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At least 127 records · Page 7

Heterogeneous Supramolecular Catalysis through Immobilization of Anionic M 4 L 6 Assemblies on Cationic Polymers

Although most of the currently developed supramolecular catalysts that emulate enzymatic reactivity with unique selectivity and activity through specific host-guest interactions work under homogeneous conditions, enzymes in nature can operate under heterogeneous conditions as membrane-bound enzymes. In order to develop such a heterogeneous system, an immobilized chiral supramolecular cluster Ga 4 1 6 ( 2 ) was introduced into cross-linked polymers with cationic functionalities. These heterogeneous supramolecular catalysts were used in aza-Prins and aza-Cope reactions and successfully applied to continuous-flow reactions. Additionally, they showed high durability and maintained high turnovers for long periods of time. In sharp contrast to the majority of examples of heterogenized homogeneous catalysts, the newly developed catalysts showed enhanced activity and robustness compared to those exhibited by the corresponding soluble cluster catalyst. An enantioenriched cluster was also immobilized to enable asymmetric catalysis, and activity and enantioselectivity of the supported chiral catalyst were maintained during recovery and reuse experiments and under a continuous-flow process. Significantly, the structure of the ammonium cations in the polymers affected stability, reactivity, and enantioselectivity, which is consistent with the hypothesis that the cationic moieties in the polymer support interact with cluster as an exohedral protecting shell, thereby influencing their catalytic performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Symmetry in Seeded Metal Nanocrystal Growth

Symmetry underpins the structure and function of the world around us and is also captured in modern nanomaterials, where changing the symmetry of a nanocrystal or the interparticle spacing and orientation of nanocrystal building blocks in a superlattice can give new function. However, the synthesis and assembly of nanocrystals have been limited largely to simple compositions and structures. It remains a grand challenge to achieve nanocrystals with compositional and structural complexity while maintaining the monodispersity required for their use. This Account will illustrate through recent examples that seeded methods enable the synthesis of compositionally and structurally complex multimetallic crystals with defined and predictable symmetries for applications in plasmonics and catalysis. This outcome arises because the barrier for heterogeneous nucleation (i.e., seeded) is lower than that of homogeneous nucleation, where seeds can serve as preferential sites for the growth of complex structures and crystal phases. Our analysis begins by considering metal overgrowth from single-crystalline seeds of different shapes and symmetries, where the kinetics of adatom addition to seeds relative to their diffusion across seeds accounts for the expressed nanocrystal shapes. These results are then compared to overgrowth from seeds with different internal structures (i.e., planar defects), where the relationships between nanocrystal size and volumetric strain energy and surface energy are discussed. A major finding from this analysis is that often the underlying symmetry of seeds can be predictably transferred to the final crystals during overgrowth processes. Consequences of this finding are the predictable syntheses of crystals with different hierarchies akin to snowcrystals as well as nanocrystals with complex compositions (e.g., quaternary nanoparticles). Yet, there are subtle aspects to seeded growth that pave a path toward examples where nanocrystal symmetry has been reduced compared to the original seeds in a controlled manner. As we found, both the concentrations of metal precursors and capping agents can impact whether symmetry is transferred or reduced during overgrowth. Examples from our laboratory will be placed in context to other reported strategies for symmetry breaking. As will be argued, understanding what conditions favor symmetry preservation versus symmetry reduction during seeded crystal growth is central to accessing next-generation crystal forms. The Account concludes by outlining synthetic challenges associated with forming nanoscale heterostructures with precise 3-D placement of different materials within a given nanocrystal as well as facet control within different material domain and interface engineering. Furthermore, we envision meeting these challenges through regioselective and chemoselective seeded syntheses for which a foundation is outlined herein.

36 MATERIALS SCIENCE↗

Mineral surface-catalyzed oxidation of Mn(II) by bromate: Implications for the occurrence of Mn oxides on Mars

