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The role of H–H interactions and impurities on the structure and energetics of H/Pd(111)

Understanding hydrogen incorporation into palladium requires detailed knowledge of surface and subsurface structure and atomic interactions as surface hydrogen is being embedded. Using density functional theory (DFT), we examine the energies of hydrogen layers of varying coverage adsorbed on Pd(111). Here we find that H–H and H–Pd interactions promote the formation of the well-known ($\sqrt{3}$ x $\sqrt{3}$) phases but also favor an unreported (3 × 3) phase at high H coverages for which we present experimental evidence. We relate the stability of isolated H vacancies of the (3 × 3) phase to the need of H 2 molecules to access bare Pd before they can dissociate. Following higher hydrogen dosage, we observe initial steps of hydride formation, starting with small clusters of subsurface hydrogen. The interaction between H and Pd is complicated by the persistent presence of carbon at the surface. X-ray photoelectron spectroscopy experiments show that trace amounts of carbon, emerging from the Pd bulk despite many surface cleaning cycles, become mobile enough to repopulate the C-depleted surface at temperatures above 200 K. When exposed to hydrogen, these surface carbon atoms react to form benzene, as evidenced by scanning tunneling microscopy observations interpreted with DFT.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

One-dimensional Rashba states with unconventional spin texture in Bi chains

Spin-polarized electrons confined in low-dimensional structures are of high interest for spintronics applications. Here, in this study, we investigate the electronic structure of an ordered array of Bi monomer and dimer chains on the Ag(110) surface. By means of spin-resolved photoemission spectroscopy, we find Rashba-Bychkov split bands crossing the Fermi level with one-dimensional constant energy contours. These bands are up-spin polarized for positive wave vectors and down-spin polarized for negative wave vectors, at variance with the Rashba-Bychkov model that predicts a pair of states with opposite spin in each half of the surface Brillouin zone. Density functional theory shows that spin-selective hybridization with the Ag bulk bands originates this unconventional spin texture.

1-dimensional spin chains↗

Passivation and Degradation of Sulfur-Treated Silicon Surfaces for Photovoltaics

Sulfur-based passivation for silicon surfaces using H2S gas is an alternative passivation method to reduce the thermal budget for Si photovoltaics. To understand the impact of the high-quality passivation and an observed passivation efficiency decrease after air exposure, we have studied the chemical surface structure by X-ray photoelectron spectroscopy (XPS), X-ray Auger electron spectroscopy (XAES), and S and Si L2,3 X-ray emission spectroscopy (XES). On the S-passivated silicon surfaces, we find the formation of S–Si bonds, in addition to some Si–O bonds. Upon air exposure, sulfur partially desorbs from the Si surface and an increased presence of Si–O and S–O bonds is observed. We identify that well-defined S–Si bonds are crucial to maintain high-quality surface passivation for Si photovoltaics, which allows further optimization of the fabrication process for S-based passivation on silicon.

Hua, Amandee↗

Reaction paths of methane activation and oxidation of surface intermediates over NiO on Ceria-Zirconia catalysts studied by In-situ FTIR spectroscopy

Methane activation over NiO/Ce 0.82 Zr 0.18 O 2 catalysts synthesized by combustion synthesis is studied by in-situ IR spectroscopy and correlated to the properties and oxygen speciation of the catalyst. Through XRD, H 2 -TPR, and pyridine adsorption followed by FTIR spectroscopy, the reducibility and Lewis acidity of the catalysts are assessed. In-situ FTIR spectroscopy is used to monitor the methane activation on catalyst surfaces. Complex IR features of methane-derived surface species are observed and are attributed to the formation of surface alkyl/alkoxy, aldehyde, formate/carbonate, and aromatic species. A data analysis algorithm is developed to evaluate the evolution of different surface species over time. The formation of formate and carbonate species is driven by adsorbed surface oxygen, while less reactive oxygen species associated with NiO allow for the production of aromatics and alkoxy intermediates. Finally, by tuning the reducibility and Lewis acidity of the catalyst, the selectivity to alkoxy intermediates can be improved.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Oxidation of Alloy X in Subcritical, Transition, and Supercritical Water

This work investigates the oxidation of a nickel-based superalloy, namely Alloy X, in water at elevated temperatures: subcritical water at 261°C and 27 MPa, the transition between subcritical and supercritical water at 374°C and 27 MPa, and supercritical water at 380°C and 27 MPa for 100 h. The morphology of the sample surfaces were studied using scanning electron microscopy coupled with focused ion beam milling, and the surface chemistry was investigated using x-ray diffraction, Raman spectroscopy, energy dispersive x-ray spectroscopy, and x-ray photoelectron spectroscopy before and after exposure studies. Surfaces of all samples were identified to comprise of a ferrite spinel containing aluminum.

