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At least 289 records · Page 16

Computational discovery of stable and metastable ternary oxynitrides

Materials design from first principles enables exploration of uncharted chemical spaces. Extensive computational searches have been performed for mixed-cation ternary compounds, but mixed-anion systems are gaining increased interest as well. Central to computational discovery is the crystal structure prediction, where the trade-off between reliance on prototype structures and size limitations of unconstrained sampling has to be navigated. We approach this challenge by letting two complementary structure sampling approaches compete. We use the kinetically limited minimization approach for high-throughput unconstrained crystal structure prediction in smaller cells up to 21 atoms. On the other hand, ternary—and, more generally, multinary—systems often assume structures formed by atomic ordering on a lattice derived from a binary parent structure. Thus, we additionally sample atomic configurations on prototype lattices with cells up to 56 atoms. Using this approach, we searched 65 different charge-balanced oxide–nitride stoichiometries, including six known systems as the control sample. The convex hull analysis is performed both for the thermodynamic limit and for the case of synthesis with activated nitrogen sources. We identified 34 phases that are either on the convex hull or within a viable energy window for potentially metastable phases. We further performed structure sampling for “missing” binary nitrides whose energies are needed for the convex hull analysis. Among these, we discovered metastable Ce3N4 as a nitride analog of the tetravalent cerium oxide, which becomes stable under slightly activated nitrogen condition µN > +0.07 eV. Given the outsize role of CeO2 in research and application, Ce3N4 is a potentially important discovery.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Unveiling the ambipolar carrier transport property of SnO 2–X for multiple-functional interlayers in perovskite solar cells

Tin oxides are the most promising electron transport layers in perovskite solar cells. An ambipolar carrier transport property has been recently demonstrated which enables a simple interconnection structure for all-perovskite tandem solar cells. However, the underlying mechanism for its ambipolar behavior is unclear which cannot be explained by the intrinsic defects in SnO 2-x . Here by using density functional theory calculations, we unveil the origin of the ambipolar carrier transport of non-stoichiometry SnO 2-x with a structure of SnO embedded in SnO 2 matrix. The hybridization of O 2p and Sn 5s orbitals of SnO introduces mid-gap states in the bandgap of SnO 2 , enabling hole transport property for SnO 2-x when x is > 0.2. Increasing the percentage of SnO in SnO 2-x significantly enhances the hole transport capability of SnO 2-x due to the enlarged Sn-O-Sn angles that increases orbital overlapping between O and Sn atoms, thus providing strategies for the further tuning of the carrier transport properties of SnO 2-x by compositional and structural designs.

14 SOLAR ENERGY↗

Molecular beam epitaxy of phase-pure antiperovskite Sr 3 SnO thin films

The antiperovskite oxide Sr 3 SnO has attracted substantial interest due to its topologically non-trivial band structure. Sr-deficient Sr3-xSnO can become superconducting, making it a candidate intrinsic topological superconductor. Here, we show that epitaxial, phase-pure Sr 3-x SnO films can be synthesized by molecular beam epitaxy (MBE) using solid Sr and SnO 2 sources. Here, we show that Sn-rich growth conditions result in a large amount of a Sn-rich impurity phase, which is challenging to detect in x-ray diffraction. Carrier densities and the amount of the impurity phase change systematically with the growth conditions, indicating that MBE provides excellent control over the films' stoichiometry. We discuss the electrical properties, including quantum interference phenomena, which support the topological nature of the films.

36 MATERIALS SCIENCE↗

Role of ripples in altering the electronic and chemical properties of graphene

Ripples of graphene are known to manipulate electronic and hydrogenation properties of graphitic materials. More detailed work is needed to elucidate the structure–property relationship of these systems. In this work, the density functional theory is used to compute the energy and electronic structure of the graphene models with respect to variable curvatures and hydrogen adsorption sites. The magnitude of finite bandgap opening depends on the orientation of ripples, and the hydrogen adsorption energy depends on the local curvature of graphene. An adsorbed hydrogen alters the local curvature, resulting in relatively weakened adsorption on the neighboring three sites, which gives a rationale to experimentally observed dynamic equilibrium stoichiometry (H:C = 1:4) of hydrogenated graphene. The surface diffusion transition state energy of adsorbed hydrogen is computed, which indicates that the Eley–Rideal surface recombination mechanism may be important to establish the dynamic equilibrium, instead of the commonly assumed Langmuir–Hinshelwood mechanism.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Understanding copper diffusion in CuInSe 2 with first-principles based atomistic and continuum models