The occurrence of manganese (Mn) oxides on Mars is believed to be an indicator of an O 2 -rich paleoenvironment of Mars because Mn oxides often form through the oxidation of Mn(II) by O 2 on the surface of Earth. An alternative formation pathway was recently proposed, in which Mn(II) is oxidized by bromate (BrO 3 - ), a common oxidant in contemporary Martian regolith. However, the oxidation of Mn(II) by bromate in solution is kinetically controlled and slow unless using very high concentrations (100 mM) of reactants that may be irrelevant to the conditions of Mars. We conducted laboratory simulations to determine whether iron (Fe) oxides (hematite and goethite) and a phyllosilicate (montmorillonite), abundant minerals on the surface of Mars, could catalyze the oxidation of Mn(II) by bromate. Hematite and goethite, but not montmorillonite, dramatically accelerated the oxidation with a low concentration (1 mM) of Mn(II) and bromate under various solution conditions. Further, the reaction system was autocatalytic with Fe oxides initiating the oxidation of Mn(II) at the early stage and the subsequent catalysis mainly provided by the Mn oxide products. In contrast to producing Mn(IV)O 2 only during the homogeneous oxidation of Mn(II) by bromate in solutions, the heterogeneous mineral-surface catalyzed oxidation resulted in a mixture of Mn(III)OOH and Mn(IV)O 2 phases. Mn(III)OOH was an intermediate product and can be further oxidized by bromate to Mn(IV)O 2 . The occurrence and accumulation of the intermediate product MnOOH can be attributed to its rapid formation due to surface-enhanced nucleation and growth on Fe oxide surfaces and to its higher resistance to oxidation by bromate than Mn(III) ions or clusters. Overall, mineralsurface catalyzed oxidation of Mn(II) by bromate is favorable from both thermodynamic and kinetic perspectives, and can be a major pathway for the occurrence of Mn oxides on Mars where microorganisms are lacking to catalyze the reaction. Our study further improves our understanding of the thermodynamic and kinetic controls on Mn(II) oxidation.

54 ENVIRONMENTAL SCIENCES↗

Templating Bicarbonate in the Second Coordination Sphere Enhances Electrochemical CO 2 Reduction Catalyzed by Iron Porphyrins

Bicarbonate-based electrolytes are ubiquitous in aqueous electrochemical CO 2 reduction, particularly in heterogenous catalysis, where they demonstrate improved catalytic performance relative to other buffers. In contrast, the presence of bicarbonate in organic electrolytes and its roles in homogeneous electrocatalysis remain underexplored. Here, we investigate the influence of bicarbonate on iron porphyrin-catalyzed electrochemical CO 2 reduction. In this work, we show that bicarbonate is a viable proton donor in organic electrolyte (p K a = 20.8 in dimethyl sulfoxide) and that urea pendants in the second coordination sphere can be used to template bicarbonate in the vicinity of a molecular iron porphyrin catalyst. The templated binding of bicarbonate increases its acidity, resulting in a 1500-fold enhancement in catalytic rates relative to unmodified parent iron porphyrin. This work emphasizes the importance of bicarbonate speciation in wet organic electrolytes and establishes second-sphere bicarbonate templating as a design strategy to harness this adventitious acid and enhance CO 2 reduction catalysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

On the integration of molecular dynamics, data science, and experiments for studying solvent effects on catalysis

Computational workflows that combine molecular dynamics (MD) simulations and emerging data-centric (DC) methods can accelerate the screening and analysis of solvent systems experimentally and computationally. Here, MD simulations provide atomic positions and velocities of reactant, solvent, and catalyst materials that can be manipulated into data representations that in turn can be used by DC techniques to conduct predictive modeling, feature extraction, and experimental design. For liquid-phase catalytic applications, emerging DC techniques such as Convolutional and Graph Neural Networks (CNN/GNN), Topological Data Analysis (TDA), and Active Learning (AL) can leverage MD and experimental data to quickly predict solvent effects on reaction outcomes. For instance, in recent studies, 3D solvent environments obtained with MD have been exploited by CNNs to predict experimental reaction rates for homogeneous acid-catalyzed lignocellulosic processes. In this perspective, we discuss basic principles of DC methods and how these can be combined with MD to enable high-throughput screening of solvent selection for diverse catalysis applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Final Technical Report

This research project aims to understand the structure and properties of hidden intermediates in amorphous oxides grown by atomic layer deposition (ALD), and apply what is learned to achieve predictive phase and property control in the ALD synthesis of amorphous oxide thin films. The one-year renewal is to further this understanding to understand how amorphous TiO2 thin films by ALD turn into crystalline phase in correlation to the presence of medium range ordering (MRO) and other impurities. This fundamental study is expected to produce a predictive synthesis science for amorphous thin films with substantially improved uniformity and thereby achieve higher stability as a new surface coating strategy used for electrochemical catalysis. In this final technical report, we summarize the key achievements in this project to meet the research goals. This includes (1) a new approach to achieve homogeneous nanometer-scale amorphous coating leading to a new record of lifetime for photoelectrochemical hydrogen fuel generation; (2) A advancement in scanning transmission electron microcopy (STEM) that led to new understanding of intermediate phase in amorphous films; and (3) a computational model for understanding the local structure ordering in amorphous TiO2 films. In addition, this project also yielded relevant technical innovations including a development of bioresorbable zinc primary batteries that can self-degrade after depletion; and a ferroelectric membrane that provides active dendrites suppression to substantially improve the lifetime of rechargeable batteries. Collaboration with Lam Research also yield a new understanding of how built-in strain influences the amorphous films’ quality, bringing direct impacts to semiconductor manufacturing industry.

