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DOE OSTI2021

Kinetic Limitations in Single‐Crystal High‐Nickel Cathodes

Abstract High‐nickel cathodes attract immense interest for use in lithium‐ion batteries to boost Li‐storage capacity while reducing cost. For overcoming the intergranular‐cracking issue in polycrystals, single‐crystals are considered an appealing alternative, but aggravating concerns on compromising the ionic transport and kinetic properties. We report here a quantitative assessment of redox reaction in single‐crystal LiNi 0.8 Mn 0.1 Co 0.1 O 2 using operando hard X‐ray microscopy/spectroscopy, revealing a strong dependence of redox kinetics on the state of charge (SOC). Specifically, the redox is sluggish at low SOC but increases rapidly as SOC increases, both in bulk electrodes and individual particles. The observation is corroborated by transport measurements and finite‐element simulation, indicating that the sluggish kinetics in single‐crystals is governed by ionic transport at low SOC and may be alleviated through synergistic interaction with polycrystals integrated into a same electrode.

Ge, Mingyuan↗

DOE OSTI2020

Kinetic Limitations in Single-Crystal High-Nickel Cathodes

High-nickel cathodes attract immense interest for use in lithium-ion batteries, to boost Li-storage capacity while reducing cost. For overcoming the intergranular-cracking issue in polycrystals, single-crystals are considered an appealing alternative, but aggravating concerns on compromising the electrochemical kinetics of electrodes. We report here a quantitative assessment of electrochemical reaction in single-crystal LiNi 0.8 Mn 0.1 Co 0.8 O 2 using operando hard X-ray microscopy/spectroscopy, revealing a strong dependence of redox kinetics on the state of charge (SOC) - being sluggish at low SOC while increasing rapidly as SOC increases both in the bulk electrode and individual particles. The observation is corroborated by transport measurements and finite-element simulation, indicating that the sluggish kinetics in single-crystals is governed by ionic transport at low SOC and may be alleviated through synergistic interaction with polycrystals integrated into a same electrode. Finally, with the elucidated mechanistic origin and alleviation solution of kinetic limitations in single-crystal high-Ni cathodes, this work constitutes a step forward in enabling their practical deployment.

25 ENERGY STORAGE↗

DOE OSTI2022

Plasma production and composition from hypervelocity impacts on solar cell cover glass

Satellites are subjected to detrimental effects from the space environment, including impacts by orbital debris and meteoroids that can cause mechanical or electrical damage. While mechanical damage is well studied, electrical effects resulting from hypervelocity impact (HVI) remain poorly understood. In HVIs, where the projectile speed exceeds the speed of sound in the target material, the impact energy ionizes the material near the surface, creating a plasma that can cause radio frequency emission. This emission is the main source of electrical anomalies in satellites, but the mechanism behind its creation is still unknown. Ground-based experiments have been used to characterize HVI plasma, including the empirical power law relations that describe the impact charge produced as a function of impactor mass and speed. Quantifying these power law relations gives us a better understanding of the species formed in the impact which can eventually lead to plasma evolution models and help us first, understand the mechanism behind radio frequency emission and second, ways to prevent its damage to the satellites. In this paper, we interpret the results of the HVI experiments on solar cell coverglass targets and identify the potential chemical or molecular reactions that form the impact ion species. This is done by looking simultaneously at multiple data sets for different species within the same impact configuration, and using a new technique for quantifying the power law relations for each emitted species. We use time of flight analysis (TOF) to detect the charged particle compositions and determine their initial speeds. The results suggest that the charge production power law is species specific, with different formation mechanisms involved in a single HVI event, some of which are associated with dissociation and some with ionization of a molecule. Furthermore, our results also show that electrons have different power laws that depend on the spacecraft surface charge. TOF measurements of ions from impact events on solar cell cover glass shows the presence of SiO + and SiO – 2 as the dominant species present in plasmas on positively and negatively charged targets, respectively, as well as the formation of FeO + .

