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At least 1,315 records · Page 73

Effect of Solvent on the Local Structure, Dynamics, and Vibrational Density of States in Sn-BEA Zeolite

Lewis acid zeolites are attractive catalysts for epoxidation and biomass valorization, as they are highly active and selective in the liquid phase and can operate at or near ambient conditions. While a rich experimental literature exists on liquid-phase Lewis acid zeolite catalysis, our understanding of the molecular organization and solvent dynamics in the vicinity of Lewis acid sites with differing metal site speciation remains limited. In this work, we investigate the molecular coordination and diffusion of two common solvents (methanol and water) around the closed and open Sn-BEA zeolite active sites using molecular dynamics simulations with a machine-learned interatomic potential trained on ab initio molecular dynamics trajectories. Molecular dynamics simulations reveal that introducing active sites significantly enhances local order in the first and second solvation shells compared to the pure silica case. For methanol, both closed and open active sites are singly coordinated, while more than two water molecules coordinate the open site. In contrast to methanol, we observed that water molecules dissociate, leading to the formation of additional Sn-OH and silanol groups away from the active site. The diffusion coefficients of water and methanol are functions of the solvent population in the pore. Here, our work provides insights into how active site speciation in Lewis acid zeolites affects solvent coordination, diffusion, and vibrational signature. This information is foundational for catalyst design and optimization of liquid-phase catalytic processes in zeolites. It also demonstrates the suitability of machine-learned interatomic potentials for modeling reactive systems, enabling sufficiently long trajectories for appropriate statistical averaging.

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Revealing CO 2 dissociation pathways at vicinal copper (997) interfaces

Size- and shape-tailored copper (Cu) nanocrystals can offer vicinal planes for facile carbon dioxide (CO 2 ) activation. Despite extensive reactivity benchmarks, a correlation between CO 2 conversion and morphology structure has not yet been established at vicinal Cu interfaces. Herein, ambient pressure scanning tunneling microscopy reveals step-broken Cu nanocluster evolutions on the Cu(997) surface under 1 mbar CO 2 (g). The CO 2 dissociation reaction produces carbon monoxide (CO) adsorbate and atomic oxygen (O) at Cu step-edges, inducing complicated restructuring of the Cu atoms to compensate for increased surface chemical potential energy at ambient pressure. The CO molecules bound at under-coordinated Cu atoms contribute to the reversible Cu clustering with the pressure gap effect, whereas the dissociated oxygen leads to irreversible Cu faceting geometries. Synchrotron-based ambient pressure X-ray photoelectron spectroscopy identifies the chemical binding energy changes in CO-Cu complexes, which proves the characterized real-space evidence for the step-broken Cu nanoclusters under CO(g) environments. Our in situ surface observations provide a more realistic insight into Cu nanocatalyst designs for efficient CO 2 conversion to renewable energy sources during C 1 chemical reactions.

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Integrated in situ spectroscopic studies on syngas production from partial oxidation of methane catalyzed by atomically dispersed rhodium cations on ceria

Catalytic reforming of methane to produce syngas is an important strategy for producing value-added chemicals. The conventional reforming catalyst relies on supported nickel nanoparticles. Here, in this work, we investigated singly dispersed Rh cations anchored on a CeO 2 catalyst (Rh 1 /CeO 2 ) for high activity and selectivity towards the production of syngas via partial oxidation of methane (POM) in the temperature range of 600–700 °C. The yields of H 2 and CO at 700 °C are 83% and 91%, respectively. The anchored Rh 1 atoms on CeO 2 of Rh 1 /CeO 2 are in the cationic state, and on an average each Rh 1 atom coordinates with 4–5 surface lattice oxygen atoms of CeO 2 . Compared to inert CeO 2 for POM, via the incorporation of single-atom sites, Rh 1 modifies the electronic state of oxygen atoms proximal to the Rh 1 atoms and thus triggers the catalytic activity of CeO 2 . The high activity of single-atom catalyst Rh 1 /CeO 2 suggests that the incorporation of single atoms of transition metals to the surface of a reducible oxide can modulate the electronic state of proximal anions of the oxide support toward forming an electronic state favorable for the selective formation of ideal products.

