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At least 163 records · Page 9

Mechanistic Study of 1,2-Dichloroethane Hydrodechlorination on Cu-Rich Pt–Cu Alloys: Combining Reaction Kinetics Experiments with DFT Calculations and Microkinetic Modeling

Cu-rich Pt–Cu bimetallic catalysts are among the most promising candidates for actively catalyzing the hydrodechlorination of 1,2-dichloroethane (1,2-DCA) toward ethylene production. Combining reaction kinetics experiments with density functional theory (DFT) calculations and mean-field microkinetic modeling, we present a systematic mechanistic study for 1,2-DCA hydrodechlorination on Cu-rich Pt–Cu alloy catalysts. Our DFT (PBE+(TS+SCS)) results suggest that increasing Cu content in the Pt–Cu alloy destabilizes C 2 -species adsorption while stabilizing the binding of atomic chlorine. The reaction energetics of all the elementary steps in the 1,2-DCA reaction network were calculated on a Pt 1 Cu 3 (111) model surface. The DFT results were then used to construct a microkinetic model, and the model-predicted reaction rates were compared with our reaction kinetics experimental results on a Cu-rich SiO 2 -supported Pt–Cu alloy catalyst through a parameter estimation procedure. Both the reaction kinetics experiments and the microkinetic model after parameter adjustments yielded 100% selectivity to ethylene. The microkinetic model pointed to a reaction pathway involving two sequential chlorine-removal steps on the Pt–Cu alloy catalyst, a mechanism distinct from the one previously identified on pure Pt/SiO 2 catalysts, which involved an initial hydrogen-removal step. Adjustments to the DFT-derived parameters indicate the possible formation of chlorine-induced Cu-enriched surface sites during 1,2-DCA hydrodechlorination conditions, sites that are more active than those encountered in the bulk Pt 1 Cu 3 (111) alloy surface. Furthermore, our study offers valuable initial insights on the 1,2-DCA hydrodechlorination reaction mechanism and the nature of the active sites on PtCu bimetallic catalysts.

1,2-Dichloroethane↗

Local Structural Disorder in Metavanadates MV 2 O 6 (M = Zn and Cu) Synthesized by the Deep Eutectic Solvent Route: Photoactive Oxides with Oxygen Vacancies

Metavanadates MV 2 O 6–δ (M = Zn and Cu) are synthesized by using a deep eutectic solvent (DES), a mixture of hydrogen bond donor and acceptor, as a reaction medium. Dissolution of stable binary metal oxides in a DES followed by a heat treatment yields phase-pure vanadates. According to in situ powder X-ray diffraction, ternary phases (α-Zn 2 V 2 O 7 and β-Cu 2–x V 2 O 7 , x ~ 0.27) are intermediates in the reaction pathway taken. Identifying a polymorphic phase transformation temperature for CuV 2 O 6 as well as the narrow temperature range between formation and decomposition for both metavanadates allows for tackling the challenge of the synthesis of these materials. The oxygen vacancy introduced by the DES route is accompanied by the formation of reduced V 4+ and Cu + in the oxide matrix, based on X-ray photoelectron spectroscopy. These oxygen vacancies modify the vibrational modes in the corresponding Raman spectra and are also responsible for broad optical absorptions in the 1.8–1.1 eV range. The optical band gaps of the materials are found at 1.8 eV (CuV 2 O 6 ) and 2.2 eV (ZnV 2 O 6 ), approximately 0.1–0.3 eV below the values reported in the literature. The reduced band gaps and sub-band gap photon absorption are key features of the oxygen-deficient metavanadates. Surface photovoltage spectroscopy reveals that all the synthesized vanadates are n-type materials with electrons as the majority charge carriers, and photoelectrochemical measurements confirm photoanodic currents for methanol oxidation. Furthermore, these results provide insight into the synthesis and structure–property relationship of the metavanadates for their potential use as photoanodes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Dimensional Evolution Guides Property Control in the A n Cu 4– n TiS 4 Semiconductor Series

