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Direct Visualization of Solid Electrolyte Interphase Formation in Lithium-Ion Batteries with In Situ Electrochemical Transmission Electron Microscopy
Complex, electrochemically driven transport processes form the basis of electrochemical energy storage devices. The direct imaging of electrochemical processes at high spatial resolution and within their native liquid electrolyte would significantly enhance our understanding of device functionality, but has remained elusive. In this work we use a recently developed liquid cell for in situ electrochemical transmission electron microscopy to obtain insight into the electrolyte decomposition mechanisms and kinetics in lithium-ion (Li-ion) batteries by characterizing the dynamics of solid electrolyte interphase (SEI) formation and evolution. Here we are able to visualize the detailed structure of the SEI that forms locally at the electrode/electrolyte interface during lithium intercalation into natural graphite from an organic Li-ion battery electrolyte. We quantify the SEI growth kinetics and observe the dynamic self-healing nature of the SEI with changes in cell potential.
A unified relation for the solid-liquid interface free energy of pure FCC, BCC, and HCP metals
We study correlations between the solid-liquid interface (SLI) free energy and bulk material properties (melting temperature, latent heat, and liquid structure) through the determination of SLI free energies for bcc and hcp metals from molecular dynamics (MD) simulation. Values obtained for the bcc metals in this study were compared to values predicted by the Turnbull, Laird, and Ewing relations on the basis of previously published MD simulation data. We found that of these three empirical relations, the Ewing relation better describes the MD simulation data. Moreover, whereas the original Ewing relation contains two constants for a particular crystal structure, we found that the first coefficient in the Ewing relation does not depend on crystal structure, taking a common value for all three phases, at least for the class of the systems described by embedded-atom method potentials (which are considered to provide a reasonable approximation for metals).
Local structural motifs and extended-range order in liquid and solid ammonia under pressure
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Glassy embedded solid-state electrode assemblies, solid-state batteries and methods of making electrode assemblies and solid-state batteries
Batteries, component structures and manufacturing methods, in particular including a glassy embedded battery electrode assembly having a composite material structure composed of interpenetrating material components including a porous electroactive network including a solid electroactive material, and a continuous glassy medium including a Li ion conducting sulfide glass, can achieve enhanced power output, reduced charging time and/or improved cycle life.
Advance optical fiber probe for simultaneous measurements of solids holdup and particles velocity using simple calibration methods for gas-solid fluidization systems
We report advanced gas-solid optical fiber probe technique that can measure simultaneously solids velocity, solids concentration related quantity, and their time series fluctuations has been implemented with simple and new calibration methods for both solids holdup and particles velocity measurements in gas-solid spouted bed and gas-solid fluidized bed. The needed signal and data processing programs have been developed in our laboratory. New, simple, and reliable calibration methods and the related experimental setups have been established to convert the solids concentration related signal to solids holdup which is a meaningful hydrodynamic parameter and to determine the effective distance between the two tips of the probe for the solids velocity measurements. The new calibration methods have been employed to cover a wide range of particle sizes which usually used in gas-solid spouted beds and gas-solid fluidized beds. Selected results have demonstrated the appropriateness of the advanced optical fiber in measuring both solids holdup and particles velocity in the experimental setups of the gas-solid spouted and fluidized beds. The measurements have been compared against independent techniques of gamma ray computed tomography (CT) and radioactive particle tracking (RPT).
Solid CO 2 -philes as potential phase-change physical solvents for CO 2
The binary phase behavior of mixtures of CO 2 and highly CO 2 -philic solids has been determined at 298 K. The solids include sugar acetates (β-d-galactose pentaacetate, β-d-ribofuranose tetraacetate, α-d(+)-glucose pentaacetate, d-(+)-sucrose octaacetate), tert-butylated aromatics (2,4-di-tert-butylphenol, 2,6-di-tert-butyl-4-methylphenol, 3,5-di-tert-butylphenol, 1,2,4-triacetoxybenzene), and a highly oxygenated cyclic compound (1,3,5-trioxane). The results are presented in the form of phase behavior (Px) diagrams at 298 K that exhibit either one (vapor–liquid–solid, VLS) or two (vapor–liquid–liquid, VL 1 L 2 and vapor–liquid–solid, VL 2 S) three-phase equilibrium lines. Ternary phase behavior at 298 K has also been determined and presented in the form of a pseudo-binary Px diagram for mixtures of an equimolar gas blend of CO 2 and H 2 and each of these CO 2 -philic solids and several other previously identified highly CO 2 -philic compounds. Only four compounds, sucrose octaacetate, 1,3,5-tri-tert-butylbenzene, 2,4-di-tert-butylbenzene, and 1,3,5-trioxane, melted at 298 K in the presence of the CO 2 /H 2 mixture at three-phase vapor–liquid–solid pressures ranging between 6 MPa and 10 MPa. These four compounds are candidates for the selective absorption of CO 2 from a CO 2 /H 2 mixture using solid compounds that can melt and selectively absorb CO{sub 2}.