Materials Science↗

Interplay of Kondo physics with incommensurate charge density waves in CeTe 3

CeTe 3 is a 2-dimensional (2D) Van der Waals (VdW) material with incommensurate charge density waves (CDW), extremely high transition temperature (T CDW ), and a large momentum-dependent CDW gap that leaves a significant portion of the Fermi surface intact. It is also considered to be a weak Kondo system, a property unexpected for a material with incommensurate CDW, where each atomic site is slightly different. Here, we study the properties of the CDW state in several RTe3 (R is rare earth) materials and examine the hybridization of itinerant states with the localized Ce 4f multiplet in CeTe 3 by using angle resolved photoemission spectroscopy. We find that the renormalization of the itinerant states originating from the hybridization with the deeper localized 4f states at −260 meV is k−dependent and extends to the Fermi level. As these localized states are far from the Fermi level, the observed hybridization affects the effective masses only marginally and does not lead to heavy fermions. However, since the same renormalizing mechanism normally leads to the heavy fermion physics when the localized 4f states are near the Fermi level, our observation of its strong k−dependence suggests that this could be the reason for discrepancy between the heavy masses in specific heat and light ones in Shubnikov de Haas oscillations, often observed in heavy fermions.

36 MATERIALS SCIENCE↗

Aluminum hydroxide, bayerite, boehmite, and gibbsite ToF-SIMS spectra in the negative ion mode. I

We report time-of-flight secondary ion mass spectrometry (ToF-SIMS) was performed for boehmite (AOH-60) and its potential products of oxidation including pseudo-boehmite (AOH-180), α- and γ-Al 2 O 3 , and α- and γ-Al(OH) 3 . Since boehmite is often incorporated on cladding materials to prevent corrosion, surface analysis techniques are performed to determine the amount of oxidation present. This ToF-SIMS spectral library is of significance because it includes boehmite and its potential oxidation products (i.e., aluminum oxide and hydroxide), which can be used to compare to spectra obtained for real-world samples containing boehmite. Furthermore, ToF-SIMS is often used as a complementary technique to x-ray photoelectron spectroscopy due to its surface sensitivity and ability to compare spectra via a multivariate analysis, therefore establishing that the molecular signatures of boehmite and relevant compounds are essential for peak identification. The SIMS spectra shown are acquired from commercially available powders, which were deposited onto a silicon wafer substrate via liquid slurry drop casting. This library of SIMS mass spectra will serve as a comparison of boehmite [γ-AlO(OH)], pseudo-boehmite [AlOOH∙nH 2 O], α- and γ-Al 2 O 3 aluminum oxide, and α- and γ-Al 2 O 3 aluminum hydroxide in the negative ion mode, which compliments those reported in the positive ion mode.

36 MATERIALS SCIENCE↗

Surface Ligand Effects on Energetics, Charge Transfer, and Stability at Interfaces Between Metal Halide Perovskites and Organic Semiconductors

Chemistry at organic-inorganic interfaces plays a major role in determining the performance of electronic and optoelectronic devices. Understanding, developing, and using surface chemistry is thus essential for creating improved and novel materials and devices. Organic metal halide perovskites (HPs) are inexpensive semiconductors that can be printed from solution to make efficient photovoltaic cells for harvesting solar energy, light emitting diodes for energy efficient solid-state lighting applications, solid-state lasers, and even spin selective devices with applications to quantum computing. To realize the potential of HPs, their surface chemistry and interfacial properties must be better understood and appropriately adjusted to meet the needs of the targeted application. For example, surface chemistry influences non-radiative recombination, which influences the efficiency of light emission and solar energy conversion, charge-carrier injection and extraction from optoelectronic devices, and material and device stability. This research project centered around determining how the surface chemistry of HP thin films and nanoparticles influences optical properties, charge transfer processes, energetics, and stability. In this project we characterized ligand binding strengths to HPs; determined how surface ligand chemistry influences photoluminescence properties, energetics, and charge transfer processes; determined that surface ligands often penetrate into HPs and uncovered methods of reducing surface ligand penetration through structural modifications; and discovered how interfacial energetics impact charge transfer processes and photovoltaic performance parameters. Overall, this research established important insights into how surface ligands interact with HPs to influence their optical properties, electronic properties, stability, and device level performance.

