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All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Interphase Stabilization of LiNi 0.5 Mn 1.5 O 4 Cathode for 5 V–Class All–Solid–State Batteries

Employing high voltage cobalt-free spinel LiNi 0.5 Mn 1.5 O 4 (LNMO) as a cathode is promising for high energy density and cost-effectiveness, but it has challenges in all-solid-state batteries (ASSBs). Here, it is revealed that the limitation of lithium argyrodite sulfide solid electrolyte (Li 6 PS 5 Cl) with the LNMO cathode is due to the intrinsic chemical incompatibility and poor oxidative stability. Through a careful analysis of the interphase of LNMO, it is elucidated that even the halide solid electrolyte (Li 3 InCl 6 ) with high oxidative stability can be decomposed to form resistive interphase layers with LNMO in ASSBs. Interestingly, with Fe-doping and a Li 3 PO 4 protective layer coating, LNMO with Li 3 InCl 6 displays stable cycle performance with a stabilized interphase at a high voltage (≈4.7 V) in ASSBs. The enhanced interfacial stability with the extended electrochemical stability window through doping and coating enables high electrochemical stability with LNMO in ASSBs. Furthermore, this work provides guidance for employing high-voltage cathodes in ASSBs and highlights the importance of stable interphases to enable stable cycling in ASSBs.

25 ENERGY STORAGE↗
DOE OSTI2023

A Deep Potential model for liquid–vapor equilibrium and cavitation rates of water

Computational studies of liquid water and its phase transition into vapor have traditionally been performed using classical water models. Here, we utilize the Deep Potential methodology—a machine learning approach—to study this ubiquitous phase transition, starting from the phase diagram in the liquid–vapor coexistence regime. The machine learning model is trained on ab initio energies and forces based on the SCAN density functional, which has been previously shown to reproduce solid phases and other properties of water. Here, we compute the surface tension, saturation pressure, and enthalpy of vaporization for a range of temperatures spanning from 300 to 600 K and evaluate the Deep Potential model performance against experimental results and the semiempirical TIP4P/2005 classical model. Moreover, by employing the seeding technique, we evaluate the free energy barrier and nucleation rate at negative pressures for the isotherm of 296.4 K. Further, we find that the nucleation rates obtained from the Deep Potential model deviate from those computed for the TIP4P/2005 water model due to an underestimation in the surface tension from the Deep Potential model. From analysis of the seeding simulations, we also evaluate the Tolman length for the Deep Potential water model, which is (0.091 ± 0.008) nm at 296.4 K. Finally, we identify that water molecules display a preferential orientation in the liquid–vapor interface, in which H atoms tend to point toward the vapor phase to maximize the enthalpic gain of interfacial molecules. We find that this behavior is more pronounced for planar interfaces than for the curved interfaces in bubbles. This work represents the first application of Deep Potential models to the study of liquid–vapor coexistence and water cavitation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Suppressing electrolyte-lithium metal reactivity via Li + -desolvation in uniform nano-porous separator

Lithium reactivity with electrolytes leads to their continuous consumption and dendrite growth, which constitute major obstacles to harnessing the tremendous energy of lithium-metal anode in a reversible manner. Considerable attention has been focused on inhibiting dendrite via interface and electrolyte engineering, while admitting electrolyte-lithium metal reactivity as a thermodynamic inevitability. Here, we report the effective suppression of such reactivity through a nano-porous separator. Calculation assisted by diversified characterizations reveals that the separator partially desolvates Li + in confinement created by its uniform nanopores, and deactivates solvents for electrochemical reduction before Li 0 -deposition occurs. The consequence of such deactivation is realizing dendrite-free lithium-metal electrode, which even retaining its metallic lustre after long-term cycling in both Li-symmetric cell and high-voltage Li-metal battery with LiNi 0.6 Mn 0.2 Co 0.2 O 2 as cathode. The discovery that a nano-structured separator alters both bulk and interfacial behaviors of electrolytes points us toward a new direction to harness lithium-metal as the most promising anode.

