannah River Site (SRS). A key safety function of salt-stone is maintaining a low-flow, chemically reducing environment that will attenuate the release of redox-sensitive radioelements such as Tc. Salt-stone also provides a physical barrier due to its low intrinsic permeability, which limits both water and oxygen ingress. These release experiments, conducted to support the U.S. Nuclear Regulatory Commission's monitoring role during tank closure, are designed to provide independent information on how well salt-stone will perform its safety function. The dynamic leach tests were conducted in a Hassler-type core-holder permeameter system that allows an accelerated flow rate of simulated SRS groundwater through an intact cylinder of salt-stone spiked with Tc-99 at a concentration of approximately 2,100 Bq/g (3 ppm). The first salt-stone specimen to be tested (Specimen 2) was prepared with Grade 100 ground granulated blast-furnace slag and aged for 119 days in a temperature-controlled, low-oxygen, high-humidity environment. Before test completion, 9.5 pore volumes (PV) of simulated SRS groundwater were passed through the salt-stone cylinder. After a few PV, apparent saturated hydraulic conductivity (K{sub sat}) values calculated from flow data reached a steady-state value of approximately 1.0 x 10{sup -9} cm/s, which is within the range of previously reported data. Tc-99 concentrations in leachate peaked early during the leach test at 2.0 x 10{sup -7} M and then declined to approximately 4 x 10{sup -8} M after 9.5 PV. The leachate Tc-99 concentration after elution of 9.5 PV is broadly consistent with a Tc solution concentration controlled by the solubility of reduced Tc solids. The range of Tc-99 concentrations is similar to the range reported for a column test that was sponsored by DOE, but the time pattern of release differs. The second salt-stone specimen tested (Specimen 3) was aged for 372 days and it further differed from the first specimen in that its Grade 100 slag component had been finely ground using a mortar and pestle in an attempt to make it more reactive. This second test yielded Tc release behavior broadly similar to that observed during the first test, except that the early Tc peak (at 1.2 x 10{sup -6} M) was six times higher and the concentration after 6.7 PV (8.8 x 10{sup -8} M) was approximately two times higher than in the first test. In addition, the steady-state K{sub sat} was an order of magnitude lower than that of the first specimen. During the second test, the injection pump was intentionally turned off for a period of 11 days (i.e., approximate residence time for 1 PV) and a Tc spike was observed when pumping resumed, suggesting that longer residence times may promote higher Tc effluent concentrations. During a second intentional shut-down of the pump for 25 days (approximate residence time for 2 PV), another Tc spike was observed. An unplanned excursion to higher confining pressure physically affected the specimen, temporarily lowering the apparent K{sub sat} followed by a subsequent increase in both K{sub sat} and Tc effluent concentration. One hypothesis is that the transient spike in confining pressure and resulting salt-stone compression and later decompression may have induced Tc release from otherwise inactive pores. (authors)
Electrolyte–Electrocatalyst Interfacial Effects of Polymeric Materials for Tandem CO 2 Capture and Conversion Elucidated Using In Situ Electrochemical AFM
Integrating CO 2 capture and electrochemical conversion has been proposed as a strategy to reduce the net energy required for CO 2 regeneration in traditional CO 2 capture and conversion schemes and can be coupled with carbon-free renewable electricity. Polyethylenimine (PEI)-based materials have been previously studied as CO 2 capture materials and can be integrated in these reactive capture processes. PEI-based electrolytes have been found to significantly increase the CO 2 loading, and impact selectivity and rate of product formation when compared to the conventional aqueous electrolytes. However, the influence of these materials at the catalyst–electrode interface is currently not well understood. In this study, PEI-based electrolytes were prepared and their impact on the morphology of a silver electrode performing electrochemical CO 2 reduction (CO 2 R) was studied using in situ electrochemical atomic force microscopy (EC-AFM). The presence of PEI on the electrode surface could be distinguished based on nanomechanical properties (DMT modulus), and changes were observed as negative polarization was applied, revealing a reorganization of the PEI chains due to electrostatic interactions. These changes were impacted by the electrolyte composition, including the addition of supporting electrolyte KHCO 3 salt, as well as CO 2 captured by the PEI-based electrolyte, which minimized the change in surface mechanical properties and degree of PEI alignment on the electrode surface. The changes in surface mechanical properties were also dependent on the PEI polymer length, with higher molecular weight PEI showing different reconfiguration than the shorter polymer brushes. The study highlights that the choice of polymer material, the electrolyte composition, and CO 2 captured impact the nearelectrode environment, which has implications for CO 2 R, and presents EC-AFM as a new tool that can be used to probe the dynamic behavior of these interfaces during electrocatalysis.
Phenomena Important in Molten Salt Reactor Simulations
The U.S. Nuclear Regulatory Commission (NRC) is preparing for the future licensing of advanced reactors that will be very different from current light water reactors. Part of the NRC preparation strategy is to identify the simulation tools that will be used for confirmatory safety analysis of normal operation and abnormal situations in those reactors. This report advances that strategy for reactors that will use molten salts (MSRs). This includes reactors with the fuel within the salt as well as reactors using solid fuel. Although both types are discussed in this report, the emphasis is on those reactors with liquid fuel because of the perception that solid-fuel MSRs will be significantly easier to simulate. These liquid-fuel reactors include thermal and fast neutron spectrum alternatives. The specific designs discussed in the report are a subset of many designs being considered in the U.S. and elsewhere but they are considered the most likely to submit information to the NRC in the near future. The objective herein, is to understand the design of proposed molten salt reactors, how they will operate under normal or transient/accident conditions, and what will be the corresponding modeling needs of simulation tools that consider neutronics, heat transfer, fluid dynamics, and material composition changes in the molten salt. These tools will enable the NRC to eventually carry out confirmatory analyses that examine the validity and accuracy of applicant’s calculations and help determine the margin of safety in plant design.
Production and Injection data for NV Binary facilities
Excel files are provided with well production and injection data for binary facilities in Nevada. The files contain the data that reported montly to the Nevada Bureau of Mines and Geology (NBMG) by the facility operators. this data has been complied into Excel spreadsheets for each of the facilities given on the NBMG web site.