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DOE OSTI2014

Raman Evidence for Late Stage Disproportionation in a Li–O 2 Battery

Raman spectroscopy is used to characterize the composition of toroids formed in an aprotic Li-O2 cell based on an activated carbon cathode. The trends in the Raman data as a function of discharge current density and charging cutoff voltage provide evidence that the toroids are made up of outer LiO2-like and inner Li2O2 regions, consistent with a disproportionation reaction occurring in the solid phase. The LiO2-like component is found to be associated with a new Raman peak identified in the carbon stretching region at ~1505 cm-1, which appears only when the LiO2 peak at 1123 cm-1 is present. The new peak is assigned to distortion of the graphitic ring stretching due to coupling with the LiO2-like component based on density functional calculations. The interface of the LiO2-like component with carbon surface should provide good electronic contact and is consistent with the low charge voltage plateau observed for it. These new results on the LiO2-like component from Raman spectroscopy provide evidence that a late stage disproportionation mechanism can occur during discharge and adds new understanding to the complexities of possible processes occurring in Li-O2 batteries.

25 ENERGY STORAGE↗

DOE OSTI2021

Design and physics basis for the upcoming DIII-D SAS-VW campaign to quantify tungsten leakage and transport in a new slot divertor geometry

A set of experiments are planned to exploit the high SOL collisionality enabled by a tightly baffled slot divertor geometry to suppress tungsten leakage in DIII-D. A toroidal row of graphite tiles from the Small Angle Slot (SAS) divertor is being coated with 10–15 μ m of tungsten. New spectroscopic viewing chords with in-vacuo optics will measure the W gross erosion source from the divertor surface with high spatial and temporal resolution. In parallel, the bottom of the SAS divertor is changed from a flat to a ‘V’ shape. New SOLPS-ITER/DIVIMP simulations conducted with drifts using the planned ‘V’ shape predict a substantial reduction in W sourcing and SOL accumulation in either B × ∇B direction relative to either the old SAS divertor shape or the open, lower divertor. Dedicated studies are planned to carefully characterize the level of W sourcing, leakage, and scrape-off-layer (SOL) accumulation in DIII-D over a wide range of plasma scenarios. Various actuators will be assessed for their efficacy in further reducing high-Z impurity sources and leakage from the slot divertor geometry. Finally, this coupled code-experiment validation effort will be used to stress-test physics models and build confidence in extrapolations to advanced, high-Z divertor geometries for next-step devices.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2023

High-throughput Li plating quantification for fast-charging battery design

Fast charging of most commercial lithium-ion batteries is limited due to fear of lithium plating on the graphite anode, which is difficult to detect and poses considerable safety risk. In this report we demonstrate the power of simple, accessible and high-throughput cycling techniques to quantify irreversible Li plating spanning data from over 200 cells. We first observe the effects of energy density, charge rate, temperature and state of charge on lithium plating, use the results to refine a mature physics-based electrochemical model and provide an interpretable empirical equation for predicting the plating onset state of charge. We then explore the reversibility of lithium plating and its connection to electrolyte design for preventing irreversible Li accumulation. Finally, we design a method to quantify in situ Li plating for commercially relevant graphite|LiNi 0.5 Mn 0.3 Co 0.2 O 2 (NMC) cells and compare with results from the experimentally convenient Li|graphite configuration. The hypotheses and abundant data herein were generated primarily with equipment universal to the battery researcher, encouraging further development of innovative testing methods and data processing that enable rapid battery engineering.

