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At least 181 records · Page 10

N 2 O deconstruction of polycyclooctene to generate carbonyl-functionalized macromonomers

Deconstruction of polyolefins into functionalized macromonomers presents a compelling strategy for polyolefin upcycling by creating macromonomers through dehydrogenation/depolymerization. We show that nitrous oxide (N 2 O), a greenhouse gas waste product from the production of nylon, mediates the deconstruction of polycyclooctene (PCOE) and generates carbonyl-functionalized macromonomers. Carbonyl incorporation and macromonomer molar mass were well controlled by reaction time, and subsequent hydrogenation readily removed residual carbon-carbon double bonds. Here, we also demonstrated that the reaction could progress efficiently with substrates of moderate levels of unsaturation, closely mimicking partially dehydrogenated polyethylene. Such carbonyl-functionalized macromonomers could serve as feedstock for preparing vitrimers and other functional polymers.

36 MATERIALS SCIENCE↗

Stability and Activity of Cobalt Antimonate for Oxygen Reduction in Strong Acid

Guided by computational Pourbaix screening and high-throughput experiments aimed at the development of precious-metal-free fuel cells, we investigate rutile CoSb 2 O 6 as an electrocatalyst for oxygen reduction in 1 M sulfuric acid. Following 4 h of catalyst conditioning at 0.7 V vs RHE, operation at this potential for 20 h yielded an average current density of –0.17 mA cm –2 with corrosion at a rate of 0.04 nm hour –1 that is stoichiometric with catalyst composition. Surface Pourbaix analysis of the (111) surface identified partial H coverage under operating conditions. The Sb active site has an HO* binding free energy of 0.49 eV, which is near the peak of the kinetic 4e – ORR volcano for transition-metal oxides in acidic conditions. Furthermore, the experimental demonstration of operational stability and computational identification of a reaction pathway with favorable energetics place rutile CoSb 2 O 6 among the most promising precious-metal-free electrocatalysts for oxygen reduction in acidic media.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Thermal Gradient Effects on Redox Evolution and Volatility-Driven Fractionation in Ternary U/Ce/Cs Condensates

Understanding how thermal history influences redox evolution and chemical fractionation is essential for characterizing high-temperature condensation in complex materials, including nuclear debris. Here, we tested the hypothesis that distinct thermal regimes in a plasma flow reactor influence redox pathways and elemental partitioning in ternary U/Ce/Cs systems. A configurable plasma flow reactor was modified with an external tube furnace to impose two distinct thermal gradients: continuous ambient cooling and a furnace-assisted thermal hold-up near 1400 K followed by rapid cooling. Transmission electron microscopy characterized phase identity, morphology, and nanoscale element distributions, while inductively coupled plasma-mass spectrometry quantified bulk elemental ratios. Across both thermal regimes, uranium and cerium condensed as UO 2 and CeO 2 as dominant refractory oxide products. Uranium partially oxidized to α-UO 3 during extended ambient cooling, while furnace-assisted hold-up preserved UO 2 and produced partial reduction of cerium to Ce 2 O 3 . Cesium remained volatile upstream and condensed later in the reactor, forming Cs 2 O and Cs-uranate phases with the highest incorporation after thermal hold-up. Bulk ICP-MS measurements supported these observations. U/Ce ratios remained comparatively stable and Cs displayed delayed and apparent transient enrichment that matched the nanoscale measurements. This integrated approach provides a quantitative method for linking thermal gradients to redox evolution and volatility-driven fractionation. These results show how the plasma flow reactor can identify where equilibrium descriptions remain adequate and where kinetic effects from residence time and temperature history must be considered when interpreting condensation behavior in multicomponent systems.

and nuclear chemistry↗

Bio‐Inspired In Situ Tuning of the Hydrophobic Environment Around Catalytically Active Organic Ligand‐Stabilized Ruthenium Nanoparticles

