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At least 289 records · Page 16

Triggering Anionic Redox Activity in Li 3 NbS 4 Through Cationic Disordering or Substitution

Extensive utilization of Li-ion batteries for varieties of applications necessitates ceaseless improvements of electrode materials for achieving higher energy density. Towards this goal, Li-rich layered oxides exhibiting high capacity due to cumulated cationic and anionic redox activities are under study for nearly a decade. Still, several unanswered questions remain with respect to these Li-driven anionic redox reactions in terms of the activation process and long-term consequences upon cycling. Here, the Li-rich Li 3 NbS 4 phase is focused, and synthesized as two different polymorphs, namely ordered and disordered phases. From analyses of their chemical and electrochemical properties, a crystal-electronic structure relationship is unraveled that triggers the anionic redox activity in these compounds. Moreover, through complementary theoretical calculations, the capability of cationic disorder to trigger anionic redox activity via the hybridization of cationic and non-bonding anionic energy levels is shown. This finding is further supported by the appearance of anionic redox activity by introducing the disorder through cationic substitution. Altogether, the insights derived here can help in designing new anionic redox materials with optimum performances for practical applications.

25 ENERGY STORAGE↗

Iron-iminopyridine complexes as charge carriers for non-aqueous redox flow battery applications

Non-aqueous redox flow batteries (RFBs) have been gaining increased attention in the energy storage arena. Some of their attractive features include the promise for high energy densities, wider voltage windows compared to aqueous systems, as well as wider operating temperature ranges. One of the major challenges in the development of these systems is the lack of electroactive materials that can undergo reversible redox events within the larger potential window of organic solvents. In this paper, we present the design, synthesis, and measurement of electrochemical properties of some iron-based imine- and iminopyridine complexes as promising candidates for RFB applications. Synthesized complexes afforded three reversible redox couples over a ~3 V range. The redox events were also computationally explored and are in good agreement with experimental data. Theoretical calculations show that the redox event at the positive potential can be characterized as metal-centered event corresponding to Fe 3+ → Fe 2+ reduction, while the two redox events at negative potentials are associated with the consecutive reductions of iminopyridine or diimine moieties. This work has led to the identification of a promising anolyte material, [tris(imino)pyridine)Fe][OTf] 2 (1), which is soluble in acetonitrile and is synthesized in two simple steps. This species shows outstanding performance when cycled between 1.0 V and 2.35 V, with 93% coulombic efficiency, 84% energy efficiency, and a capacity decay rate of 0.61% per cycle at 5 mA cm –2 . Further modifications to this kind of charge carrier may lead to the development of high energy density materials for grid scale energy storage applications.

25 ENERGY STORAGE↗

Fluorination Enables Simultaneous Improvements of a Dialkoxybenzene-Based Redoxmer for Nonaqueous Redox Flow Batteries

Redoxmers or redox-active organic materials, arc one critical component for nonaqueous redox flow batteries (RFBs), which hold high promise in enabling the time domain of the grid. While tuning redox potentials of redoxmers is a very effective way to enhance energy densities of NRFBs, those improvements often accompany accelerated kinetics of the charged species, undermining stability and cycling performance. In this paper, a strategy for designing redoxmers with simultaneous improvements in redox potential and stability is proposed. Specifically, the redoxmer 1,4-di-tert-butyl-2,5-bis(2,2,2-trifluoroethoxy)benzene (ANL-C46) is developed by incorporating fluorinated substitutions into the dialkoxybenzene-based platform. Compared to the non-fluorinated analogue, ANL-C46 demonstrates not only an increased (similar to 0.41 V) redox potential but also much enhanced stability (1.6 times) and cyclability (4 times) evidenced by electron paramagnetic resonance kinetic study, H-cell and flow cell cycling. In fact, the cycling performance of ANL-C46 is among the best of high potential (>1.0 V vs Ag/Ag + ) redoxmers ever reported. Density functional theory calculations suggest that while the introduced fluorine substitutions elevate the redox potentials, they also help to depress the decomposition reactions of the charged redoxmers, affording excellent stability. The findings represent an interesting strategy for simultaneously improving energy density and stability, which could further prompt the development of high-performance redoxmers.

