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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Tailoring Solvation Solvent in Localized High-Concentration Electrolytes for Lithium||Sulfurized Polyacrylonitrile

Sulfurized polyacrylonitrile (SPAN) is a promising cathode material for lithium-sulfur (Li-S) batteries due to its significantly reduced polysulfide (PS) dissolution compared to the elemental S cathode. Although conventional carbonate-based electrolytes is stable with SPAN electrodes, it is less stable with Li metal anode (LMA). Recently, localized high-concentration electrolytes (LHCEs) have been developed to improve the stability of LMA. Here, we report a new strategy to further improve the performance of LI||SPAN batteries by replacing the conventional solvating solvent 1,2-dimethoxyethane (DME) in the LHCE with a new solvating solvent, 1,2-diethoxyethane (DEE), the new LHCEs exhibits less reactivity against Li 2 S 2 , alleviates PS dissolution, forms a better cathode-electrolyte interphase layer on the SPAN, and enhances structure reversibility even at elevated temperature (ET, 45°C). With the same salt and diluent as in other LHCEs, the LHCE with DEE leads to better performance in Li||SPAN batteries (with 82.9% capacity retention after 300 cycles at ET), preservation of SPAN cathode structure, and suppression of the volume change of LMA. The similar strategy on tailoring the solvating solvents in LHCEs can also be used in other rechargeable batteries to improve their performances.

1,2-diethoxyethane↗
DOE OSTI2015

PdCu Nanoalloy Electrocatalysts in Oxygen Reduction Reaction: Role of Composition and Phase State in Catalytic Synergy

The catalytic synergy of nanoalloy catalysts depends on the nanoscale size, composition, phase state, and surface properties. This report describes findings of an investigation of their roles in the enhancement of electrocatalytic activity of PdCu alloy nanoparticle catalysts for oxygen reduction reaction (ORR). In this work Pd n Cu 100–n nanoalloys with controlled composition and subtle differences in size and phase state were synthesized by two different wet chemical methods. Detailed electrochemical characterization was performed to determine the surface properties and the catalytic activities. The atomic-scale structures of these catalysts were also characterized by high-energy synchrotron X-ray diffraction coupled with atomic pair distribution function analysis. The electrocatalytic activity and stability were shown to depend on the size, composition, and phase structure. With Pd n Cu 100–n catalysts from both methods, a maximum ORR activity was revealed at Pd/Cu ratio close to 50:50. Structurally, Pd 50 Cu 50 nanoalloys feature a mixed phase consisting of chemically ordered (body-centered cubic type) and disordered (face-centered cubic type) domains. The phase-segregated structure is shown to change to a single phase upon electrochemical potential cycling in ORR condition. While the surface Cu dissolution occurred in PdCu catalysts from the two different synthesis methods, the PdCu with a singlephase character is found to exhibit a tendency of a much greater dissolution than that with the phase segregation. Analysis of the results, along theoretical modeling based on density functional theory calculation, has provided new insights for the correlation between the electrocatalytic activity and the catalyst structures.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Boosting the Oxygen Evolution Reaction by Tuning the Interfacial Iron Adsorption on Layered Double Hydroxide

Understanding the interaction between ions in the electrolyte and electrode materials plays an important role in optimizing the water electrolysis performance for hydrogen production. Herein, the synergistic effect of iron (Fe) in the electrolyte and interlayer anions within the layered structure on the oxygen evolution reaction (OER) has been investigated by combining material synthesis with controlled structure, multiple characterization techniques, and first-principles calculations. Nickel aluminum layered double hydroxides (NiAl-LDHs) with different interlayer anions (CO 3 2– , Cl – , and Br – ) show similar oxygen evolution activity in the absence of Fe species in the electrolyte. The addition of Fe into the electrolyte results in improved performance for all of the NiAl-LDHs, following the rank LDH-Br > LDH-Cl > LDH-CO 3 , under all of the conditions with varied concentration of Fe. X-ray absorption spectroscopy and identical location electron microscopy analyses show that the LDH structure remains unchanged after the OER activity test, while in situ stationary probe rotating disk electrode inductively coupled plasma mass spectrometry (SPRDE-ICP-MS) measurements show partial dissolution of the intercalating halide ions during cycling, with less dissolution for Br-intercalated materials. Insights from theoretical calculations demonstrate the thermodynamic preference of Br – to remain intercalated in the presence of Fe, while the stronger adsorption of Fe(OH) 3 species on the LDH-Br sample promotes the OER activity. In conclusion, these results provide mechanistic insights into the rational design of active layered materials with an enhanced OER performance for efficient water electrolysis.

