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At least 397 records · Page 22

Influence of crossover on capacity fade of symmetric redox flow cells

Volumetrically unbalanced compositionally symmetric cell cycling with potentiostatic (CV) or galvanostatic-with-potential-hold (CCCV) protocols is a rigorous technique for evaluating the calendar lifetime of reactants for redox flow batteries. Here, we evaluate the influence of reactant crossover through the membrane on symmetric cell cycling behavior. We tested symmetric cells of anthraquinone disulfonic acid (AQDS) with Nafion membranes of varied thickness and manufacture (NR211, NR212, N115, and N117, ranging 25–183 μm). Membranes were tested both as-received and pretreated with a common procedure of soaking in water at elevated temperature and then in dilute hydrogen peroxide. We found no significant difference in capacity fade rates of symmetric cells with any of the membranes as-received, indicating a negligible influence of crossover. However, we observed increased capacity fade with increased permeability through pretreated membranes. Supported by zero-dimensional modeling and operando UV-vis spectrophotometry, we propose a mechanism for net crossover in AQDS symmetric cells based on a higher time-averaged concentration of quinhydrone dimers in the non-capacity limiting side (NCLS) compared to the capacity limiting side (CLS), driving net crossover of AQDS reactants out of the CLS. Further, we illustrate other hypothetical scenarios of net crossover using the zero-dimensional model. Overall, many membrane–electrolyte systems used in symmetric cell studies have sufficiently low crossover flux as to avoid the influence of crossover on capacity fade, but under conditions of higher crossover flux, complex interactions of crossover and chemical reactions may result in diverse capacity fade trajectories, the mechanisms of which may be untangled with operando characterization and modeling.

25 ENERGY STORAGE↗

A Free-Standing Boron-Doped Diamond Grid Electrode for Fundamental Spectroelectrochemistry

Spectroelectrochemistry (SEC) is a powerful technique that enables a variety of redox properties to be studied, including formal potential (E o ), thermodynamic values (ΔG, ΔH, ΔS), diffusion coefficient (D), electron transfer stoichiometry (n), and others. SEC requires an electrode which light can pass through while maintaining sufficient electrical conductivity. This has been traditionally composed of metal or metal oxide films atop transparent substrates like glass, quartz, or metallic mesh. Robust electrode materials like boron-doped diamond (BDD) could help expand the environments in which SEC can be performed, but most designs are limited to thin films (~100–200 nm) on transparent substrates less resilient than free-standing BDD. Here, this work presents a free-standing BDD grid electrode (G-BDD) for fundamental SEC measurements, using the well-characterized Fe(CN) 6 3–/4– redox couple as proof-of-concept. With a combination of cyclic voltammetry (CV), thin-layer SEC, and chronoabsorptometry, several of the redox properties mentioned above were calculated and compared. For E o' , n, and D, similar results were obtained when comparing the CV [E o' = +0.279 (±0.002) V vs Ag/AgCl; n = 0.97; D = 4.1 × 10 –6 cm 2 ·s –1 ] and SEC [E o' = +0.278 (±0.001) V vs Ag/AgCl; n = 0.91; D = 5.2 × 10 –6 cm 2 ·s –1 ] techniques. Both values align with what has been previously reported. To calculate D from the SEC data, modification of the classical equation used in chronoabsorptometry was required to accommodate the G-BDD electrode geometry. Overall, this work expands on the applicability of SEC techniques and BDD as a versatile electrode material.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Deciphering the Oxygen Absorption Pre-edge: A Caveat on its Application for Probing Oxygen Redox Reactions in Batteries