25 ENERGY STORAGE↗
DOE OSTI2024

Hybrid Density Functional Theory Comparison of Oxygen Release and Solvent Decomposition Kinetics on Li x NiO 2 Surfaces

High-nickel-content layered oxides are among the most promising electric vehicle battery cathode materials. However, their interfacial reactivity with electrolytes and tendency toward oxygen release (possibly yielding reactive 1 O 2 ) remain degradation concerns. Elucidating the most relevant (i.e., fastest) interfacial degradation mechanism will facilitate future mitigation strategies. We apply screened hybrid density functional (HSE06) calculations to compare the reaction kinetics of Li x NiO 2 surfaces with ethylene carbonate (EC) with those of O 2 release. Further, on both the (001) and (104) facets, EC oxidative decomposition exhibits lower activation energies than O 2 release. Our calculations, coupled with previously computed liquid-phase reaction rates of 1 O 2 with EC, strongly question the role of “reactive 1 O 2 ” species in electrolyte oxidative degradation. The possible role of other oxygen species is discussed. To deal with the challenges of modeling Li x NiO 2 surface reactivity, we emphasize a “local structure” approach instead of pursuing the global energy minimum.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Modulating the Lattice Stability in Sodium-Layered Oxide Cathodes through Inductive Effect

Stability and safety of sodium layered oxide cathodes relative to lithium analogs remain a critical concern, yet its fundamental origin remains poorly understood. Here, we examine the role of sodium – oxygen bond ionicity in governing outgassing by introducing 5% lithium (Li), potassium (K), or both into layered NaNiO 2 (NNO), yielding Na 0.95 Li 0.05 NiO 2 , Na 0.95 K 0.05 NiO 2 , and Na 0.90 Li 0.05 K 0.05 NiO 2 . Online electrochemical mass spectrometry at 4.3 V reveals that K substitution increases gas evolution with similar charge capacity, whereas Li substitution reduces gas evolution by nearly 80% with only a 16% capacity decrease. Capacity-controlled experiments show that NNO must be charged to only 3.8 V (144 mA h g -1 ) to achieve gas evolution comparable to Na 0.95 Li 0.05 NiO 2 charged to 4.3 V (175 mA h g -1 ). These results demonstrate that tuning alkali-metal–oxygen bond ionicity through the inductive effect regulates Ni–O covalency, lattice oxygen stability, and interfacial reactivity, providing design guidance for safer sodium layered oxide cathodes.

25 ENERGY STORAGE↗
DOE OSTI2022

An embedded interfacial network stabilizes inorganic CsPbI3 perovskite thin films

Abstract The black perovskite phase of CsPbI 3 is promising for optoelectronic applications; however, it is unstable under ambient conditions, transforming within minutes into an optically inactive yellow phase, a fact that has so far prevented its widespread adoption. Here we use coarse photolithography to embed a PbI 2 -based interfacial microstructure into otherwise-unstable CsPbI 3 perovskite thin films and devices. Films fitted with a tessellating microgrid are rendered resistant to moisture-triggered decay and exhibit enhanced long-term stability of the black phase (beyond 2.5 years in a dry environment), due to increasing the phase transition energy barrier and limiting the spread of potential yellow phase formation to structurally isolated domains of the grid. This stabilizing effect is readily achieved at the device level, where unencapsulated CsPbI 3 perovskite photodetectors display ambient-stable operation. These findings provide insights into the nature of phase destabilization in emerging CsPbI 3 perovskite devices and demonstrate an effective stabilization procedure which is entirely orthogonal to existing approaches.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Stabilization of garnet/Li interphase by diluting the electronic conductor

The high interfacial resistance and lithium (Li) dendrite growth are two major challenges for solid-state Li batteries (SSLBs). The lack of understanding on the correlations between electronic conductivity and Li dendrite formation limits the success of SSLBs. Here, by diluting the electronic conductor from the interphase to bulk Li during annealing of the aluminium nitride (AlN) interlayer, we changed the interphase from mixed ionic/electronic conductive to solely ionic conductive, and from lithiophilic to lithiophobic to fundamentally understand the correlation among electronic conductivity, Li dendrite, and interfacial resistance. During the conversion-alloy reaction between AlN and Li, the lithiophilic and electronic conductive Li x Al diffused into Li, forming a compact lithiophobic and ionic conductive Li 3 N, which achieved an ultrahigh critical current density of 2.6/14.0 mA/cm 2 in the time/capacity-constant mode, respectively. The fundamental understanding on the effect of interphase nature on interfacial resistance and Li dendrite suppression will provide guidelines for designing high-performance SSLBs.