58 GEOSCIENCES↗
DOE OSTI2018

High-Rate and Long-Term Cycle Stability of Li–S Batteries Enabled by Li 2 S/TiO 2 -Impregnated Hollow Carbon Nanofiber Cathodes

The high theoretical energy density of lithium-sulfur (Li-S) batteries makes them an alternative battery technology to lithium ion batteries. However, Li-S batteries suffer from low sulfur loading, poor charge transport, and dissolution of lithium polysulfide. Here, we use the lithiated S, Li 2 S, as the cathode material, coupled with electrospun TiO 2 -impregnated hollow carbon nanofibers (TiO 2 -HCFs), which serve as the conductive agent and protective barrier for Li 2 S in Li-S batteries. TiO 2 -HCFs provide much improved electron/ionic conductivity and serve as a physical barrier, which prevents the dissolution of lithium polysulfides. The Li 2 S/TiO 2 -HCF composite delivers a discharge capacity of 851 mA h g Li2S -1 at 0.1C and the bilayer TiO 2- HCFs/Li 2 S/TiO 2- HCF composite delivers a high specific capacity of 400 mA h g Li2S -1 at 5C.

25 ENERGY STORAGE↗
DOE OSTI2023

Pt Nanoparticles on Atomic-Metal-Rich Carbon for Heavy-Duty Fuel Cell Catalysts: Durability Enhancement and Degradation Behavior in Membrane Electrode Assemblies

Proton exchange membrane fuel cells (PEMFCs) are a promising zero-emission power source for heavy-duty vehicles (HDVs). However, long-term durability of up to 25,000 h is challenging because current carbon support, catalyst, membrane, and ionomer developed for traditional light-duty vehicles cannot meet the stringent requirement. Therefore, understanding catalyst degradation mechanisms under the HDV condition is crucial for rationally designing highly active and durable platinum group metal (PGM) catalysts for high-performance membrane electrode assemblies (MEAs). Herein, we report a PGM catalyst consisting of platinum nanoparticles with a high content (40 wt %) on atomic-metal-site (e.g., MnN 4 )-rich carbon support. MEAs with the Pt (40 wt %)/Mn–N–C cathode catalyst achieved significantly enhanced performance and durability, generating 1.41 A cm –2 at 0.7 V under HDV conditions (0.25 mgPt cm –2 and 250 kPa abs pressure) and retaining 1.20 A cm –2 after an extended and accelerated stress test up to 150,000 voltage cycles. Electron microscopy studies indicate that most fine Pt nanoparticles are retained on or/and in the carbon support covered with the ionomer throughout the catalyst layer at the end of life. During the long-term stability test, the observed electrochemical active surface area reduction and performance loss primarily result from Pt depletion in the catalyst layer due to Pt dissolution and redeposition at the interface of the cathode and membrane. Importantly, the first-principle density functional theory calculations further reveal a support entrapment effect of the Mn–N–C, in which the MnN 4 site can specifically adsorb the Pt atom and further retard the Pt dissolution and migration, therefore enhancing long-term MEA durability.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Sorption and Oxidative Degradation of Small Organic Molecules on Mn-Oxides-Effects of pH and Mineral Structures