25 ENERGY STORAGE↗

DOE OSTI2021

Methodologies for Design, Characterization and Testing of Electrolytes that Enable Extreme Fast Charging of Lithium-ion Cells

Selection, testing and validation of electrolyte candidates for Li-ion cells are discussed, based on a 10-minute target for extreme fast charge (XFC). A combination of modeling and laboratory measurements create a timely and synergistic approach to identifying candidate electrolyte formulations. Multi-solvent systems provide a balanced set of properties, wherein lower molecular-weight solvents offer reduced viscosity, increased species diffusivity, and mitigation of concentration polarization at high charge rates. Carefully selected formulations can exhibit peak conductivity and usable conductivity range of two to three times that of the baseline EC-EMC (3:7, wt.) + LiPF 6 . Candidates are also chosen based on stability and longevity within the cell environment. Lab testing coincides with property predictions from the Advanced Electrolyte Model (AEM) and a macro-scale cell model. Furthermore, cell testing utilized coin and pouch cells having NMC532 or NMC811 cathodes with graphite electrodes. Results indicate combinations of low-molecular weight solvents are key for fast-charge electrolytes as they extend the useful conductivity range to both low and higher salt concentrations, and possess higher self-diffusivities compared to conventional solvents. This reduces impacts from concentration polarization. The choice of electrolyte also influences the tendency for lithium metal deposition at the anode, as showcased by experimental and modeling results herein.

25 ENERGY STORAGE↗

DOE OSTI2023

X-ray absorption spectroscopic study of the alumina supported Fe and FeMo catalysts for methane dehydrogenation

Nanoscale Fe (5%Fe/Al 2 O 3 ) and FeMo (4.5%Fe-0.5%Mo/Al 2 O 3 ) catalysts are prepared by precipitating metal components onto alumina and then reducing in hydrogen at 700 °C for 2 hrs. Here, the catalysts are characterized before and after their exposures to methane at 700 °C, employing ex-situ X-ray absorption spectroscopy (XAS) and X-ray diffraction techniques. XAS data of the as-prepared catalysts shows that, iron precipitates onto alumina as 6L-ferrihydrite, and Mo is present as molybdate (Mo(VI)O 4 2- ). The molybdate, which binds the alumina in the as-prepared FeMo catalyst, is partially reduced to MoO 2 . The reduction of iron to metallic state is incomplete because the ferrous iron binds the alumina, forming hercynite. After several hrs of methane exposure to both the catalysts at 700 °C, a major Fe 3 C and a graphite phase are observed only in the FeMo catalyst. The observation confirms that the Mo promotes more iron to an active Fe metal, a part of that metal converts to Fe 3 C and austenite (Fe x C). Concurrently, the MoO 2 converts to Mo-oxycarbide (MoO x C y ), the latter then carburize to Mo 2 C in the FeMo catalyst. The Fe metal, Mo-oxycarbide and metal carbides are mainly responsible for the conversion of methane to H 2 and carbon. At reaction temperature > 900 °C, the Mo carbide particles agglomerate, and the excess carbon deposits on this agglomerate leading to catalyst deactivation. The deactivated catalyst is regenerated with CO 2 treatment at 1000 °C to restore its initial oxide structure.

30 DIRECT ENERGY CONVERSION↗

DOE OSTI2013

Lithium Metal Anodes for Rechargeable Batteries

Rechargeable lithium metal batteries have much higher energy density than those of lithium ion batteries using graphite anode. Unfortunately, uncontrollable dendritic lithium growth inherent in these batteries (upon repeated charge/discharge cycling) and limited Coulombic efficiency during lithium deposition/striping has prevented their practical application over the past 40 years. With the emerging of post Li-ion batteries, safe and efficient operation of lithium metal anode has become an enabling technology which may determine the fate of several promising candidates for the next generation of energy storage systems, including rechargeable Li-air battery, Li-S battery, and Li metal battery which utilize lithium intercalation compounds as cathode. In this work, various factors which affect the morphology and Coulombic efficiency of lithium anode will be analyzed. Technologies used to characterize the morphology of lithium deposition and the results obtained by modeling of lithium dendrite growth will also be reviewed. At last, recent development in this filed and urgent need in this field will also be discussed.