14 SOLAR ENERGY↗

Mixed Ligand Passivation as the Origin of Near-Unity Emission Quantum Yields in CsPbBr 3 Nanocrystals

Key features of syntheses, involving the quaternary ammonium passivation of CsPbBr 3 nanocrystals (NCs), include stable, reproducible and large (often near-unity) emission quantum yields (QYs). The archetypical example involves didodecyl dimethyl ammonium (DDDMA + ) passivated CsPbBr 3 NCs where robust QYs stem from interactions between DDDMA + and NC surfaces. Despite widespread adoption of this synthesis, specific ligand-NC surface interactions responsible for large DDDMA + -passivated NC QYs have not been fully established. Multidimensional nuclear magnetic resonance experiments now reveal a new DDDMA + -NC surface interaction, beyond established “tightly-bound” DDDMA + interactions, which strongly affects observed emission QYs. Depending upon the existence of this new DDDMA + coordination, NC QYs vary broadly between 60% and 85%. More importantly, these measurements reveal surface passivation through unexpected didodecyl ammonium (DDA + ) that works in concert with DDDMA + , to produce near unity (i.e. >90%) QYs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

All-epitaxial long-range surface plasmon polariton structures with integrated active materials

We demonstrate all-epitaxial structures capable of supporting short- and long-range surface plasmon polariton (SRSPP and LRSPP) modes in the long-wave infrared region of the electromagnetic spectrum. The SRSPP and LRSPP modes are bound to the interfaces of a buried heavily doped (n ++ ) semiconductor layer and surrounding quantum-engineered type-II superlattice (T2SL) materials. The surrounding T2SLs are designed to allow optical transitions across the frequency dispersion of the SPP modes. We map the SPP dispersion in our structure using grating-coupled angle- and polarization-dependent reflection and photoluminescence spectroscopy. The epitaxial structures are analytically described using a simplified three-layer system (T2SL/n ++ /T2SL) and modeled using rigorous coupled wave analysis with excellent agreement to our experimental results. The presented structures offer the potential to serve as long-range interconnects or waveguides in all-epitaxial plasmonic/optoelectronic systems operating in the long-wave infrared.

36 MATERIALS SCIENCE↗

Observation of spin-momentum locked surface states in amorphous Bi 2 Se 3

Crystalline symmetries have played a central role in the identification and understanding of quantum materials. Here we investigate whether an amorphous analogue of a well-known three-dimensional strong topological insulator has topological properties in the solid state. We show that amorphous Bi 2 Se 3 thin films host a number of two-dimensional surface conduction channels. Our angle-resolved photoemission spectroscopy data are consistent with a dispersive two-dimensional surface state that crosses the bulk gap. Spin-resolved photoemission spectroscopy shows this state has an anti-symmetric spin texture, confirming the existence of spin-momentum locked surface states. We discuss these experimental results in light of theoretical photoemission spectra obtained with an amorphous topological insulator tight-binding model, contrasting it with alternative explanations. In conclusion, the discovery of spin-momentum locked surface states in amorphous materials opens a new avenue to characterize amorphous matter and triggers the search for an overlooked subset of quantum materials outside of current classification schemes.