25 ENERGY STORAGE↗

Heterometallic Ce IV / V V Oxo Clusters with Adjustable Catalytic Reactivities

Heterometallic Ce IV /M oxo clusters are underexplored yet and can benefit from synergistic properties from combining cerium and other metal cations to produce efficient redox catalysts. Herein, we designed and synthesized a series of new Ce 12 V 6 oxo clusters with different capping ligands: Ce 12 V 6 -SO 4 , Ce 12 V 6 -OTs (OTs: toluenesulfonic acid), and Ce 12 V 6 -NBSA (NBSA: nitrobenzenesulfonic acid). Single crystal X-ray diffraction (SCXRD) for all three structures reveals a Ce 12 V 6 cubane core formulated [Ce 12 (VO) 6 O 24 ] 18+ with cerium on the edges of the cube, vanadyl capping the faces, and sulfate on the corners. While infrared spectroscopy (IR), ultraviolet–visible spectroscopy (UV–vis), electrospray ionization mass spectrometry (ESI-MS), and proton nuclear magnetic resonance ( 1 H NMR) proved the successful coordination of the organic ligands to the Ce 12 V 6 core, liquid phase 51 V NMR and small-angle X-ray scattering (SAXS) confirmed the integrity of the clusters in the organic solutions. Furthermore, functionalization of the Ce 12 V 6 core with organic ligands both provides increased solubility in term of homogeneous application and introduces porosity to the assemblies of Ce 12 V 6 -OTs and Ce 12 V 6 -NBSA in term of heterogeneous application, thus allowing more catalytic sites to be accessible and improving reactivity as compared to the nonporous and less soluble Ce 12 V 6 -SO 4 . Meanwhile, the coordinated ligands also influenced the electronic environment of the catalytic sites, in turn affecting the reactivity of the cluster, which we probed by the selective oxidation of 2-chloroethyl ethyl sulfide (CEES). Furthermore, this work provides a strategy to make full use of the catalytic sites within a class of inorganic sulfate capped clusters via organic ligand introduction.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Partitioning of Fe(II) in reduced nontronite (NAu-2) to reactive sites: Reactivity in terms of Tc(VII) reduction