The pre-edges of oxygen-K X-ray absorption spectra have been ubiquitous in transition metal (TM) oxide studies in various fields, especially on the fervent topic of oxygen redox states in battery electrodes. However, critical debates remain on the use of the O-K pre-edge variations upon electrochemical cycling as evidences of oxygen redox reactions, which has been a popular practice in the battery field. This study presents an investigation of the O-K pre-edge of 55 oxides covering all 3d TMs with different elements, structures, and electrochemical states through combined experimental and theoretical analyses. It is shown unambiguously that the O-K pre-edge variation in battery cathodes is dominated by changing TM-d states. Furthermore, the pre-edge enables a unique opportunity to project the lowest unoccupied TM-d states onto one common energy window, leading to a summary map of the relative energy positions of the low-lying TM states, with higher TM oxidation states at lower energies, corresponding to higher electrochemical potentials. The results naturally clarify some unusual redox reactions, such as Cr 3+/6+ . This work provides a critical clarification on O-K pre-edge interpretation and more importantly a benchmark database of O-K pre-edge for characterizing redox reactions in batteries and other energy materials.

36 MATERIALS SCIENCE↗

Promotion and Tuning of the Electrochemical Reduction of Hetero‐ and Homobimetallic Zinc Complexes**

Abstract Compounds containing multiple metals attract significant interest due to the useful redox and reactivity properties of such species. Here, the electrochemical properties of a family of macrocyclic complexes that feature a zinc(II) center paired with a secondary redox‐inactive metal cation in heterobimetallic (Na + , Ca 2+ , Nd 3+ , Y 3+ ) motifs or homobimetallic (Zn 2+ ) motifs have been investigated. The new complexes were prepared via a divergent strategy, isolated, and structurally characterized with single‐crystal X‐ray diffraction (XRD) analysis. XRD results show that the structures of the complexes are modulated by the identity of the incorporated secondary metal ions. Cyclic voltammetry data reveal that ligand‐centered reduction is promoted in the bimetallic complexes and that the paired metal ions synergistically influence the redox properties of the complexes. Similar to prior work from our group and others, the bimetallic complexes containing stronger Lewis acids undergo more significant reduction potential shifts; contrasting with prior work on complexes containing redox‐active metals, however, the zinc(II) complexes studied here display faster electron transfer (as judged by lower reorganization energies, λ) when incorporating di‐ or tri‐valent Lewis acids in contrast to monovalent (and more weakly acidic) sodium. The quantified trends in these data offer insights that could help distinguish metal‐ versus ligand‐centered reduction of bimetallic complexes.

Kelsey, Shaun R.↗

Thermodynamic Limits of Redox-Based Thermochemical Processes (REDOTHERM)

Solar thermochemical fuel production is a potential pathway for the production of sustain liquid drop-in fuels, which can help decarbonize the aviation and maritime sectors. In an attempt to analyze the commercial viability of this technology, several studies have been conducted, including system and technoeconomic analysis (TEA) modeling. However, most studies to date simply assume a given redox reactor efficiency, which is significantly higher than demonstrated values to date. While it is widely recognized that utilizing a counter-current flow (CF) configuration could increase the redox reactor efficiency, an over-simplification in the thermodynamic modeling may lead to unphysical results which has been included in multiple publications. The fact that the solar redox reactor is the least developed component in the process chain makes it hard to identify technology gaps and evaluate pathways to deployment at scale using this approach. In this work, a thermodynamic model for a moving oxide system has been developed, in a general form that allows to analyze the system for different redox-active materials, under a wide range of operating conditions, for both parallel and countercurrent flows. The model capabilites are demonstrated, and the model's code will be shared as an open-source on GitHub in the next few months.

chemical looping↗

The impact of alkali‐ion intercalation on redox chemistry and mechanical deformations: Case study on intercalation of Li, Na, and K ions into FePO 4 cathode