25 ENERGY STORAGE↗
DOE OSTI2021

Interfacial Effects on Transport Coefficient Measurements in Li-ion Battery Electrolytes

Development of Li + -containing electrolytes with improved transport properties requires reliable, reproducible, and ideally low volume techniques to rigorously understand ion-transport with varying composition. Precisely measuring the complete set of transport coefficients in liquid electrolytes under battery-relevant operating conditions is difficult and the reliability of these methods are sparsely described in electrolyte transport literature. In this work, we apply a potentiostatic polarization-based transport characterization approach typically used for polymer electrolytes to liquid electrolyte systems in an attempt to fully measure all transport coefficients (conductivity, total salt diffusion coefficient, thermodynamic factor and transference number) for the model system of LiPF 6 in an ethylene carbonate—ethyl methyl carbonate (EC:EMC) mixture. Using systematic timescale and statistical analyses, we find that transport coefficients measured using potentiostatic polarization of Li-Li symmetric cells exhibit strong correlation to Li electrode interfacial resistance, indicating that such methods are probing both bulk and interfacial phenomena. This reveals a major roadblock in characterizing electrolyte systems where the interfacial resistance is significantly larger than ohmic electrolyte resistance. As a result, we find that methods that rely on potentiostatic Li metal stripping/plating do not readily result in reliable liquid electrolyte transport coefficients, unlike similar methods for solid polymer electrolytes, where interfacial resistances are typically smaller than electrolyte resistances at the elevated temperatures typically of interest for such electrolytes.

25 ENERGY STORAGE↗
DOE OSTI2023

In-situ thermodynamics measurements at metal oxides-solution interfaces using Flow Adsorption Microcalorimetry.

Mineral-fluid interfaces are the principal sites of geochemical processes near Earth’s surface, hosting chemical reactions that play a fundamental role in (bio)geochemical cycles and in the fate and transport of anthropogenic contaminants, and that effectively control the compositions of soil and water environments. These complex interfaces are critical for our energy and environmental future. The mineral-fluid interface has been studied in an unprecedented level of detail with both experimental and computational approaches, separately and in combination. However, conspicuously missing from studies of the mineral-fluid interface are direct measurements of the energies of ion sorption and exchange. The literature on energetics and enthalpies of exchange, adsorption, dissolution, precipitation, and surface protonation reactions, especially those directly supported by experimental data, remains scarce despite their fundamental nature. The overarching goal of this project is to complete a systematic study of the thermodynamics properties of interfacial reactions at four MO surfaces (Rutile (α-TiO2), Quartz (SiO2), boehmite (γ-AlOOH) and goethite (α-FeOOH)) through the application and construction of novel flow adsorption microcalorimetry techniques and instrumentations. These unique and specialized microcalorimeters will operate at various temperatures and solution chemical compositions allowing for in-situ measurements across metal oxides and ligands of various characteristics. The overall research goal will be accomplished by completing the following three specific objectives (O): O1) Determine the energetics of surface protonation and deprotonation, ion exchange and ligand sorption reactions; O2) Investigate the surface charge thermodynamic properties under a range of temperature and solution chemical compositions; and O3) Develop predictive trends of the interplay between MO structure, surface coverage and surface reactivity. In addition to key thermodynamics parameters, calorimetric measurements provide a wealth of mechanistic information about reactions energetics and kinetics, surface charge characteristics, and structure-reactivity or selectivity relationships, all obtained in-situ and in real-time. This report includes science highlights from various projects completed over the performance period of the project. Also listed are dissemination opportunities, people supported on the grant and the impact on available physical resources and the discipline as a whole.