We investigate the diffusion of copper in CuInSe 2 using thermodynamic and kinetic models based on density functional theory calculations, attempting to reconcile large differences in reported experimental diffusivities. We find that observations of rapid chemical diffusion can be explained by large thermodynamic factors, which we calculate using a compositionally constrained model of intrinsic point defect formation. We further characterize how copper diffusion coefficients depend on material synthesis conditions and exhibit their variation across the CuInSe 2 secondary phase diagram. In doing so, we identify stable off-stoichiometries that are dominated by either vacancy- or interstitial-mediated diffusion mechanisms. These results are employed in the development of a continuum reaction–diffusion model, which we use to simulate experimental depth profiles.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Lattice and electronic structure of ScN observed by angle-resolved photoemission spectroscopy measurements

Scandium nitride (ScN) has recently attracted much attention for its potential applications in thermoelectric energy conversion, as a semiconductor in epitaxial metal/semiconductor superlattices, as a substrate for GaN growth, and alloying it with AlN for 5G technology. This study was undertaken to better understand its stoichiometry and electronic structure. ScN (100) single crystals 2 mm thick were grown on a single crystal tungsten (100) substrate by a physical vapor transport method over a temperature range of 1900–2000 °C and a pressure of 20 Torr. The core level spectra of Sc 2p 3/2,1/2 and N 1s were obtained by x-ray photoelectron spectroscopy (XPS). The XPS core levels were shifted by 1.1 eV toward higher values as the [Sc]:[N] ratio varied from 1.4 at 1900 °C to ~1.0 at 2000 °C due to the higher binding energies in stoichiometric ScN. Angle-resolved photoemission spectroscopy measurements confirmed that ScN has an indirect bandgap of ~1.2 eV.

42 ENGINEERING↗

Quantum paramagnetism in a non-Kramers rare-earth oxide: Monoclinic Pr 2 Ti 2 O 7

Little is so far known about the magnetism of the A 2 B 2 O 7 monoclinic layered perovskites that replace the spin-ice supporting pyrochlore structure for r A /r B > 1.78. We show that high quality monoclinic Pr 2 Ti 2 O 7 single crystals with a three-dimensional network of non-Kramers Pr 3+ ions that interact through edge-sharing superexchange interactions, form a singlet ground-state quantum paramagnet that does not undergo any magnetic phase transitions down to, at least, 1.8 K. The chemical phase stability, structure, and magnetic properties of the layered perovskite Pr 2 Ti 2 O 7 were investigated using x-ray diffraction, transmission electron microscopy, and magnetization measurements. Synthesis of polycrystalline samples with the nominal compositions of Pr 2 Ti 2+x O 7 (–0.16 ≤ x ≤ 0.16 ) showed that deviations from the Pr 2 Ti 2 O 7 stoichiometry lead to secondary phases of related structures including the perovskite phase Pr 2/3 TiO 3 and the orthorhombic phases Pr 4 Ti 9 O 24 and Pr 2 TiO 5 . No indications of site disordering (stuffing and antistuffing) or vacancy defects were observed in the Pr 2 Ti 2 O 7 majority phase. A procedure for growth of high-structural-quality stoichiometric single crystals of Pr 2 Ti 2 O 7 by the traveling solvent floating zone method is reported. Thermomagnetic measurements of single-crystalline Pr 2 Ti 2 O 7 reveal an isolated singlet ground state that we associate with the low-symmetry crystal electric-field environments that split the (2J + 1 = 9)-fold degenerate spin-orbital multiplets of the four differently coordinated Pr 3+ ions into 36 isolated singlets resulting in an anisotropic temperature-independent van Vleck susceptibility at low T. Here, a small isotropic Curie term is associated with 0.96(2)% noninteracting Pr 4+ impurities.

36 MATERIALS SCIENCE↗

Revisiting the growth rate hypothesis: Towards a holistic stoichiometric understanding of growth

The growth rate hypothesis (GRH) posits that variation in organismal stoichiometry (C:P and N:P ratios) is driven by growth-dependent allocation of P to ribosomal RNA. The GRH has found broad but not uniform support in studies across diverse biota and habitats. We synthesise information on how and why the tripartite growth-RNA-P relationship predicted by the GRH may be uncoupled and outline paths for both theoretical and empirical work needed to broaden the working domain of the GRH. We found strong support for growth to RNA (r 2 = 0.59) and RNA-P to P (r 2 = 0.63) relationships across taxa, but growth to P relationships were relatively weaker (r 2 = 0.09). Together, the GRH was supported in ~50% of studies. Mechanisms behind GRH uncoupling were diverse but could generally be attributed to physiological (P accumulation in non-RNA pools, inactive ribosomes, translation elongation rates and protein turnover rates), ecological (limitation by resources other than P), and evolutionary (adaptation to different nutrient supply regimes) causes. These factors should be accounted for in empirical tests of the GRH and formalised mathematically to facilitate a predictive understanding of growth.