Abstract Batteries made of charge carriers from Earth‐crust abundant materials (e.g., Na, K, and Mg) have received extensive attention as an alternative to Li‐ion batteries for grid storage. However, a lack of understanding of the behavior of these larger ions in the electrode materials hinders the development of electrode structures suitable for these large ions. In this study, we investigate the impact of alkali ions (Li, Na, and K) on the redox chemistry and mechanical deformations of iron phosphate composite cathodes by using electrochemical techniques and in situ digital image correlation. Na‐ion and Li‐ion intercalation demonstrate a nearly linear correlation between electrochemical strains and the state of charge and discharge. The strain development shows nonlinear dependance on the state of charge and discharge for K ions. Strain rate calculations show that K ion intercalation results in a progressive increase in the strain rate for all cycles. Li and Na intercalation induce nearly constant strain rates with the exception of the first discharge cycle of Na intercalation. When the same amount of ions are inserted into the electrode, the electrode shows the lowest strain generation upon Li intercalation compared to larger alkali ions. Na and K ions induce similar volumetric changes in the electrode when the state of charge and discharge is around 30%. Although the electrode experiences larger absolute strain generation at the end of the discharge cycles upon Na intercalation, strain rates were found to be greater for K ions. Potential‐dependent behaviors also demonstrate more sluggish redox reactions during K intercalation, compared to Li and Na. Our quantitative analysis suggests that the strain rate, rather than the absolute value of strain, is the critical factor in amorphization of the crystalline electrode.

25 ENERGY STORAGE↗

Photocatalytic Oxidation of Dissolved Mn 2+ by TiO 2 and the Formation of Tunnel Structured Manganese Oxides

The redox reaction of manganese (Mn) is of great environmental, geological, and public health significance, as Mn oxides control the distribution and electron flow of numerous nutrients and contaminants in natural and engineered environments. Current understanding on the oxidation pathways of Mn(II) to Mn(III/IV) mainly focuses on biotic processes due to their much higher oxidation rates than those of abiotic processes. This study demonstrates rapid photocatalytic oxidation of Mn 2+ (aq) under circumneutral conditions catalyzed by naturally abundant semiconducting TiO 2 minerals. Notably, the photocatalytic oxidation rates are comparable to or even higher than those of reported biotic/abiotic processes. In addition, the rapid photocatalytic oxidation leads to the formation of large tunnel structured Mn oxides (todorokite and romanechite) on the surface of TiO 2 . These findings suggest that photocatalytic oxidation of Mn 2+ (aq) by natural semiconducting minerals is likely an important yet previously overlooked pathway for understanding the occurrence of natural Mn oxide coatings on rock surfaces. In addition, considering the increasing input of photoreactive engineered nanoparticles into environmental systems, this work shows the potential impacts of nanoparticles on influencing natural redox cycles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Unlocking the Potential of A-Site Ca-Doped LaCo 0.2 Fe 0.8 O 3-δ : A Redox-Stable Cathode Material Enabling High Current Density in Direct CO 2 Electrolysis

Massive carbon dioxide (CO 2 ) emission from recent human industrialization has affected the global ecosystem and raised great concern for environmental sustainability. The solid oxide electrolysis cell (SOEC) is a promising energy conversion device capable of efficiently converting CO 2 into valuable chemicals using renewable energy sources. However, Sr-containing cathode materials face the challenge of Sr carbonation during CO 2 electrolysis, which greatly affects the energy conversion efficiency and long-term stability. Thus, A-site Ca-doped La1– x CaxCo 0.2 Fe 0.8 O 3-δ (0.2 ≤ x ≤ 0.6) oxides are developed for direct CO 2 conversion to carbon monoxide (CO) in an intermediate-temperature SOEC (IT-SOEC). With a polarization resistance as low as 0.18 O cm 2 in pure CO 2 atmosphere, a remarkable current density of 2.24 A cm –2 was achieved at 1.5 V with La 0.6 Ca 0.4 Co 0.2 Fe 0.8 O 3-δ (LCCF64) as the cathode in La 0.8 Sr 0.2 Ga 0.83 Mg 0.17 O 3-δ (LSGM) electrolyte (300 µm) supported electrolysis cells using La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3-δ (LSCF) as the air electrode at 800 °C. Furthermore, symmetrical cells with LCCF64 as the electrodes also show promising electrolysis performance of 1.78 A cm –2 at 1.5 V at 800 °C. In addition, stable cell performance has been achieved on direct CO 2 electrolysis at an applied constant current of 0.5 A cm –2 at 800 °C. The easily removable carbonate intermediate produced during direct CO 2 electrolysis makes LCCF64 a promising regenerable cathode. The outstanding electrocatalytic performance of the LCCF64 cathode is ascribed to the highly active and stable metal/perovskite interfaces that resulted from the in situ exsolved Co/CoFe nanoparticles and the additional oxygen vacancies originated from the Ca 2 Fe 2 O 5 phase synergistically providing active sites for CO 2 adsorption and electrolysis. Here this study offers a novel approach to design catalysts with high performance for direct CO 2 electrolysis.