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2025

Complex Adsorption Behavior of Neodymium and Ytterbium on Structurally-Distinct Alumina Surfaces

New sources of rare earth elements (REEs) are needed to support a green energy transition. REEs adsorbed to aluminum-rich clays in weathering deposits represent important resources but the mechanisms responsible for their retention and ease of extraction are unresolved. Disordered coordination and co-occurrence of multiple species pose challenges to investigating REE adsorption processes via established spectroscopic methods. In this study, we applied element-specific surface crystallography methods to obtain a new perspective on the complexity of REE adsorption mechanisms and affinities. Alumina (001) and (012) crystal surfaces were utilized to evaluate surface-specific controls on Nd(III) and Yb(III) adsorption behavior. The REEs displayed similar total adsorption to alumina (001) as a mixture of inner- and outer-sphere complexes, but Nd displayed a greater proportion of inner-sphere binding. Adsorption of ordered inner- and outer-sphere REE species was substantially lower on alumina (012). These distinct behaviors reflect differences in the surface functional group charging and topography of the two surfaces. However, alumina (012) also hosted a substantial population of disordered adsorbed species, especially for Nd, potentially associated with Al vacancy surface defects. Here, the accumulation of light versus heavy REEs via adsorption in weathering deposits likely results from multiple, competing reactions affected by clay particle morphology. Leaching procedures for resource recovery should account for differential rates of desorption by coexisting inner- and outer-sphere REE surface complexes.

58 GEOSCIENCES↗

DOE OSTI2022

The Jefferson Lab Eta Factory (JEF) experiment

The Jefferson Lab Eta Factory (JEF) experiment is an upcoming experiment designed to run in Hall D at Jefferson Lab using an upgraded GlueX spectrometer to study various decays of the ? meson. The GlueX spectrometer consists of a ?2 Tesla solenoid magnet housing a liquid hydrogen target and drift chambers used for tracking charged particles and an array of lead glass blocks (the Forward Calorimeter (FCAL)) downstream of the magnet for detecting neutral particles. The decays of the ? meson can be used to measure the light quark mass ratio via the ???+???0 channel and allow access to higher-order terms in Chiral Perturbation Theory via the ???0?? channel. The decays can also be used to constrain new charge-conjugation violating/parity conserving (CVPC) reactions and to search for signatures of dark matter. In particular, the ???0?? channel can be used to search for lepto-phobic dark vector (B) bosons in the reaction ??B? (B??0?) or dark scalar (S) bosons in the reaction ???0S (S???). Studying the rare radiative decay channel ???0?? requires replacing the 4×4×45 cm3 lead glass blocks in the inner region of the FCAL with 2×2×20 cm3 lead tungstate crystals, which will provide twice better position and energy resolution. This talk will describe the JEF physics program and the upgrade to the FCAL.

Taylor, Simon↗

DOE OSTI2025

Oxidation and recharge of reactive structural Fe( II ) in titanomagnetite (Fe 3− x Ti x O 4 ) nanoparticles

Mixed-valent iron oxide minerals, such as magnetite (Fe(II)(Fe(III)) 2 O 4 ), are an important source of solid-state ferrous iron (Fe(II)) that can impact the speciation and transport of electron accepting contaminants in the Earth’s subsurface, such as radioactive pertechnetate ( 99 Tc(VII)O 4 − ). However, when oxidizing conditions are encountered, structural Fe(II) at the mineral surface is consumed yielding a maghemite (γ-Fe(III) 2 O 3 )-like layer that limits further electron transfer. This oxidized surface layer can be recharged back to the original Fe(II)/(III) ratio by re-exposure to reducing conditions, i.e., aqueous solutions containing Fe 2+ . However, for substituted magnetite (Fe 3−x M x O 4 , M = transition metal cation), the extent of this redox recyclability is unclear. Here, we examine oxidation and recharge for titanomagnetite (Fe 3−x Ti x O 4 ) nanoparticles, where the Fe(II)/Fe(III) ratio varies by the amount of Fe(II) required to charge balance the titanium (Ti(IV)) substituted into the structure. The nanoparticles were synthesized by aqueous precipitation from a solution containing ferrous, ferric and titanium chloride at room temperature. Transmission electron microscopy combined with electron energy loss spectroscopy revealed that rapid precipitation formed core–shell-like nanoparticles consisting of a hyperstoichiometric magnetite core, with Ti(IV) and charge balancing Fe(II) enriched at the surface. This surface enrichment made Fe(II) more available for electron transfer reactions with redox active solution species. Examination of oxidation by H 2 O 2 followed by recharge with aqueous Fe 2+ indicates recyclability of reducing equivalents in the nanoparticles, yielding a core recrystallized to stoichiometric magnetite and a shell bearing excess Fe(II) to charge balance the substituted Ti(IV). The recharged particles are shown to have restored redox reactivity with 99 Tc(VII)O 4 − resulting in reduction to 99 Tc(IV)O 2 and oxidation of the structural Fe(II) to Fe(III).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Proton Quenching in Rare-Earth Inorganic Scintillators: GAGG:Ce and YSO:Ce

