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At least 1,351 records · Page 75

Trickier than It Looks: Isomerization between Five- and Six-Coordinated Zinc in Heterometallic Li 2 Zn 2 Molecule

This report describes the synthesis and characterization of two hetero bi metallic Li–Zn coordination isomers [Li 2 Zn 2 (tbaoac) 6 ] (tbaoac = tert -butyl acetoacetato) that have been isolated separately by the same stoichiometric reaction run in different organic solvents. The 6-coordinated zinc isomer ( 6-Zn ) was synthesized in acetone with high yield, while the 5-coordinated one ( 5-Zn ) was readily obtained from ethanol. The 5-Zn isomer has a low solubility in organic solvents such as alkanes and haloalkanes, while its 6-Zn counterpart exhibits a good solubility in almost all common solvents. Two isomeric molecules feature similar centrosymmetric tetranuclear cyclic assemblies, which are different in their arrangement of tbaoac ligands. While all ligands act as μ 2 -type in the structure of 5-Zn , the two tbaoac groups chelating Li appear as μ 3 -type in 6-Zn , thus providing an additional coordination for Zn ions. However, the real structural transformation between these isomers was shown to be more complex than simply making or breaking a couple of Zn–O bonds. X-ray single-crystal structure analysis, powder X-ray diffraction, multinuclear NMR, DART mass spectrometry, ICP-OES analysis, and TGA have been employed for the characterization of the isomers. The combination of powder X-ray diffraction and 1 H NMR investigation revealed that 6-Zn isomer can be quantitatively transformed to 5-Zn in ethanol, while the reverse conversion instantly takes place in acetone.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Subsurface spectroscopy of heterogeneous materials using optical wavefront shaping

Plastic-bonded explosives and propellants consist of energetic molecular crystals embedded in a polymer matrix that also includes additives, such as taggants, plasticizers, grit, antioxidants, etc. Furthermore, this heterogeneous composition renders these materials optically opaque, limiting optical characterization techniques (e.g., Raman spectroscopy) to probing chemical reactions at the sur-face. However, many reactions of interest are believed to occur inside the material where current optical techniques can not probe. To address this challenge, we have developed a new optical technique that utilizes feedback assisted wavefront shaping (using spatial light modulators) to focus probe light inside a heterogeneous material, such that we can perform subsurface spectroscopy. Recently, we demonstrated this technique by monitoring subsurface photodegradation and thermal degradation of Eu-doped molecular crystals using both fluorescence and Raman spectroscopy. Based off these successes we are now looking into improvements to this technique to allow for greater time resolution, including replacing our spatial light modulators with fast digital mirror devices, using ns optical phase conjugation, and self-healing optical beams.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

The superior hydrothermal stability of Pd/SSZ-39 in low temperature passive NOx adsorption (PNA) and methane combustion

We successfully synthesized uniform SSZ-39 with an average crystal size of about a micron. Pd (0.7 - 3 wt%) was supported on SSZ-39 with Si/Al ratio ~12. The as-synthesized materials were characterized by FTIR, XRD, Helium Ion Microscopy, HAADF-STEM imaging, 27 Al, 29 Si and H solid state NMR spectroscopic techniques. FTIR studies with CO and NO probe molecules reveal that the 0.7 wt% Pd/SSZ-39 material with Si/Al ~12 has the majority of Pd dispersed atomically as isolated Pd(II) and Pd(II)-OH centers, and thus can be used as a low-temperature passive NOx adsorber. Pd(II)-NO, Pd(II)(OH)(NO) and Pd(II)(CO)(NO) complexes form during PNA in this material. We compare this PNA material directly with the Pd/SSZ-13 system (with Si/Al ratio ~12) and show its superior hydrothermal stability. Remarkably, Pd/SSZ-39 with Si/Al ratio ~12 survives hydrothermal aging up to 815 ºC in 10% H 2 O/Air vapor for 16 hours without significant loss in activity. The SSZ-39 crystal structure remains intact during hydrothermal aging up to 1,000 ºC as we elucidate it with XRD and HAADF-STEM imaging/EDS mapping. However, changes to the framework during such harsh hydrothermal treatment significantly change the NOx release profiles during PNA as evidenced by high-field 27 Al NMR on fresh and aged Pd/SSZ-39 samples as well as PNA performance measurements. Besides PNA application, these hydrothermally very stable materials (3 wt% Pd on SSZ-39 with Si/Al ratio ~12) can be used as a robust methane combustion catalyst under industrially relevant conditions (GHSV~600,000hr -1 ). This catalyst shows minimal deactivation after both harsh hydrothermal aging at 750 and 800 ºC, and prolonged time on stream (105 hrs) at 425 °C. In contrast, both 3wt% Pd/alumina and 3wt% SSZ-13 supported samples lose a significant portion of their activity. Our study opens new avenues to prepare the most hydrothermally stable known Pd/zeolite materials with applications for adsorption and catalytic hydrocarbon combustion under industrially relevant conditions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Virtual texture analysis to investigate the deformation mechanisms in metal microstructures at the atomic scale