25 ENERGY STORAGE↗

NASA NTRS1986

Fracture mechanics of matrix cracking and delamination in glass/epoxy laminates

This study focused on characterizing matrix cracking and delamination behavior in multidirectional laminates. Static tension and tension-tension fatigue tests were conducted on two different layups. Damage onset, accumulation, and residual properties were measured. Matrix cracking was shown to have a considerable influence on residual stiffness of glass epoxy laminates, and could be predicted reasonably well for cracks in 90 deg piles using a simple shear lag analysis. A fracture mechanics analysis for the strain energy release rate associated with 90 deg ply-matrix crack formation was developed and was shown to correlate the onset of 90 deg ply cracks in different laminates. The linear degradation of laminate modulus with delamination area, previously observed for graphite epoxy laminates, was predicted for glass epoxy laminates using a simple rule of mixtures analysis. The strain energy release rate associated with edge delamination formation under static and cyclic loading was difficult to analyze because of the presence of several contemporary damage phenomena.

Caslini, M.↗

NASA NTRS1987

Study of matrix cracking and delamination in glass/epoxy laminates

Caslini, Massimo↗

DOE OSTI2015

Pyrolytic synthesis and characterization of N-doped carbon nanoflakes for electrochemical applications

Highlights: • Carbon nanoflakes doped with nitrogen were produced by a pyrolytic technique. • Quarternary, pyrrolic and pyridinic types of nitrogen are confirmed by XPS. • Nitrogen content depends on precursor used and temperature processed. • Specific surface area values decrease with increasing of synthesis duration. • N-doped carbon nanoflakes may be suitable for electrochemical applications. - Abstract: Nitrogen doped carbon nanoflakes, which are very important for many electrochemical applications, were synthesized by pyrolysis of nitrogen containing organic compounds over metal oxide template. Acetonitrile, pyridine and butylamine, which are of different volatility were tested as N-containing precursors. Morphology, structure and chemical composition of the as-synthesized materials were investigated by scanning electron microscopy (SEM), high resolution transmission electron microscopy (TEM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). It was found that materials are highly defective and consist of a few malformed graphene layers. X-ray photoelectron spectra reflect the dominant graphitic and pyridinic N-bonding configuration. It was also noted that specific surface area depends on the duration and temperature of the reaction. Increase in duration and temperature led to decrease of the specific surface area from 1000 to 160 m{sup 2}/g, 1170 to 210 m{sup 2}/g and 1180 to 480 m{sup 2}/g for acetonitrile, butylamine and pyridine precursors, respectively.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2017

Synchrotron measurements of local microstructure and residual strains in ductile cast iron

The local microstructure and distribution of thermally induced residual strains in ferrite matrix grains around an individual spherical graphite nodule in ductile cast iron (DCI) were measured using a synchrotron X-ray micro-diffraction technique. It is found that the matrix grains are deformed, containing dislocations and dislocation boundaries. Each of the residual strain components in the matrix grains exhibits a complex pattern along the circumferential direction of the nodule. Along the radial direction of the nodule, strain gradients from the interface to the grain interior are seen for some strain components, but only in some matrix grains. The observed residual strain patterns have been analysed by finite element modelling, and a comparison between the simulation and experiments is given. The present study of local residual stress by both experimental characterization and simulation provide much needed information for understanding the mechanical properties of DCI, and represent an important contribution for the microstructural design of new DCI materials.

Zhang, Y B↗

NASA NTRS1982

A simple test for the interlaminar fracture toughness of composites

A simple test method for the measurement of delamination resistance is assessed through its application to 11-ply graphite-epoxy laminates whose matrices employ the F185 and 205 resins. The F185 resin has the same base epoxy as the 205, to which liquid and solid elastomers have been added. The critical value of the mixed mode energy release rate, calculated from a closed form equation employing nominal strain measurements from the onset of edge delamination, show that addition of the elastomers to the base epoxy increases interlaminar fracture toughness. Comparison of these results with those of width-tapered double cantilever beam (WTDCB) test data for the two materials shows a similar strain energy release rate, establishing the accuracy of the novel method. Both tests are found to be needed, however, for the quantitative characterization of interlaminar fracture toughness.