Abstract The organic ligand environment surrounding enzymatic and homogeneous catalytic active sites often determines catalytic activity. Ruthenium nanoparticles, ≤1 nm in diameter, are synthesized using monodentate thiol, monodentate phosphine, and bidentate bisphosphine ligands. Even though some of the ruthenium surface is blocked by the ligands, catalytic activity is still observed for CO oxidation and H 2 O 2 decomposition. All three ligand‐stabilized ruthenium nanoparticles have similar CO oxidation rates; however, the bisphosphine‐stabilized Ru nanoparticles are approximately 2.5 times less active than the monothiol‐stabilized and monophosphine‐stabilized ruthenium nanoparticles for H 2 O 2 decomposition. It is observed that the organic ligand environment is modulated in situ during nanoparticle synthesis via partial oxidation of the bisphosphine as confirmed by 31 P NMR measurements. We hypothesize that bisphosphine‐bound Ru nanoparticles consist of a Ru core with some of the ligands bound in a monodentate manner where the other P atom is oxidized and not bound to the Ru surface leading to a thicker hydrophobic layer around the Ru nanoparticles. The increase in hydrophobicity is confirmed via contact angle and zeta potential measurements. H 2 O 2 decomposition rates are known to decrease with increasing hydrophobicity, and this work illustrates a pathway for increasing hydrophobicity in situ using ligand‐bound metallic nanoparticles.

Sufyan, Sayed Abu [Department of Chemical Engineer↗

A Multicopper Oxidase from Paenibacillus Polyethylenelyticus JNU01 Oxidizes Polyethylene

Polyethylene (PE) is a widely used plastic that persists in the environment and resists breakdown via microbial degradation. In this work, we discovered a new bacterium, Paenibacillus polyethylenelyticus JNU01, that grows on a PE-like wax (PELW, 4 kDa) as its sole carbon source, causing chemical modifications to the substrate and releasing small-molecule products. Genomic and transcriptomic analyses identified a multicopper oxidase (PpMmcO) as a key enzyme candidate for this observed activity. PpMmcO promoted surface oxidation, increased hydrophilicity, and the release of small-molecule products such as ketones, alkanes, and alkenoic acids. Scanning electron microscopy confirmed surface damage on both PELW and post-use greenhouse PE films. Weight loss analysis showed mass losses of 5.2% for the PELW powder and 1.6% for the greenhouse PE film after treatment with wild-type PpMmcO. We propose a radical-mediated pathway catalyzed by PpMmcO. These findings identify a new bacterium and enzyme capable of promoting partial PE oxidation and provide insight into biological processes that may act on polyethylene.

36 MATERIALS SCIENCE↗

Tuning 3-D Nanomaterial Architectures Using Atomic Layer Deposition to Direct Solution Synthesis

The ability to synthesize nanoarchitected materials with tunable geometries provides a means to control their functional properties, with applications in biological, environmental, and energy fields. To this end, various bottom-up and top-down synthesis processes have been developed. However, many of these processes require prepatterning or etching steps, making them challenging to scale-up to complex, nonplanar substrates. Furthermore, the ability to integrate nanomaterials into hierarchical arrays with precise control of feature spacing and orientation remains a challenge. One approach to overcome these patterning challenges is the use of surface modification layers to guide the resulting geometry of nanomaterial architectures grown from the substrate. A powerful strategy to accomplish this is what we will refer to as “surface-directed assembly,” where the resulting geometric parameters (feature size, shape, orientation) are predetermined by the initial surface layer. In particular, the use of Atomic Layer Deposition (ALD) to form a surface layer, followed by solution-based growth processes, has the ability to synthesize architected structures with tunable geometries on complex, nonplanar surfaces. Over the past decade, we have reported a series of studies where surface-directed assembly is used to synthesize ZnO nanowires (NWs) on top of a variety of substrates. In this case, a thin film of ZnO is deposited onto the substrate using ALD, which can guide the NW diameter, spacing, and angular orientation with respect to the substrate by controlling epitaxial relationships. Furthermore, we have shown that by depositing a submonolayer overcoat of a secondary material (e.g., amorphous TiO 2 ), nucleation sites are partially blocked, which can further tune the spacing between nanowires while minimizing changes to their other geometric properties. This approach can be used to generate multilevel hierarchical structures, such as hyperbranched NW arrays with tunable control of each level of hierarchy using ALD. Finally, we have demonstrated that the tunable control of geometric parameters can be scaled-up to curved, nonplanar substrates. This highlights the power of ALD to conformally and uniformly deposit the seed layers on complex substrates with subnanometer precision. To complement these seeded hydrothermal approaches, we expanded this strategy to include conversion chemistry of the initial ALD seed layers. For example, by replacing ZnO with Al 2 O 3 as the seed layer without changing the hydrothermal growth conditions, Al–Zn layered-double hydroxide nanosheets can be formed instead of nanowires. In another example of conversion chemistry, a solution anion-exchange process was used to incorporate sulfur into ALD metal oxide films. In both of these conversion processes, the properties of the initial ALD film enabled tuning of the resulting nanostructure geometry. In this Account, we describe the use of ALD to guide the growth of diverse nanomaterial systems, with tunable control over their geometry and composition. We further show how these approaches can be used to tune functional properties for a range of applications, including superomniphobic surfaces, antibiofouling coatings, and photocatalysis. In conclusion, we conclude with an outlook on how the combination of ALD and solution synthesis can enable future directions in scalable nanomanufacturing to overcome the limitations of traditional top-down and bottom-up approaches.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