54 ENVIRONMENTAL SCIENCES↗

Modified atomic layer deposition of MoS 2 thin films

As one of the most attractive transition metal dichalcogenides (TMDs), the growth of molybdenum disulfide (MoS 2 ) with industrial compatibility is of great importance. Atomic layer deposition (ALD) has been shown to be a promising method to achieve the growth of high-quality TMD materials. However, MoS 2 films deposited by ALD often are amorphous with nonideal stoichiometry and require high-temperature post-deposition annealing. Here, we introduce a modified ALD recipe using Mo(CO) 6 and H 2 S, resulting in controllable linear growth behavior, a S-to-Mo ratio of 2:1, and crystalline films at a temperature as low as 190 °C. The growth mechanisms and key factors leading to this improvement are proposed and complemented by kinetics calculations. This newly developed methodology relies on aligning the process time with the reaction kinetics of carbonyl disassociation. The MoS 2 films prepared herein were shown to be active hydrogen evolution reaction catalysts.

2D materials↗

Shake loss intensities in x-ray photoelectron spectroscopy: Theory, experiment, and atomic composition accuracy for MgO and related compounds

The relative intensities of XPS core levels, scaled by their photoionization cross sections, are regularly used to determine sample atomic composition. Cross sections, however, give the intensity to all possible final states for the core ionizations, not just to the main peak. This includes all intrinsic satellite structure (shake states and, for open shell systems, the different ionic multiplets). In practice, for solids, this is usually experimentally impossible to determine accurately because such a satellite structure sits on the inelastically scattered electron background and cannot be easily separated. Therefore, usually, only the intensity of the main peak is used. This limits the ultimate possible accuracy of XPS composition determination. The purpose of the present paper is to examine the contributions that a theoretical analysis of losses of intensity can make to improve quantitation. For an MgO single crystal, we show that the correct stoichiometry of 1:1 can be recovered using the theoretical analysis of the experimental MgO peak ratio intensities. For materials with a sufficient bandgap for the XPS main peaks to be separated from the scattered background, the intensity of main peaks can often be accurately determined. Thus, if one uses theory to calculate that fraction of the total intensity lost from a main peak into all its satellite structure, the intensity of just main peaks could then be used to more accurately determine relative atom % composition. This work tests this approach using a single crystal MgO (50% Mg, 50% O) standard. Ab initio electronic structure theory of representative MgO clusters is used to determine Hartree–Fock wave functions for the ground state and final ionized states corresponding to the main Mg 2p and O1s XPS peaks of the oxide. The sudden approximation, SA, is used to determine the fractional losses from these main peaks to shake satellites, which is found to be greater for O1s than Mg2p. This results in predicted “apparent composition” for stoichiometric MgO of 55.2% Mg, 44.8% O instead of the true 50% Mg, 50% O. Equivalent theory for CaO results in a predicted apparent Ca value of 53.4%. Experimentally, using Mg2s or 2p intensity ratio to O1s, we find values between 52.2% and 56.0% Mg using two crystals and four different instrument electron pass energies. The average value of the measurements is 54.5% Mg when corrected for the presence of an adventitious carbon overlayer and slight surface hydroxide. Though this agreement with theory may be somewhat fortuitous, given the potential experimental errors, which are fully discussed, it is similar to that in our earlier study on LiF. We also present preliminary experimental data on Mg(OH) 2 and MgSO 4 , which show a similar trend of apparently higher than 50% Mg, but we have no theory values. We are not yet able to experimentally test for validation of the difference between apparent composition for MgO (55.2% Mg) and CaO (53.4% Ca), owing to significant carbonate formation at the surface of the single crystal CaO. Here, an important conclusion is that the theoretical determination of shake losses, obtained with ab initio wavefunctions and the SA, is likely to be a useful way to calibrate the accuracy and reliability of compositions obtained from XPS intensities and merits further study.