Through progressive reduction of the three-dimensional (3D) covalent network of Cu 4 TiS 4 , we isolate seven new members of the A n Cu 4–n TiS 4 family (A = alkali metal; n = 0–4), spanning 3D, 2D, 1D, and 0D structural fragments. The dimensional reduction is rational, as it preserves the edge-sharing connectivity between [CuS 4 ] 7– and [TiS 4 ] 4– tetrahedra across the series. This structural evolution is driven by the stepwise substitution of Cu with alkali metals, guiding the formation of fragments with reduced dimensionality. The effects of “n” and “A” on the crystal structures, stabilities, electronic structures, and optoelectronic properties are profound, demonstrating that the manipulation of alkali metal size and A n Cu 4–n TiS 4 stoichiometry enables predictable variations in structure and properties. For example, the n = 0 and n = 4 end members of the A n Cu 4–n TiS 4 family set the range of achievable band gaps with 2.00 eV for Cu 4 TiS 4 , 2.60 eV for Na 4 TiS 4 , and intermediate values for the n = 1–3 members. Notably, CsCu 3 TiS 4 exhibits exceptional air stability and congruent melting, with density functional theory (DFT) calculating moderate hole and electron effective masses in specific crystallographic directions (mh = 1.24m 0 , me = 0.87m 0 ). Additionally, A 3 CuTiS 4 (A = Na, K, Rb) displays direct band gap behavior and long photoluminescence lifetimes of 2.3–8.6 μs, and K 3 CuTiS 4 has a PLQY of 5.19%. These findings underscore the potential of the A n Cu 4–n TiS 4 family for applications in optoelectronics and demonstrate widely applicable design concepts that unveil rational stoichiometries within a given composition space to generate a series of crystal structures related through an evolving covalent dimensionality that corresponds to a predictable electronic structure and property progression.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Ethanol Conversion to C 4+ Olefins over Bimetallic Copper- And Lanthanum-Containing Beta Zeolite Catalysts

We report ethanol conversion to C 4+ olefins remains a critical yet nonselective process for producing renewable middle distillates. Here, Cu–La/Beta catalysts composed of copper and lanthanum incorporated onto a dealuminated Beta support are reported for ethanol conversion to C 4+ olefins (73% selectivity, ~98% ethanol conversion, 623 K,<4% C 1 –C 3 hydrocarbons) which particularly favors C 5+ olefin formation (43% selectivity) as a distinction from the benchmarking Cu–Y/Beta catalyst. Monometallic Cu/Beta or La/Beta samples are insufficient to catalyze the C 4+ olefin formation and primarily form dehydration products (e.g., ethylene and diethyl ether), indicating the necessity of both Cu and La species for butene and C 5+ olefin formation. Increasing the bulk La loading at a fixed Cu content yields higher C 5+ olefins until the La/Cu molar ratio reaches 3.6. These findings indicate Cu–La/Beta as an effective ethanol conversion catalyst that facilitates multiple C–C bond formation events required for synthesizing C 5+ olefins (i.e., hexenes and octenes).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Ab Initio Studies of Discharge Mechanism of MnO 2 in Deep-Cycled Rechargeable Zn/MnO 2 Batteries

Rechargeable alkaline Zn/MnO 2 batteries are an attractive solution for large-scale energy storage applications. Recently, Bi and Cu additives have been used to increase the cycle life and capacity of rechargeable Zn/MnO 2 batteries, with an equivalent of the full two-electron capacity realized for many cycles, in the absence of zinc. However, the mechanism of the effect of Bi and Cu on the performance of rechargeable Zn/MnO 2 batteries has not been investigated in detail. We apply first-principles density functional computational methods to study the discharge mechanisms of the unmodified and Bi/Cu-modified γ -MnO 2 electrodes in rechargeable alkaline Zn/MnO 2 batteries. Using the results of our calculations, we analyze the possible redox reaction pathways in the γ -MnO 2 electrode and identify the electrochemical processes leading to the formation of irreversible discharge reaction products, such as hausmannite and hetaerolite. Our study demonstrates the possibility of formation of intermediate Bi-Mn and Cu-Mn oxides in deep-cycled Bi/Cu-modified MnO 2 electrodes. The formation of intermediate Bi-Mn and Cu-Mn oxides could reduce the rate of accumulation of irreversible reaction products in the MnO 2 electrode and improve the rechargeability and cyclability of Zn/MnO 2 batteries.