Obrien, T. K.↗

DOE OSTI2019

Experimental and Computational Analysis of NEAMS Pebble Bed Reactors

The Advanced High-Temperature Pebble Bed Reactor concept leverages a particle-based fuel format consisting of discrete spherical graphite pebbles arrayed in a packed bed architecture. Thermal regulation achieved via flow of gas (e.g., helium) or liquid (e.g., molten salt) coolants through the void spaces between pebbles in the bed (characteristic pebble diameters: ~ 6 cm, gas cooled; ~ 3 cm, liquid cooled). This design is of interest owing to inherent advantages including passive safety features and highly efficient heat transfer characteristics that enable high power densities to be achieved. Fully leveraging these advantages requires a fundamental understanding of the complex coolant flow structure within the pebble-shaped fuel bed. Unfortunately, complexities associated with non-invasively probing the micro-scale flow phenomena within the complex network of void spaces between pebbles have hindered efforts to characterize the underlying transport phenomena. Without this fundamental foundation, it becomes challenging to rationally construct macroscopic transport models based upon volume averages of micro-scale parameters that accurately capture the observed flow behavior. Consequently, this lack of fundamental knowledge has limited previous work to coarse comparisons between theory and extremely limited experimental data. Moreover, these comparisons have been made only in terms of integral or macroscopic results. Therefore, multipoint measurements with a high level of spatial and temporal resolution are critically needed to fully map the complex flow patterns and to provide data at high spatial density to permit accurate volume averaging in the pebble bed. For this project, we performed a coordinated experimental and computational effort to quantitatively map the full-field velocity and temperature fields in the interstitial spaces within the pebble bed. The major accomplishments of this project included the important knowledge acquired for the flow mixing and heat transfer in the interstitial pore scales, the effects of flow mixing in the near-wall and far-wall regions, and the by-pass flows of pebble bed systems. The produced high-resolution experimental data (not broadly available in existing literature) were then used for the numerical studies enabling the refinement and validation of standard simulation tools (Nek5000).

42 ENGINEERING↗

NASA NTRS2004

Lithium Polymer Electrolytes and Solid State NMR

Research is being done at the Glenn Research Center (GRC) developing new kinds of batteries that do not depend on a solution. Currently, batteries use liquid electrolytes containing lithium. Problems with the liquid electrolyte are (1) solvents used can leak out of the battery, so larger, more restrictive, packages have to be made, inhibiting the diversity of application and decreasing the power density; (2) the liquid is incompatible with the lithium metal anode, so alternative, less efficient, anodes are required. The Materials Department at GRC has been working to synthesize polymer electrolytes that can replace the liquid electrolytes. The advantages are that polymer electrolytes do not have the potential to leak so they can be used for a variety of tasks, small or large, including in the space rover or in space suits. The polymers generated by Dr. Mary Ann Meador's group are in the form of rod -coil structures. The rod aspect gives the polymer structural integrity, while the coil makes it flexible. Lithium ions are used in these polymers because of their high mobility. The coils have repeating units of oxygen which stabilize the positive lithium by donating electron density. This aids in the movement of the lithium within the polymer, which contributes to higher conductivity. In addition to conductivity testing, these polymers are characterized using DSC, TGA, FTIR, and solid state NMR. Solid state NMR is used in classifying materials that are not soluble in solvents, such as polymers. The NMR spins the sample at a magic angle (54.7') allowing the significant peaks to emerge. Although solid state NMR is a helpful technique in determining bonding, the process of preparing the sample and tuning it properly are intricate jobs that require patience; especially since each run takes about six hours. The NMR allows for the advancement of polymer synthesis by showing if the expected results were achieved. Using the NMR, in addition to looking at polymers, allows for participation on a variety of other projects, including aero-gels and carbon graphite mat en als. The goals of the polymer electrolyte research are to improve the physical properties of the polymers. This includes improving conductivity, durability, and expanding the temperature range over which it is effective. Currently, good conductivity is only present at high temperatures. My goals are to experiment with different arrangements of rods and coils to achieve these desirable properties. Some of my experiments include changing the number of repeat units in the polymer, the size of the diamines, and the types of coil. Analysis of these new polymers indicates improvement in some properties, such as lower glass transition temperature; however, they are not as flexible as desired. With further research we hope to produce polymers that encompass all of these properties to a high degree.