58 GEOSCIENCES↗
NASA NTRS2009

Calculation of Stress Intensity Factors for Interfacial Cracks in Fiber Metal Laminates

Stress intensity factors for interfacial cracks in Fiber Metal Laminates (FML) are computed by using the displacement ratio method recently developed by Sun and Qian (1997, Int. J. Solids. Struct. 34, 2595-2609). Various FML configurations with single and multiple delaminations subjected to different loading conditions are investigated. The displacement ratio method requires the total energy release rate, bimaterial parameters, and relative crack surface displacements as input. Details of generating the energy release rates, defining bimaterial parameters with anisotropic elasticity, and selecting proper crack surface locations for obtaining relative crack surface displacements are discussed in the paper. Even though the individual energy release rates are nonconvergent, mesh-size-independent stress intensity factors can be obtained. This study also finds that the selection of reference length can affect the magnitudes and the mode mixity angles of the stress intensity factors; thus, it is important to report the reference length used with the calculated stress intensity factors.

Wang, John T.↗
DOE OSTI2024

NaSICON-type materials for lithium-ion battery applications: Progress and challenges

Lithium-ion batteries (LIBs) are widely used in electric vehicles, energy storage, smart grids, and portable devices due to their high average output voltage and energy density. NaSICON-type materials have been identified as potential candidates for electrode and solid electrolyte materials for LIBs due to their 3D framework, which contains Li + ions, excellent ionic conductivity, and thermal stability. NaSICON-type materials have a 3D framework and a fast Li + diffusion pathway, making them suitable for use in LIBs. However, their application as solid electrolytes is limited due to poorer ionic conductivity and interfacial stability compared to commercialized liquid electrolytes. Furthermore, their use as electrode materials is restricted by their low electronic conductivity. Here, this review provides an overview of NaSICON-type materials, including their common structure, Li + diffusion mechanism, and preparation strategies. The article also discusses the application and modification strategies of NaSICON-type materials for LIBs, classifying them as anode materials, cathode materials, and solid electrolyte materials. Additionally, the potential use of NaSICON-type materials as modification materials for cathode materials for LIBs is briefly mentioned. Building on previous work on NaSICON-type materials, we propose potential areas for further development and wider applications of these materials in LIBs.

25 ENERGY STORAGE↗
DOE OSTI2023

Reaction Current Heterogeneity at the Interface between a Lithium Electrode and Polymer/Ceramic Composite Electrolytes

Although lithium metal anodes are expected to increase the energy density of next-generation batteries, dendrite growth during charge remains a major bottleneck preventing widespread implementation. Composite solid electrolytes with ceramic particles embedded in a polymer matrix have the potential to prevent dendrites owing to the higher mechanical stiffness while also possessing the flexibility to maintain contact with the electrode. However, microscopically, the different mechanical and electrochemical properties of the polymer and ceramic domains can cause inhomogeneous charge transfer at the Li/electrolyte interface, which can lead to nonuniform Li deposition and propagation of dendrites. Here, we computationally examine the coupled electrochemical, transport, and mechanical processes at the interface to determine the propensity for dendrite formation and possible approaches to mitigate this issue. Predictions of two possible microstructures at the interface, namely, (i) where both the polymer and ceramic come in contact with Li metal and (ii) when only the polymer comes in contact with Li metal, suggest that the former has a greater tendency for nonuniform plating. In addition, predictions suggest that minimizing the interfacial resistance between polymers and ceramics and incorporating interlayers between the electrode and electrolyte help mitigate current heterogeneity. In conclusion, these predictions provide guidance for experimental approaches to prevent dendrites in composite electrolytes.

25 ENERGY STORAGE↗
DOE OSTI2023

Accelerating Manufacturing of Powder-Processed Strong, Lightweight and Thermally Stable Bulk Nanocrystalline Al Alloys via Engineered Interface States