Understanding the deformation behavior of metallic materials at high strain rates requires the characterization of plasticity contributors such as twins, phase transformed regions, and dislocations. However, predicting the contributions from phase transformation and twinning relies on a complete understanding of the selection of variants for various loading orientations and the evolution of their volume fractions. This manuscript presents a new virtual texture (VirTex) analysis approach to characterize phase transformation and twinning variants in deformed microstructures generated using molecular dynamics (MD) simulations. Furthermore, the VirTex method involves the construction of a rotation matrix to calculate the angle/axis pairs and misorientation angles for each atom in the microstructure. Any changes in the orientation angle from angle/axis pairs and/or structure types are analyzed to determine the nucleation and evolution of variants in the microstructure. The study uses shock deformed single-crystal Fe, Ta, and Cu to analyze the variant selections for phase transformation or twinning or both in BCC and FCC systems. In addition, the VirTex analysis is able to characterize the phase transformation and twinning variants in nanocrystalline Fe and Ta microstructures. Besides characterizing variants, orientation mapping also provides an accelerated and on-the-fly approach for quantifying twin fractions in MD microstructures.

36 MATERIALS SCIENCE↗

Insights into the Structure–Activity Relationships in Metal–Organic Framework-Supported Nickel Catalysts for Ethylene Hydrogenation

Solid supports play an indispensable role in heterogeneous catalysis, as they can directly affect the catalytic activity and selectivity of supported catalysts. However, the specific roles of such supports remain to be demystified owing to the difficulties in obtaining precise structural information on supported catalysts. To understand the effects of MOF topology, pore environment, and metal identity of node supports on the catalytic activity, a Ni catalyst was supported on eight Zr- or Hf-MOFs based on 8-connected nodes: namely M-NU-1200, M-NU-1000, M-NU-1008, and M-NU-1010 (M = Zr, Hf). Single-crystal X-ray diffraction (SCXRD), diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), and X-ray photoelectron spectroscopy (XPS) were employed to characterize the supported catalyst structures. To investigate the support effects on their activities, the supported Ni catalysts were evaluated by using ethylene hydrogenation as a model reaction. The results revealed that all Hf-based-MOF-supported Ni catalysts exhibited higher catalytic reactivity with TOF (turnover frequency) values at least double of those isostructural Zr counterparts. Additionally, MOFs with less congested metal anchoring sites, as a result of the topology and surrounding pore environment, yielded higher TOFs, suggesting the importance of supports in dictating both the catalyst accessibility and activity. Computational analysis complemented the experimental observations and provided insights into reaction barrier differences and their performance variation. Furthermore, this study demonstrates the essential role of the supports and provides a thought for selecting/designing suitable supports in heterogeneous catalysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Decoding the Atomic Structure of Ga 2 Te 5 Pulsed Laser Deposition Films for Memory Applications Using Diffraction and First-Principles Simulations