30 DIRECT ENERGY CONVERSION↗

Systems and methods of long-duration energy storage and regeneration of energy-bearing redox pairs

Described herein are systems and methods of storing and delivering electrical using hydrogen at low-cost and for long-durations. The systems and methods use energy-bearing redox pairs that electrochemically bear energy through decoupled hydrogen and oxygen consumption and/or evolution reactions, which are typically associated with fuel cells. Each species of the energy-bearing redox pair is associated with a standard electrode potential within a water electrolysis voltage window for the electrolyte solution. Electrical energy delivery, hydrogen generation, electrolyte regeneration, or combinations thereof can be performed by logically or physically separated unit operations in a continuous manner, batch manner, or semi-batch manner facilitated by the energy-bearing redox pair.

08 HYDROGEN↗

Iodine Immobilization by Materials through Sorption and Redox-Driven Processes: A Literature Review

Radioiodine-129 (129I) in the subsurface is mobile and limited information is available on treatment technologies. Scientific literature was reviewed to compile information on materials that could potentially be used to immobilize 129I through sorption and redox-driven processes, with an emphasis on ex-situ processes. Candidate materials to immobilize 129I include iron minerals, sulfur-based materials, silver-based materials, bismuth-based materials, ion exchange resins, activated carbon, modified clays, and tailored materials (metal organic frameworks (MOFS), layered double hydroxides (LDHs) and aerogels). Where available, compiled information includes material performance in terms of (i) capacity for 129I uptake; (ii) long-term performance (i.e., solubility of a precipitated phase); (iii) technology maturity; (iv) cost; (v) available quantity; (vi) environmental impact; (vii) ability to emplace the technology for in situ use at the field-scale; and (viii) ex situ treatment (for media extracted from the subsurface or secondary waste streams). Because it can be difficult to compare materials due to differences in experimental conditions applied in the literature, Part II of this review describes results of laboratory studies for selected materials using a standardized batch loading test.

Moore, Robert C.↗

Single‐Site, Single‐Metal‐Atom, Heterogeneous Electrocatalyst: Metal–Organic‐Framework Supported Molybdenum Sulfide for Redox Mediator‐Assisted Hydrogen Evolution Reaction

Abstract Synthesis of single‐site catalysts, whereby the local structure and surrounding chemical environments are identical, has been challenging, particularly in heterogeneous catalysis, as the support often presents spectrum of chemically distinct binding sites. Yet, the above criteria are crucial in attributing the apparent catalytic performance to the structural motif. The presented work augments on our previous work using monometallic molybdenum sulfide tethered within a zirconium‐based metal‐organic framework (MOF), NU‐1000; the monometallic nature enables all presented sites to be catalytically addressable. As the molybdenum sulfide species resided within two distinct pores (micro‐ and mesopores) of the MOF support, we have imparted uniformity in the local chemical environment by reducing the pore heterogeneity down to a single mesopore. Single‐site and single‐atom nature of the candidate catalyst was established via X‐ray diffraction measurements. Redox mediators were implemented, which, under reductive potentials, provide reduced species; they can effectively deliver the necessary reducing equivalences to the catalytic units that can otherwise not be addressed electrochemically due to the low electron mobility within the framework. Our results indicate the micropore‐allocated molybdenum sulfide is approximately four times more active as that in mesopores, whereas its catalytic mechanism is identical, underscoring the importance of controlling chemical environment beyond the active site.