The overarching goal of this program is to develop an integrated materials by design framework enabling a simple, scalable, and efficient manufacturing route for thermally stable nanocrystalline Al-based alloys with high specific strength over a range of service temperatures. The central scientific principle underpinning this program is the elucidation, and ultimately implementation in novel alloy design, of unique interfacial structures and chemistries driven by segregation in multi-component systems that give rise to unprecedented processability and properties. This program targeted nanocrystalline Al-based ternary alloys produced by mechanical alloying of powders followed by compaction and sintering with hot pressing, which are inherently scalable and inexpensive manufacturing routes, but when applied to nanocrystalline alloys are usually plagued by low density and/or poor retention of the intended nanostructures during processing. This program successfully demonstrated manufacturing of a bulk (>1 cm 3 ) nanocrystalline Al-based alloy with a combination of thermal stability, high temperature strength retention, and specific strength that exceeds the current-state-of-the-art of Al alloys. It is anticipated that the greatest technological impact will occur by demonstration of rapid and scalable manufacturing of bulk nanocrystalline Al alloys with exceptional thermal stability and mechanical performance, thus enabling increased energy efficiency in high performance power generation systems via: (i) replacement of existing components with lightweight Al-based alloys and (ii) increasing operating temperatures with property retention. The program focused on the development of a simple and efficient manufacturing route for thermally stable nanocrystalline Al-based alloys with high specific strength over a range of service temperatures. The program is expected to have direct impact on scalable and economic manufacturing of bulk nanocrystalline alloys. This program profited from the recent discovery by the project team of segregation-driven amorphous intergranular films in nanocrystalline metallic alloys that can be kinetically frozen-in at sub-solidus temperatures. These interfacial states (also known as amorphous complexions) comprise a large fraction of the total material in nanocrystalline alloys and are responsible for two beneficial characteristics that anchor the proposed work: (1) activated sintering leading to high density and (2) retained nanostructures leading to high strengths that approach a substantial fraction of the theoretical limit. More specifically, these engineered interfaces led to a three-fold benefit: (i) high-throughput materials processing with low energy budget and cost, (ii) exceptional thermal stability, and (iii) high specific strength at both room temperature and intermediate temperatures experienced during service.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
DOE OSTI2022

Topological Antiferromagnetic Van der Waals Phase in Topological Insulator/Ferromagnet Heterostructures Synthesized by a CMOS-Compatible Sputtering Technique

Breaking time-reversal symmetry by introducing magnetic order, thereby opening a gap in the topological surface state bands, is essential for realizing useful topological properties such as the quantum anomalous Hall and axion insulator states. In this work, a novel topological antiferromagnetic (AFM) phase is created at the interface of a sputtered, c-axis-oriented, topological insulator/ferromagnet heterostructure—Bi 2 Te 3 /Ni 80 Fe 20 because of diffusion of Ni in Bi 2 Te 3 (Ni-Bi 2 Te 3 ). The AFM property of the Ni-Bi2Te3 interfacial layer is established by observation of spontaneous exchange bias in the magnetic hysteresis loop and compensated moments in the depth profile of the magnetization using polarized neutron reflectometry. Analysis of the structural and chemical properties of the Ni-Bi2Te3 layer is carried out using selected-area electron diffraction, electron energy loss spectroscopy, and X-ray photoelectron spectroscopy. These studies, in parallel with first-principles calculations, indicate a solid-state chemical reaction that leads to the formation of Ni=Te bonds and the presence of topological antiferromagnetic (AFM) compound NiBi 2 Te 4 in the Ni-Bi 2 Te 3 interface layer. The Neél temperature of the Ni-Bi 2 Te 3 layer is ≈ 63 K, which is higher than that of typical magnetic topological insulators (MTIs). The presented results provide a pathway toward industrial complementary metal-oxide-semiconductor (CMOS)-process-compatible sputtered-MTI heterostructures, leading to novel materials for topological quantum devices.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Microstructural, Corrosion and Mechanical Characterization of Friction-Stir Welded Joints Between Aluminum and Magnesium Alloys

Friction Stir Welding (FSW) of Aluminum-Magnesium (Al-Mg) alloys has garnered increasing attention due to its wide-ranging applications in the automotive and aerospace industries. The microstructural, corrosion, and mechanical properties of FSW Al-Mg welds under selected conditions are critical factors that must be well-investigated to ensure their durability and performance. In this study, electrochemical tests, including Open Circuit Potential (OCP), Linear Polarization Resistance (LPR), Potentiodynamic Polarization Scan (PD), and Electrochemical Impedance Spectroscopy (EIS), have been used to analyze the corrosion resistance of these welds, along with weight loss measurements through cyclic corrosion testing (CCT) and surface evolution via SEM over an 8-week period. Mechanical properties are evaluated through microindentation, nanoindentation, fatigue, and lap-shear tests. The results of the electrochemical tests reveal that the corrosion properties of the center weld zone differ from those of the two base alloys. Indentation tests indicate that the weld zone behaves differently from the base alloys. Surprisingly, the lap shear strength did not decrease significantly even after 8 weeks of cyclic corrosion testing, indicating that the joint prevented any ingress of the electrolyte. Fatigue testing showed that applying an adhesive between the Al and Mg joint improved the fatigue life to some extent, although the corrosion resistance reduced due to the discontinuous bonding of the adhesive layer. Overall, these findings highlight the importance of investigating the corrosion and mechanical properties of FSW Al-Mg welds and provide valuable insights for future modeling works.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
DOE OSTI2022