Berkeley, Emily R.↗

DOE OSTI2014

Fabrication and long-wavelength characterization of neat and chemically modified graphene

Graphene, a single- or several layer-thick carbon, attracts significant research activity because of its exceptional material properties. Graphene is a promising material for optoelectronic applications. Neat graphene demonstrates potential as a material for long wavelength photodetectors working at elevated temperatures. Chemical modification of graphene opens up many new applications of this material in electronics, in new composite materials, and in new catalysts for different chemical processes. Chemical vapor deposition-grown large-area graphene can be successfully modified with the creation of benzyne attachments. The investigation of microwave properties is an important part of graphene research. Two variants of near-field long wavelength microscopy were found efficient with graphene. Measurements with a probe formed by an electrically open end of a 4 GHz half-lambda parallel-strip transmission line resonator allow the implementation of an electrodynamic model of graphene microwave impedance. The results of near-field scanning superconducting quantum interference device (SQUID) RF microscopy of graphite and graphene at 200 MHz shed light on mechanisms of AC graphene response: screening currents induced in graphene by an external RF magnetic field tend to localize near structural defects.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Integrative Additive Design for Robust SEI Formation in NMC811||Silicon Batteries

Silicon (Si) is considered a promising replacement for graphite anodes in lithium-ion batteries (LIBs) due to its high abundance and exceptional specific capacity, but its widespread commercialization has been hindered by poor electrochemical performance. Among various strategies, the use of functional additives has emerged as one of the most effective and cost-efficient methods to enhance the electrochemical properties of LIBs. In this study, several additives—vinylene carbonate (VC), vinyl ethylene carbonate (VEC), lithium difluorophosphate (LiDFP), lithium difluoro(oxalato)borate (LiDFOB), lithium tetrafluorooxalatophosphate (LiTFOP), and lithium difluorobis(oxalato)phosphate (LiDFBOP)—were systematically investigated in LiNi₀.₈Mn₀.₁Co₀.₁O₂ (NMC811)||Si full cells. Notably, LiDFBOP, a lithium salt containing two oxalate groups, outperformed all other additives, delivering the best capacity retention after 300 cycles. Comprehensive characterizations, including FTIR, SEM, and XPS, revealed that LiDFBOP's superior performance stems from its ability to form a more stable solid electrolyte interphase (SEI) on the Si anode, owing to its favorable molecular structure that integrates the beneficial features of the other additives.

25 ENERGY STORAGE↗

DOE OSTI2022

Raman spectroscopy of thermally perturbed carbon fibers: Discriminating spectral responses of modulus classes and defect types

The mechanical strength properties of carbon fibers are generally thought to be correlated with the presence of underlying atomic-level defects. These defects serve to break the underlying translational symmetry of the graphitic or graphene subunits of the fiber construction, resulting in the emergence of new Raman-active spectral features. However, historical attempts to classify the precise origin of defect contributions to the Raman spectra have been challenging because of indistinct and overlapping features in the carbon fiber Raman spectra. Further, while substantial research exists on high-temperature exposure in inert atmospheres for carbon fiber composites, comparatively less addresses microscale behaviors and Raman spectral alterations to monofilament carbon fibers exposed to high-temperature atmospheric environments. Here, we report Raman spectral responses of nine commercially available high-performance, polyacrylonitrile-based carbon fibers exposed to various atmospheric heat treatments. In this work, we introduce a model-independent characterization method, the integrated absolute difference, to quantify the spectral responses to heat treatment of different fiber modulus classes. We combine this new method with a newly reported strategy to standardize spectral fitting for carbon fibers. With this approach, we show that atomic-scale defects in the underlying fiber microstructure manifest in measurably distinct manners and have distinct responses to thermal perturbation. These combined approaches may lay the foundation for disentangling contributions from specific defects in the Raman spectra of carbon fibers.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Polymorphic, Porous, and Host–Guest Nanostructures Directed by Monolayer–Substrate Interactions: Epitaxial Self-Assembly Study of Cyclic Trinuclear Au(I) Complexes on HOPG at the Solution–Solid Interface