25 ENERGY STORAGE↗

Critical roles of Cu(OH)2 in low-temperature moisture-induced degradation of Cu-SAPO-34 SCR catalyst: Correlating reversible and irreversible deactivation

Cu-SAPO-34 selective catalytic reduction (SCR) catalyst deactivates upon exposure to water vapor at temperatures lower than 100 °C, which deteriorates its application prospects. The deactivation under cycled aging-regeneration conditions can be categorized into two stages, namely reversible and irreversible deactivation. Based on SCR reaction tests, and characterizations with diffuse reflection infrared Fourier transform spectroscopy (DRIFTS), NH3 temperature-programmed desorption (NH3-TPD) and H2 temperature-programmed reduction (H2-TPR), it is concluded that the transformation of SCR active isolated Cu(II) ions to Cu(OH)2 is critical to both types of deactivation. Within the frame of reversible deactivation, Cu(OH)2 is converted back to SCR active Cu(II) ions by interacting with Brønsted acid sites during high-temperature regeneration. However, interactions between Cu(OH)2 and hydrolyzed framework Al lead to the formation of CuAl2O4-like species, causing permanent loss of active Cu(II) ions and thus, irreversible deactivation. The authors from Tsinghua University would like to acknowledge the financial support from projects of China Science and Technology Exchange Centre (No. 2016YFE0126600) and the National Key R&D Program of China (No. 2017YFC0211102). YM also acknowledges Tsinghua Scholarship for Overseas Graduate Studies for a visit to the Pacific Northwest National Laboratory (PNNL). PNNL is operated by Battelle for the US Department of Energy (DOE) under contract DE-AC05-76RL01830. FG is supported by DOE, Office of Energy Efficiency and Renewable Energy, Vehicle Technologies Office.

Cu-SAPO-34, low-temperature deactivation, reversib↗

Kinetic control of phase evolution and defect-mediated recombination in AACVD-grown copper antimony sulphide thin films

Copper antimony sulphide (CAS) is a multinary chalcogenide semiconductor in which small deviations from stoichiometry can drive phase competition and strong defect-mediated modulation of optoelectronic properties. However, the systematic roles of copper precursor fraction and deposition time in governing phase evolution, off-stoichiometry, and recombination dynamics in aerosol-assisted chemical vapour deposition (AACVD)-grown undoped CAS thin films remain insufficiently understood. In this work, undoped CAS thin films were deposited by AACVD using Cu(dedtc)2 and Sb(dedtc)3 single-source precursors at 550 °C and a carrier gas flow rate of 150 sccm, while the Cu(dedtc)2 mole fraction (x = 0.15 – 0.55) and deposition time (1 – 2 hours) were systematically varied to probe how growth kinetics influence phase composition, microstructure, and defect-mediated optical properties without post-deposition annealing or extrinsic doping. Increasing copper precursor content drives phase evolution toward tetrahedrite-dominant CAS films at intermediate Cu(dedtc)2 mole fractions, with the film deposited at x = 0.35 exhibiting the strongest tetrahedrite character within the parameter space examined. The films are also copper-rich, antimony-poor, and sulphur-deficient, consistent with off-stoichiometric growth and intrinsic defect formation, plausibly including copper interstitials, Cu-on-Sb antisites, and sulphur vacancies. These growth-dependent compositional deviations are accompanied by tunable indirect optical bandgaps of approximately 1.60 – 2.18 eV and weak visible photoluminescence governed by defect-mediated recombination. Time-resolved photoluminescence reveals bi-exponential decay behaviour with lifetimes of approximately 0.1 – 3.6 ns, with emission dominated by slower donor–acceptor pair recombination and a smaller contribution from faster trap-assisted pathways. Collectively, these results establish an explicit kinetic process–structure–defect–property relationship for AACVD-grown CAS thin films and provide a growth–structure–property framework relevant to future optimization of CAS-based optoelectronic and energy materials.