CsO x Nanostructures on Au(111): Morphology- and Size-dependent Activity for the Water–Gas Shift Reaction

Alkali oxides are typically used as promoters of heterogeneous catalysts for the water–gas shift (WGS; H 2 O + CO → H 2 + CO 2 ) reaction. On Au(111), CsO x exhibits diverse nanostructures at varying coverages, as revealed by scanning tunneling microscopy. Clusters of cesium oxide (Cs 2 O 2 ) nucleate at elbow sites of the Au(111) herringbone when θ Cs is less than 0.1 ML. Subsequently, these clusters transform into two-dimensional (2D) islands (Cs 2 O, Cs 2 O 2 , CsO 2 ) as the cesium coverage increases (θ Cs > 0.1 ML). Both types of CsO x nanostructures enable the WGS process on Au(111). The highest activity was seen for the cesium oxide clusters which facilitated the partial dissociation of water and binding of CO. The CO ads and OH ads groups were not strongly bound and probably reacted to yield a short-lived HOCO intermediate that led to gaseous H 2 and CO 2 . The 2D islands of CsO x also enabled the WGS but their efficiency was reduced due to the formation of cesium hydroxide compounds (limiting mobility of OH groups) and the generation of CO 3 and C species (blocking of active centers). The fact that the performance of the CsO x /Au(111) catalysts changed dramatically with variations in the chemical properties of the CsO x nanostructures indicates that the alkali oxide was an integral part of the active phase, playing a central role in the activation and conversion of the reactants. To attach the label of “promoter” to CsO x is a simplification that does not help in the design and optimization of catalysts for C1 chemistry. In conclusion, to achieve a rational design, one must consider the structural and chemical properties of the alkali oxide.

36 MATERIALS SCIENCE↗

Influence of soil depth, irrigation, and plant genotype on the soil microbiome, metaphenome, and carbon chemistry

ABSTRACT Climate change is causing an increase in drought in many soil ecosystems and a loss of soil organic carbon. Calcareous soils may partially mitigate these losses via carbon capture and storage. Here, we aimed to determine how irrigation-supplied soil moisture and perennial plants impact biotic and abiotic soil properties that underpin deep soil carbon chemistry in an unfertilized calcareous soil. Soil was sampled up to 1 m in depth from irrigated and planted field treatments and was analyzed using a suite of omics and chemical analyses. The soil microbial community composition was impacted more by irrigation and plant cover treatments than by soil depth. By contrast, metabolomes, lipidomes, and proteomes differed more with soil depth than treatments. Deep soil (>50 cm) had higher soil pH and calcium concentrations and higher levels of organic acids, bicarbonate, and triacylglycerides. By contrast, surface soil (0–5 cm) had higher concentrations of soil organic matter, organic carbon, oxidizable carbon, and total nitrogen. Surface soils also had higher amounts of sugars, sugar alcohols, phosphocholines, and proteins that reflect osmotic and oxidative stress responses. The lipidome was more responsive to perennial tall wheatgrass treatments compared to the metabolome or proteome, with a striking change in diacylglyceride composition. Permanganate oxidizable carbon was more consistently correlated to metabolites and proteins than soil organic and inorganic carbon and soil organic matter. This study reveals specific compounds that reflect differences in organic, inorganic, and oxidizable soil carbon fractions that are impacted by interactions between irrigation-supplied moisture and plant cover in calcareous soil profiles. IMPORTANCE Carbon is cycled through the air, plants, and belowground environment. Understanding soil carbon cycling in deep soil profiles will be important to mitigate climate change. Soil carbon cycling is impacted by water, plants, and soil microorganisms, in addition to soil mineralogy. Measuring biotic and abiotic soil properties provides a perspective of how soil microorganisms interact with the surrounding chemical environment. This study emphasizes the importance of considering biotic interactions with inorganic and oxidizable soil carbon in addition to total organic carbon in carbonate-containing soils for better informing soil carbon management decisions.