47 OTHER INSTRUMENTATION↗

Jahn–Teller-driven phase segregation in Mn x Co 3–x O 4 spinel thin films

Transition metal spinel oxides comprised of earth-abundant Mn and Co have long been explored for their use in catalytic reactions and energy storage. However, understanding functional properties can be challenging due to differences in sample preparation and the ultimate structural properties of the materials. Epitaxial thin film synthesis provides a novel means of producing precisely controlled materials to explore the variations reported in the literature. In this work, Mn x Co 3–x O 4 samples from x = 0 to x = 1.28 were synthesized through molecular beam epitaxy and characterized to develop a material properties map as a function of stoichiometry. Here, films were characterized via in situ x-ray photoelectron spectroscopy, x-ray diffraction, scanning transmission electron microscopy, and polarized K-edge x-ray absorption spectroscopy. Mn cations within this range were found to be octahedrally coordinated, in line with an inverse spinel structure. Samples largely show mixed Mn 3+ and Mn 4+ character with evidence of phase segregation tendencies with the increasing Mn content and increasing Mn 3+ formal charge. Phase segregation may occur due to structural incompatibility between cubic and tetragonal crystal structures associated with Mn 4+ and Jahn–Teller active Mn 3+ octahedra, respectively. Our results help in explaining the reported differences across samples in these promising materials for renewable energy technologies.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Development of a two-zone zero-dimensional mixing model for actively fueled prechamber engines

In this numerical work, a zero-dimensional, two-zone mixing model was developed and validated to capture the mixture preparation process of an actively fueled prechamber engine. The model was developed for ethanol-gasoline fuel blends but is applicable to various fuels of interest relevant to prechamber applications. The model was exercised to demonstrate the effects of boundary conditions, fuel composition, and residual content on the mixture stoichiometry predictions. The 0D model showed reasonable agreement in prechamber equivalence ratio predictions with higher fidelity computational fluid dynamics modeling, but the accuracy of model was constrained to the governing assumptions of the injection process. The modeling assumptions surrounding the non-dimensional injection of mass into the prechamber were scrutinized to identify key areas of model improvement. The results indicate heat transfer effects play a crucial role in the evaporation of the fuel within the confined auxiliary chamber, especially when considering fuels with high latent heat of vaporization. Additionally, the presence of fuel films that collect on the prechamber surfaces complicated the modeled evaporative cooling loses as the modeling suggests the films evaporate primarily by means of conduction from the boundary. Furthermore, the developed model serves as a simplified framework to generate calibration maps of prechamber fueling or run real time as an open loop control strategy such that desired prechamber mixture proportions are effectively targeted.

Zero-dimensional↗

Charge Compensation by Iodine Covalent Bonding in Lead Iodide Perovskite Materials

Metal halide perovskite materials (MHPs) are a family of next-generation semiconductors that are enabling low-cost, high-performance solar cells and optoelectronic devices. The most-used halogen in MHPs, iodine, can supplement its octet by covalent bonding resulting in atomic charges intermediate to I− and I0. Here, we examine theoretically stabilized defects of iodine using density functional theory (DFT); defect formation enthalpies and iodine Bader charges which illustrate how MHPs adapt to stoichiometry changes. Experimentally, X-ray photoelectron spectroscopy (XPS) is used to identify perovskite defects and their relative binding energies, and validate the predicted chemical environments of iodine defects. Examining MHP samples with excess iodine compared with near stoichiometric samples, we discern additional spectral intensity in the I 3d5/2 XPS data arising from defects, and support the presence of iodine trimers. I 3d5/2 defect peak areas reveal a ratio of 2:1, matching the number of atoms at the ends and middle of the trimer, whereas their binding energies agree with calculated Bader charges. Results suggest the iodine trimer is the preferred structural motif for incorporation of excess iodine into the perovskite lattice. Understanding these easily formed photoactive defects and how to identify their presence is essential for stabilizing MHPs against photodecomposition.

36 MATERIALS SCIENCE↗

Oxidation of Glycolate in the Defense Waste Processing Facility (DWPF) Recycle Collection Tank - 20305