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A Conical Intersection Influences the Ground State Rearrangement of Fulvene to Benzene

The rearrangement of fulvene to benzene is believed to play an important role in the formation of soot during hydrocarbon combustion. Previous work has identified two possible mechanisms for the rearrangement-a unimolecular path and a hydrogen-atom-assisted, bimolecular path. Computational results to date have suggested that the unimolecular mechanism faces a barrier of about 74 kcal/mol, which makes it unable to compete with the bimolecular mechanism under typical combustion conditions. This computed barrier is about 10 kcal/mol higher than the experimental value, which is an unusually large discrepancy for modern electronic structure theory. In the present work, we have reinvestigated the unimolecular mechanism computationally, and we have found a second transition state that is approximately 10 kcal/mol lower in energy than the previously identified one and, therefore, in excellent agreement with the experimental value. The existence of two transition states for the same rearrangement arises because there is a conical intersection between the two lowest singlet states which occurs in the vicinity of the reaction coordinates. The two possible paths around the cone on the lower adiabatic surface give rise to the two distinct saddle points. The lower barrier for the unimolecular mechanism now makes it competitive with the bimolecular one, according to our calculations. In support of this conclusion, we have reanalyzed some previous experimental results on anisole pyrolysis, which leads to benzene as a significant product and have shown that the unimolecular and bimolecular mechanisms for fulvene ? benzene must be occurring competitively in that system. Finally, we have identified that similar conical intersections arise during the isomerizations of benzofulvene and isobenzofulvene to naphthalene.

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Skeletal Ni electrode-catalyzed C-O cleavage of diaryl ethers entails direct elimination via benzyne intermediates

Diaryl ethers undergo electrocatalytic hydrogenolysis (ECH) over skeletal Ni cathodes in a mild, aqueous process that achieves direct C-O cleavage without initial benzene ring saturation. Mechanistic studies find that aryl phenyl ethers with a single para or meta functional group (methyl, methoxy, or hydroxy) are selectively cleaved to the substituted benzene and phenol, in contrast to recently reported homogeneous catalytic cleavage processes. Ortho positioning of substituents reverses this C-O bond selectivity, except for the 2-phenoxyphenol case. Together with isotope labeling and co-solvent studies, these results point to two distinct cleavage mechanisms: (a) dual-ring coordination and C-H activation, leading to vicinal elimination to form phenol and a surface-bound aryne intermediate which is then hydrogenated and released as the arene; and (b) surface binding in keto form by the phenolic ring of the hydroxy-substituted substrates, followed by direct displacement of the departing phenol. Notably, acetone inhibits the well-known reduction of phenol to cyclohexanol, affording control of product ring saturation. A byproduct of this work is the discovery that the ECH treatment completely defluorinates substrates bearing aromatic C-F and C-CF 3 groupings.

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Materials Engineering of Violin Soundboards by Stradivari and Guarneri

Abstract We investigated the material properties of Cremonese soundboards using a wide range of spectroscopic, microscopic, and chemical techniques. We found similar types of spruce in Cremonese soundboards as in modern instruments, but Cremonese spruces exhibit unnatural elemental compositions and oxidation patterns that suggest artificial manipulation. Combining analytical data and historical information, we may deduce the minerals being added and their potential functions—borax and metal sulfates for fungal suppression, table salt for moisture control, alum for molecular crosslinking, and potash or quicklime for alkaline treatment. The overall purpose may have been wood preservation or acoustic tuning. Hemicellulose fragmentation and altered cellulose nanostructures are observed in heavily treated Stradivari specimens, which show diminished second‐harmonic generation signals. Guarneri's practice of crosslinking wood fibers via aluminum coordination may also affect mechanical and acoustic properties. Our data suggest that old masters undertook materials engineering experiments to produce soundboards with unique properties.