Synthesis, crystallographic characterization, and molecular self-assembly of two novel cyclotrimeric gold(I) complexes, Au 3 [3,5-(COOEt) 2 Pz] 3 (Au 3 Pz 3 ) and Au 3 [(n-Pr–O)C=N(Me)] 3 (Au 3 Cb 3 ) was studied. Single crystal X-ray crystallography data reveal that both gold(I) complexes have one-dimensional stacking patterns caused by intermolecular Au(I)···Au(I) aurophilic interactions. The Au 3 Pz 3 trimer units stack with two alternate and symmetrical Au(I)···Au(I) interactions while the Au 3 Cb 3 units have three alternating and nonsymmetrical Au(I)···Au(I) interactions. Molecular self-assembly of the gold(I) complexes on the 1-phenyloctane/highly ordered pyrolytic graphite (HOPG) (0001) solution–solid interface is studied with scanning tunneling microscopy (STM). The gold(I) cyclotrimers form epitaxial nanostructures on the HOPG surface. At a concentration of ~1 × 10 –4 M, Au 3 Pz 3 complexes exhibit a single morphology, while Au 3 Cb 3 complexes exhibit polymorphology. Two polymorphs, one nonporous and the other porous, are observed at 22.0 ± 2.0 °C for Au 3 Cb 3 complexes. A nonporous, low-surface-density (0.82 molecules/nm 2 ) Au 3 Cb 3 nanostructure forms first and then transforms into a high-density (1.43 molecules/nm2) porous nanostructure. This is the first time any porous surface nanostructure is reported for an organometallic system. The porous structure is thought to be stabilized by a combination of hydrogen bonding and monolayer–substrate interactions. These pores are utilized to incorporate pyrene into the film, rendering this the first organometallic host–guest system imaged at the solid–solution interface. In conclusion, molecular and periodic density functional theory (DFT) calculations shed light on the two-dimensional topography and polymorphic self-assembly revealed by STM; these calculations suggest significant electronic hybridization of the Au 3 trimer orbitals and HOPG. The multiple-technique approach used herein provides insights concerning molecule–substrate and molecule–molecule interactions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Quantification of Uncoupled Spin Domains in Spin-Abundant Disordered Solids

Materials often contain minor heterogeneous phases that are difficult to characterize yet nonetheless significantly influence important properties. Here we describe a solid-state NMR strategy for quantifying minor heterogenous sample regions containing dilute, essentially uncoupled nuclei in materials where the remaining nuclei experience heteronuclear dipolar couplings. NMR signals from the coupled nuclei are dephased while NMR signals from the uncoupled nuclei can be amplified by one or two orders of magnitude using Carr-Meiboom-Purcell-Gill (CPMG) acquisition. The signal amplification by CPMG can be estimated allowing the concentration of the uncoupled spin regions to be determined even when direct observation of the uncoupled spin NMR signal in a single pulse experiment would require an impractically long duration of signal averaging. We use this method to quantify residual graphitic carbon using 13 C CPMG NMR in poly(carbon monofluoride) samples synthesized by direct fluorination of carbon from various sources. Our detection limit for graphitic carbon in these materials is better than 0.05 mol%. The accuracy of the method is discussed and comparisons to other methods are drawn.

36 MATERIALS SCIENCE↗