36 MATERIALS SCIENCE↗

Investigating Spillover Energy as a Descriptor for Single-Atom Alloy Catalyst Design

The identification of thermodynamic descriptors of catalytic performance is essential for the rational design of heterogeneous catalysts. Here, we investigate how spillover energy, a descriptor quantifying whether intermediates are more stable at the dopant or host metal sites, can be used to design single-atom alloys (SAAs) for formic acid dehydrogenation. Further, using theoretical calculations, we identify NiCu as a SAA with favorable spillover energy and demonstrate that formate intermediates produced after the initial O–H activation are more stable at Ni sites where rate-determining C–H activation occurs. Surface science experiments demonstrated that NiCu(111) SAAs are more reactive than Cu(111) while they still follow the formate reaction pathway. However, reactor studies of silica-supported NiCu SAA nanoparticles showed only a modest improvement over Cu resulting from surface coverage effects. Overall, this study demonstrates the potential of engineering SAAs using spillover energy as a design parameter and highlights the importance of adsorbate–adsorbate interactions under steady-state operation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Electronic structure of the honeycomb iridate Cu 2 ⁢IrO 3 at high pressure

Cu 2 IrO 3 has attracted recent interest due to its proximity to the Kitaev quantum spin liquid state and the complex structural response observed at high pressures. We use x-ray spectroscopy and scattering as well as electrical transport techniques to unveil the electronic structure of Cu 2 IrO 3 at ambient and high pressures. Despite featuring a Ir 4+ J eff = 1/2 state at ambient pressure, Ir L 3 -edge resonant inelastic x-ray scattering reveals broadened electronic excitations that point to the importance of Ir 5d-Cu 3d interaction. High pressure first drives an Ir-Ir dimer state with collapsed < L · S > and < L z >/< S z >, signaling the formation of 5d molecular orbitals. A novel Cu → Ir charge transfer is observed above 30 GPa at low temperatures, leading to an approximate Ir 3+ and Cu 1.5+ valence, with persistent insulating electrical transport seemingly driven by charge segregation of Cu 1+ /Cu 2+ ions into distinct sites. Concomitant x-ray spectroscopy and diffraction measurements through different thermodynamic paths demonstrate a strong electron-lattice coupling, with J eff = 1/2 and Ir 3+ /Cu 1.5+ electronic states occurring only in phases 1 and 5, respectively. Remarkably, the charge-transfer state can only be reached if Cu 2 IrO 3 is pressurized at low temperature, suggesting that phonons play an important role in the inhibiting this phase. Furthermore, these results point to the choice of thermodynamic path across interplanar collapse transition as a key parameter to access novel states in intercalated iridates.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

From Micro-environments to Macroscopic Effects: How the Alkaline Hydrogen Evolution Reaction Drives Cu Cathodic Corrosion

Cathodic corrosion of copper (Cu) has posed a significant challenge for over a century, impeding various technological progresses such as electrochemical conversion of CO 2 (eCO 2 RR) into fuels and other value-added carbon products. Here, in this study, employing a combined Density Functional Theory (DFT) and kinetic Monte Carlo (kMC) simulation approach, we delve into the atomistic level mechanism driving this phenomenon in Cu. Our hypothesis posits the pivotal role of alkaline hydrogen evolution reaction (HER) in facilitating cathodic corrosion in Cu. We rigorously develop a pH-dependent hydroxide (OH) adsorption mechanism and calculate the equilibrium OH coverage (𝜃 OH ) at varying pH levels, the thermodynamic stability of subsurface oxygen (O sub ), as well as the Cu-vacancy mediated diffusion of subsurface oxygens (O sub ). Through comprehensive analysis, we establish correlation among various microenvironments, including oxygen diffusion in subsurface layers, pH-dependent OH adsorption, and Cu dissolution into the electrolyte as (Cu-OH) complexes. Furthermore, our investigation explores the correlation between surface coordination environment of active sites and cathodic corrosion of Cu. Finally, by integrating DFT-derived thermodynamic data into a kMC model, we successfully predict the formation of experimentally observed corrosion pits on Cu-surfaces. This combined approach not only advances our fundamental understanding of Cu cathodic corrosion but also offers insights crucial for developing effective corrosion mitigation strategies.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Structure of Charge Density Waves in La1.875Ba0.125CuO4