36 MATERIALS SCIENCE↗

Role of Axial Ligation in Gating the Reactivity of Dimethylplatinum(III) Diimine Radical Cations

Electrochemical methods are coupled with chemical oxidant-based analytical strategies to evaluate the oxidative reactivity of the platinum(II) diimine complex (bpy)Pt II (CH 3 ) 2 (bpy = 2,2'-bipyridine) in coordinating and non-coordinating media. Through this mechanistic analysis, we show that the one-electron oxidation of (bpy)Pt II (CH 3 ) 2 generates a highly reactive, 15-electron Pt III radical cation and identify three reaction pathways that can follow this oxidation: radical–substrate dimerization, radical-radical dimerization, and oxidative disproportionation. Axial ligation of the initially generated [(bpy)Pt III (CH 3 ) 2 ] •+ species is a critical driver of this reactivity, gating the available mechanistic pathways and tuning the competition between radical–radical dimerization and oxidative disproportionation.

14 SOLAR ENERGY↗

Interactions of Oxide Surfaces with Water Revealed with Solid-State NMR Spectroscopy

Hydrous materials are ubiquitous in the natural environment and efforts have previously been made to investigate the structures and dynamics of hydrated surfaces for their key roles in various chemical and physical applications, with the help of theoretical modeling and microscopy techniques. However, an overall atomic-scale understanding of the water–solid interface, including the effect of water on surface ions, is still lacking. Herein, we employ ceria nanorods with different amounts of water as an example and demonstrate a new approach to explore the water–surface interactions by using solid-state NMR in combination with density functional theory. NMR shifts and relaxation time analysis provide detailed information on the local structure of oxygen ions and the nature of water motion on the surface: the amount of molecularly adsorbed water decreases rapidly with increasing temperature (from room temperature to 150 °C), whereas hydroxyl groups are stable up to 150 °C, and dynamic water molecules are found to instantaneously coordinate to the surface oxygen ions. Additionally, the applicability of dynamic nuclear polarization for selective detection of surface oxygen species is also compared to conventional NMR with surface selective isotopic-labeling: the optimal method depends on the feasibility of enrichment and the concentration of protons in the sample. These results provide new insight into the interfacial structure of hydrated oxide nanostructures, which is important to improve performance for various applications.

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Influence of near-surface oxide layers on TiFe hydrogenation: mechanistic insights and implications for hydrogen storage applications

The inevitable formation of passivating oxide films on the surface of the TiFe intermetallic compound limits its performance as a stationary hydrogen storage material. Extensive experimental efforts have been dedicated to the activation of TiFe, i.e. oxide layer removal prior to utilization for hydrogen storage. However, development of an efficient activation protocol necessitates a fundamental understanding of the composition and structure of the air-exposed surface and its interaction with hydrogen, which is currently absent. Therefore, in this study we explored the growth and nature of oxide films on the most exposed TiFe surface (110) in depth using static and dynamic first-principles methods. We identified the lowest energy structures for six oxygen coverages up to approximately 1.12 nm of thickness with a global optimization method and studied the temperature effects and structural evolution of the oxide phases in detail via ab initio molecular dynamics (AIMD). Based on structural similarity and coordination analysis, motifs for TiO 2 and TiFeO 3 as well as Ti(FeO 2 ) x (x = 2, 3 or 5) phases were identified. On evaluating the interaction of the oxidized surface with hydrogen, a minimal energy barrier of 0.172 eV was predicted for H 2 dissociation while H migration from the top of the oxidized surface to the bulk TiFe was limited by several high-lying energy barriers above 1.4 eV. Our mechanistic insights will prove themselves valuable for informed designs towards new activation methods of TiFe and related systems as hydrogen storage materials.