Noh, Hyunho↗

Multi-omics of NET formation and correlations with CNDP1, PSPB, and L-cystine levels in severe and mild COVID-19 infections

We report that we performed a multi-omics analysis of an immunologically naïve SARS-CoV-2 clinical cohort to characterize overall changes in plasma among control (uninfected), mild, and severe infections. A comparison of healthy controls and patient samples showed activation of neutrophil degranulation pathways. Consistent with this observation, we characterized neutrophil extracellular trap (NET) complexes that were partially initiated in a subset of the mild infections (showing partially formed NETs) and fully-formed NETs in a subset of severe infections (containing multiple NET proteins in individual patient samples). As a potential mechanism to suppress NET formation, multiple redox enzymes were elevated in the mild and severe population. Analysis of metabolites from the same cohort showed a 24 and 60-fold elevation in plasma L-cystine, the oxidized form of cysteine and substrate of the powerful antioxidant glutathione in mild and severe patients, respectively. Unique to patients with mild infections, the carnosine dipeptidase modifying enzyme (CNDP1) was up-regulated. The strong protein and metabolite oxidation signatures suggest multiple compensatory pathways working to suppress both free radical and NET formation in SARS-CoV-2 infections.

60 APPLIED LIFE SCIENCES↗

Iron-rich microstructure records of high temperature multi-component silicate melt behavior in nuclear fallout

Above-ground nuclear explosions that interact with the surface of the earth entrain materials from the surrounding environment, influencing the resulting physical and chemical evolution of the fireball, which can affect the final chemical phase and mobility of hazardous radionuclides that are dispersed in the environment as fallout particles. The interaction of iron with a nuclear explosion is of specific interest due to the potential for iron to act as a redox buffer and because of the likelihood of significant masses of metals to be present in urban environments. We investigated fallout from a historic surface interacting nuclear explosion conducted on a steel tower and report the discovery of widespread and diverse iron-rich micro-structures preserved within the samples, including crystalline dendrites and micron-scale iron-rich spheres with liquid immiscibility textures. We assert these micro-structures reflect local redox conditions and cooling rates and can inform interpretation of high temperature events, enabling new insights into fireball condensation physics and chemistry when metals from the local environment (i.e. structural steel) are vaporized or entrained. Finally, these observations also significantly expand the availability of silicate immiscibility datasets applicable to rapidly quenched systems such as meteorite impact melt glass.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

On the Structural Origin of Fast Li-Ion Cycling in Tetragonal Bronze-Type Nb 8 W 9 O 47

Bronze and bronze-derived, mixed metal oxides are materials of growing interest for lithium-ion battery anodes due to their high-rate capabilities and the potential for high energy densities via multielectron redox. We report on the synthesis and electrochemical properties of the tetragonal tungsten bronzetype phase Nb 8 W 9 O 47 and our investigation into the structural evolution of this phase upon lithium (de)intercalation, with particular attention to how it relates to the fast-cycling capabilities. Electrochemical cycling shows Nb 8 W 9 O 47 can achieve greater than one Li + per transition metal at rates of C/2 or slower and maintains a capacity equivalent to 0.65 Li + per transition metal at a rate of 20C. Sequential Rietveld analysis of operando X-ray diffraction data reveals anisotropic changes to the unit cell parameters during discharge, accompanied by an off-centering of the transition metals within their octahedral environments. While higher capacities can be accessed below 1.2 V, cells discharged to 1.0 V exhibit a significant expansion of the unit cell volume and reduced Coulombic efficiencies. This report suggests that rigid crystal structures incapable of undergoing polyhedral rotational deformations can instead exploit displacive distortions of the transition metal redox center to enable fast Li-ion cycling with minimal atomic rearrangements.