Abstract Clay minerals impart important chemical properties to soils, in part, by virtue of changes in the redox state of Fe in their crystal structures. Therefore, measurement of Fe(III)/Fe(II) and partitioning of Fe(II) in different reactive sites in clay minerals (during biological and chemical Fe(III) reduction) is essential to understand their role and their relative reactivity in terms of reduction and immobilization of heavy metal contaminants such as technetium. This study had three objectives: (1) to understand the degree of dissolution of nontronite (Fe-rich smectite) as a result of chemical and biological reduction of Fe(III) in the structure; (2) to quantify partitioning of chemically and biologically produced Fe(II) into different reactive sites in reduced nontronite, including aqueous Fe 2+ , ammonium chloride-extractable Fe(II) (mainly from the ion-exchangeable sites, denoted as Fe ( II ) NH 4 Cl ${\rm{Fe}}{\left( {{\rm{II}}} \right)_{{\rm{N}}{{\rm{H}}_4}{\rm{Cl}}}}$ ), sodium acetate-extractable Fe(II) (mainly from the surface complexation sites, denoted as Fe(II) acetate ), and structural Fe(II) (denoted as Fe(II) str ); and (3) to evaluate the reactivity of these Fe(II) species in terms of Tc(VII) reduction. Chemical and biological reduction of Fe(III) in nontronite (NAu-2) was performed, and reduced nontronite samples with different extents of Fe(III) reduction (1.2–71%) were prepared. The extent of reductive dissolution was measured as a function of the extent of Fe(III) reduction. Our results demonstrated that chemically and biologically produced Fe(II) in NAu-2 may be accommodated in the NAu-2 structure if the extent of Fe(III) reduction is small (< ∼30%). When the extent of reduction was >∼30%, dissolution of nontronite occurred with a corresponding decrease in crystallinity of residual nontronite. The Fe(II) produced was available for partitioning into four species: Fe ( ab ) 2 + ${\rm{Fe}}_{\left( {{\rm{ab}}} \right)}^{2 + }$ , Fe(II) acetate , Fe ( II ) NH 4 Cl ${\rm{Fe}}{\left( {{\rm{II}}} \right)_{{\rm{N}}{{\rm{H}}_4}{\rm{Cl}}}}$ , and Fe(II) str . The increase in Fe(II) acetate during the early stages of Fe(III) reduction indicated that the Fe(II) released had the greatest affinity for the surface-complexation sites, but this site had a limited capacity (∼60 µmol of Fe(II)/g of NAu-2). The subsequent increase in Fe ( II ) NH 4 Cl ${\rm{Fe}}{\left( {{\rm{II}}} \right)_{{\rm{N}}{{\rm{H}}_4}{\rm{Cl}}}}$ indicated that the released Fe(II) partitioned into the exchangeable sites once the amount of Fe at the surface-complexation sites reached half of its maximum site capacity. The fraction of Fe(II) str decreased concomitantly, as a result of Fe(II) release from the NAu-2 structure, from 100% when the extent of Fe(III) reduction was <30% to nearly 65% when the extent of Fe(III) reduction reached 71%. The Fe(II) acetate and Fe(II) str exhibited greater reactivity in terms of Tc(VII) reduction than the Fe ( II ) NH 4 Cl ${\rm{Fe}}{\left( {{\rm{II}}} \right)_{{\rm{N}}{{\rm{H}}_4}{\rm{Cl}}}}$ . Clearly, the surface-complexed and structural Fe(II) are the desirable species when reduced clay minerals are used to reduce and immobilize soluble heavy metals in contaminated groundwater and soils. These results have important implications for understanding microbe—clay mineral interactions and heavy metal immobilization in clay-rich natural environments.

54 ENVIRONMENTAL SCIENCES↗

Coupled Thermal-Hydraulic Analysis and Species Mass Transport in a Versatile Experimental Salt Irradiation Loop (VESIL) using COBRA-TF

With the resurgence of interest in Molten Salt Reactor (MSR) technology among commercial and governmental agencies, there is a need for new experiments and new modelling capabilities to characterize the unique phenomena present in this fluid fuel system. A Versatile Experimental Salt Irradiation Loop (VESIL) is currently under investigation at Idaho National Laboratory. It is designed to be a dynamic fuel-bearing salt loop placed in the Advanced Test Reactor. One of the key phenomena this proposed experiment plans to elucidate is fission product speciation in the fuel-salt and the subsequent effects this can have on fuel-salt properties, fission product transport and interactions, source term generation, corrosion and redox potential control. Specifically, noble gases (Xe & Kr) will bubble out to a plenum or off-gas system and noble metals (Mo, Tc, Te etc.) will precipitate and deposit in specific zones in the loop. This work extends the mass transfer and species interaction models in the general species transport capability of COBRA-TF (CTF) and applies these models to give a preliminary estimation of fission product behavior in the proposed VESIL design.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Inclusion of Biological Targets in the Analysis of Electrical Characteristics of Non-Thermal Plasma Discharge

