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At least 397 records · Page 22

Polymer Dynamics in Block Copolymer Electrolytes Detected by Neutron Spin Echo

Polymer chain dynamics of a nanostructured block copolymer electrolyte, polystyrene- block -poly(ethylene oxide) (SEO) mixed with lithium bis(trifluoromethanesulfonyl)imide (LiTFSI) salt, are investigated by neutron spin echo (NSE) spectroscopy on the 0.1–100 ns time scale and analyzed using the Rouse model at short times ( t ≤ 10 ns) and the reptation tube model at long times ( t ≥ 50 ns). In the Rouse regime, the monomeric friction coefficient increases with increasing salt concentration, as seen previously in homopolymer electrolytes. In the reptation regime, the tube diameters, which represent entanglement constraints, decrease with increasing salt concentration. The normalized longest molecular relaxation time, calculated from the NSE results, increases with increasing salt concentration. We argue that quantifying chain motion in the presence of ions is essential for predicting the behavior of polymer-electrolyte-based batteries operating at large currents.

25 ENERGY STORAGE↗

Effects of catholyte aging on high-nickel NMC cathodes in sulfide all-solid-state batteries

Sulfide solid-state electrolytes (SSEs) in all-solid-state batteries (SSBs) are recognized for their high ionic conductivity and inherent safety. The LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811) cathode offers a high thermodynamic potential of approximately 3.8 V vs. Li/Li + and a theoretical specific capacity of 200 mA h g −1 . However, the practical utilization of NMC811 in sulfide SSBs faces significant interfacial challenges. The oxidation instability of sulfide solid electrolytes against NMC811 and the formation of the cathode electrolyte interphase (CEI) during cycling lead to degradation and reduced cell performance. Volumetric changes in NMC during lithiation and de-lithiation can also cause detachment from sulfide electrolytes or internal particle cracking. Despite extensive galvanostatic cycling studies to address the issues, the calendar life of sulfide SSBs remains poorly understood. Here, we systematically studied the effects of four different catholytes on the calendar aging of LiNbO 3 (LNO)-coated NMC811, including Li 6 PS 5 Cl (LPSCl), Li 3 InCl 6 –Li 6 PS 5 Cl (LIC–LPSCl), Li 3 YCl 6 –Li 6 PS 5 Cl (LYC–LPSCl), and Li 10 GeP 2 S 12 (LGPS). Our results indicate that LPSCl provides optimal capacity retention when stored at high state-of-charge (SOC) at room temperature, but the LIC–LPSCl cathode shows significant capacity degradation and chemical incompatibility. We also established an effective electrochemical calendar aging testing protocol to simulate daily usage, enabling quick inference of the calendar life of SSBs. In conclusion, this new testing approach accelerates materials selection strategies for high-nickel NMC composite cathodes in sulfide SSBs.

25 ENERGY STORAGE↗

Polysilaketals: High‐Performance Polyether‐Based Electrolytes with Tunable Disubstituted Silane Linkers

Abstract Polymer electrolytes exhibit higher energy density and improved safety in lithium‐ion batteries relative to traditionally used liquid electrolytes but are currently limited by their lower electrochemical performance. Aiming to access polymer electrolytes with competitive electrochemical properties, we developed the anionic ring‐opening polymerization (AROP) of cyclic silaketals to synthesize amorphous silicon‐containing polyether‐based electrolytes with varying substituent bulk of the general formula [OSi(R) 2 (CH 2 CH 2 O) 2 ] n (R=alkyl, phenyl). As opposed to previously reported uncontrolled polycondensation routes toward low molecular weight polysilaketals, AROP allows access to targeted molecular weights above the entanglement threshold of the polymers. The polysilaketal with the lowest steric bulk (P(OSi Me,Me ‐2EO)) exceeds the conductivity of poly(ethylene oxide) (PEO), a leading polymer electrolyte. To the best of our knowledge, this is the first solid polymer electrolyte to achieve this benchmark. Steric bulk in polysilaketals was found to impart stability and two bulkier polysilaketals, P(OSi Et,Et ‐2EO) and P(OSi Me,Ph ‐2EO), exhibited higher current fractions than PEO over a wide range of salt loadings. Moreover, the efficacy of P(OSi Et,Et ‐2EO) was competitive with that of PEO. Taken together, the tunable and competitive electrochemical properties of polysilaketals validate the systematic incorporation of silyl groups as a strategy to access high performance polymer electrolytes.