Although charge-density wave (CDW) correlations exist in several families of cuprate superconductors, they exhibit substantial variation in CDW wavevector and correlation length, indicating a key role for CDW-lattice interactions. We investigated this interaction in La1.875Ba0.125CuO4 using single crystal x-ray diffraction to collect a large number of CDW peak intensities, and determined the Cu and La/Ba atomic distortions induced by the formation of CDW order. Within the CuO2 planes, the distortions involve a periodic modulation of the Cu-Cu spacing along the direction of the ordering wave vector. The charge ordering within the copper-oxygen layer induces an out-of-plane breathing modulation of the surrounding lanthanum layers, which leads to a related distortion on the adjacent copper-oxygen layer. Our result implies that the CDW-related structural distortions do not remain confined to a single layer but rather propagate an appreciable distance through the crystal. This leads to overlapping structural modulations, in which CuO2 planes exhibit distortions arising from the orthogonal CDWs in adjacent layers as well as distortions from the CDW within the layer itself. We attribute this striking effect to the weak c-axis charge screening in cuprates and suggest this effect could help couple the CDW between adjacent planes in the crystal.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Element-Specific Study of Magnetic Anisotropy and Hardening in SmCo 5– x Cu x Thin Films

This work investigates the effect of copper substitution on the magnetic properties of SmCo 5 thin films synthesized by molecular beam epitaxy. A series of thin films with varying concentrations of Cu were grown under otherwise identical conditions to disentangle structural and compositional effects on the magnetic behavior. The combined experimental and theoretical studies show that Cu substitution at the Co 3g sites not only stabilizes the formation of the SmCo 5 structure but also enhances magnetic anisotropy and coercivity. Density functional theory calculations indicate that Sm(Co 4 Cu 3g ) 5 possesses a higher single-ion anisotropy as compared to pure SmCo 5 . In addition, X-ray magnetic circular dichroism reveals that Cu substitution causes an increasing decoupling of the Sm 4f and Co 3d moments. Scanning transmission electron microscopy confirms predominantly SmCo 5 phase formation and reveals nanoscale inhomogeneities in the Cu and Co distribution. Our study based on thin film model systems and advanced characterization as well as modeling reveals novel aspects of the complex interplay of intrinsic and extrinsic contributions to magnetic hysteresis in rare-earth-based magnets, i.e., the combination of increased intrinsic anisotropy due to Cu substitution and the extrinsic effect of inhomogeneous elemental distribution of Cu and Co.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Electrochemical Hydrogenation of CO on Cu(100): Insights from Accurate Multiconfigurational Wavefunction Methods

Copper (Cu) remains the most efficacious electrocatalyst for electrochemical CO 2 reduction (CO 2 R). Its activity and selectivity are highly facet-dependent. We recently examined the commonly proposed rate-limiting CO hydrogenation step on Cu(111) via embedded correlated wavefunction (ECW) theory and demonstrated that only this higher-level theory yields predictions consistent with potential-dependent experimental kinetics. Here, to understand the differing activities of Cu(111) and Cu(100) in catalyzing CO 2 R, we explore CO hydrogenation on Cu(100) using ECW theory. We predict that the preferred pathway involves the reduction of adsorbed CO (*CO) to *COH via proton-coupled electron transfer (PCET) at working potentials, although *CHO also may form with a kinetically accessible but higher barrier. In contrast, our earlier work on Cu(111) concluded that *COH and *CHO formation via PCET are equally feasible. Furthermore, this work illustrates one possible origin of the facet dependence of CO 2 R mechanisms and products on Cu electrodes and sheds light on how the selectivity of CO 2 R electrocatalysts can be controlled by the surface morphology.