Scintillator detectors are an integral component of radiation detection systems for a variety of applications such as medical imaging, accelerator diagnostics, and space science. Typically, a scintillator detector’s response is characterized using gamma sources to understand the detection response to different types of radiation, including charged particle detection. However, there exists a nonlinearity of the amount of light produced from an incident gamma ray of specific energy and the light produced from an incident charged particle of the same energy. This important effect, known as quenching, must be accounted for to interpret energies from charged particles incident on detectors. In this article, we present results of quenching parameterization for two types of cerium-doped inorganic scintillators, Y2SiO5:Ce (YSO:Ce) and Gd3Al2Ga3O12:Ce (GAGG:Ce). We measured the light output from incident proton energies from 1 to 25 MeV using a 3-MV tandem accelerator and two reactions: Au(p,p)Au and 3He(d,p)⁴He. Using gamma-ray sources to calibrate the detectors, we compared the measured electron-equivalent energy versus the incident energy expected. Using an adaptation of the Birks semi-empirical formula, we extracted the Birks parameter (kB) to understand quenching. For one of the GAGG:Ce samples, the kB parameter of 0.0072 [g cm-2 MeV-1] is comparable to a similar study where the value of kB was 0.0065 [g cm-2 MeV-1]. For YSO:Ce, no other kB values were found in the literature. Three different types of GAGG:Ce were used to collect measurements of kB as a function of dopant concentration.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2023

A Reaction Mechanism for Carbon Soot in Post-Detonation Flows

This report documents the generation of a mechanism to predict the inclusion of carbon soot particles in a high explosive flow. The mechanism includes gasification and oxidation reactions, formation, sublimation, radiation, and agglomeration. Each part of the mechanism is derived from properties in the literature. The influence of each part of the mechanism is explored using simple, example simulations consisting of a 12 mm diameter 2,4,6-Trinitrotoluene charge detonated in ambient air. The mechanism has not been quantitatively compared to experiments. Additional efforts will be required to tune and validate it, which will require continued advancements in experimental diagnostics and simulation techniques.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

NASA NTRS2016

Electromagnetic Dissociation and Spacecraft Electronics Damage

When protons or heavy ions from galactic cosmic rays (GCR) or solar particle events (SPE) interact with target nuclei in spacecraft, there can be two different types of interactions. The more familiar strong nuclear interaction often dominates and is responsible for nuclear fragmentation in either the GCR or SPE projectile nucleus or the spacecraft target nucleus. (Of course, the proton does not break up, except possibly to produce pions or other hadrons.) The less familiar, second type of interaction is due to the very strong electromagnetic fields that exist when two charged nuclei pass very close to each other. This process is called electromagnetic dissociation (EMD) and primarily results in the emission of neutrons, protons and light ions (isotopes of hydrogen and helium). The cross section for particle production is approximately defined as the number of particles produced in nucleus-nucleus collisions or other types of reactions. (There are various kinematic and other factors which multiply the particle number to arrive at the cross section.) Strong, nuclear interactions usually dominate the nuclear reactions of most interest that occur between GCR and target nuclei. However, for heavy nuclei (near Fe and beyond) at high energy the EMD cross section can be much larger than the strong nuclear interaction cross section. This paper poses a question: Are there projectile or target nuclei combinations in the interaction of GCR or SPE where the EMD reaction cross section plays a dominant role? If the answer is affirmative, then EMD mechanisms should be an integral part of codes that are used to predict damage to spacecraft electronics. The question can become more fine-tuned and one can ask about total reaction cross sections as compared to double differential cross sections. These issues will be addressed in the present paper.

Norbury, John W.↗

DOE OSTI2022

Towards fast-charging high-energy lithium-ion batteries: From nano- to micro-structuring perspectives

Electric vehicles (EVs) have been playing an indispensable role in reducing greenhouse gas emissions for our modern society. However, current EVs are difficult to meet people’s diverse travel needs, especially in long endurance and fast-charging capacities. At the heart of this issue is the physicochemical limit of current lithium-ion batteries (LIBs), which are the core parts for powering the vehicles. Hence, LIBs with simultaneous high energy and power are critically required to further promote the development of EVs. Here, in this review, we first summarize the key electrochemical processes in electrochemical reactions which lead to the corresponding overpotentials in or between multiple battery components. Furthermore, numerical simulations are employed to quantitatively analyze the effects of versatile electrode parameters on electrochemical properties in high-energy NMC811//graphite systems. On the basis of the in-depth understandings from simulation, recent experimental efforts on designing electroactive materials and electrode architectures across multiple length scales are discussed. Among them, nano-structuring can promote local mass transport and stabilize the interfaces at the particle level, while micro-structuring can establish efficient pathways for charge carriers at the electrode level. Finally, we conclude that a tight feedback loop among structure engineering, characterization and simulation should be followed to speed up the understanding of the deficiencies existing in current electrode designs as well as point out the possible electrode optimization routes for next-generation fast-charging LIBs.