Rugh, Haley J.↗

Effects of Plasticizer Content and Ceramic Addition on Electrochemical Properties of Cross-Linked Polymer Electrolyte

The development of a safe electrolyte is the key to improving energy density for next generation lithium batteries. In this work, UV-crosslinked poly(ethylene oxide) (PEO) -based polymer and composite electrolytes are systematically investigated on their ionic conductivity, mechanical and electrochemical properties. The polymer electrolytes are plasticized with non-flammable linear short-chain PEO. In the composite electrolytes, a doped lithium aluminum titanium phosphate (LATP) ceramic, LICGC™, is used as the ceramic filler. It is found that the addition of the plasticizer leads to a tradeoff between ion transport and mechanical properties. In contrast, the addition of ceramic fillers improves both the ionic conductivity and mechanical properties. The sample with 20 wt% of LICGC™ shows a conductivity of ~0.6 mS cm –1 at 50 °C. This sample also demonstrates much longer cycle life than the neat polymer electrolyte in Li platting/stripping test with a capacity of 1 mAh cm –2 . Further, a full cell made with this composite electrolyte against Li metal anode and high voltage LiNi 0.6 Mn 0.2 Co 0.2 O 2 cathode shows 94% capacity retention after 30 cycles, compared to 58% capacity retention with the neat polymer electrolyte. These results demonstrate that a hybrid of polymer/ceramic/non-flammable plasticizer is a promising path to high energy density, high voltage lithium batteries.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

SISGR: Chemomechanics of Far-From-Equilibrium Interfaces (COFFEI)

Portable, reliable, and deployable devices for energy storage and conversion require fundamental changes in design of solid-state composites comprising ceramics and metals. These materials comprise the electrodes and electrolytes of next-generation solid-oxide fuel cells and all solid-state batteries, forming solid-state functional composites. The advent of solid-state batteries – which replace liquid electrolytes with solid electrolytes capable of lithium ion transport for reliable energy storage in portable batteries – and the increased demand space for all solid-state fuel cells capable of oxygen reduction at intermediate temperatures remain important challenges for improved material stability and decreased system cost. However, little is understood about three fundamental facets of materials that enable such solid-state energy applications. First, how do such materials deform, fracture, or delaminate under operando conditions? Second, how does such mechanical deformation limit or facilitate electronic and ionic transport within and across such material interfaces? Third, how we can predictably design interface-rich composites to engineer both structural and electrochemical stability? This COFFEI Group comprised expertise from Materials Science & Engineering and Nuclear Science & Engineering to integrate unique in situ experiments, simulations, and fabricated interfaces that address these fundamental questions in solid-state interfaces of nanoscale composites that will guide solid-state electrochemistry, transport kinetics, and mechanical deformation for nonstoichiometric materials that enable such applications. In particular, we built on COFFEI’s understanding of chemomechanical coupling among defect concentrations, ionic transport, electron transport, and stored elastic energy that is particularly acute in the far-from-equilibrium conditions typical of energy device applications. By tailoring our focus to solid-state interfaces, we addressed these important issues by (a) developing and applying advanced in situ and ex situ characterization tools to characterize model materials and interfaces synthesized with molecular-level control, under both laboratory-controlled and extreme environments representative of energy device operation; and (b) employing computational modeling and simulation frameworks to predict transport mechanisms, reactivity and stability of these model materials and interfaces under significant chemical strains typical of energy device operation. Recent progress provided insights to additional materials systems and electrochemomechanical fatigue and fracture that were not fully envisioned when the program was initiated. Specifically, in the final three years of COFFEI we pursued two integrated thrusts, with complementary focus. Thrust I focused on failure-resistant electrochemomechanical composites, while Thrust II focused on strain-modulated conductivity and reactivity across interfaces. In contrast to our initial COFFEI focus, these thrusts concentrated wholly on solid-state material interfacial interactions and included greater integration of multiscale visualization including in situ electron microscopy of strained structures/interactions and mesoscale simulations. Successful development of functionally superior and long-lived battery and fuel cell systems and stress adaptable oxides requires a deeper, fundamental understanding of the coupling among the historically important subfields of solid-state electrochemistry, transport kinetics, and mechanical deformation for nonstoichiometric metal oxide electrodes. In this program, the understanding and the application of chemomechanical coupling of defect concentrations, ionic transport, electro-catalytic activity and stored elastic energy, particularly acute in the far-from-equilibrium conditions typical of energy device applications, are being refined and implications for device operation clarified, including for miniaturized solid-state batteries and fuel cells.