Manganese (Mn)-oxides regulate carbon (C) cycling in soils by sorbing and oxidizing organic compounds. The composition of soil organic matter varies widely, and little is known about the reactivity of individual organic compounds with structurally diverse Mn-oxides under various environmentally relevant pH conditions. Here, in this study, we examined the affinity of six organic compounds for three Mn-oxides, comprised of layer (birnessite and hydrous Mn oxide HMO) or tunnel (cryptomelane) structures, at acidic (pH 4), slightly acidic (pH 6), and slightly alkaline (pH 8) conditions. Cryptomelane, with a higher specific surface area and point of zero charge, showed higher reactivity than that of HMO and birnessite. Interestingly, these Mn-oxides, although different in structures, decomposed each organic compound to form the same products. Citrate, pyruvate, ascorbate, and catechol induced reduction and dissolution of Mn-oxides. After the reaction, the average oxidation state of Mn in the solids was much lower at pH 4 than at pH 6 and 8, suggesting more reduction under more acidic conditions. Even when reacting with phthalate and propanol, which only sorbed to Mn-oxides but did not degrade, there was proton-promoted Mn dissolution under acidic conditions. These results suggest the significance of environmental pH and mineral structures in affecting the Mn–organic interactions and provide fundamental insights into a better understanding of the roles of Mn-oxides in regulating soil C cycling.

58 GEOSCIENCES↗
DOE OSTI2017

Solubility Model for Ferrous Iron Hydroxide, Hibbingite, Siderite, and Chukanovite in High Saline Solutions of Sodium Chloride, Sodium Sulfate, and Sodium Carbonate

Here, a solubility model is presented for ferrous iron hydroxide (Fe(OH) 2 (s)), hibbingite (Fe 2 Cl(OH) 3 (s)), siderite (FeCO 3 (s)), and chukanovite (Fe 2 CO 3 (OH) 2 (s)). The Pitzer activity coefficient equation was utilized in developing the model to account for the excess free energies of aqueous species in the background solutions of high ionic strength. Solubility limiting minerals were analyzed before and after experiments using X-ray diffraction. Formation of Fe(OH) 2 (s) was observed in the experiments that were initiated with Fe 2 Cl(OH) 3 (s) in Na 2 SO 4 solution. Coexistence of siderite and chukanovite was observed in the experiments in Na 2 CO 3 + NaCl solutions. Two equilibrium constants that had been reported by us for the dissolution of Fe(OH) 2 (s) and Fe 2 Cl(OH) 3 (s) (Nemer et al.) were rederived in this paper, using newer thermodynamic data selected from the literature to maintain internal consistency of the series of our data analyses in preparation, including this paper. Three additional equilibrium constants for the following reactions were determined in this paper: dissolution of siderite and chukanovite and dissociation of the aqueous species Fe(CO 3 ) 2 –2 . Five Pitzer interaction parameters were derived in this paper: β (0) , β (1) , and C φ parameters for the species pair Fe +2 /SO 4 –2 ; β (0) and β (1) parameters for the species pair Na+/Fe(CO3)2–2. Our model predicts that, among the four inorganic ferrous iron minerals, siderite is the stable mineral in two WIPP-related brines (WIPP: Waste Isolation Pilot Plant), i.e., GWB and ERDA6 (Brush and Domski), and the electrochemical equilibrium between elemental iron and siderite provides a low oxygen fugacity (10 –91.2 atm) that can keep the actinides at their lowest oxidation states. (Nemer et al., Brush and Domski; references numbered 1 and 2 in the main text).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

Effects of Phosphonate Structures on Brine–Biotite Interactions under Subsurface Relevant Conditions

Phosphonates have been widely used as scale inhibitors in energy-related subsurface operations, where their performance is greatly affected by interactions with rocks and minerals. However, information about commonly used phosphonate scale inhibitor–shale interactions is limited. In this study, using Fe-bearing mica (biotite) as a model phyllosilicate mineral, the effects of three common phosphonates, namely, iminodi(methylene)phosphonate (IDMP), nitrilotris(methylene)phosphonate (NTMP), and diethylenetriaminepenta(methylene)phosphonate (DTPMP), were studied at 95 °C and 102 atm CO2. During the experiments (0–70 h), IDMP remained stable, while NTMP and DTPMP were degraded and released phosphate, formate, and new phosphonates with smaller molecular weights. As a result of the differences in complexation capability, IDMP, with the fewest phosphonate functional groups, promoted biotite dissolution mainly through surface complexation and DTPMP, with the most functional groups, promoted biotite dissolution mainly through aqueous complexation. Furthermore, the presence of phosphonates enhanced secondary precipitation of P-, Fe-, and Al-bearing minerals, and their phosphonate structures affected the morphologies, phases, and distributions of secondary precipitates. Owing to phosphonate–biotite interactions (mainly as a result of surface adsorption), the biotite surfaces became much more hydrophilic. This study provides new insights into structure-dependent phosphonate–mineral interactions, and the results have important implications for the safety and efficiency of energy-related subsurface operations.