08 HYDROGEN↗

Designing electrolytes with polymerlike glass-forming properties and fast ion transport at low temperatures

Significance Liquid electrolytes with thermophysical properties analogous to solid polymers, but with exceptional liquidlike ionic conductivities, are formed spontaneously when moderate amounts (≤1 M) of inorganic salts coordinate strongly with small molecules in a conventional aprotic solvent. Specifically, we report that electrolytes composed of the cyclic liquid ether, dioxolane (DOL), and containing the simple salt LiNO 3 are able to completely bypass the liquid → crystalline solid thermal transition, and to exhibit abnormally high bulk and interfacial ionic conductivities down to temperatures as low as −50 °C. Through physical, spectroscopic, and ion-transport measurements it is shown that strong interactions between LiNO 3 and DOL distort bonds in DOL, couple motions of individual solvent molecules, and lower the thermodynamic activity of the electrolyte.

36 MATERIALS SCIENCE↗

The kagomé metals RbTi 3 Bi 5 and CsTi 3 Bi 5

Abstract The kagomé metals RbTi 3 Bi 5 and CsTi 3 Bi 5 were synthesized both as polycrystalline powders by heating the elements in an argon atmosphere and as single crystals grown using a self-flux method. The compounds crystallize in the hexagonal crystal system isotypically to KV 3 Sb 5 ( P 6/ mmm , Z = 1, CsTi 3 Bi 5 : a = 5.7873(1), c = 9.2062(1) Å; RbTi 3 Bi 5 : a = 5.773(1), c = 9.065(1) Å). The titanium atoms form a kagomé net with bismuth atoms in the hexagons as well as above and below the triangles. The alkali metal atoms are coordinated by 12 bismuth atoms and form AlB 2 -like slabs between the kagomé layers. Magnetic susceptibility measurements with CsTi 3 Bi 5 and RbTi 3 Bi 5 single crystals reveal Pauli-paramagnetism and traces of superconductivity caused by CsBi 2 /RbBi 2 impurities. Magnetotransport measurements reveal conventional Fermi liquid behavior and quantum oscillations indicative of a single dominant orbit at low temperature. DFT calculations show the characteristic metallic kagomé band structure similar to that of CsV 3 Sb 5 with reduced band filling. A symmetry analysis of the band structure does not reveal an obvious and unique signature of a nontrivial topology.

Chemistry↗

Modulating Electronic Structure of Atomically Dispersed Nickel Sites through Boron and Nitrogen Dual Coordination Boosts Oxygen Reduction

Abstract Atomically dispersed 3D transitional metal active sites with nitrogen coordination anchored on carbon support have emerged as a kind of promising electrocatalyst toward oxygen reduction reaction (ORR) in the field of fuel cells and metal–air cells. However, it is still a challenge to accurately modulate the coordination structure of single‐atom metal sites, especially first‐shell coordination, as well as identify the relationship between the geometric/electronic structure and ORR performance. Herein, a carbon‐supported single‐atom nickel catalyst is fabricated with boron and nitrogen dual coordination (denoted as Ni‐B/N‐C). The hard X‐ray absorption spectrum result reveals that atomically dispersed Ni active sites are coordinated with one B atom and three N atoms in the first shell (denoted as Ni‐B 1 N 3 ). The Ni‐B/N‐C catalyst exhibits a half‐wave potential ( E 1/2 ) of 0.87 V versus RHE, along with a distinguished long‐term durability in alkaline media, which is superior to commercial Pt/C. Density functional theory calculations indicate that the Ni‐B 1 N 3 active sites are more favorable for the adsorption of ORR intermediates relative to Ni‐N 4 , leading to the reduction of thermodynamic barrier and the acceleration of reaction kinetics, which accounts for the increased intrinsic activity.

