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At least 667 records · Page 37

Ensembles of Metastable States Govern Heterogeneous Catalysis on Dynamic Interfaces

Heterogeneous catalysis is at the heart of chemical industry. Being able to tune and design efficient catalysts for processes of interest is of an utmost importance, and for this, the molecular-level understanding of heterogeneous catalysts is the first step, and indeed a prime focus of the modern catalysis research. For a long time, a single most thermodynamically stable structure of the catalytic interface attained in reaction conditions had been envisioned as the reactive phase. However, some catalytic interfaces continue to undergo structural dynamics in the steady state, triggered by high temperatures, pressures, and binding and changing reagents. Among particularly dynamic interfaces are such widely-used catalysts as crystalline and amorphous surfaced supporting (sub-)nano metallic clusters. Recently, it became clear that this dynamic fluxionality causes the supported clusters to populate many distinct structural and stoichiometric states in catalytic conditions. Hence, the catalytic interface should be viewed as an evolving statistical ensemble of many (not one) structures. As such, every member in the ensemble contributes to the properties of the catalyst differently, and in proportion to its probability to be populated. This new notion flips the established paradigm and calls for new theory, modeling approaches, operando measurements, and updated design strategies. The statistical ensemble nature of surface-supported sub-nano cluster catalysts can be exemplified by oxide-supported and adsorbate-covered Pt, Pd, Cu, CuPd clusters, catalytic toward oxidative and non-oxidative dehydrogenation. They have access to a variety of 3D and quasi-2D shapes. The compositions of their thermal ensembles are dependent on the cluster size, leading to size-specific catalytic activities and the famous “every atom counts” phenomenon. The support and adsorbates affect catalyst structures, and state of the reacting species causes the ensemble to change in every reaction intermediate. The most stable member of the ensemble dominates the thermodynamic properties of the corresponding intermediate, whereas the kinetics can be determined by more active but less populated metastable catalyst states, and that suggests that many earlier studies might have overlooked the actual active sites. Both effects depend on the relative time-scales of catalyst restructuring and reaction dynamics. The catalyst may routinely operate off-equilibrium. Ensemble phenomena lead to surprising exceptions from established rules of catalysis, such as scaling relations, and Arrhenius behavior. Catalyst deactivation is also an ensemble property, and its extent of mitigation can be predicted through the new paradigm. These findings were enabled by advances in theory, such as global optimization and subsequent utilization of multiple local minima, and pathways sampling, as well as operando catalyst characterization. The fact that the per-site and per-species resolution is needed for the description and predicting of catalyst properties gives theory the central role in catalysis research, as most experiments provide ensemble-average information and cannot detect the crucial minority species that may be responsible for the catalytic activity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Ultrasonic characterization of Ti-5Al-5Mo-5V-3Cr

Metastable β titanium alloys such as Ti-5Al-5Mo-5V-3Cr are of increasing interest due to their excellent corrosion resistance, high strength, and in particular, the ability to manipulate microstructure to a high degree to control the mechanical properties of the material. It is therefore important to consider how this manipulation of mechanical properties will affect the inspection of this material with ultrasonic testing both for the purposes of flaw detection and material characterization. The connection between material properties and ultrasonic characterization techniques will be discussed and then dissected in the context of Ti-5553. This metastable alloy was shown to exhibit remarkable variation in microstructure as well as ultrasonic velocity and attenuation demonstrating these techniques as potential candidates for characterizing Ti-5553 and Ti-5553 as a good candidate for aiding in future studies aimed at learning more about the role of secondary phases in ultrasonic wave propagation.

Sunderman, Ruth↗

Uncovering the predictive pathways of lithium and sodium interchange in layered oxides

Ion exchange is a powerful method to access metastable materials with advanced functionalities for energy storage applications. However, high concentrations and unfavourably large excesses of lithium are always used for synthesizing lithium cathodes from parent sodium material, and the reaction pathways remain elusive. Here, using layered oxides as model materials, we demonstrate that vacancy level and its corresponding lithium preference are critical in determining the accessible and inaccessible ion exchange pathways. Taking advantage of the strong lithium preference at the right vacancy level, we establish predictive compositional and structural evolution at extremely dilute and low excess lithium based on the phase equilibrium between Li 0.94 CoO 2 and Na 0.48 CoO 2 . Such phase separation behaviour is general in both surface reaction-limited and diffusion-limited exchange conditions and is accomplished with the charge redistribution on transition metals. Guided by this understanding, we demonstrate the synthesis of Na y CoO 2 from the parent Li x CoO 2 and the synthesis of Li 0.94 CoO 2 from Na y CoO 2 at 1-1,000 Li/Na (molar ratio) with an electrochemical assisted ion exchange method by mitigating the kinetic barriers. Our study opens new opportunities for ion exchange in predictive synthesis and separation applications. Ion exchange is a powerful method to access metastable materials for energy storage, but identifying lithium and sodium interchange in layered oxides remains challenging. Using such model materials, vacancy level and corresponding lithium preference are shown to be crucial for ion exchange pathway accessibility.