bio-inspired, mechanical behavior, carbon sequestr↗
DOE OSTI2019

Energetics and the Role of Defects in Fe(II)-Catalyzed Goethite Recrystallization from Molecular Simulations

Goethite is one of the most stable and common iron (III) minerals at the Earth’s near surface. However, recent isotope- tracer studies suggest that goethite continuously recrystallizes in the presence of aqueous Fe(II) ions. Such studies often indicate the presence of two regimes of atom exchange kinetics, a rapid stage assigned to reactive defect sites initially available at particle surfaces, followed by slower continuous exchange. An autocatalytic solid-state electron conduction model coupling Fe(II) oxidative adsorption to its reductive release at spatially distinct sites has been proposed, but the thermodynamic driving force has yet to be pinpointed. Here, using a novel hybrid/reactive molecular simulation method, for goethite (110) surfaces at circumneutral pH, we rigorously tested whether surface free energy minimization, including examining the role of structural defects, is sufficient to overcome the activation energy for interfacial electron transfer and conduction. The simulations quantitatively show that: (i). on smooth stable surfaces the available thermal energy at dynamic equilibrium is sufficient to sustain the slow continuous regime of atom exchange kinetics via short intra-surface electron conduction pathways of 1-2 nm (3-5 Fe site hops); (ii). in this slower regime, the model converges to atom exchange kinetics of 10 -5 Fe s -1 cm -2 , a rate recently deduced from stochastic modeling of experimental data and linked to the reductive dissolution rate of goethite; (iii). the driving force for initially rough defective goethite surfaces to smoothen can accelerate atom exchange to an extent quantitatively consistent with that observed in the initial rapid stage, in this case accessing conduction pathways of up to 8 nm. The findings suggest that the interaction of Fe(II) with initially defective goethite surfaces can drive, by the conduction model, atom exchange that is capable of recrystallizing the interiors of nanoscale particles, and that, closer to equilibrium on smooth surfaces, slower atom exchange continues in perpetuity but likely involving only the outermost atomic layers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

Chemical Trapping of CO2 by Clay Minerals at Reservoir Conditions: Two Mechanisms Observed by In Situ High Pressure and Temperature Experiments

The reaction of clay minerals in sedimentary rocks with supercritical CO2-rich fluids is poorly understood, but has potential implications for enhanced oil and gas production and geological C-sequestration. Experiments performed in situ at temperature and pressure relevant to reservoir conditions (T = 323 K and Pfluid = 90 bar) show that trioctahedral clay minerals can react with supercritical CO2 to produce carbonate phases by both ion exchange/precipitation reactions and dissolution/reprecipitation on a timescale of hours under certain conditions. The dissolution/reprecipitation reactions were observed in a synthetic, high surface area/high edge site surface area smectite (laponite) exchanged with Ca2+, Cs+, and tetramethyl ammonium (TMA+), and the ion exchange/precipitation mechanism was observed for a Pb-exchanged natural smectite (hectorite). Novel X-ray diffraction and NMR and infrared spectroscopic tools provide in situ observation of the reactions in real time supported by a suite of ex situ analyses. For the laponites, IR data show that HCO3- ion forms at water contents as small as ~5 H2O molecules/exchangeable cation. When the exchangeable cation is Ca2+, the IR data show the formation of carbonate as well, and the NMR results show formation of amorphous calcium carbonate at low water contents in addition to HCO3-. Laponites equilibrated at 100% R.H. at atmospheric conditions and then exposed to scCO2 generate additional, more mobile HCO3- ion and exhibit evidence of clay dissolution leading to a poorly crystalline or amorphous hydrous magnesium carbonate/bicarbonate that forms from Mg2+ released by dissolution of the octahedral sheet. The 100% R.H. sample with exchangeable Ca2+ also forms calcite, vaterite and aragonite precipitates. Comparison of these results with those already published in the literature suggest that a high edge site surface area is crucial to this process occurring on a short timescale. In the Pb-exchanged hectorite exposed to scCO2, once a critical humidity threshold is reached, cerussite (PbCO3) rapidly forms concurrent with exchange of interlayer Pb2+ with H3O+ formed by reaction of CO2 with water on the clay surface. Given that such a reaction is not observed on a similar timescale with more common Ca2+ or Na+ in hectorite and other smectites, the low solubility of cerussite appears to be the thermodynamic driving force for this process, meaning that such reactions are expected to occur more slowly in most natural samples. However, the results suggest that both types of CO2-capturing processes could occur on short and/or geological timescales during CO2 flooding of oil and gas reservoirs, in C-sequestration reservoirs, and as the result of fracking using CO2-based fluids.