25 ENERGY STORAGE↗

DOE OSTI2020

The GlueX beamline and detector

The GlueX experiment at Jefferson Lab has been designed to study photoproduction reactions with a 9-GeV linearly polarized photon beam. The energy and arrival time of beam photons are tagged using a scintillator hodoscope and a scintillating fiber array. The photon flux is determined using a pair spectrometer, while the linear polarization of the photon beam is determined using a polarimeter based on triplet photoproduction. Charged-particle tracks from interactions in the central target are analyzed in a solenoidal field using a central straw-tube drift chamber and six packages of planar chambers with cathode strips and drift wires. Electromagnetic showers are reconstructed in a cylindrical scintillating fiber calorimeter inside the magnet and a lead-glass array downstream. Charged particle identification is achieved by measuring energy loss in the wire chambers and using the flight time of particles between the target and detectors outside the magnet. The signals from all detectors are recorded with flash ADCs and/or pipeline TDCs into memories allowing trigger decisions with a latency of 3.3 $μs$. The detector operates routinely at trigger rates of 40 kHz and data rates of 600 megabytes per second. Here, we describe the photon beam, the GlueX detector components, electronics, data-acquisition and monitoring systems, and the performance of the experiment during the first three years of operation.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2021

Nonresonant Diffusion in Alpha Channeling

The gradient of fusion-born alpha particles that arises in a fusion reactor can be exploited to amplify waves, which cool the alpha particles while diffusively extracting them from the reactor. Furthermore, the corresponding extraction of the resonant alpha particle charge has been suggested as a mechanism to drive rotation. By deriving a coupled linear-quasilinear theory of alpha channeling, we show that, for a time-growing wave with a purely poloidal wave vector, a current in the nonresonant ions cancels the resonant alpha particle current, preventing the rotation drive but fueling the fusion reaction.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

NASA NTRS1989

Biophysical aspects of heavy ion interactions in matter

The biological effects of high energy, high charge nuclei (HZE particles) occupy a central role in the management of space radiation hazards due to galactic cosmic rays. For the energy range of interest, the mean free path for nuclear interactions of these heavy ions is comparable to the thickness of the material traversed, and a significant fraction of stopping particles will undergo a nuclear reaction with the nuclei of the stopping material. Transport methods for HZE particles are dependent on models of the interaction of man-made systems with the space environment to an even greater extent than methods used for other types of radiation. Hence, there is a major need to validate these transport codes by comparison with experimental data. The basic physical properties of HZE particles will be reviewed and illustrated with the results of nuclear fragmentation experiments performed with 670A MeV neon ions incident on a water absorber and with measurements of multiple Coulomb scattering of uranium beams in copper. Finally, the extent to which physical measurements yield radiobiological predictions is illustrated for the example of neon.

Schimmerling, Walter↗

NASA NTRS2009

Observation and Interpretation of Energetic Neutral Hydrogen Atoms from the December 5, 2006 Solar Event

We report the first observations of energetic neutral atoms (ENAs) from a solar flare/coronal mass ejection event. The observations were made during the December 5, 2006 X9 solar flare, located at E79, by the Low Energy Telescopes (LETs) on the STEREO A and B spacecraft. Within 1-2 hours of the flare onset, both LETs observed a sudden burst of 1.6 to 15 MeV protons arriving hours before the onset of the main solar energetic particle (SEP) event at Earth. More than 70% of these particles arrived from a longitude within +-10 degrees of the Sun. The derived emission profile at the Sun lasted for more than an hour and had a profile remarkably similar to the GOES soft X-ray profile. The observed arrival directions and energy spectrum argue strongly that the particle events <5 MeV were due to energetic neutral hydrogen atoms that were stripped of their electrons upon entering the LET sensor. To our knowledge, this is the first reported observation of ENA emission from a solar flare/coronal mass ejection. We discuss possible origins for the production of ENAs in solar events, including charge-transfer reactions involving both flare and shock-accelerated protons. Assuming isotropic emission, we find that ~2 x 10E28 ENAs escaped from the Sun in the upper hemisphere. Based on the 2.2 MeV gamma-ray emission observed by RHESSI in this event, and using measured and theoretical cross sections, we estimate that ~3 x 10E31 ENAs with 1.8 - 5 MeV could be produced by protons accelerated in the flare. CME-driven shock acceleration is also a possible ENA source, but unfortunately there were no CME observations available from this event. Taking into account ENA losses, we conclude that the observed ENAs were most likely produced in the high corona at heliocentric distances 1.6 solar radii.