30 DIRECT ENERGY CONVERSION↗

Catalytic Water Electrolysis by Co–Cu–W Mixed Metal Oxides: Insights from X-ray Absorption Spectroelectrochemistry

Mixed metal oxides (MMOs) are a promising class of electrocatalysts for the oxygen evolution reaction (OER) and hydrogen evolution reaction (HER). Despite their importance for sustainable energy schemes, our understanding of relevant reaction pathways, catalytically active sites, and synergistic effects is rather limited. Here, we applied synchrotron-based X-ray absorption spectroscopy (XAS) to explore the evolution of the amorphous Co–Cu–W MMO electrocatalyst, shown previously to be an efficient bifunctional OER and HER catalyst for water splitting. Ex situ XAS measurements provided structural environments and the oxidation state of the metals involved, revealing Co 2+ (octahedral), Cu + / 2+ (tetrahedral/square-planar), and W 6+ (octahedral) centers. Operando XAS investigations, including X-ray absorption near-edge structure (XANES) and extended X-ray absorption fine structure (EXAFS), elucidated the dynamic structural transformations of Co, Cu, and W metal centers during the OER and HER. The experimental results indicate that Co 3+ and Cu 0 are the active catalytic sites involved in the OER and HER, respectively, while Cu 2+ and W 6+ play crucial roles as structure stabilizers, suggesting strong synergistic interactions within the Co–Cu–W MMO system. In conclusion, these results, combined with the Tafel slope analysis, revealed that the bottleneck intermediate during the OER is Co 3+ hydroperoxide, whose formation is accompanied by changes in the Cu–O bond lengths, pointing to a possible synergistic effect between Co and Cu ions. Our study reveals important structural effects taking place during MMO-driven OER/HER electrocatalysis and provides essential experimental insights into the complex catalytic mechanism of emerging noble-metal-free MMO electrocatalysts for full water splitting.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Clarifying the formation of equiaxed grains and microstructural refinement in the additive manufacturing of Ti-Cu

Controlling microstructural evolution in metallic additive manufacturing (AM) is difficult, especially in producing refined as-built grains instead of coarse, directional grains. Traditional solutions involve adding inoculants to AM feedstocks, but titanium (Ti) alloys cannot employ this approach without producing detrimental secondary phases. Ti-Cu (Ti-copper) alloys offer a solution through constitutional supercooling and/or solid state thermal cycling under AM conditions. This work analyzes a compositionally graded directed energy deposition (DED) Ti-Cu build, single-melt laser tracks, and dilatometric heat treatments to evaluate if, when, and by what mechanism(s) microstructural refinement occurs. Refinement by inoculation of unmelted powder particles was also considered. Constitutional supercooling produced no net microstructural refinement as any equiaxed dendrites which form are remelted with new deposition. This finding agreed with solidification modeling of powder bed fusion-laser beam (PBF-LB) and DED builds. Solid state thermal cycling refined microstructures only during ex-situ dilatometric heat treatments, suggesting build parameter optimization is needed to achieve refinement in-situ. Accidental heterogeneous nucleation on unmelted Ti powder, originating from the different thermophysical properties of Ti and Cu, provided the most significant microstructural refinement. This work systematically assesses the microstructural refinement mechanisms of Ti-Cu in AM builds and offers insights into microstructural control in eutectoid alloys.