In Plasma Medicine studies, the effect of non-thermal plasma (NTP) on biological targets is typically correlated with the amount of stable reactive oxygen and nitrogen species produced in a liquid medium. The effect of NTP and the response of the biological target on cellular redox mechanisms is overlooked in these investigations. Additionally, the influence of electrical properties of cells on the physical properties of NTP is neglected. Therefore, we used a floating electrode dielectric barrier discharge plasma to explore the impact of cell structure, size, and viability of the biological target on the physical properties of NTP. Lissajous figures were used to determine circuit capacitance and energy per cycle during NTP exposure of different cell suspensions. We show that both, structural integrity and active enzymic processes of cells change the electrical properties of NTP. Correlations were also drawn between NTP-produced hydrogen peroxide and nitrite with measured capacitance. Our studies indicate that the observed changes between different cell suspensions may be due to a feedback loop between the biological target and the NTP source. In future studies, a more detailed analysis is needed to improve the control of clinical NTP devices.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Stabilized Oxygen Vacancy Chemistry toward High-Performance Layered Oxide Cathodes for Sodium-Ion Batteries

Anionic redox has emerged as a transformative paradigm for high-energy layered transition-metal (TM) oxide cathodes, but it is usually accompanied by the formation of anionic redox-mediated oxygen vacancies (OVs) due to irreversible oxygen release. Additionally, external factor-induced OVs (defined as intrinsic OVs) also play a pivotal role in the physicochemical properties of layered TM oxides. However, an in-depth understanding of the interplay between intrinsic and anionic redox-mediated OVs and the corresponding regulation mechanism of the dynamic evolution of OVs is still missing. Herein, we disclose the strong interrelationship between these OVs and demonstrate that the presence of intrinsic OVs in the TMO2 layers could induce weak integrity of the TM-O frameworks and unlock additional diffusion paths to trigger the generation and migration of anionic redox-mediated OVs. Accordingly, an OV stabilization strategy is proposed by deliberately introducing high-valence Nb5+, which could serve as an important building block in anchoring the oxygen sublattice and preventing the formation of a percolating OV migration network, thereby suppressing the formation/diffusion of anionic redox-mediated OVs. Consequently, superb structural integrity and improved electrochemical performance with reversible anionic redox chemistry are achieved. This work advances our understanding of the role of OVs for developing high-performance energy storage systems utilizing anionic redox.

anionic redox↗

Atomic-Scale Structure of Chemically Distinct Surface Oxygens in Redox Reactions

During redox reactions, oxide-supported catalytic systems undergo structural and chemical changes. Improving subsequent catalytic properties requires an understanding of the atomic-scale structure with chemical state specificity under reaction conditions. For the case of 1/2 monolayer vanadia on α-TiO 2 (110), we use X-ray standing wave (XSW) excited X-ray photoelectron spectroscopy to follow the redox induced atomic positional and chemical state changes of this interface. Furthermore, while the resulting XSW 3D composite atomic maps include the Ti and O substrate atoms and V surface atoms, our focus in this report is on the previously unseen surface oxygen species with comparison to density functional theory predictions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Experimental determination of the electrochemical properties of bismuth chloride in eutectic LiCl–KCl and LiCl–KCl–CaCl 2 molten salts

Bismuth has been investigated as a potential liquid electrode for molten salt electrorefining, but the electrochemical behavior of Bi 3+ /Bi redox couple has received scant attention in LiCl–KCl and LiCl–KCl–CaCl 2 eutectics. Electroanalytical techniques were used to determine properties of Bi 3+ /Bi. Diffusivities of 6.71 and 8.93 × 10 –6 cm 2 s –1 and standard apparent potentials of 0.1166 and 0.1187 V versus Ag/AgCl (4.75 mol%) were recommended for BiCl 3 in LiCl–KCl and LiCl–KCl–CaCl 2 eutectics, respectively, at 680 ± 3.1 K. The ICP-MS analysis of BiCl 3 content limited the accuracy of the results. Furthermore, the reliability of the results improved with a more thorough drying procedure for CaCl 2 .