Mewaldt, R. A.↗

DOE OSTI2024

WDM-SP-25A: Development of a stopping power platform using secondary nuclear reactions in Warm Dense Matter (Director’s Post-Doc Shot Request) [Slides]

Motivation: Recent theoretical modeling at LANL has demonstrated that the ignition criteria is a strong function of the temperature of the DT ice that surrounds the hot spot [Daughton et al. PoP 2023]. Alpha heating of the DT shell can raise the ignition threshold. Critical to modeling the alpha-particle deposition in the shell is understanding charged particle stopping in warm dense matter.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2020

Ultrahigh temperature in situ transmission electron microscopy based bicrystal coble creep in Zirconia II: Interfacial thermodynamics and transport mechanisms

This work uses a combination of stress dependent single grain boundary Coble creep and zero-creep experiments to measure interfacial energies, along with grain boundary point defect formation and migration volumes in cubic ZrO 2 . These data, along with interfacial diffusivities measured in a companion paper are then applied to analyzing two-particle sintering. The analysis presented here indicates that the large activation volume, v * = v f + v m primarily derives from a large migration volume and suggests that the grain boundary rate limiting defects are delocalized, possibly due to electrostatic interactions between charge compensating defects. The discrete nature of the sintering and creep process observed in the small-scale experiments supports the hypothesis that grain boundary dislocations serve as sources and sinks for grain boundary point defects and facilitate strain during sintering and Coble creep. Model two-particle sintering experiments demonstrate that initial-stage densification follows interface reaction rate-limited kinetics.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Multiplicity trigger detector for the S π RIT experiment

A multiplicity trigger detector (MTD) was developed for the SπRIT experiment that aims to probe the high- density symmetry energy via heavy-ion collisions (HICs). The MTD is designed to measure the charged-particle multiplicity in HICs to provide a trigger signal that can be used to select high-multiplicity events induced by central collisions. The MTD consists of two side-walls segmented into 30 plastic scintillation paddles, each equipped with a multi-pixel photon counter. A custom board with EASIROC front-end ASIC is used as readout electronics. A multiplicity logic signal is generated by an on-board FPGA that processes the discriminated signals from EASIROCs. The overall latency of the whole detector system for outputting the trigger is less than 100 ns, including 52 ns of electronics latency for processing the signals. During the measurement of 112 Sn + 124 Sn reactions at an incident energy of 270 MeV/nucleon, the minimum multiplicity threshold of the MTD was set to 4, where the overall trigger efficiency was obtained to be about 39 % for inclusive nuclear reactions. Furthermore, a simulation study with a numerical calculation of HICs found that the central collisions of impact parameters of less than 4 fm can be triggered with a high efficiency of more than 95 % by the experimental trigger condition.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2022

Chemical Challenges that the Peroxide Dianion Presents to Rechargeable Lithium–Air Batteries

Understanding the fundamental redox reactions and processes that occur in lithium–air and, more generally, metal–air batteries is important to the progress of this promising energy-storage technology. Knowledge of the chemistry of the peroxide dianion, O 2 2– , is especially crucial, as the dianion is at the nexus of the charge/discharge cycle of lithium–air batteries. The intrinsic electron transfer properties and redox chemistry of peroxide dianion are poorly defined because it is difficult to isolate the dianion free of protons and metal ions. We review the results of (i) the electron transfer kinetics and (ii) the redox reaction chemistry of isolated peroxide dianion encapsulated within the cavity of a hexacarboxamide cryptand. With regard to the former, electron transfer kinetics measurements provide fundamental Marcus parameters that will be useful for models that seek to disentangle the precise contributions of Li + ion-coupled electron transfer, electron transfer across the Li 2 O 2 solid particle interface, and charge hopping among Li 2 O 2 particles. With regard to the latter, an underappreciated chemistry of peroxide dianion with CO 2 produces peroxymonocarbonate (OOCO 2 2– ) and peroxydicarbonate (O 2 COOCO 2 2– ). An autocatalytic cycle will lead to oxidative degradation of traditional organic electrolytes and other vulnerable cell components employed in lithium–air batteries. Furthermore, this peroxycarbonate-derived chemistry, in addition to more commonly recognized solution-based oxidation chemistry, will need to be mitigated to realize the long-term cyclability of rechargeable lithium–air batteries.

25 ENERGY STORAGE↗