59 BASIC BIOLOGICAL SCIENCES↗

Influence of strain on SrFeO 3-δ oxidation, reduction, and water dissociation: Insights from ambient pressure X-ray photoelectron spectroscopy

The oxidation and reduction of metal oxides and their interaction with the environment play a critical role in their use for energy storage and conversion applications. The formation of surface adsorbates and their impact on oxide electronic structure can be challenging to probe experimentally, particularly for thin films which enable the study of epitaxial strain but have low surface areas. Here we present a detailed study using ambient pressure X-ray photoelectron spectroscopy of the reduction and oxidation of strained SrFeO 3-δ , induced by changes in temperature, oxygen partial pressure, and water vapor exposure. We find that in comparison to the oxidized lattice, application of tensile strain promotes the formation of oxygen vacancies at the surface, facilitating the subsequent incorporation of oxygen into the lattice in an oxygen environment. While tensile strain does promote the formation of hydroxyls from water dissociation, the kinetics of this process appear more sluggish than on less-strained surfaces, likely due to a competitive surface interaction with oxygen or bulk absorption of hydroxyl species. These findings relating strain, oxygen vacancies, and surface reactivity yield important insight into the surface functionality of oxides for energy conversion and storage applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Radically Engineered Modular Air Separation System with Tailored Oxygen Sorbents

The commercial energy sector relies heavily on fossil fuel conversion, and in the process releases a significant amount of CO 2 . A promising technology to utilize fossil fuels with relatively affordable CO 2 capture is gasification. However, it requires a pure oxygen stream. The current state of the art method to produce oxygen is cryogenic air separation, which supercools air to a liquid, and then using distillation columns to separate the components. While this method has been thoroughly studied, it only has a 25% efficiency from a second law standpoint and therefore requires a significant amount of energy (and associated emissions) for oxygen production. This, then, lowers the incentive for carbon capture within a plant, so alternative methods need to be investigated. One potential method, chemical looping air separation (CLAS), is a promising method to replace state of the art oxygen generation technologies. CLAS utilizes a cyclic redox scheme with an oxygen sorbent to create pure oxygen streams. This approach typically utilizes a dual reactor scheme where the oxygen deficient sorbent enters the first reactor and is subjected to high oxygen partial pressures to re-oxidize the sorbent. Then the sorbent is sent to the reducing reactor, where it is subjected to low oxygen partial pressure (steam or vacuum) to releases oxygen. The overarching objective of this project was to discover the principles for rational design and optimization of oxygen sorbents and process design to ensure the process is a viable replacement for cryogenic air separation, especially in the context of modular gasification systems. This was done through development, characterization, testing, and analyses of (a) high temperature mixed composite oxides; (b) low temperature doped perovskite oxides (A1 x A2 1-x B1 y B2 1-y O 3 ); (c) scale up synthesis and testing of the optimized sorbent particles; (d) process design and analyses of the CLAS system in the context of modular gasification applications.