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Layered Transition Metal Oxides as Ca Intercalation Cathodes: A Systematic First-Principles Evaluation

Finding high-voltage Ca cathode materials is a critical step to unleashing the full potential of high-energy-density Ca-ion batteries. Therefore, first-principles calculations are used to demonstrate that P-type layered calcium transition metal (TM) oxide materials (CaTM 2 O 4 ) with a range of TM substitutions (TM = Ti, V, Cr, Mn, Fe, Co, and Ni) have excellent battery-related properties including thermodynamic stability, average voltage, energy density, synthesizability, ionic mobility, and electronic structure. However, the thermodynamic stability of the charged phase and TM redox activity are shown to be sensitive to TM selection, with CaCo 2 O 4 having the best balance of all considered properties. The utility of combining multiple TMs to expand the chemical search space for TM substitutions is demonstrated by mixing Co and Ni in layered CaTM 2 O 4 .

25 ENERGY STORAGE↗

Understanding capacity fade in organic redox-flow batteries by combining spectroscopy with statistical inference techniques

Organic redox-active molecules are attractive as redox-flow battery (RFB) reactants because of their low anticipated costs and widely tunable properties. Unfortunately, many lab-scale flow cells experience rapid material degradation (from chemical and electrochemical decay mechanisms) and capacity fade during cycling (>0.1%/day) hindering their commercial deployment. In this work, we combine ultraviolet-visible spectrophotometry and statistical inference techniques to elucidate the Michael attack decay mechanism for 4,5-dihydroxy-1,3-benzenedisulfonic acid (BQDS), a once-promising positive electrolyte reactant for aqueous organic redox-flow batteries. We use Bayesian inference and multivariate curve resolution on the spectroscopic data to derive uncertainty-quantified reaction orders and rates for Michael attack, estimate the spectra of intermediate species and establish a quantitative connection between molecular decay and capacity fade. Our work illustrates the promise of using statistical inference to elucidate chemical and electrochemical mechanisms of capacity fade in organic redox-flow battery together with uncertainty quantification, in flow cell-based electrochemical systems.

25 ENERGY STORAGE↗

Materials Design Directions for Solar Thermochemical Water Splitting

The sustainable, economical production of molecular hydrogen is a crucial component of a net zero-greenhouse-gas-emissions future. Solar thermochemical water splitting (STWS) offers a renewable route to hydrogen with the potential to help decarbonize several industries, including transportation, manufacturing, mining, metals processing, and electricity generation, as well as provide sustainable hydrogen as a chemical feedstock. STWS uses high temperatures generated from concentrated sunlight or other sustainable means for high-temperature heat to produce hydrogen and oxygen from steam. For example, in its simplest form of a two-step thermochemical cycle, a redox-active metal oxide is heated to ≈1700-2000 K, driving off molecular oxygen while producing oxygen vacancies in the material. The reduced metal oxide then cools (ideally with the extracted heat recuperated for re-use) and, in a separate step, comes into contact with steam, which reacts with oxygen vacancies to produce molecular hydrogen while recovering the original state of the metal oxide. Despite its promising use of the entire solar spectrum to split water thermochemically, the current estimated cost of hydrogen produced via STWS is ≈4-6× the U.S. Department of Energy (DOE) Hydrogen Shot target value of $1/kg. One contributing approach to bridging this cost gap is the design of new materials with improved thermodynamic properties to enable higher efficiencies. The state-of-the-art (SOA) redox-active metal oxide for STWS is ceria (CeO 2 ), due to its close to optimal, although too high, oxygen vacancy formation enthalpy and large configurational and electronic entropy of reduction. However, ceria requires high operating temperatures and its efficiency is insufficient. Therefore, efforts to increase the efficiency of STWS cycles have focused on further optimizing oxygen vacancy formation enthalpies and augmenting the reduction entropy via substitution or doping and materials discovery schemes. Examples of the latter include the perovskites BaCe 0.25 Mn 0.75 O 3 and (Ca,Ce)(Ti,Mn)O 3 . These efforts and others have revealed intuitive chemical principles for the efficient and systematic design of more effective materials, such as the strong correlation between the enthalpies of crystal bond dissociation and solid-state cation reduction with the enthalpy of oxygen vacancy formation, as well as configurational entropy augmentation via the coexistence of two or more redox-active cation sublattices. The purpose of this chapter is to prepare the reader with an up-to-date account of STWS redox-active materials, both the SOA and promising newcomers, as well as to provide chemically intuitive strategies for improving their cycle efficiencies through materials design – in conjunction with ongoing efforts in reactor engineering and gas separations – to reach the cost points for commercial viability. First, we will introduce the thermodynamics of STWS using a two-step, metal-oxide, thermochemical cycle with economics in mind. We also will compare the pros and cons of processes that do or do not involve phase changes. Second, we will describe the qualities that make ceria the SOA STWS redox-active material, as well as its limitations. Third, we will survey some of the most promising candidates to date in the search for materials to supplant ceria, emphasizing the post-ternary, metal-oxide-perovskite alloys. Lastly, we will enumerate and discuss the following materials design directions for STWS redox-active materials: crystal reduction potentials as a proxy for oxygen vacancy formation enthalpies, engineering the electronic and configurational entropy of reduction via f-shells and simultaneous redox, and vetting materials stability via temperature-dependent phase diagrams and melting-point prediction.