Neuromorphic computing, reconfigurable optical metamaterials that are operational over a wide spectral range, holographic and nonvolatile displays of extremely high resolution, integrated smart photonics, and many other applications need next-generation phase-change materials (PCMs) with better energy efficiency and wider temperature and spectral ranges to increase reliability compared to current flagship PCMs, such as Ge 2 Sb 2 Te 5 or doped Sb 2 Te. Gallium tellurides are favorable compounds to achieve the necessary requirements because of their higher melting and crystallization temperatures, combined with low switching power and fast switching rate. Ga 2 Te 3 and non-stoichiometric alloys appear to be atypical PCMs; they are characterized by regular tetrahedral structures and the absence of metavalent bonding. The sp 3 gallium hybridization in cubic and amorphous Ga 2 Te 3 is also different from conventional p-bonding in flagship PCMs, raising questions about its phase-change mechanism. Furthermore, gallium tellurides exhibit a number of unexpected and highly unusual phenomena, such as nanotectonic compression and viscosity anomalies just above their melting points. Using high-energy X-ray diffraction, supported by first-principles simulations, we will elucidate the atomic structure of amorphous Ga 2 Te 5 PLD films, compare it with the crystal structure of tetragonal gallium pentatelluride, and investigate the electrical, optical, and thermal properties of these two materials to assess their potential for memory applications, among others.

36 MATERIALS SCIENCE↗

Structure-property relationships in directionally solidified single crystal NiAl

The ordered intermetallic alloy NiAl is being considered as a potential high temperature structural material, but lack of ductility at ambient temperatures, especially in polycrystalline form, is presently a major obstacle in achieving this goal. Even general agreement of the intrinsic ductility that can be achieved in monocrystals is in dispute. In order to understand this problem, two directionally solidified ingots of NiAl which displayed known differences in ductility were characterized in sufficient detail to identify the corresponding microstructural differences. It was found that the type and size of casting defects, i.e., porosity, present in the material were the major factors in controlling ductility of NiAl single crystals and could explain the order of magnitude variance in fracture strains reported in the literature.

Noebe, R. D.↗

Atomic-Scale Surface Studies of Bulk Metallic Glasses. Final Report

Bulk metallic glasses (BMGs) are of both scientific and technological interest because the absence of periodic atomic arrangements provides them with unique physical, chemical, and mechanical properties. Their high strength, superior elasticity, and an ability to be easily formed into virtually unlimited shapes with feature sizes from centimeters to Angstroms by blow molding and thermoplastic forming makes them an attractive choice for more and more practical applications and products. Due to their complex internal structure, however, experiments that yield insight into their exact atomic arrangements have been scarce. As a result, glass physics is one of the last remaining unexplored fields of materials science despite the scientific and technological importance of glasses in our daily lives, and the question how to characterize and control matter away from equilibrium, as glasses are, was listed as one of five Grand Challenges in a recent DoE report. The main reason for the slow progress in glass physics is the lack of experimental tools that enable access to atomic-scale structural and behavioral information for disordered materials. Such atomic-scale knowledge is mandatory to establish structure-property relationships that ultimately could allow to custom-design alloys featuring specific desired characteristics. With no such relationships available, theory development in glass remains basic and the few that exist are often untested. The aim of this research was to enable progress in our understanding of BMGs by developing a new approach that will allow a meaningful application of local surface science methods to specially prepared BMG samples to obtain a wealth of quantitative information on their atomic arrangements. Key was the availability of specially prepared samples whose surfaces feature large atomically flat terraces despite being entirely amorphous, which we have produced from a Pt 57.5 Cu 14.7 Ni 5.3 P 22.5 alloy (‘Pt-BMG’) both under ambient conditions as well as in ultrahigh vacuum using a unique setup that has been specially developed within this grant. Our approach starts with the in-situ preparation of oxide crystals that are terminated by large terraces, from which exact mirror images out of BMG will be produced using thermoplastic forming (TPF); for the research within this grant, we have successfully used (001)-oriented SrTiO 3 single crystal surfaces as well as (100)-, (110)-, and (111)-oriented single crystals made from LaAlO 3 . Since the resulting BMG replicas display all features of the original crystal with sub-Angstrom fidelity, thereby mimicking the original crystal’s termination by atomically flat terraces without being crystalline themselves, they are ideally suited for further investigation. The following atomic-scale local studies were then carried within this proposal: (i) high-resolution surface imaging and local spectroscopy using scanning probe microscopy, which showed disordered atom-like features and revealed changes in the gradient of the local surface potential on a 1-2 nm length scale; (ii) characterization of atomic-scale plastic flow with affected volumes as low as 1000 atoms, which showed local hardness near or above the theoretically predicted maximum and, once plastic deformation was initiated, homogeneous flow of the atoms involved; (iii) characterization of surface relaxation processes and the onset of crystallization induced by annealing, which showed that upon heating over the material’s glass transition temperature, the surface rearranges and relaxes towards a more stable, denser packed glass, which increases on-terrace surface roughness, while surface tension smoothens step edges; and (iv) studies that investigate the dependence of the material’s mechanical properties and structure on processing parameters, revealing that relaxed glasses get denser, harder, and more elastic. In combination, this information allows to combine structural models with mechanical properties and preparation history, thereby facilitating the development of preparation-structure-property relationships for metallic glasses. With the availability of such information, bulk metallic glasses can be further optimized to be used in more and more applications in industry.