25 ENERGY STORAGE↗

Electron microscopic determination of the metastable dissociation region in the system Li sub 2SiO3-SiO sub 2

Seven glasses with an alkali oxide content in the range 9.57 to 29.53 mole percent were investigated. The temperature at which the transition of microheterogeneous mixing to the condition of mutual solubility occurs on heating is found. It is found that the altered constituent composition results in the alteration in the percentage amount of the coexisting phases.

Marinov, M.↗

Waveform effects of a metastable olivine tongue in subducting slabs

Velocity models of subducting slabs with a kinetically-depressed olivine to beta- and gamma-spinel transition are constructed, and the effect that such structures would have on teleseismic P waveforms are examined using a full-wave finite-difference method. These 2D calculations yielded waveforms at a range of distances in the downdip direction. The slab models included a wedge-shaped, low-velocity metastable olivine tongue (MOTO) to a depth of 670 km, as well as a plausible thermal anomaly; one model further included a 10-km-thick fast layer on the surface of the slab. The principal effect of MOTO is to produce grazing reflections at wide angles off the phase boundary, generating a secondary arrival 0 to 4 seconds after the initial arrival depending on the take-off angle. The amplitude and timing of this feature vary with the lateral location of the seismic source within the slab cross-section.

Vidale, John E.↗

Atomic Structure and Dynamics of Unusual and Wide-Gap Phase-Change Chalcogenides: A GeTe 2 Case

Brain-inspired computing, reconfigurable optical metamaterials, photonic tensor cores, and many other advanced applications require next-generation phase-change materials (PCMs) with better energy efficiency and a wider thermal and spectral range for reliable operations. Germanium ditelluride (GeTe 2 ), with higher thermal stability and a larger bandgap compared to current benchmark PCMs, appears promising for THz metasurfaces and the controlled crystallization of atomically thin 2D materials. Using high-energy X-Ray diffraction supported by first-principles simulation, the atomic structure in semiconducting pulsed laser deposition films and metallic high-temperature liquids is investigated. The results suggest that the structural and chemical metastability of GeTe 2 , leading to disproportionation into GeTe and Te, is related to high internal pressure during a semiconductor–metal transition, presumably occurring in the supercooled melt. Similar phenomena are expected for canonical GeS 2 and GeSe 2 under high temperatures and pressures.

74 ATOMIC AND MOLECULAR PHYSICS↗

Generalization of low pressure, gas-liquid, metastable sound speed to high pressures

A theory is developed for isentropic metastable sound propagation in high pressure gas-liquid mixtures. Without simplification, it also correctly predicts the minimum speed for low pressure air-water measurements where other authors are forced to postulate isothermal propagation. This is accomplished by a mixture heat capacity ratio which automatically adjusts from its single phase values to approximately the isothermal value of unity needed for the minimum speed. Computations are made for the pure components parahydrogen and nitrogen, with emphasis on the latter. With simplifying assumptions, the theory reduces to a well known approximate formula limited to low pressure.

Bursik, J. W.↗

Challenging thermodynamics: combining immiscible elements in a single-phase nano-ceramic

Abstract The Hume-Rothery rules governing solid-state miscibility limit the compositional space for new inorganic material discovery. Here, we report a non-equilibrium, one-step, and scalable flame synthesis method to overcome thermodynamic limits and incorporate immiscible elements into single phase ceramic nanoshells. Starting from prototype examples including (NiMg)O, (NiAl)O x , and (NiZr)O x , we then extend this method to a broad range of Ni-containing ceramic solid solutions, and finally to general binary combinations of elements. Furthermore, we report an “encapsulated exsolution” phenomenon observed upon reducing the metastable porous (Ni 0.07 Al 0.93 )O x to create ultra-stable Ni nanoparticles embedded within the walls of porous Al 2 O 3 nanoshells. This nanoconfined structure demonstrated high sintering resistance during 640 h of catalysis of CO 2 reforming of methane, maintaining constant 96% CH 4 and CO 2 conversion at 800 °C and dramatically outperforming conventional catalysts. Our findings could greatly expand opportunities to develop novel inorganic energy, structural, and functional materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Rapid solidification of high-conductivity copper alloys