08 HYDROGEN↗

Electronic Structure Distortions in Chromium Chelates Impair Redox Kinetics in Flow Batteries

Aminopolycarboxylate chelates are emerging as a promising class of electrolyte materials for aqueous redox flow batteries, offering tunable redox potentials, solubility, and pH stability through careful selection of ligands and transition metal ions. Despite their potential, the impact of molecular structure modifications on the electronic and electrochemical properties of these chelates remains underexplored. Here, in this study, we examine how introducing a hydroxyl group, often employed for its solubilizing properties, to the backbone of CrPDTA, a reference chelate material, significantly changes the thermodynamics and kinetics of the chelate's redox process. We correlate changes in molecular and electronic structures to different electrochemical responses resulting from the hydroxyl addition and show that the introduction of this functional group leads to a distortion in the octahedral coordination of chromium. Furthermore, increased anisotropic spin density and nonintegral oxidation state changes in the Cr metal center result in a larger barrier for electron transfer in CrPDTA‐OH. It is demonstrated that preserving a hexacoordinate chelate structure across a broad pH range is crucial for efficient flow battery application and it is emphasized that ligand modifications must avoid distorting the octahedral coordination of the transition metal.

25 ENERGY STORAGE↗

Dynamical Change of Valence States and Structure in NiCu 3 Nanoparticles during Redox Cycling

Alloyed materials are promising candidates to improve catalytic processes. Ni–Cu nanoparticles are used for various reactions, including processes with biomass-derived components. However, dynamical restructuring effects alter the catalytic properties and can deactivate the sample. To understand these structural modifications, a multimodal investigation of NiCu 3 /C was performed to determine compositional and morphological changes during a redox cycle to simulate reduction and oxidation of the catalyst during reaction. We exploit a novel correlative, multimodal approach that combines in situ X-ray absorption spectroscopy (XAS) and in situ scanning transmission electron microscopy and electron energy-loss spectroscopy (STEM-EELS) to describe changes that occur in the sample in realistic conditions. In the fresh sample, there are two morphologies present: core–shell and hollow. Segregation of Cu was observed in both types of particles after synthesis, with Cu being more oxidized in the hollow structures. Upon reduction for 2 h under H 2 at 400 °C, the Cu was reduced, although segregation of Cu and Ni was still observed. Subsequent exposure to O 2 at 400 °C led to a strong reoxidation of Cu with the formation of hollow particles with compositional heterogeneities. The oxidation of metals and segregation phenomena can be related to known catalytic properties of NiCu 3 /C particles, especially regarding the hydrodeoxygenation of 5-hydroxymethylfurfural to 2,5-dimethylfuran.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