36 MATERIALS SCIENCE↗

Electrode Design for Low Temperature Direct-Hydrocarbon Solid Oxide Fuel Cells

In certain embodiments of the present disclosure, a solid oxide fuel cell is described. The solid oxide fuel cell includes a hierarchically porous cathode support having an impregnated cobaltite cathode deposited thereon, an electrolyte, and an anode support. The anode support includes hydrocarbon oxidation catalyst deposited thereon, wherein the cathode support, electrolyte, and anode support are joined together and wherein the solid oxide fuel cell operates a temperature of 600.degree. C. or less.

Chen, Fanglin↗

Mechanistic origin of solvent-dependent thermal stability in sodiated Sn anodes for sodium-ion batteries

Understanding the thermal stability of high-energy density alloy anodes is critical for the safe deployment of sodium-ion batteries (SIBs). Here, accelerating rate calorimetry (ARC), post-mortem characterizations, and density functional theory (DFT) calculations are combined to understand the thermal reactivity of fully sodiated Sn, Sn-hard carbon (HC) blends, and HC anodes in carbonate- and ether-based electrolytes. ARC measurements show that propylene carbonate (PC) causes earlier self-heating rate (SHR) onset and higher reactivity than tetraethylene glycol dimethyl ether (TEGDME), indicating inferior thermal stability. Sodiated Sn exhibits better thermal stability than sodiated HC, while Sn-HC blends show intermediate behavior that improves with increasing Sn content. Post-ARC analyses reveal desodiation of Na15Sn4 to metallic Sn with particle coalescence, whereas Sn-HC blends and HC retain finer morphologies. PC promotes Sn oxidation to SnO, while TEGDME suppresses oxide formation; NaPF6-containing electrolytes additionally form NaF. DFT calculations show that PC adsorption lowers Na extraction energy and enhances interfacial electronic interactions, facilitating Na release and reductive decomposition. These results establish a direct correlation between solvent-dependent reaction pathways and thermal stability in SIB alloy anodes.

Accelerating rate calorimetry↗

Stable Solid Electrolyte Interphase Layer Formed by Electrochemical Pretreatment of Gel Polymer Coating on Li Metal Anode for Lithium–Oxygen Batteries

Lithium (Li)-oxygen (O2) batteries (LOBs) exhibit the highest theoretical specific energy density among candidates of the next-generation energy storage systems, but the instability of Li metal anode (LMA), air electrode, and electrolyte largely limit the practical energy density of these batteries. Herein, we report an effective method to protect LMA against side reactions between LMA and crossover contaminants such as highly reactive oxygen moieties. A solid electrolyte interphase (SEI) layer rich in inorganic components was formed on a LMA coated with polyethylene oxide thin-film through an in-situ electrochemical pre-charging step under oxygen atmosphere. This uniformly distributed stiff SEI layer interacted with flexible polymer matrix and formed a submicron-sized gel-like polymer layer. This polymer supported SEI layer leads to much longer cycle life (130 vs. 65 cycles) as compared to those of pristine cell under the same testing conditions (1.0 mAh cm-2 at 0.2 mA cm-2 in the voltage range of 2 to 5 V without any catalysts). It is also very effective during low voltage (2 to 4.5 V) cycling with a redox mediator (0.1 and 0.15M (2,2,6,6-tetramethylpiperidin-1-yl) oxidanyl). Therefore, this approach can be used to stabilize LMA/electrolytes interphase and improve the cycle life of rechargeable LOBs.

lithium-oxygen batteries, lithium metal anodes, ar↗

Hydrogen bonds enhanced composite polymer electrolyte for high-voltage cathode of solid-state lithium battery

Polymer electrolyte is one of the important components for developing advanced solid-state lithium batteries (SSLBs). However, the narrow electrochemical stability window restricts the practical application with high-voltage cathodes. In this study, a series of composite solid electrolytes (CSEs), possessing both wide electrochemical stability window (up to 5.0 V vs. Li + /Li) and high ionic conductivity (over 1.35×10 -3 S/cm at 25 °C), were reported by integrating SiO 2 nanoparticles into poly(vinyl ethylene carbonate) polymer electrolyte. The enhanced anti-oxidation performances are mainly caused and confirmed by the local intermolecular interactions of hydrogen bonds in CSE. Based on this CSE, the SSLBs with LiCoO 2 cathode present good cycle stability at high voltage, and the capacity retention with 4.5 V cut-off voltage is about 94% after 200 cycles. This work not only proves the importance of intermolecular interactions in CSE, but also provides an effective method for achieving high-energy SSLBs with enhanced interface compatibility between polymer electrolyte and highvoltage cathodes