The main objective was to develop improved copper alloys of high strength and high thermal and electric conductivity. Chill block melt spinning was used to produce binary alloys of Cu-Cr and Cu-Zr, and ternary alloys of Cu-Cr-Ag. By quenching from the liquid state, up to 5 atomic percent of Cr and Zr were retained in metastable extended solid solution during the rapid solidification process. Eutectic solidification was avoided and the full strengthening benefits of the large volume fraction of precipitates were realized by subsequent aging treatment. The very low solid solubility of Cr and Zr in Cu result in a high conductivity Cu matrix strengthened by second phase precipitates. Tensile properties on as-cast and aged ribbons were measured at room and elevated temperatures. Precipitate coarsening of Cr in Cu was studied by changes in electrical resistance during aging. X-ray diffraction was used to measure the lattice parameter and the degree of supersaturation of the matrix. The microstructures were characterized by optical and electron microscopy.

Bloom, Theodore Atlas↗

The 3-D description of vertical current sheets with application to solar flares

Following a brief review of the processes which have been suggested for explaining the occurrence of solar flares we suggest a new scenario which builds on the achievements of the previous suggestion that the current sheets, which develop naturally in 3-D cases with gravity from impacting independent magnetic structures (i.e., approaching current systems), do not consist of horizontal currents but are instead predominantly vertical current systems. This suggestion is based on the fact that as the subphotospheric sources of the magnetic field displace the upper photosphere and lower chromosphere regions, where plasma beta is near unity, will experience predominantly horizontal mass motions which will lead to a distorted 3-D configurations of the magnetic field having stored free energy. In our scenario, a vertically flowing current sheet separates the plasma regions associated with either of the subphotospheric sources. This reflects the balanced tension of the two stressed fields which twist around each other. This leads naturally to a metastable or unstable situation as the twisted field emerges into a low beta region where vertical motions are not inhibited by gravity. In our flare scenario the impulsive energy release occurs, initially, not by reconnection but mainly by the rapid change of the magnetic field which has become unstable. During the impulsive phase the field lines contort in such way as to realign the electric current sheet into a minimum energy horizontal flow. This contortion produces very large electric fields which will accelerate particles. As the current evolves to a horizontal configuration the magnetic field expands vertically, which can be accompanied by eruptions of material. The instability of a horizontal current is well known and causes the magnetic field to undergo a rapid outward expansion. In our scenario, fast reconnection is not necessary to trigger the flare, however, slow reconnection would occur continuously in the current layer at the locations of potential flaring. During the initial rearrangement of the field strong plasma turbulence develops. Following the impulsive phase, the final current sheet will experience faster reconnection which we believe responsible for the gradual phase of the flare. The reconnection will dissipate part of the current and will produce sustained and extended heating in the flare region and in the postflare loops.

Fontenla, Juan M.↗

Linear-in-temperature resistivity for optimally superconducting (Nd,Sr)NiO 2

The occurrence of superconductivity in proximity to various strongly correlated phases of matter has drawn extensive focus on their normal state properties, to develop an understanding of the state from which superconductivity emerges. The recent finding of superconductivity in layered nickelates raises similar interests. However, transport measurements of doped infinite-layer nickelate thin films have been hampered by materials limitations of these metastable compounds: in particular, a high density of extended defects. Here, by moving to a substrate (LaAlO 3 ) 0.3 (Sr 2 TaAlO 6 ) 0.7 that better stabilizes the growth and reduction conditions, we can synthesize the doping series of Nd 1– x Sr x NiO 2 essentially free from extended defects. In their absence, the normal state resistivity shows a low-temperature upturn in the underdoped regime, linear behaviour near optimal doping and quadratic temperature dependence for overdoping. This is phenomenologically similar to the copper oxides despite key distinctions—namely, the absence of an insulating parent compound, multiband electronic structure and a Mott–Hubbard orbital alignment rather than the charge-transfer insulator of the copper oxides. In this study, we further observe an enhancement of superconductivity, both in terms of transition temperature and range of doping. These results indicate a convergence in the electronic properties of both superconducting families as the scale of disorder in the nickelates is reduced.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Jarosite in Gale Crater, Mars: The Importance of Temporal and Spatial Variability and Implications for Habitiability