Chemistry↗

Mechanisms of Zn removal from water by amorphous geopolymer: Molecular-level insights from X-ray absorption spectroscopy, isotope fractionation, and surface complexation modeling

Porous geopolymers have attracted widespread attention as promising heavy metal adsorbents that can be synthesized from aluminosilicate solid wastes. However, the precise microstructural evidence for adsorbed heavy metals on geopolymers remains unclear due to the insensitivity of conventional characterization techniques on minerals with amorphous structure and surface disorder. Batch adsorption and column experiments coupled with X-ray absorption spectroscopy (XAS), Zn stable isotope, and surface complexation model (SCM) were employed to reveal the Zn removal mechanisms with coal fly ash porous geopolymer (CFAPG) at a molecular scale. The macroscopic kinetic and isothermal adsorption of Zn on CFAPG were well described by the pseudo-second-order model and Bi_Langmuir equation, respectively, indicating the presence of abundant heterogeneous active sites on the CFAPG surface. Further, two types of active sites on the CFAPG surface were identified by XAS coupled with Zn isotopes in batch experiments at pH <= 6.0: one is pH-dependent and associated with tetrahedral zinc coordi-nation, and the other is pH-insensitive and associated with octahedral zinc coordination; these sites were confirmed by the bidentate SCM as the variable charge site (surface complexation, >S-OH) and the permanent negative charge site (cation exchange, >X - ), respectively. Furthermore, the important contribution of surface co -precipitation besides surface complexation and cation exchange to the Zn adsorption on CFAPG was identified by XAS coupled with SCM in a flow-through column experiment at pH >6.0. These investigations provide a systemic understanding of the Zn adsorption mechanisms on CFAPG and an SCM reference for the application and prediction of geopolymers in heavy metal-contaminated water remediations.

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Active Learning Accelerated Discovery of Stable Iridium Oxide Polymorphs for the Oxygen Evolution Reaction

The discovery of high-performing and stable materials for sustainable energy applications is a pressing goal in catalysis and materials science. Understanding the relationship between a material’s structure and functionality is an important step in the process, such that viable polymorphs for a given chemical composition need to be identified. Machine-learning-based surrogate models have the potential to accelerate the search for polymorphs that target specific applications. Herein, we report a readily generalizable active-learning (AL) accelerated algorithm for identification of electrochemically stable iridium oxide polymorphs of IrO 2 and IrO 3 . The search is coupled to a subsequent analysis of the electrochemical stability of the discovered structures for the acidic oxygen evolution reaction (OER). Structural candidates are generated by identifying all 956 structurally unique AB2 and AB3 prototypes in existing materials databases (more than 38000). Next, using an active learning approach, we find 196 IrO 2 polymorphs within the thermodynamic amorphous synthesizability limit and reaffirm the global stability of the rutile structure. We find 75 synthesizable IrO 3 polymorphs and report a previously unknown FeF 3 -type structure as the most stable, termed α-IrO 3 . To test the algorithms performance, we compare to a random search of the candidate space and report at least a 2-fold increase in the rate of discovery. Additionally, the AL approach can acquire the most stable polymorphs of IrO 2 and IrO 3 with fewer than 30 density functional theory optimizations. Analysis of the structural properties of the discovered polymorphs reveals that octahedral local coordination environments are preferred for nearly all low-energy structures. Subsequent Pourbaix Ir–H 2 O analysis shows that α-IrO3 is the globally stable solid phase under acidic OER conditions and supersedes the stability of rutile IrO 2 . Calculation of theoretical OER surface activities reveal ideal weaker binding of the OER intermediates on α-IrO 3 than on any other considered iridium oxide. We emphasize that the proposed AL algorithm can be easily generalized to search for any binary metal oxide structure with a defined stoichiometry.