25 ENERGY STORAGE↗

Study of the Segmental Dynamics and Ion Transport of Solid Polymer Electrolytes in the Semi-crystalline State

Solid polymer electrolytes are promising in fulfilling the requirements for a stable lithium metal anode toward higher energy and power densities. In this work, we investigate the segmental dynamics, ionic conductivity, and crystallinity of a polymer electrolyte consisting of poly(ethylene oxide) (PEO) and lithium triflate salt, in the semi-crystalline state. Using quasi-elastic neutron scattering, the segmental dynamics of PEO chains confined between the crystalline lamellae is quantified, using Cole–Cole analysis. We show that the structural relaxation time, τ 0 , of PEO equilibrated near room temperature is six-fold longer than the same sample that had just cooled down to room temperature. This corresponds to a three-fold smaller ionic conductivity in the equilibrated condition. This work reveals that the segmental dynamics of semi-crystalline polymer electrolytes is very sensitive to thermal history. We demonstrate that quasi-elastic neutron scattering can be used to characterize the ion transport and segmental dynamics in the semi-crystalline state.

36 MATERIALS SCIENCE↗

Novel Elastomeric Membranes Developed for Polymer Electrolytes in Lithium Batteries

Lithium-based polymer batteries for aerospace applications need to be highly conductive from -70 to 70 C. State-of-the-art polymer electrolytes are based on polyethylene oxide (PEO) because of the ability of its ether linkages to solvate lithium ions. Unfortunately, PEO has a tendency to form crystalline regions below 60 C, dramatically lowering conductivity below this temperature. PEO has acceptable ionic conductivities (10(exp -4) to 10(exp -3) S/cm) above 60 C, but it is not mechanically strong. The room-temperature conductivity of PEO can be increased by adding solvent or plasticizers, but this comes at the expense of thermal and mechanical stability. One of NASA Glenn Research Center s objectives in the Polymer Rechargeable System program (PERS) is to develop novel polymer electrolytes that are highly conductive at and below room temperature without added solvents or plasticizers.

Tigelaar, Dean M.↗

Achieving Stable Molybdenum Oxide Cathodes for Aqueous Zinc-Ion Batteries in Water-in-Salt Electrolyte

A layered MoO 3 material with large interlayer spacing represents a promising cathode for aqueous rechargeable Zn-ion batteries (ARZIBs), but the implementation of this material is limited due to the intrinsically low conductivity and poor structural stability. A 30 m ZnCl 2 water-in-salt electrolyte (WISE) was introduced to a MoO 3 nanobelt cathode for the first time, significantly increasing the stability of MoO 3 cathodes compared to those in 3 M ZnSO 4 and 3 M ZnCl2 electrolyte. The Zn/MoO 3 cell in WISE unambiguously demonstrated significantly improved rate performance delivering 349, 253, and 222 mAh/g at 100, 500, and 1000 mA/g, denoting a 2×, and 12× capacity increase of those achieved in 3 M electrolytes at 500 and 1000 mA/g, respectively. A capacity retention rate of 73% was achieved after (dis)charging at 100 mA/g for 100 cycles, and no obvious capacity fading was observed at higher current densities of 500 mA/g and 2A/g. A compilation of structural and morphological characterization was systematically performed to provide insight into the mechanisms of the improved performance in ZnCl 2 WISE for the MoO3 cathode materials. Specifically, our data collectively suggested that the drastic fading in 3M electrolytes can be attributed to the parasitic surface deposits on Zn originated from Mo dissolution and H 2 formation due to Zn corrosion and hydrogen evolution reaction (HER), which were significantly suppressed in the ZnCl 2 WISE. The direct visualization of these side reactions was achieved for the first time in the Zn-MoO 3 system, using an in situ optoelectrochemical measurement.

25 ENERGY STORAGE↗

Advances in Molten Oxide Electrolysis for the Production of Oxygen and Metals from Lunar Regolith

As part of an In-Situ Resource Utilization infrastructure to sustain long term-human presence on the lunar surface, the production of oxygen and metals by electrolysis of lunar regolith has been the subject of major scrutiny. There is a reasonably large body of literature characterizing the candidate solvent electrolytes, including ionic liquids, molten salts, fluxed oxides, and pure molten regolith itself. In the light of this information and in consideration of available electrolytic technologies, the authors have determined that direct molten oxide electrolysis at temperatures of approx 1600 C is the most promising avenue for further development. Results from ongoing studies as well as those of previous workers will be presented. Topics include materials selection and testing, electrode stability, gas capture and analysis, and cell operation during feeding and tapping.