36 MATERIALS SCIENCE↗

Titanium-doped sapphire laser research and design study

Three main topics were considered in this study: the fundamental laser parameters of titanium-doped sapphire, characterization of commercially grown material, and design of a tunable, narrow-linewidth laser. Fundamental parameters investigated included the gain cross section, upper-state lifetime as a function of temperature and the surface-damage threshold. Commercial material was found to vary widely in the level of absorption of the laser wavelength with the highest absorption in Czochralski-grown crystals. Several Yi:sapphire lasers were constructed, including a multimode laser with greater than 50mJ of output energy and a single-transverse-mode ring laser, whose spectral and temporal characteristics were completely characterized. A design for a narrow-linewidth (single-frequency) Ti:sapphire laser was developed, based on the results of the experimental work. The design involves the use of a single-frequency, quasi-cw master oscillator, employed as an injection source for a pulsed ring laser.

Moulton, Peter F.↗

Compositional variation in late-stage differentiates in mare lavas, as indicated by silicate melt inclusions

Questions regarding an interpretation of data from silicate melt inclusions are considered, taking into account the fragmental nature of the record, the possible effects of cooling rate on late-stage melt composition, and the crystallization of the trapped melt. New data related to 484 new analyses are provided in a separate table. Textural and mineralogical features and bulk chemical composition for an overall characterization of late-stage differentiates are discussed. A description is presented of a grouping and recognition of rock types on the basis of late-stage inclusion analyses. Attention is given to the bimodality of potassium values and the delineation of differentiation trends. It is found that many of the problems in interpretation and much of the scatter found in the composition of silicate melt inclusions in lunar samples can be attributed to the incomplete nature of the record and to crystallization after trapping.

Roedder, E.↗

Duration of a Magma Ocean and Subsequent Mantle Overturn in Mars: Evidence from Nakhlites