Bowers, Geoffrey M.↗
DOE OSTI2025

Electrochemical Behavior of Cerium at an Indium Tin-Doped Oxide Electrode in Acidic Media

The redox behavior and speciation of cerium at mesoporous thin films composed of nanoparticles of indium tin-doped oxide (nITO) electrodes were characterized in pH 4.8, 0.1 M acetate buffer and both 0.1 and 1 M HNO 3 using electrochemical techniques and X-ray photoelectron spectroscopy. Anodic deposition of ceria species from Ce(III) to the nITO electrode was achieved under all solvent conditions via spontaneous condensation of electrochemically generated ceric hydroxide species. In 1 M nitric acid, the rate of CeO 2 dissolution is on the same order as CeO 2 deposition, resulting in negligible amounts of CeO 2 electrodeposited at the nITO surface. The cathodic stripping of CeO 2 from the nITO substrate deposited in 0.1 M nitric acid or pH 4.8 acetate buffer follows a 2-step process where Ce(IV)-oxide is initially reduced to an unstable Ce(III)-oxide species that rapidly undergoes acid catalyzed dissolution to yield soluble Ce(III) (aq) . These findings provide a foundation for the pH and anodic potential controlled deposition of CeO 2 thin films to ITO substrates, which can aid in the development of materials composed of ceria. As a result, they can also be used to infer likely analogous actinide redox behavior and speciation at these electrodes.

Cerium↗
DOE OSTI2021

Chemical Modulation of Local Transition Metal Environment Enables Reversible Oxygen Redox in Mn-Based Layered Cathodes

Oxygen redox plays a prominent role in enhancing the energy density of Mn-based layered cathodes. However, understanding the factors affecting the reversibility of oxygen redox is nontrivial due to complicated structural and chemical transformations. Here in this paper, we show that local Mn–O symmetry induced structural/chemical evolutions majorly dictate the reversibility of oxygen redox of Na x Li y Mn 1–y O 2 in Na cells. Na x Li y Mn 1–y O 2 with Jahn–Teller distorted MnO 6 octahedra undergoes severe Mn dissolution during cycling, which destabilizes the transition metal layer resulting in poor Li retention and irreversible oxygen redox. Jahn–Teller distortion of MnO 6 octahedra can be suppressed by modulating the local charge of Mn and Mn–O distance through Mg/Ti dual doping. This leads to reduced Mn dissolution and more reversible oxygen redox. Such stabilization significantly improves the electrochemical performance of Mg/Ti dual doped Na x Li y Mn 1–y O 2 . Through this work, we show that local structural stabilization through local chemical environment modification can promote reversible oxygen redox in layered cathodes.

25 ENERGY STORAGE↗
DOE OSTI2022

Dual Passivation of Cathode and Anode through Electrode–Electrolyte Interface Engineering Enables Long-Lifespan Li Metal–SPAN Batteries