The Curiosity rover has recently found evidence for small amounts of jarosite, a ferric sulfate, in the Pahrump Hills region at the base of Aeolis Mons (Mount Sharp), Gale crater. While jarosite has been described previously at other locations on Mars, including several sites at Meridiani Planum (explored by the Opportunity rover; and Mawrth Vallis (by remote MRO-CRISM observations; this is the first identification in Gale. Jarosite is interpreted to be a mineral indicator of acidic conditions (pH less than 4; on Earth, it is most commonly found in acid rock-drainage or acid sulfate soil environments. However, jarosite has also been described from a number of terrestrial environments where widespread acidic conditions are not prevalent. As a case study, we describe here an occurrence of sedimentary pyrite nodules that have been variably oxidized in situ to gypsum, schwertmannite, K-/Na-jarosite and iron oxides in a polar desert environment on Devon Island, Nunavut, Canada. Remarkably, these nodules occur in loosely consolidated carbonate sediments, which would have required a higher pH environment at their time of formation and deposition. Thus, acidic conditions may only exist at a small (sub-cm) scale or in a restricted temporal window in an otherwise well-buffered environment. On Devon Island, the jarosite occurs in the most oxidized nodules and is never associated directly with pyrite. Schwertmannite, a metastable iron oxyhydroxysulfate that can form at pH higher than that required for jarosite, occurs in association with partially oxidized pyrite. The paragenetic sequence observed here suggests initial formation of schwertmannite and late-stage precipitation of jarosite in restricted micro-environments, possibly forming via transformation of an amorphous schwertmannite-like phase. While the carbonate environment on Devon Island differs significantly from that of Gale crater, i.e., where we find predominantly basaltic sedimentary rocks, this terrestrial analog provides insight into the significance of jarosite with respect to habitability. For example, the variable abundance of jarosite on Mars and possibly in Gale crater points to potentially localized conditions favorable for jarosite formation. Interestingly, small amounts of sulfide minerals have also been detected by Curiosity at Yellowknife Bay; oxidation of sulfide minerals at Pahrump could explain the presence of small amounts of jarosite. The iron-rich rocks at Pahrump may also represent relatively altered basaltic sediments, or they could be sediments that were altered further by a fluid with a distinct, possibly more acidic, composition. In addition, the abundance of iron-rich amorphous material in Gale rocks allows for the possibility that pre-cursor, iron-bearing phases transform to jarosite post-depositionally. Thus, the occurrence of jarosite at Pahrump could reflect changing paleoenvironmental conditions, though continuing study of its context and textural relationships should provide a fuller understanding of the significance of this mineral to past fluid compositions and past habitability at Gale crater.

Leveille, R. J.↗

Metastable oxygen emission bands

Recombination of ground-state oxygen atoms populates six different bound electronic states of molecular oxygen. Of the six optical transitions expected between the three upper states at 4 to 4.5 electron volts and the two lowest states, five have been observed in the afterglow of a conventional helium-oxygen microwave discharge in both (O-16)2 and (O-18)2, three of them for the first time in gas-phase spectra. Generation of these emissions from oxygen atoms in a system free of molecular oxygen establishes that atom recombination is the production mechanism.

Slanger, T. G.↗

RbB 3 Si 3 : An Alkali Metal Borosilicide that is Metastable and Superconducting at 1 atm

The stability, electronic structure and potential superconductivity in AB 3 Si 3 (A = Na, K, Rb, and Cs) compounds that assume the clathrate-based sodalite structure whose frameworks consists of covalent B-Si bonds is investigated via first-principles calculations. This structure type has recently been predicted in a number of high temperature superconducting hydrides, but these are only stable under megabar pressures. Herein, we predict a novel superconducting phase, RbB 3 Si 3 , that could be synthesized under pressures that are a factor of ten smaller, ~10 GPa, and quenched to atmospheric conditions. Electron-phonon coupling calculations predict that RbB 3 Si 3 possesses a superconducting critical temperature, T c , of 14 K at 1 atm. Here, the dynamic stability of RbB 3 Si 3 and CsB 3 Si 3 at ambient pressure can be explained by considering the chemical pressure exerted on the B-Si framework that is caused by the size effect of the alkali metal atom.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Ion implantation of magnesium guests into type II silicon clathrate films: an alternate approach to doping a cage-like silicon allotrope