36 MATERIALS SCIENCE↗

Activating magnetite ores for aqueous ironmaking at high current densities

Low-temperature electrochemical cells reducing iron oxides to metal in alkaline electrolytes can support fully electrified steelmaking processes. Previous studies on these cells have primarily focused on high-surface-area hematite, Fe 2 O 3 , reactants whereas attempts to reduce suspensions of magnetite, Fe 3 O 4 —one of the two feedstocks for existing ironmaking reactors—have generally been limited to low rates of reaction (<30 mA cm −2 ). Here, in this study, we control the crystalline domain size of Fe 2 O 3 and Fe 3 O 4 particles in 10 M NaOH electrolytes to study how the nanoscale morphology of oxides controls the rate of electrochemical ironmaking. Rotating-ring disk electrode measurements of Fe 2+ , in situ Raman spectroscopy of the electrode surface, and ex situ electron microscopy were consistent with a hypothesized passivation process at Fe 3 O 4 surfaces that may prevent the continuous formation of soluble intermediates. Sufficiently small (<100 nm diameter) oxide particles yielded Fe partial current densities >160 mA cm −2 , a fivefold increase relative to previously reported rates for Fe 3 O 4 suspensions and comparable to active Fe 2 O 3 . Electron microscopy revealed that electrodeposited films were composed of micron-scale crystalline Fe domains with a porous film of Fe 3 O 4 nanoparticles and supports a model where Fe is grown primarily from soluble Fe 2+ intermediates. Based on these insights, inactive blast-furnace-grade iron-oxides were transformed into high surface area nanoparticles (1.6 to 229.2 m 2 g −1 ) via reprecipitation, leading to a ninefold enhancement in faradaic efficiency and an Fe partial current density of 120 mA cm −2 . When integrated with chlor-iron cells producing reagents for reprecipitation, this approach could lead to a cost-competitive process for electrochemical ironmaking from industrially relevant feedstocks.

TEM↗

Electrocatalytic Isoxazoline–Nanocarbon Metal Complexes

In this work, we report the synthesis of new carbon-nanomaterial-based metal chelates that enable effective electronic coupling to electrocatalytic transition metals. In particular, multiwalled carbon nanotubes (MWCNTs) and few-layered graphene (FLG) were covalently functionalized by a microwave-assisted cyclo-addition with nitrile oxides to form metal-binding isoxazoline functional groups with high densities. The covalent attachment was evidenced by Raman spectroscopy, and the chemical identity of the surface functional groups was confirmed by X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). The functional carbon nanomaterials effectively chelate precious metals Ir(III), Pt(II), and Ru(III), as well as earth-abundant metals such as Ni(II), to afford materials with metal contents as high as 3.0 atom %. The molecularly dispersed nature of the catalysts was confirmed by X-ray absorption spectroscopy (XAS) and energy-dispersive X-ray spectroscopy (STEM-EDS) elemental mapping. The interplay between the chelate structure on the graphene surface and its metal binding ability has also been investigated by a combination of experimental and computational studies. The defined ligands on the graphene surfaces enable the formation of structurally precise heterogeneous molecular catalysts. The direct attachment of the isoxazoline functional group on the graphene surfaces provides strong electronic coupling between the chelated metal species and the conductive carbon nanomaterial support. We demonstrate that the metal-chelated carbon nanomaterials are effective heterogeneous catalysts in the oxygen evolution reaction with low overpotentials and tunable catalytic activity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Selective hybridization between the main band and the superstructure band in the Bi 2 Sr 2 CaCu 2 O 8 + δ superconductor

High-resolution laser-based angle-resolved photoemission measurements have been carried out on Bi 2 Sr 2 CaCu 2 O 8+δ (Bi2212) and Bi 2 Sr 2–x La x CuO 6+δ (Bi2201) superconductors. Unexpected hybridization between the main band and the superstructure band in Bi2212 is clearly revealed. In the momentum space where one main Fermi surface intersects with one superstructure Fermi surface, four bands are observed instead of two. The hybridization exists in both the superconducting state and the normal state, and in Bi2212 samples with different doping levels. Such a hybridization is not observed in Bi2201. This phenomenon can be understood by considering the bilayer splitting in Bi2212, the selective hybridization of two bands with peculiar combinations, and the altered matrix element effects of the hybridized bands. These observations indicate that the origin of the superstructure bands is intrinsic to the CuO 2 planes. Furthermore, understanding physical properties and superconductivity in Bi2212 should consider the complete Fermi surface topology which involves the main bands, the superstructure bands, and their interactions.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Observation of a Flat and Extended Surface State in a Topological Semimetal

A flat band structure in momentum space is considered key for the realization of novel phenomena. A topological flat band, also known as a drumhead state, is an ideal platform to drive new exotic topological quantum phases. Using angle-resolved photoemission spectroscopy experiments, we reveal the emergence of a highly localized surface state in a topological semimetal BaAl4 and provide its full energy and momentum space topology. We find that the observed surface state is localized in momentum, inside a square-shaped bulk Dirac nodal loop, and in energy, leading to a flat band and a peak in the density of state. These results imply this class of materials as an experimental realization of drumhead surface states and provide an important reference for future studies of the fundamental physics of correlated quantum effects in topological materials.