It is now generally accepted that the heat produced by accretion, short-lived radioactive elements such as Al-26, and gravitational energy from core formation was sufficient to at least partially melt the silicate portions of terrestrial planets resulting in a global-scale magma ocean. More particularly, in Mars, the geochemical signatures displayed by shergottites, are likely inherited from the crystallization of this magma ocean. Using the short-lived chronometer Sm-146 - Nd-142 (t(sup 1/2) = 103 Myr), the duration of the Martian magma ocean (MMO) has been evaluated to being less than 40 Myr, while recent and more precise ND-142/ND-144 data were used to evaluate the longevity of the MMO to approximately 100 Myr after the solar system formation. In addition, it has been proposed that the end of the crystallization of the MMO may have triggered a mantle overturn, as a result of a density gradient in the cumulate layers crystallized at different levels. Dating the mantle overturn could hence provide additional constraint on the duration of the MMO. Among SNC meteorites, nakhlites are characterized by high epsilon W-182 of approximately +3 and an epsilon Nd-142 similar to depleted shergottites of +0.6-0.9. It has hence been proposed that the source of nakhlites was established very early in Mars history (approximately 8-10 Myr). However, the times recorded in HF-182-W-182 isotope system, i.e. when 182Hf became effectively extinct (approximately 50 Myr after solar system formation) are less than closure times recorded in the Sm-146-Nd-142 isotope system (with a full coverage of approximately 500 Myr after solar system formation). This could result in decoupling between the present-day measured epsilon W-182 and epsilon Nd-142 as the SM-146 may have recorded later differentiation events in epsilon ND-142 not observed in epsilon W-182 values. With these potential complexities in short-lived chronological data for SNC's in mind, new Hf-176/Hf-177, Nd-143/Nd-144 and Nd-142/Nd-144 were obtained for three nakhlites (Nakhla, MIL03346 and Yamato000593). These new data are combined with previous epsilon W-182 data, to investigate potential discrepancies between the Hf-182-W-182 and Sm-146-Nd-142 systematics, and the relationship between the source of nakhlites and a crystallizing magma ocean

Debaille, V.↗

Femtosecond resolution of soft mode dynamics in structural phase transitions

The microscopic pathway along which ions or molecules in a crystal move during structural phase transition can often be described in terms of a collective vibrational mode of the lattice. In many cases, this mode, called a 'soft' phonon mode because of its characteristically low frequency near the phase transition temperature, is difficult to characterize through conventional frequency-domain spectroscopies such as light or neutron scattering. A femtosecond time-domain analog of light-scattering spectroscopy called impulsive stimulated Raman scattering (ISRS) has been used to examine the soft modes of two perovskite ferroelectric crystals. The low-frequency lattice dynamics of KNbO3 and BaTiO3 are clarified in a manner that permits critical evaluation of microscopic models for their ferroelectric transitions. The results illustrate the advantages of ISRS over conventional Raman spectroscopy of low-frequency, heavily damped soft modes.

Dougherty, Thomas P.↗

Control of nucleation and growth in protein crystal growth

The potential advantages of nucleation and growth control through temperature, rather than the addition of precipitants or removal of solvent, are discussed. A simple light scattering arrangement for the characterization of nucleation and growth conditions in solutions is described. The temperature dependence of the solubility of low ionic strength lysozyme solutions is applied in preliminary nucleation and growth experiments.

Rosenberger, Franz↗

Insights into Copper Sulfide Formation from Cu and S K edge XAS and DFT studies

An understanding of the fundamentals of the reaction between CuO with trace amounts of H 2 S to form CuS products is critical for the optimal utilization of this process in sulfur removal applications. Unfortunately, CuS is a complex material, featuring various Cu 2-x S compounds (with 0 ≤ x ≤ 1), distorted crystal phases, and varying electronic structures and coordination environments of Cu and S ions. In this work, we combine ex situ and in situ X-ray absorption spectroscopy (XAS) at S and Cu K edges, fixed bed sorption experiments, DFT simulations, and other characterization techniques to speciate the CuS products formed at different temperatures (298–383 K) and from CuO sorbents with different crystallite sizes (2.8–40 nm). The results of our analysis identify the formation of a distorted CuS layer at the surface of CuO crystals with disulfide groups with shorter Cu–S bonds and higher delocalization of the positive charge of the Cu center into (S 1– )2. This distorted CuS layer dominates the XAS signal at lower temperatures (298–323 K) and at the initial stages of sulfidation at higher temperatures (353 and 383 K) where conversion is low (<40%). First-principles atomistic simulations confirm the thermodynamic favorability of the formation of surface (S 1– )2 on both CuO (111) and ($\bar{1}11$) surfaces, providing further support for our experimental observations. Furthermore, these simulations reveal that the presence of disulfide bonds stabilized surface hydroxyl groups, leading to lower Gibbs Free Energies of their surface migration.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Micro-spectroscopic and freezing characterization of ice-nucleating particles collected in the marine boundary layer in the eastern North Atlantic