01 COAL, LIGNITE, AND PEAT↗

Workshop on Oxygen in the Terrestrial Planets

This volume contains abstracts that have been accepted for presentation at the Workshop on Oxygen in the Terrestrial Planets, July 20-23,2004, Santa Fe, New Mexico. The contents include: 1) Experimental Constraints on Oxygen and Other Light Element Partitioning During Planetary Core Formation; 2) In Situ Determination of Fe(3+)/SigmaFe of Spinels by Electron Microprobe: An Evaluation of the Flank Method; 3) The Effect of Oxygen Fugacity on Large-Strain Deformation and Recrystallization of Olivine; 4) Plagioclase-Liquid Trace Element Oxygen Barometry and Oxygen Behaviour in Closed and Open System Magmatic Processes; 5) Core Formation in the Earth: Constraints from Ni and Co; 6) Oxygen Isotopic Compositions of the Terrestrial Planets; 7) The Effect of Oxygen Fugacity on Electrical Conduction of Olivine and Implications for Earth s Mantle; 8) Redox Chemical Diffusion in Silicate Melts: The Impact of the Semiconductor Condition; 9) Ultra-High Temperature Effects in Earth s Magma Ocean: Pt and W Partitioning; 10) Terrestrial Oxygen and Hydrogen Isotope Variations: Primordial Values, Systematics, Subsolidus Effects, Planetary Comparisons, and the Role of Water; 11) Redox State of the Moon s Interior; 12) How did the Terrestrial Planets Acquire Their Water?; 13) Molecular Oxygen Mixing Ratio and Its Seasonal Variability in the Martian Atmosphere; 14) Exchange Between the Atmosphere and the Regolith of Mars: Discussion of Oxygen and Sulfur Isotope Evidence; 15) Oxygen and Hydrogen Isotope Systematics of Atmospheric Water Vapor and Meteoric Waters: Evidence from North Texas; 16) Implications of Isotopic and Redox Heterogeneities in Silicate Reservoirs on Mars; 17) Oxygen Isotopic Variation of the Terrestrial Planets; 18) Redox Exchanges in Hydrous Magma; 19) Hydrothermal Systems on Terrestrial Planets: Lessons from Earth; 20) Oxygen in Martian Meteorites: A Review of Results from Mineral Equilibria Oxybarometers; 21) Non-Linear Fractionation of Oxygen Isotopes Implanted in Lunar Metal Grains: Solar, Lunar or Terrestrial Origin? 22) Isotopic Zoning in the Inner Solar System; 23) Redox Conditions on Small Bodies; 24) Determining the Oxygen Fugacity of Lunar Pyroclastic Glasses Using Vanadium Valence - An Update; 25) Mantle Redox Evolution and the Rise of Atmospheric O2; 26) Variation of Kd for Fe-Mg Exchange Between Olivine and Melt for Compositions Ranging from Alkaline Basalt to Rhyolite; 27) Determining the Partial Pressure of Oxygen (PO,) in Solutions on Mars; 28) The Influence of Oxygen Environment on Kinetic Properties of Silicate Rocks and Minerals; 29) Redox Evolution of Magmatic Systems; 30) The Constancy of Upper Mantlefo, Through Time Inferred from V/Sc Ratios in Basalts: Implications for the Rise in Atmospheric 0 2; 31) Nitrogen Solubility in Basaltic Melt. Effects of Oxygen Fugacity, Melt Composition and Gas Speciation; 32) Oxygen Isotope Anomalies in the Atmospheres of Earth and Mars; 33) The Effect of Oxygen Fugacity on Interdiffusion of Iron and Magnesium in Magnesiowiistite 34) The Calibration of the Pyroxene Eu-Oxybarometer for the Martian Meteorites; 35) The Europium Oxybarometer: Power and Pitfalls; 36) Oxygen Fugacity of the Martian Mantle from PigeoniteMelt Partitioning of Samarium, Europium and Gadolinium; 37) Oxidation-Reduction Processes on the Moon: Experimental Verification of Graphite Oxidation in the Apollo 17 Orange Glasses; 38) Oxygen and Core Formation in the Earth; 39) Geologic Record of the Atmospheric Sulfur Chemistry Before the Oxygenation of the Early Earth s Atmosphere; 40) Comparative Planetary Mineralogy: V/(CrCAl) Systematics in Chromite as an Indicator of Relative Oxygen Fugacity; 41) How Well do Sulfur Isotopes Constrain Oxygen Abundance in the Ancient Atmospheres? 42) Experimental Constraints on the Oxygen Isotope (O-18/ O-16) Fractionation in the Ice vapor and Adsorbant vapor Systems of CO2 at Conditions Relevant to the Surface of Mars; 43) Micro-XANES Measurements on Experimental Spinels andhe Oxidation State of Vanadium in Spinel-Melt Pairs; 44) Testing the Magma Ocean Hypothesis Using Metal-Silicate Partitioning of Te, Se and S; 45) Solubility of Oxygen in Liquid Iron at High Pressure and Consequences for the Early Differentiation of Earth and Mars Metallic Liquid Segregation in Planetesimals; 46) Oxygen Fugacity of Lunar Basalts and the Lunar Mantle. Range of fo2 and the Effectiveness of Oxybarometers; 47) Thermodynamic Study of Dissociation Processes of Molecular Oxygen in Vapor over Oxide Compounds; 48) Oxygen Profile of a Thermo-Haliophilic Community in the Badwater Salt Flat; 49) Oxygen Barometry Using Synchrotron MicroXANES of Vanadium; 50) Mass-Independent Isotopic Fractionation of Sulfur from Sulfides in the Huronian Supergroup, Canada; 51) Mass Independent Isotopes and Applications to Planetary Atmospheres; 52) Electrical Conductivity, Oxygen Fugacity, and Mantle Materials; 53) Crustal Evolution and Maturation on Earth: Oxygen Isotope Evidence; 54) The Oxygen Isotope Composition of the Moon: Implications for Planet Formation; 55) Oxygen Isotope Composition of Eucrites and Implications for the Formation of Crust on the HED Parent Body; and 56) The Role of Water in Determining the Oxygen Isotopic Composition of Planets.