36 MATERIALS SCIENCE↗

Highly Sensitive Measurements of Methylene Dynamics With a Frequency-Selective Double-Quantum Sideband Method

Probing the fast dynamics of surface sites using NMR spectroscopy is highly challenging owing to the sites’ high dilution and the difficulties often associated with isotopic enrichment. Intra-CH 2 1 H- 1 H dipolar couplings are ideal probes of motions given that they only involve 1 H’s and the tensor has a well-defined size and orientation. Here, we introduce a frequency-selective variant of the double-quantum sideband method to measure like-spin 1 H- 1 H dipolar coupling constants. The experiment dramatically reduces the instrument time required to measure dynamically-averaged intra-CH 2 dipolar couplings. We demonstrate the performance of the sequence using silica-supported silanes as model highly-mobile surface species.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Characterization of plasma catalytic decomposition of methane: role of atomic O and reaction mechanism

In this work, we investigated atmospheric pressure plasma jet (APPJ)-assisted methane oxidation over a Ni-SiO 2 /Al 2 O 3 catalyst. We evaluated possible reaction mechanisms by analyzing the correlation of gas phase, surface and plasma-produced species. Plasma feed gas compositions, plasma powers, and catalyst temperatures were varied to expand the experimental parameters. Real-time Fourier-transform infrared spectroscopy was applied to quantify gas phase species from the reactions. The reactive incident fluxes generated by plasma were measured by molecular beam mass spectroscopy using an identical APPJ operating at the same conditions. A strong correlation of the quantified fluxes of plasma-produced atomic oxygen with that of CH 4 consumption, and CO and CO 2 formation implies that O atoms play an essential role in CH 4 oxidation for the investigated conditions. With the integration of APPJ, the apparent activation energy was lowered and a synergistic effect of 30% was observed. We also performed in-situ diffuse reflectance infrared Fourier-transform spectroscopy to analyze the catalyst surface. The surface analysis showed that surface CO abundance mirrored the surface coverage of CH n at 25 °C. This suggests that CH n adsorbed on the catalyst surface as an intermediate species that was subsequently transformed into surface CO. We observed very little surface CH n absorbance at 500 °C, while a ten-fold increase of surface CO and stronger CO 2 absorption were seen. This indicates that for a nickel catalyst at 500 °C, the dissociation of CH 4 to CHn may be the rate-determining step in the plasma-assisted CH 4 oxidation for our conditions. We also found the CO vibrational frequency changes from 2143 cm –1 for gas phase CO to 2196 cm –1 for CO on a 25 °C catalyst surface, whereas the frequency of CO on a 500 °C catalyst was 2188 cm –1 . Here, the change in CO vibrational frequency may be related to the oxidation of the catalyst.

methane oxidation↗

Spectroscopic determination of metal redox and segregation effects during CO and CO/NO oxidation over silica-supported Pd and PdCu catalysts

Here, we report the effects of alloying Cu into silica supported Pd nanoparticles on the catalytic activity, surface composition, and particle structure during CO oxidation Pd is highly active for CO oxidation but is inhibited by relevant competitive reagents (e.g. NO) at low temperatures (< 150 °C). By alloying Cu into Pd nanoparticles, NO inhibition is suppressed without any CO oxidation activity loss. Infrared spectroscopy illustrates the formation of surface nitrosyl (NO-Pd) is eliminated in the PdCu alloy catalyst, preventing CO oxidation inhibition by NO. X-ray absorption spectroscopy studies show that Pd in the monometallic catalyst forms a surface oxide after light-off. Conversely, in the PdCu catalyst, Pd remains metallic during reaction, independent of temperature, whereas the Cu oxidizes when the catalyst becomes active, after light-off. Furthermore, DRIFTS studies show that the Cu segregates to the surface as the catalyst becomes active for diesel oxidation, presumably becoming the O 2 adsorption site.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