An added-mass partition algorithm for fluid–structure interactions of compressible fluids and nonlinear solids
We describe an added-mass partitioned (AMP) algorithm for solving fluid–structure interaction (FSI) problems involving inviscid compressible fluids interacting with nonlinear solids that undergo large rotations and displacements. The computational approach is a mixed Eulerian–Lagrangian scheme that makes use of deforming composite grids (DCG) to treat large changes in the geometry in an accurate, flexible, and robust manner. The current work extends the AMP algorithm developed in Banks et al. [1] for linearly elasticity to the case of nonlinear solids. To ensure stability for the case of light solids, the new AMP algorithm embeds an approximate solution of a nonlinear fluid–solid Riemann (FSR) problem into the interface treatment. The solution to the FSR problem is derived and shown to be of a similar form to that derived for linear solids: the state on the interface being fundamentally an impedance-weighted average of the fluid and solid states. Numerical simulations demonstrate that the AMP algorithm is stable even for light solids when added-mass effects are large. The accuracy and stability of the AMP scheme is verified by comparison to an exact solution using the method of analytical solutions and to a semi-analytical solution that is obtained for a rotating solid disk immersed in a fluid. The scheme is applied to the simulation of a planar shock impacting a light elliptical-shaped solid, and comparisons are made between solutions of the FSI problem for a neo-Hookean solid, a linearly elastic solid, and a rigid solid. The ability of the approach to handle large deformations is demonstrated for a problem of a high-speed flow past a light, thin, and flexible solid beam.
The Energy Frontier Research Center for Solid-State Lighting Sci-ence: Exploring New Materials Architectures and Light Emission Phenomena
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Magnitude of the Förster Radius in Colloidal Quantum Dot Solids
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On the Mechanism of the Vapor–Solid–Solid Growth of Au-Catalyzed GaAs Nanowires
The mechanism of the vapor–solid–solid growth of Au-catalyzed GaAs nanowires in the temperature range of 420–450°C is investigated. For the first time, the effect of elastic stresses caused by a difference in the atomic densities of the catalyst and nanowire material on the solid-phase nucleation rate is considered. By assuming that the growth of the GaAs nucleus at the catalyst–nanowire interface is limited by the As-diffusion flux in the catalyst, it is shown that vapor–solid–solid growth can be implemented through the polycentric-nucleation mode in the temperature range under consideration. The intensity of the nucleation of coherent islands upon vapor–solid–solid growth is shown to be higher than the intensity of nucleation in the case of vapor–liquid–solid growth because a low interphase surface energy is implemented at coherent solid–solid conjugation. It is proved that the nucleation of Au-catalyzed GaAs nanowires by the vapor–solid–solid mechanism is possible only when GaAs-island growth proceeds due to As diffusion along the catalyst–nanowire interface.
Effect of La{sub 2}O{sub 3}-treatment on textural and solid-solid interactions in ferric/cobaltic oxides system
Pure and La{sub 2}O{sub 3}-containing (0.75-3.0 mol%) Fe{sub 2}O{sub 3}/Co{sub 3}O{sub 4} solids were prepared by thermal treatment of their carbonates at 500-700 Degree-Sign C. The produced solids were characterized using XRD, HRTEM, EDX and nitrogen adsorption at -196 Degree-Sign C. The results revealed that pure solids calcined at 600 and 700 Degree-Sign C consisted of nanosized CoFe{sub 2}O{sub 4} phase, while pure mixed solids calcined at 500 Degree-Sign C consisted of trace amount of CoFe{sub 2}O{sub 4} and unreacted Fe{sub 2}O{sub 3}, Co{sub 3}O{sub 4} phases. The presence of 0.75 mol% La{sub 2}O{sub 3} enhanced solid-solid interaction between Fe{sub 2}O{sub 3} and Co{sub 3}O{sub 4} at 500 Degree-Sign C yielding CoFe{sub 2}O{sub 4}. The ferrite phase existed also in all mixed oxides upon treated with La{sub 2}O{sub 3} besides LaCoO{sub 3} phase. LaCoO{sub 3} existed as a major phase in all mixed oxides treated with 3 mol% La{sub 2}O{sub 3}. La{sub 2}O{sub 3}-treatment modified the crystallite size of all phases present to an extent dependent on calcination temperature and amount of La{sub 2}O{sub 3} content. This treatment decreased effectively the S{sub BET} of all mixed solids. - Graphical Abstract: TEM photographs of pure mixed oxides calcined at 500 Degree-Sign C. Highlights: Black-Right-Pointing-Pointer Cobalt ferrite exhibit chemical stability, low electric loss and high coercivity. Black-Right-Pointing-Pointer Cobalt ferrite is used in microwave devices, computer memories and magnetic storage. Black-Right-Pointing-Pointer Solid-solid interactions in ferric/cobaltic oxides system were investigated. Black-Right-Pointing-Pointer La{sub 2}O{sub 3}-treatment modified surface compositions of the system investigated. Black-Right-Pointing-Pointer All phases present in various solids existed as nanosized solids.