The Savannah River Site's Defense Waste Processing Facility (DWPF) operations are being upgraded with the introduction of the Nitric-Glycolic Flowsheet. Glycolic acid has been shown superior to formic acid as the reducing acid used during chemical processing. The new flowsheet improves or maintains necessary parameters such as 1) reduction of mercury, 2) adjustment of feed rheology and 3) adjustment of melter oxidation/reduction potential. Further, the potential for catalytic hydrogen generation in DWPF processing is virtually eliminated. DWPF process condensates are collected and returned to the SRS Concentration, Storage and Transfer Facilities (CSTF). The Recycle Collection Tank (RCT) collects off-gas condensate during chemical processing, vitrification, and other unit operations performed in DWPF and is the singular return vessel delivering recycle effluent back to CSTF. Each batch of recycle may contain a small amount of glycolate from chemical processing and melter off-gas condensates. To avoid potential flammability issues due to thermolysis of glycolate in the CSTF, chemical oxidation within the RCT has been investigated as an option for mitigating the transfer of glycolate. Sodium permanganate has been down-selected as the best option for oxidation of glycolate. Testing was performed using both 2-L and 22-L reactors (16,800:1 and 1,530:1 scale by volume) with non-radioactive waste simulants to approximate the expected RCT compositions. RCT simulants were evaluated at various process pH and temperature conditions. Also, RCT operations, namely the sequence of addition of corrosion inhibitors (NaOH and NaNO{sub 2}) versus a permanganate strike, were evaluated. Glycolate was introduced via a sludge simulant to mimic both expected entrainment and abnormal process foam-over conditions - the range being between 68 and 5100 mg/kg glycolate. Glycolate destruction was monitored by ion chromatography (IC). The corresponding manganese behavior was monitored in real-time using in situ ultraviolet-visible (UV-Vis) spectroscopy. RCT glycolate content can be reduced to below the IC detection limit within 90 minutes for all concentrations investigated. Ion Chromatography analysis revealed that under alkaline conditions, glycolate is primarily oxidized to oxalate with no significant formation of CO{sub 2} or carbonate, and nitrite is not oxidized to nitrate. Initially, complete oxidation of organics species and nitrite was assumed. Determination of the mechanistic chemical reaction has allowed the required amount of permanganate to be more accurately predicted and the total addition to be significantly reduced. UV-Vis measurements reveal that permanganate (Mn{sup 7+}) is reduced to manganate (Mn{sup 6+}) in the RCT. The oxidant stoichiometry is defined by using the initial permanganate to glycolate (P/G) molar ratio. At low initial glycolate concentration (68 and 140 mg/kg), the minimum required initial permanganate to glycolate (P/G) molar ratio was found to be 5-6. With high initial glycolate concentrations (5100 mg/kg) a lower (P/G) molar ratio of ∼2.5 was needed. The final portion of this effort supporting the nitric/glycolic flowsheet will be to test actual (fully radioactive) RCT samples as per the above simulant tests. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Lipocalin Blc is a potential heme-binding protein

Lipocalins are a superfamily of functionally diverse proteins defined by a well-conserved tertiary structure despite variation in sequence. Lipocalins bind and transport small hydrophobic molecules in organisms of all kingdoms. However, there is still uncertainty regarding the function of some members of the family, including bacterial lipocalin Blc from Escherichia coli. Here, we present evidence that lipocalin Blc may be involved in heme binding, trans-periplasmic transport, or heme storage. This conclusion is supported by a cocrystal structure, mass-spectrometric data, absorption titration, and in silico analysis. Binding of heme is observed at low micromolar range with one-to-one ligand-to-protein stoichiometry. However, the absence of classical coordination to the iron atom leaves the possibility that the primary ligand of Blc is another tetrapyrrole.

59 BASIC BIOLOGICAL SCIENCES↗

Impact of Processing on Structural and Compositional Evolution in Mixed Metal Halide Perovskites during Film Formation

Understanding crystallization processes and their pathways in metal-halide perovskites is of crucial importance as this strongly affects the film microstructure, its stability, and device performance. While many approaches are developed to control perovskite formation, the mechanisms of film formation are still poorly known. Using time-resolved in situ grazing incidence wideangle X-ray scattering, the film formation of perovskites is investigated with average stoichiometry Cs 0.15 FA 0.85 PbI 3 , where FA is formamidinium, using the popular antisolvent dropping and gas jet treatments and this is contrasted with untreated films. i) The crystallization pathways during spin coating, ii) the subsequent postdeposition thermal annealing, and iii) crystallization during blade coating are studied. The findings reveal that the formation of a nonperovskite FAPbI 3 phase during spin coating is initially dominant regardless of the processing and that the processing treatment (e.g., antisolvent dropping, gas jet) has a significant impact on the as-cast film structure and affects the phase evolution during subsequent thermal treatment. It is shown that blade coating can be used to overcome the nonperovskite phase formation via solvothermal direct crystallization of perovskite phase. This work shows how real-time investigation of perovskite formation can help to establish processing–microstructure–functionality relationships.

36 MATERIALS SCIENCE↗