Wet chemical synthesis and properties of argyrodite sulfide solid electrolytes for solid state lithium batteries

The commercialization of the lithium-ion battery (LIB) in 1991 was responsible for the explosion in portable electronic technologies that has been seen over the past 30 years. With the advent of electric vehicles and other high-powered technologies, there is tremendous demand for LIBs with higher energy density and high safety. To achieve this, new electrode materials must be explored. The obvious choice of anode material would be pure metal lithium, which has a theoretical specific capacity of 3860 mAh g-1 . Unfortunately, metal lithium anodes have not been widely commercialized due to their tendency to react violently with the flammable liquid electrolytes used in today’s batteries. Battery safety can best be achieved by adopting solid electrolytes in place of liquid electrolytes. Solid electrolytes are nonvolatile and nonflammable, safely allowing for the combination of high-capacity cathode materials with a Li metal anode. Argyrodite sulfide solid electrolytes such as halogen-doped Li6PS5X (X = Cl, Br, I) are noted for their high ionic conductivity. But before sulfides can be commercially adopted, they possess several disadvantages which must be addressed, including time- and energy-consuming synthesis processes, poor electrochemical stability, and intrinsically poor air stability. This dissertation seeks to address each of these challenges through materials design an synthesis strategies. In this work, we pioneer a solvent-based approach for the synthesis of argyrodite solid electrolytes Li7PS6 and Li6PS5Xinstead of a stringent solid-state synthesis. Nontoxic ethanol is employed as the solvent, enabling a rapid synthetic approach to produce argyrodite solid electrolytes with high phase purity and compositional flexibility. Compared with Li7PS6, halogen doping (i.e. X = F, Cl, Br, I) not only increases the ionic conductivity, but also enhances the electrochemical stability at the interface towards Li metal. Specifically, F-doped argyrodites produce a robust SEI layer containing LiF, contributing to enhanced interfacial stability. Finally, to address the air instability challenge, argyrodite-incorporated composite solid electrolytes (CSEs) are designed and prepared to produce stable and flexible membranes that are demonstrated in solid-state Li metal batteries. These advances push argyrodite sulfide solid electrolyte research further and pave the way for the proliferation of next generation lithium metal batteries.

25 ENERGY STORAGE↗
DOE OSTI2021

Electrolyte Regulating toward Stabilization of Cobalt-Free Ultrahigh-Nickel Layered Oxide Cathode in Lithium-Ion Batteries

Cobalt (Co)-free ultrahigh-nickel (Ni) layered oxides exhibit a double-edged competitive advantages in reducing the cathode cost and boosting the energy density, promising the sustainable development of batteries for electric vehicles. However, the increased Ni content, resultantly more highly oxidative Ni 4+ , potentially induces severe capacity fading due to the aggravated side reactions, limiting the practical applications. Here, we evaluate the compatibility of two localized high-concentration electrolytes (LHCEs) with LiNi 0.96 Mg 0.02 Ti 0.02 O 2 (NMT) cathode under a high charging voltage of 4.4 V in lithium ion batteries. The LHCE with EC additive enables the formation of stable interfacial layers on both NMT cathode and graphite anode, thus realizing a capacity retention of 97.2% over 200 cycles at 25 °C and high reversible capacities of ~180.2 and ~185.8 mAh g -1 , respectively, at 5C charge rate and 5C discharge rate. This study offers a promising approach to enable Co-free ultrahigh-Ni layered oxides for practical applications.

25 ENERGY STORAGE↗