Abstract. Formation of atmospheric ice plays a crucial role in the microphysical evolution of mixed-phase and cirrus clouds and thus climate. How aerosol particles impact ice crystal formation by acting as ice-nucleating particles (INPs) is a subject of intense research activities. To improve understanding of atmospheric INPs, we examined daytime and nighttime particles collected during the Aerosol and Cloud Experiments in the Eastern North Atlantic (ACE-ENA) field campaign conducted in summer 2017. Collected particles, representative of a remote marine environment, were investigated for their propensity to serve as INPs in the immersion freezing (IMF) and deposition ice nucleation (DIN) modes. The particle population was characterized by chemical imaging techniques such as computer-controlled scanning electron microscopy with energy-dispersive X-ray analysis (CCSEM/EDX) and scanning transmission X-ray microscopy with near-edge X-ray absorption fine-structure spectroscopy (STXM/NEXAFS). Four major particle-type classes were identified where internally mixed inorganic–organic particles make up the majority of the analyzed particles. Following ice nucleation experiments, individual INPs were identified and characterized by SEM/EDX. The identified INP types belong to the major particle-type classes consisting of fresh sea salt with organics or processed sea salt containing dust and sulfur with organics. Ice nucleation experiments show IMF events at temperatures as low as 231 K, including the subsaturated regime. DIN events were observed at lower temperatures of 210 to 231 K. IMF and DIN observations were analyzed with regard to activated INP fraction, ice-nucleation active site (INAS) densities, and a water activity-based immersion freezing model (ABIFM) yielding heterogeneous ice nucleation rate coefficients. Observed IMF and DIN events of ice formation and corresponding derived freezing rates demonstrate that the marine boundary layer aerosol particles can serve as INPs under typical mixed-phase and cirrus cloud conditions. The derived IMF and DIN parameterizations allow for implementation in cloud and climate models to evaluate predictive effects of atmospheric ice crystal formation.

54 ENVIRONMENTAL SCIENCES↗

Elusive Double Perovskite Iodides: Structural, Optical, and Magnetic Properties

Halide double perovskites [A 2 M I M III X 6 ] are an important class of materials that have garnered substantial interest as non-toxic alternatives to conventional lead iodide perovskites for optoelectronic applications. While numerous studies have examined chloride and bromide double perovskites, reports of iodide double perovskites are rare, and their definitive structural characterization has not been reported. Predictive models have aided us here in the synthesis and characterization of five iodide double perovskites of general formula Cs 2 NaLnI 6 (Ln=Ce, Nd, Gd, Tb, Dy). Finally, the complete crystal structures, structural phase transitions, optical, photoluminescent, and magnetic properties of these compounds are reported.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Bridging the gap between NMR measured mean silicate chain length and nano-scale silicate polymorphism of calcium silicate hydrates

Variable stoichiometry and silicate polymorphism in calcium-silicate-hydrates (C-S-H) has impeded the revelation of point defects distribution in the silicate tetrahedral network of C-S-H, which resembles tobermorite crystal structure with some bridging tetrahedra (BT) and paired tetrahedra (PT) vacancies in dreierketten chains. Here we use a computational approach to characterize silicate polymorphism by introducing the vacancy ratio of BT to PT (α) and establishing a three-term empirical mean chain length (MCL) formula for different calcium-to‑silicon ratios (Ca/Si) ranging from 1.2 to 2.3. The formula identifies BT and PT controls at low and high α respectively and allows an inverse mapping of polymorphic range based on NMR experiments. The proposed computational framework quantitatively describes silicate polymorphs and links NMR-measured MCL to C-S-H atomistic configurations at the molecular level.

36 MATERIALS SCIENCE↗