25 ENERGY STORAGE↗

Subsurface hydrocarbon degradation strategies in low- and high-sulfate coal seam communities identified with activity-based metagenomics

Environmentally relevant metagenomes and BONCAT-FACS derived translationally active metagenomes from Powder River Basin coal seams were investigated to elucidate potential genes and functional groups involved in hydrocarbon degradation to methane in coal seams with high- and low-sulfate levels. An advanced subsurface environmental sampler allowed the establishment of coal-associated microbial communities under in situ conditions for metagenomic analyses from environmental and translationally active populations. Metagenomic sequencing demonstrated that biosurfactants, aerobic dioxygenases, and anaerobic phenol degradation pathways were present in active populations across the sampled coal seams. In particular, results suggested the importance of anaerobic degradation pathways under high-sulfate conditions with an emphasis on fumarate addition. Under low-sulfate conditions, a mixture of both aerobic and anaerobic pathways was observed but with a predominance of aerobic dioxygenases. The putative low-molecular-weight biosurfactant, lichysein, appeared to play a more important role compared to rhamnolipids. The methods used in this study—subsurface environmental samplers in combination with metagenomic sequencing of both total and translationally active metagenomes—offer a deeper and environmentally relevant perspective on community genetic potential from coal seams poised at different redox conditions broadening the understanding of degradation strategies for subsurface carbon.

59 BASIC BIOLOGICAL SCIENCES↗

A multi-omic characterization of the physiological responses to salt stress in Scenedesmus obliquus UTEX393

Scenedesmus obliquus UTEX393 is a promising microalgal candidate for sustainable biomanufacturing but its limited halotolerance hinders large-scale cultivation in saline environments. To investigate the molecular basis of salt stress responses, we conducted a comprehensive multi-omic analysis integrating genomics, transcriptomics, proteomics, lipidomics, metabolomics, and DNA affinity purification sequencing (DAP-seq). An improved nuclear genome assembly and annotation yielded 19,017 gene models and a 97% BUSCO completeness score, enabling construction of a genome-scale metabolic model. Comparing 15 ppt salinity stress to 5 ppt control, growth and productivity were significantly reduced, accompanied by widespread transcriptomic and proteomic changes. Transcriptomic analysis revealed downregulation of photosynthetic machinery and energy conservation genes, and upregulation of stress-responsive elements such as expansins, flavodoxins, and osmoprotectants. Lipidomic profiling showed accumulation of triacylglycerols (TAGs) and degradation of galactosyl lipids, consistent with a shift toward lipid biosynthesis to mitigate redox imbalance. Depletion of key polar metabolites and branched-chain amino acids suggested a rerouting of central carbon metabolism under stress. DAP-seq identified key transcription factors, including LHY1 and SPL12, that target central metabolic enzymes involved in redox balancing, such as glyceraldehyde-3-phosphate dehydrogenase (GAPDH) and malate dehydrogenase (MDH). These findings establish a regulatory-metabolic framework linking redox stress to lipid accumulation and reveal potential engineering targets to enhance salt tolerance. Overall, the multi-omic analysis supports the “overflow” hypothesis, where impaired photosynthesis results in excess reducing equivalents being diverted into TAG synthesis and highlights transcriptional regulators as candidates for improving algal robustness in brackish environments.

09 BIOMASS FUELS↗

Mathematical Framework Underlying the In Situ Electrochemical Diagnosis of Adsorbed Intermediates Formed during Redox Reactions at Electrode Surfaces

Previously, we have presented an electrochemical technique wherein an electroactive tracer species is employed to probe the rate-limiting factors governing redox reactions at an electrode surface. In this technique, the electrode is first held potentiostatically to facilitate a redox process (step 1), and then the potential is released to open circuit conditions (step 2) so as to monitor the time-dependent re-equilibration of the electrode potential in the presence of the tracer. The time-dependent potential response in step 2 has been shown to contain information about diffusion—limited or desorption—limited steps, enabling in situ probing of the electrochemistry at the electrode surface during step 1. In the present contribution, a theoretical model governing the transient response in step 2 is developed for two limiting cases: diffusion—limited and desorption—limited recovery of the electrode potential. Mathematical modeling shows that, during re-equilibration, the step 2 potential transient corresponding to a case where step 1 involves surface adsorbed species which undergo desorption in step 2 exhibits a much longer time constant than that when re-equilibration occurs under diffusion limitations. The mathematical framework presented herein provides a sound fundamental basis for applying the aforementioned technique to studying adsorption-desorption processes during electrochemistry. Also, technique limitations are presented in light of the modeling findings.

25 ENERGY STORAGE↗