36 MATERIALS SCIENCE↗

Microstructural evolution in shear-punch tests: A comparative study of pure Cu and Cu-Cr alloy

Understanding the mechanisms behind microstructural evolution during shear deformation has been a long-standing area of interest. However, establishing a connection between microstructure, mechanical properties, and extent of shear deformation is challenging and requires refined experimental approaches. Shear-punch testing (SPT) provides a controlled method to introduce shear into small volumes of material that later can be subjected to detailed microstructural characterization. In this study, we utilize an SPT device to induce shear deformation to pure copper and a binary copper-chromium alloy. Electron backscatter diffraction and transmission electron microscopy were used to study the mechanisms of plastic deformation after SPT. Our results indicate that shear deformation of pure Cu produces a dense network of intercepting microshear bands upon sustained deformation. Twin boundaries undergo degradation into high angle grain boundaries due to simultaneous deviation from the axis-angle pair condition of 60° misorientation on [111] direction. The presence of 50% volume Cr particles in the soft Cu matrix fundamentally altered the shear deformation mechanism. Preferential deformation of the Cu matrix led to accelerated shear-induced formation of low and high angle grain boundaries, and subsequent grain refinement. Comparatively, no grain refinement occurred in pure Cu at a strain ~10 times larger (ϵ = 4.73) than that of the copper-chromium case (ϵ = 0.42). Overall, our study sheds light on the microstructural evolution during shear deformation and highlights the significant influence of particle reinforcements on the shear deformation mechanisms of metals.

36 MATERIALS SCIENCE↗

Isolation and Structural Elucidation of 15–Nuclear Copper Dihydride Clusters: An Intermediate in the Formation of a Two–Electron Copper Superatom

Highly reactive copper-dihydride clusters, [Cu 15 (H) 2 (S 2 CNR 2 ) 6 (C 2 Ph) 6 ](PF 6 ) {R = n Bu (1 H ), n Pr (2 H ), i Bu (3 H )}, are isolated during the reaction of [Cu 28 H 15 {S 2 CN n Bu 2 } 12 ](PF 6 ) with ten equivalents of phenylacetylene. They are found to be intermediates in the formation of the earlier reported two-electron superatom [Cu 13 (S 2 CNR 2 ) 6 (C 2 Ph) 4 ] + . Better yields are obtained by reacting dithiocarbamate sodium salts, [Cu(CH 3 CN) 4 ](PF 6 ), BH 4 – and phenylacetylene. The presence of two hydrides in the isolated clusters is confirmed by the synthesis and characterization of its deuteride analogue [Cu 15 (D) 2 (S 2 CNR 2 ) 6 (C 2 Ph) 6 ] + , and a single-crystal neutron structure of 2 H . Structural characterization of 1 H reveals a new bicapped icosahedral copper(I) cage encapsulating a linear copper dihydride (CuH 2 ) – unit. In conclusion, reaction of 3 H with Au(I) salts yields a highly luminescent [AuCu 12 (S 2 CNiBu 2 ) 6 (C 2 Ph) 4 ] + cluster.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Phase evolution during conventional and reactive flash sintering of (Mg,Ni,Co,Cu,Zn)O via in situ X-ray diffraction

Reactive flash sintering (RFS) enables the simultaneous synthesis and sintering of ceramics and has been shown to affect the reaction pathway of different materials. Herein, in situ synchrotron X-ray diffraction (XRD) is used to investigate the (Mg,Ni,Co,Cu,Zn)O entropy-stabilized oxide formation during: (i) conventional heating and (ii) RFS under current rate-controlled mode. The same reaction pathway is verified in both instances: the starting rock-salt (RS), spinel (Co 3 O 4 ), tenorite (CuO), and wurtzite (ZnO) phases transform into a single RS phase with a (1 1 1) to (2 0 0) intensity ratio of 0.67, consistent with a random distribution of the cations into the structure. Pt lattice peak shift from the XRD patterns is used as standard to monitor the sample surface temperature, revealing a strong endothermic reaction during the RS single-phase formation (Pt peaks shift toward higher angles while increasing sample temperature/current density). Furthermore, in RFS, the single-phase RS structure is formed in just 60 s at a furnace temperature of 600°C and a current rate of 220 mA mm -2 /min. Therefore, RFS greatly accelerates the synthesis of (Mg,Ni,Co,Cu,Zn)O, however, it does not play a role in the reaction pathway for this material formation.

36 MATERIALS SCIENCE↗