The reliability and durability of lithium metal (Li 0 )–sulfur batteries are largely limited by the undesired Li 0 plating-stripping irreversibility and the detrimental polysulfide dissolution, yet approaches that can simultaneously address the above anodic and cathodic problems are scarce. In this study, we report the stable operation of a Li 0 -SPAN (sulfurized polyacrylonitrile) battery via an anode–cathode dual-passivation approach. By combination of a fluorinated localized high concentration electrolyte (LHCE) and a Li 3 N-forming additive (TMS-N 3 ), robust and highly conductive electrode passivation layers are formed in situ on the surface of both the Li 0 anode and the SPAN cathode. The resulting highly reversible, dendrite-free, and high-density Li 0 plating morphology enables a high Coulombic efficiency of 99.4%. Advanced tender energy X-ray spectroscopy also reveals the eliminated Li 2 S formation and minimized polysulfide dissolution in SPAN cathodes, leading to a high capacity of 580 mAh/g SPAN and stable cycling with negligible capacity decay (0.7%) for 800 cycles. This electrode–electrolyte interphase engineering strategy has tackled the major limitations of Li–S batteries in both ether- and carbonate-based electrolyte systems and under a wide temperature range from –10 to +50 °C, thus providing insightful guidelines for the rational design of highly durable and high-energy-density Li 0 -S batteries.

25 ENERGY STORAGE↗
DOE OSTI2016

Sparingly solvating electrolytes for high energy density Lithium–sulfur batteries

Moving to lighter and less expensive battery chemistries compared to lithium-ion requires the control of energy storage mechanisms based on chemical transformations rather than intercalation. Lithium sulfur (Li/S) has tremendous theoretical specific energy, but contemporary approaches to control this solution-mediated, precipitation-dissolution chemistry requires using large excesses of electrolyte to fully solubilize the polysulfide intermediate. Achieving reversible electrochemistry under lean electrolyte operation is the only path for Li/S to move beyond niche applications to potentially transformational performance. An emerging topic for Li/S research is the use of sparingly solvating electrolytes and the creation of design rules for discovering new electrolyte systems that fundamentally decouple electrolyte volume from reaction mechanism. Furthermore, this perspective presents an outlook for sparingly solvating electrolytes as the key path forward for longer-lived, high-energy density Li/S batteries including an overview of this promising new concept and some strategies for accomplishing it.

25 ENERGY STORAGE↗
DOE OSTI2024

Physical and Electrochemical Characterization of Aluminum Electrodes during Electrocoagulation

Electrocoagulation (EC) of synthetic groundwater was conducted using a sacrificial aluminum electrode in a flow-through EC reactor with short retention times (<1 min) under varying hydrodynamic and electrochemical conditions. The treated water was allowed to settle for 24 h and achieved silicate removal of up to 50 ± 4%, and hardness removal of 11 ± 1%. Physical, chemical, and electrochemical characterization was performed to explore changes in electrode surface morphology and composition. Electrochemical impedance spectroscopy (EIS) showed that chemical reactions at the electrode/water interface are sensitive to changes in the immediate chemical environment. We demonstrate that the most energy-intensive step in EC is aluminum dissolution at the anode, which remained fairly constant due to the continuous renewal of the anode’s surface, a result of aluminum dissolution. At the cathode, a structural change in the oxide layer, from γ-Al 2 O 3 to gibbsite, was detected by grazing-incidence X-ray diffraction, which decreased the resistance to charge transfer at the cathode surface, resulting in decreased electrode resistance. The high flow rate in the system minimized the accumulation of aluminum hydroxide solids and aluminum ions at the electrode/water interface, which minimized the formation of thick scalants and amorphous Al(OH) 3 on the cathode and anode, respectively. In conclusion, it was further demonstrated by EIS that under these conditions the resistance to charge transfer was constant throughout the duration of the experiment.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Cast Film Production with Polyethylene Recycled from a Post-Industrial Printed Multilayer Film by Solvent-Targeted Recovery and Precipitation

The solvent-targeted recovery and precipitation (STRAP) process separates and recovers the constituent resins in multilayer plastic packaging films by selective polymer dissolution. In this work, three different experimental methods were considered to recover a polyethylene (PE) resin from a printed multilayer film by STRAP. The methods consisted of (1) a filter bag system, (2) a Soxhlet extraction, and (3) a jacketed dissolution vessel. Cast films were produced with the PE recovered from each method and were analyzed for color, mechanical properties, and number of impurities. High-quality recycled PE cast films can be produced by increasing the solvent to plastic ratio, including a filter pore size of 100 μm, and optimizing temperature control in STRAP. Furthermore, this study demonstrates that STRAP polymers can be recycled back into plastic films, enabling the potential circularity of these packaging materials.

36 MATERIALS SCIENCE↗