Type II silicon clathrates, with their unique cage-like structure, offer exciting potential for applications in thermoelectrics, photovoltaics, and quantum materials due to their tunable electronic and thermal properties. This study investigates the use of ion implantation to introduce targeted guest atoms, which act as dopants, into type II Si clathrate films. The focus is on Mg as a test case for implantation, a dopant previously unreported in type II Si clathrates. The effects of ion implantation on the metastable Si clathrate structure were examined through systematic investigation of implant parameters. Time-of-flight secondary ion mass spectrometry depth profiling confirmed the successful implantation of Mg, while X-ray diffraction and confocal Raman spectroscopy demonstrated minimal structural damage at lower fluences, with the clathrate framework retaining its integrity without converting to other phases. At the higher end of the fluence range implantation caused localized transitions from clathrate to amorphous silicon. Implant activation using rapid thermal annealing was examined with the clathrate structure stable up to 500 °C and being converted to diamond silicon above this temperature. Post-implantation and activation structural characterization showed evidence of damage reversal. Electron paramagnetic resonance studies provided indirect evidence of dopant incorporation. These findings establish a foundation for introducing alternative guests/dopants into the Si clathrate cages through ion implantation, advancing their tunability for next-generation quantum and optoelectronic devices.

36 MATERIALS SCIENCE↗

Forming mechanism of equilibrium and non-equilibrium metallurgical phases in dissimilar aluminum/steel (Al–Fe) joints

Abstract Forming metallurgical phases has a critical impact on the performance of dissimilar materials joints. Here, we shed light on the forming mechanism of equilibrium and non-equilibrium intermetallic compounds (IMCs) in dissimilar aluminum/steel joints with respect to processing history (e.g., the pressure and temperature profiles) and chemical composition, where the knowledge of free energy and atomic diffusion in the Al–Fe system was taken from first-principles phonon calculations and data available in the literature. We found that the metastable and ductile (judged by the presently predicted elastic constants) Al 6 Fe is a pressure ( P ) favored IMC observed in processes involving high pressures. The MoSi 2 -type Al 2 Fe is brittle and a strong P -favored IMC observed at high pressures. The stable, brittle η-Al 5 Fe 2 is the most observed IMC (followed by θ-Al 13 Fe 4 ) in almost all processes, such as fusion/solid-state welding and additive manufacturing (AM), since η-Al 5 Fe 2 is temperature-favored, possessing high thermodynamic driving force of formation and the fastest atomic diffusivity among all Al–Fe IMCs. Notably, the ductile AlFe 3 , the less ductile AlFe, and most of the other IMCs can be formed during AM, making AM a superior process to achieve desired IMCs in dissimilar materials. In addition, the unknown configurations of Al 2 Fe and Al 5 Fe 2 were also examined by machine learning based datamining together with first-principles verifications and structure predictions. All the IMCs that are not P- favored can be identified using the conventional equilibrium phase diagram and the Scheil-Gulliver non-equilibrium simulations.

36 MATERIALS SCIENCE↗

Thermal stability of dopants in boron carbide

Undoped (B 4 C), B rich (B 5.5 C), and B/Si co-doped (Si-B 6.5 C) boron carbides were annealed at 500 °C for up to 21 days to investigate the thermal stability of primary dopants, B and Si. Structural changes associated with dedoping were investigated by X-ray diffraction (XRD) and Raman spectroscopy. The stable phase B 4 C showed no microstructural or lattice parameter changes. Similarly, lattice parameters of B 5.5 C remained constant, suggesting that B dopant is stable at the given conditions. However, the shortened lattice parameters and reduced Si content of Si-B 6.5 C over the annealing time indicated that Si dopant was in a metastable state at the annealing temperature. Consequently, Si dedoping led to an increase in amorphization (a loss of local crystalline order) which degrades the ballistic performance of boron carbide. The insight highlights the importance of Si dopant in boron carbide and suggests that rapid processing may be necessary to retain more silicon for better performance.

36 MATERIALS SCIENCE↗

Magnetic properties of Martian surface material

The hypothesis that the magnetic properties of the Martian surface material are due to the production of a magnetic phase in the clay mineral nontronite by transient shock heating is examined. In the course of the investigation a magnetic material is produced with rather unusual properties. Heating from 900 C to 1000 C, of natural samples of nontronite leads first to the production of what appears to be Si doped maghemite gamma (-Fe2O3). Although apparently metastable, the growth of gamma -Fe2O3 at these temprtures is unexpected, and its relative persistence of several hours at 1000 C is most surprising. Continued annealing of this material for longer periods promote the crystallization of alpha Fe2O3 and cristobalite (high temperature polymorph of SiO2). All available data correlate this new magnetic material with the cristobalite hence our naming it magnetic ferri cristobalite. Formation of this magnetic cristobalite, however, may require topotactic growth from a smectite precursor.

Hargraves, R. B.↗