Source record↗

Probing O 2 -dependence of tetrahydrofuranyl reactions via isomer-resolved speciation

Low-temperature oxidation of tetrahydrofuran involves competing reactions that depend on temperature, pressure, and oxygen concentration, including ring-opening and subsequent oxidation of initial radicals ($\dot{R}$), HOO-elimination yielding dihydrofuran isomers, and the formation of peroxy radicals ($RO\dot{O}$). Here, the latter species, upon isomerization, lead to hydroperoxy-substituted radicals ($\dot{Q}OOH$) that undergo reaction either via unimolecular decomposition or second-O 2 -addition. Quantitative measurements of partially oxidized intermediates formed from each type of reaction provide critical constraints that are required for accurate modeling of combustion. To examine the influence of temperature and oxygen concentration on intermediates from tetrahydrofuran, isomer-resolved speciation measurements were conducted at 810 Torr in a jet-stirred reactor (JSR) from 500 – 1000 K. Resulting from negative-temperature coefficient behavior, species concentrations peaked at two temperatures, 600 K and 800 K, which were then selected for separate experiments to quantify O 2 -dependence using concentrations of 0.37 • 10 18 – 7.40 • 10 18 molecules cm –3 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Tuning Fluorination of Linear Carbonate for Lithium-Ion Batteries

Liquid electrolyte engineering plays a critical role in modern lithium-ion batteries. However, the existing electrolytes fall short when used with some trending battery chemistries such as high-voltage and high-energy-density electrodes. Fluorination of electrolyte solvents has been identified as an effective approach for improved cyclability, but few works systematically studied the effects of fluorination extent of carbonate solvents on battery performance. Here we design and synthesize a family of fluorinated ethyl methyl carbonates. Different numbers of F atoms are finely tuned to yield monofluoroethyl methyl carbonate (F1EMC), difluoroethyl methyl carbonate (F2EMC) and trifluoroethyl methyl carbonate (F3EMC). The cycling behavior of several types of lithium-ion pouch cells, including graphite (Gr)/single-crystalline LiNi 0.8 Mn 0.1 Co 0.1 O 2 (SC-NMC811), Gr-SiO x /LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622), high-voltage Gr/LiNi 0.5 Mn 1.5 O 4 (LNMO), Gr/layered Li-rich Mn-based oxide (LLMO) and fast-charging Gr/NMC622, were systematically investigated to understand the impact of fluorination degree. Compared to the commercially available F3EMC, we found that the partially-fluorinated F1EMC and F2EMC in some cases showed improved cycling stability, which we attribute to their locally-polar –CH 2 F and –CHF 2 groups and thus fast ion conduction than –CF 3 . This work suggests that highly or fully fluorinated solvents are not necessarily desirable; instead, fluorination degree needs to be rationally and finely tuned for optimized lithium-ion cell performance.

25 ENERGY STORAGE↗

Additive‐Free Oxidized Spiro‐MeOTAD Hole Transport Layer Significantly Improves Thermal Solar Cell Stability

Perovskite solar cells are among the most promising new solar technologies, already surpassing polycrystalline silicon solar cell efficiencies. The stability of the highest efficiency devices at elevated temperature is, however, poor. These cells typically use Spiro-MeOTAD as the hole transporting layer. It is generally believed that additives, required for enhancing electrical conductivity and optimizing energy level alignment, are responsible for the reduced stability—inferring that Spiro-MeOTAD based hole transporting layers are intrinsically unstable. Here, a reliable noble metal free synthesis of Spiro-MeOTAD (bis(trifluoromethane)sulfonimide) 4 is presented which is used as the oxidizing agent. No additives are added to the partially oxidized Spiro-MeOTAD hole-transporting layer. Device efficiencies up to 24.2% are achieved. Electrical conductivity is largely developed by the first 1% oxidation. Further oxidation shifts the energy levels away from the vacuum level, which allows tuning of the energy level alignment without the use of additives—contradicting the current understanding of this system. Without additives, devices demonstrate significant improvement in stability at elevated temperatures up to 85 °C under one sun over 1400 h continuous illumination. The remaining degradation is pinpointed to ion migration and reactions in the perovskite layer which may be further suppressed with compositional engineering and adequate ion barrier layers.