Solid matrix transformation and tracer addition using molten ammonium bifluoride salt as a sample preparation method for laser ablation inductively coupled plasma mass spectrometry
Solid sampling and analysis methods, such as laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), are challenged by matrix effects and calibration difficulties. Matrix-matched standards for external calibration are seldom available and it is difficult to distribute spikes evenly into a solid matrix as internal standards. While isotopic ratios of the same element can be measured to high precision, matrix-dependent effects in the sampling and analysis process frustrate accurate quantification and elemental ratio determinations. Here we introduce a potentially general solid matrix transformation approach entailing chemical reactions in molten ammonium bifluoride (ABF) salt that enables the introduction of spikes as tracers or internal standards. Proof of principle experiments show that the decomposition of uranium ore in sealed PFA fluoropolymer vials at 230 °C yields, after cooling, new solids suitable for direct solid sampling by LA. When spikes are included in the molten salt reaction, subsequent LA-ICP-MS sampling at several spots indicate that the spikes are evenly distributed, and that U-235 tracer dramatically improves reproducibility in U-238 analysis. Precisions improved from 17% relative standard deviation for U-238 signals to 0.1% for the ratio of sample U-238 to spiked U-235, a factor of over two orders of magnitude. These results introduce the concept of solid matrix transformation (SMT) using ABF, and provide proof of principle for a new method of incorporating internal standards into a solid for LA-ICP-MS. This new approach, SMT-LA-ICP-MS, provides opportunities to improve calibration and quantification in solids based analysis. Finally, looking forward, tracer addition to transformed solids opens up LA-based methods to analytical methodologies such as standard addition, isotope dilution, preparation of matrix-matched solid standards, external calibration, and monitoring instrument drift against external calibration standard
Charge Transport Modulation in PbSe Nanocrystal Solids by Au x Ag 1– x Nanoparticle Doping
Nanocrystal (NC) solids are an exciting class of materials, whose physical properties are tunable by choice of the NCs as well as the strength of the interparticle coupling. One can consider these NCs as “artificial atoms” in analogy to the formation of condensed matter from atoms. Akin to atomic doping, the doping of a semiconducting NC solid with impurity NCs can drastically alter its electronic properties. A high degree of complexity is possible in these artificial structures by adjusting the size, shape, and composition of the building blocks, which enables “designer” materials with targeted properties. Here, we present the doping of the PbSe NC solids with a series of Au x Ag 1–x alloy nanoparticles (NPs). A combination of temperature-dependent electrical conductance and Seebeck coefficient measurements and room-temperature Hall effect measurements demonstrates that the incorporation of metal NPs both modifies the charge carrier density of the NC solids and introduces energy barriers for charge transport. These studies point to charge carrier injection from the metal NPs into the PbSe NC matrix. The charge carrier density and charge transport dynamics in the doped NC solids are adjustable in a wide range by employing the Au x Ag 1–x NP with different Au:Ag ratio as dopants. Furthermore, this doping strategy could be of great interest for thermoelectric applications taking advantage of the energy filtering effect introduced by the metal NPs.
Challenges and Prospects of All-Solid-State Electrodes for Solid-State Lithium Batteries
In the development of all-solid-state lithium batteries (ASSLB), progress is made with solid-state electrolytes; however, challenges regarding compatibility and stability still exist with solid electrodes. These issues result in a low battery capacity and short cycle life, which limit the commercial application of ASSLBs. Here, this review summarizes the recent research progress on solid-state electrodes in ASSLBs including the solid–solid interface phenomena such as the interface between electrode materials and electrolytes. The mechanical stability problems in solid electrodes, including fracture, brittleness, and deformation of electrode materials, are also discussed, and corresponding methods to measure the solid electrode stress are provided. In addition, strategies for mitigating stress-related issues are examined. Finally, the fabrication process of solid electrodes is introduced and their future developments, including the exploration of new electrode materials and the design of more intelligent electrode structures, are proposed.
Toward high solids loading process for lignocellulosic biofuel production at a low cost: Biofuel Production at High Solids Loading
High solids loadings (>18 wt%) in enzymatic hydrolysis and fermentation are desired for lignocellulosic biofuel production at a high titer and low cost. However, sugar conversion and ethanol yield decrease with increasing solids loading. The factor(s) limiting sugar conversion at high solids loading is not clearly understood. In the present study, we investigated the effect of solids loading on simultaneous saccharification and co-fermentation (SSCF) of AFEX™ (ammonia fiber expansion) pretreated corn stover for ethanol production using a xylose fermenting strain Saccharomyces cerevisiae 424A(LNH-ST). Decreased sugar conversion and ethanol yield with increasing solids loading were also observed. End-product (ethanol) was proven to be the major cause of this issue and increased degradation products with increasing solids loading was also a cause. For the first time, we show that with in situ removal of end-product by performing SSCF aerobically, sugar conversion stopped decreasing with increasing solids loading and monomeric sugar conversion reached as high as 93% at a high solids loading of 24.9 wt%. In this work, techno-economic analysis was employed to explore the economic possibilities of cellulosic ethanol production at high solids loadings. The results suggest that low-cost in situ removal of ethanol during SSCF would significantly improve the economics of high solids loading processes.