Sadoway, Donald R.↗

Synthesis of rhenium coatings on 316 stainless steel and their electrochemical behavior towards water oxidation in saline environments

The production of electrolytic hydrogen or Green Hydrogen has attracted the attention of scientists as a potential enabler of sustainable energy production. The cleavage of the water molecule requires high energy, in order to produce hydrogen and oxygen through their corresponding half reactions, the hydrogen evolution and oxygen evolution reactions. Further, this latter reaction has been studied in more detail, since its slow kinetics make the water electrolysis less efficient, and, for instance, delay the formation of hydrogen in the counter compartment of the electrolytic cell. In this work, a study of the oxygen evolution reaction is presented. For this, a series of rhenium catalysts deposited onto stainless steel 316 are studied with the aim of analyzing the effect of the pure metal (Re) and the metal with heteroatoms (Re-C, Re-B, and Re-O). As one of the problems worldwide is the scarcity of freshwater, the study focuses on the performance of this series of catalysts in highly saline environments, representative of seawater. The synthesis and electrochemical performance is shown, giving high expectations that these electrocatalysts could be potential electrocatalysts in marine environments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Proton Relay for the Rate Enhancement of Electrochemical Hydrogen Reactions at Heterogeneous Interfaces

Proton transfer is critically important to many electrocatalytic reactions, and directed proton delivery could open new avenues for the design of electrocatalysts. However, although this approach has been successful in molecular electrocatalysis, proton transfer has not received the same attention in heterogeneous electrocatalyst design. Here, in this work, we report that a metal oxide proton relay can be built within heterogeneous electrocatalyst architectures and improves the kinetics of electrochemical hydrogen evolution and oxidation reactions. The volcano-type relationship between activity enhancement and pK a of amine additives confirms this improvement; we observe maximum rate enhancement when the pK a of a proton relay matches the pH of the electrolyte solution. Density-functional-theory-based reactivity studies reveal a decreased proton transfer energy barrier with a metal oxide proton relay. These findings demonstrate the possibility of controlling the proton delivery and enhancing the reaction kinetics by tuning the chemical properties and structures at heterogeneous interfaces.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Gas Generation in Lithium Cells with High-Nickel Cathodes and Localized High-Concentration Electrolytes

High-nickel layered-oxide cathodes (LiNi x Mn y Co 1-x-y O 2 , x ≥ 0.8) exhibit high capacities, but also experience rapid capacity fade during cycling, and are susceptible to heat generation and gas release. Advanced electrolytes, such as localized high-concentration electrolytes (LHCE), substantially stabilize the cathode during cycling and have lower flammability than conventional electrolytes, but gas generation with these electrolytes is yet to be assessed. We demonstrate here that gas generation from a high-nickel cathode in an LHCE is half as much as in a conventional electrolyte at 4.4 V. The gas generation in LHCE is further reduced at 4.3 V, but the LHCE generates a similar amount of gas as the conventional electrolyte at 4.6 V. Neither electrolyte can prevent gas generation after cycling; cathodes after 200 cycles generate similar amounts of gas as pristine cathodes during high-voltage hold. Finally, it is shown that in both electrolytes, oxygen from the cathode lattice plays a critical role in gas generation.

25 ENERGY STORAGE↗

Comparing Experimentally-Measured Sand’s Times with Concentrated Solution Theory Predictions in a Polymer Electrolyte

We compare the electrochemically measured Sand’s time, the time required for the cell potential to diverge when the applied current density exceeds the limiting current, with theoretical predictions for a 0.47 M poly(ethylene oxide) (5 kg mol −1 )/LiTFSI electrolyte. The theoretical predictions are made using concentrated solution theory which accounts for both concentration polarization and polymer motion, using independently measured parameters that depend on concentration, c : conductivity ( κ ), salt diffusion coefficient ( D ), cationic transference number with respect to the solvent velocity ( t + 0 ), thermodynamic factor 1 + dln f ± dln c , and partial molar volume of the salt ( V ̅ ); f ± is the mean molar activity coefficient of the salt. We find quantitative agreement between experimental data and theoretical predictions. We derive a generalized analytical expression for Sand’s time for electrolytes based on dilute solution theory. This expression correctly predicts the divergence of the Sand’s time at the limiting current, in agreement with experimental data and concentrated solution theory predictions. When the applied current is large compared to the limiting current, the analytical expression approaches the standard expression for Sand’s time used in the literature.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