14 SOLAR ENERGY↗

Self-grown NiCuO x hybrids on a porous NiCuC substrate as an HER cathode in alkaline solution

Electrocatalysts converted directly from the substrates hold the key to achieve high catalytic activity and durability due to their high bonding strength, intimate electronic contact, and tunable phase composition. Herein, an electrically conductive porous NiCuC substrate was adopted to develop a multi-porous NiCuO x /NiCuC hydrogen evolution reaction (HER) catalyst using a one-step oxidation method in this research. The NiCuO x hybrids were characterized as three typical layers: an outer layer with NiCuO 2 solid solution phase, a partially oxidized intermediate layer, and an inner layer with limited stable oxygen content. Here, the NiCuO x /NiCuC possesses abundant Ni(II)–Cu(II) sites to accelerate the Volmer step via the electrostatic effect with OH – , numerous metallic NiCu sites to facilitate the H adsorption, and highly accessible channels to promote the Heyrovsky step during HER catalysis. As a result, high electrocatalytic performance was obtained with an overpotential of 116 mV at a current density of 10 mA cm –2 in 1.0 M potassium hydroxide, and a stable catalytic performance during the HER process for more than 24 h.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

CO Oxidation Mechanisms on CoO x -Pt Thin Films

The reaction of CO and O 2 with submonolayer and multilayer CoO x films on Pt(111), to produce CO 2 , was investigated at room temperature in the mTorr pressure regime. Here, using operando ambient pressure X-ray photoelectron spectroscopy and high pressure scanning tunneling microscopy, as well as density functional theory calculations, we found that the presence of oxygen vacancies in partially oxidized CoO x films significantly enhances the CO oxidation activity to form CO 2 upon exposure to mTorr pressures of CO at room temperature. In contrast, CoO films without O-vacancies are much less active for CO 2 formation at RT, and CO only adsorbed in the form of carbonate species that are stable up to 260 °C. On submonolayer CoO x islands, the carbonates form preferentially at island edges, deactivating the edge sites for CO 2 formation, even while the reaction proceeds inside the islands. These results provide a detailed understanding of CO oxidation pathways on systems where noble metals such as Pt interact with reducible oxides.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Photoelectrochemical CO 2 Reduction toward Multicarbon Products with Silicon Nanowire Photocathodes Interfaced with Copper Nanoparticles

The development of photoelectrochemical systems for converting CO 2 into chemical feedstocks offers an attractive strategy for clean energy storage by directly utilizing solar energy, but selectivity and stability for these systems have thus been limited. Here, we interface silicon nanowire (SiNW) photocathodes with a copper nanoparticle (CuNP) ensemble to drive efficient photoelectrochemical CO 2 conversion to multicarbon products. This integrated system enables CO 2 -to-C 2 H 4 conversion with faradaic efficiency approaching 25% and partial current densities above 2.5 mA/cm 2 at -0.50 V vs RHE, while the nanowire photocathodes deliver 350 mV of photovoltage under 1 sun illumination. Under 50 h of continual bias and illumination, CuNP/SiNW can sustain stable photoelectrochemical CO 2 reduction. In conclusion, these results demonstrate the nanowire/catalyst system as a powerful modular platform to achieve stable photoelectrochemical CO 2 reduction and the feasibility to facilitate complex reactions toward multicarbons using generated photocarriers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Role of catalytic nitrile decomposition in tricopper complex mediated direct partial oxidation of methane to methanol

Synthetic homogeneous system known to date performing methane to methanol conversion using O 2 as terminal oxidant is unique and based on copper complex with piperazine-based ligand (Cu 3 L in Fig. 1) in a medium of acetonitrile. Prior work have shown that in order to achieve catalytic turnover, hydrogen peroxide is needed to regenerate the active site. We show in this paper that reaction solvent based on organic nitrile decompose concurrently with methane activation and that in the absence of either acetonitrile, Cu complex or hydrogen peroxide, the catalytic turnover does not happen. We show in this manuscript that the direct methane oxidation to methanol might have been mediated by catalytic Radziszewski oxidation between acetonitrile and H 2 O 2 . Additionally we have discovered that in the absence of methane, peroxide mediated acetonitrile decomposition also makes methanol via a background reaction which was hitherto unknown.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