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Analysis of the Structure of Heavy Ion Irradiated LaFeO 3 Using Grazing Angle X-ray Absorption Spectroscopy

Crystalline ceramics are candidate materials for the immobilization of radionuclides, particularly transuranics (such as U, Pu, and Am), arising from the nuclear fuel cycle. Due to the α-decay of transuranics and the associated recoil of the parent nucleus, crystalline materials may eventually be rendered amorphous through changes to the crystal lattice caused by these recoil events. Previous work has shown irradiation of titanate-based ceramics to change the local cation environment significantly, particularly in the case of Ti which was shown to change from 6- to 5-fold coordination. Here, this work expands the Ti-based study to investigate the behavior in Fe-based materials, using LaFeO 3 as an example material. Irradiation was simulated by heavy ion implantation of the bulk LaFeO 3 ceramic, with the resulting amorphous layer characterized with grazing angle X-ray absorption spectroscopy (GA-XAS). Insights into the Fe speciation changes exhibited by the amorphized surface layer were provided through quantitative analysis, including pre-edge analysis, and modeling of the extended X-ray absorption fine structure (EXAFS), of the GA-XAS data.

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Investigation of the Deactivation and Reactivation Mechanism of a Heterogeneous Palladium(II) Catalyst in the Cycloisomerization of Acetylenic Acids by In Situ XAS

A well-studied heterogeneous palladium(II) catalyst used for the cycloisomerization of acetylenic acids is known to be susceptible to deactivation through reduction. To gain a deeper understanding of this deactivation process and to enable the design of a reactivation strategy, in situ X-ray absorption spectroscopy (XAS) was used. With this technique, changes in the palladium oxidation state and coordination environment could be studied in close detail, which provided experimental evidence that the deactivation was primarily caused by triethylamine-promoted reduction of palladium(II) to metallic palladium nanoparticles. Furthermore, it was observed that the choice of the acetylenic acid substrate influenced the distribution between palladium(II) and palladium(0) species in the heterogeneous catalyst after the reaction. From the mechanistic insight gained through XAS, an improved catalytic protocol was developed that did not suffer from deactivation and allowed for more efficient recycling of the catalyst.

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Two-State Reactivity in Iron-Catalyzed Alkene Isomerization Confers σ-Base Resistance

A low-coordinate, high spin (S = 3/2) organometallic iron(I) complex is a catalyst for the isomerization of alkenes. A combination of experimental and computational mechanistic studies supports a mechanism in which alkene isomerization occurs by the allyl mechanism. Importantly, while substrate binding occurs on the S = 3/2 surface, oxidative addition to an η 1 -allyl intermediate only occurs on the S = 1/2 surface. In conclusion, since this spin state change is only possible when the alkene substrate is bound, the catalyst has high immunity to typical σ-base poisons due to the antibonding interactions of the high spin state.

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Supramolecular Metal Halide Complexes for High-Temperature Nonlinear Optical Switches

Nonlinear optical (NLO) switching materials, which exhibit reversible intensity modulation in response to thermal stimuli, have found extensive applications across diverse fields, including sensing, photoelectronics, and photonic applications. While significant progress has been made in solid-state NLO switching materials, these materials typically showcase their highest NLO performance near room temperature. However, this performance drastically deteriorates upon heating, primarily due to the phase transition undergone by the materials from non-centrosymmetric to centrosymmetric phase. Here, we introduce a new class of NLO switching materials, solid-state supramolecular compounds 18-Crown-6 ether@Cu 2 Cl 4 ·4H 2 O (1·4H 2 O), exhibiting reversible and stable NLO switching when subjected to near-infrared (NIR) photoexcitation and/or thermal stimuli. The reversible crystal structure in response to external stimuli is attributed to the presence of a weakly coordinated bridging water molecule, facilitated by hydrogen bonding/chelation interactions between the metal halide and crown-ether supramolecules. We observed an exceptionally high second-harmonic generation (SHG) signal under continuous photoexcitation, even at temperatures exceeding 110°C. In addition, the bridging water molecules within the complex can be released and recaptured in a fully reversible manner, all without requiring excessive energy input. This feature allows for precise control of SHG signal activation and deactivation through structural transformations, resulting in a high-contrast off/on ratio, reaching values in the million-fold range.

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