36 MATERIALS SCIENCE↗

ECUT: Energy Conversion and Utilization Technologies program. Heterogeneous catalysis modeling program concept

Insufficient theoretical definition of heterogeneous catalysts is the major difficulty confronting industrial suppliers who seek catalyst systems which are more active, selective, and stable than those currently available. In contrast, progress was made in tailoring homogeneous catalysts to specific reactions because more is known about the reaction intermediates promoted and/or stabilized by these catalysts during the course of reaction. However, modeling heterogeneous catalysts on a microscopic scale requires compiling and verifying complex information on reaction intermediates and pathways. This can be achieved by adapting homogeneous catalyzed reaction intermediate species, applying theoretical quantum chemistry and computer technology, and developing a better understanding of heterogeneous catalyst system environments. Research in microscopic reaction modeling is now at a stage where computer modeling, supported by physical experimental verification, could provide information about the dynamics of the reactions that will lead to designing supported catalysts with improved selectivity and stability.

Voecks, G. E.↗

Silica Supported Organometallic Ir I Complexes Enable Efficient Catalytic Methane Borylation

Catalytic C–H borylation is an attractive method for the conversion of the most abundant hydrocarbon, methane (CH 4 ), to a mild nucleophilic building block. However, existing CH 4 borylation catalysts often suffer from low turnover numbers and conversions, which is hypothesized to result from inactive metal hydride agglomerates. Herein we report that the heterogenization of a bisphosphine molecular precatalyst, [(dmpe)Ir(cod)CH 3 ], onto amorphous silica dramatically enhances its performance, yielding a catalyst that is 12-times more efficient than the current standard for CH 4 borylation. The catalyst affords over 2000 turnovers at 150 °C in 16 h with a selectivity of 91.5% for mono- vs diborylation. Higher catalyst loadings improve yield and selectivity for the monoborylated product (H 3 CBpin) with 82.8% yield and >99% selectivity being achieved with 1255 turnovers. X-ray absorption and dynamic nuclear polarization-enhanced solid-state NMR spectroscopic studies identify the supported precatalyst as an Ir I species, and indicate that upon completion of catalysis, multinuclear Ir polyhydrides are not formed. This is consistent with the hypothesis that immobilization of the organometallic Ir species on a surface prevents bimolecular decomposition pathways. Importantly, immobilization of the homogeneous Ir I fragment onto amorphous silica represents a unique and simple strategy to improve the TON and longevity of a CH 4 borylation catalyst.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Domain-Dependent Electronic Properties of 2D Copper Boride Synthesized from Reversible Subsurface Diffusion on Cu(111)

Emerging boron-based 2D materials hold properties with potential applications ranging from electronic devices to catalysis and energy storage. Using physical vapor deposition, 2D copper borides are formed on Cu(111) at elevated temperatures. However, the as-prepared surfaces often contain boron clusters that compromise structural homogeneity, and the dynamics of their formation is not yet fully understood. Through in situ low-energy electron microscopy (LEEM), Auger electron spectroscopy (AES), and scanning tunneling microscopy/spectroscopy (STM/STS), we show that cluster-free 2D CuB x is synthesized via reversible subsurface diffusion of boron atoms. The resolved regular atomic structure aligns with the previously calculated Cu 8 B 14 model. In a rare case, possibly due to surface strain and a change of orientation, a second domain of CuB x was observed with a pronounced change in electronic properties, yet electronic states remain delocalized in both domains. In conclusion, these findings demonstrate the sensitivity of electronic properties to domain structure and highlight a potential opportunity to tune 2D CuB x for diverse applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Bicontinuous nanoporous design induced homogenization of strain localization in metallic glasses

Bicontinuous nanoporous metallic glasses (MG) synergize the outstanding properties of MGs and open-cell nanoporous materials. The low-density and high-specific-surface-area of bicontinuous nanoporous structures have the potential to enhance the applicability of MGs in catalysis, sensors, and lightweight structural designs. In this work, we report molecular dynamics simulations of tensile loading deformation and failure of bicontinuous nanoporous Cu 64 Zr 36 MG with 55% porosity and 4.4 nm ligament size. Results indicate an anomalous mechanical behavior featuring delocalized plastic deformation preceding ductile failure. The deformation follows two mechanisms: i) Necking of ligaments aligned with the loading direction and ii) progressive alignment of randomly oriented ligaments. Failure occurs at 0.16 strain, following massive rupture of ligaments. This work indicates that a bicontinuous nanoporous design is able to effectively delocalize strain localization in a MG due to a combination of size effect on the ductility of MGs resulting in nano ligaments necking and progressive asynchronous alignment of ligaments.

36 MATERIALS SCIENCE↗

Novel Homogeneous Electrocatalysts for the Nitrogen Reduction Reaction

This project funded a broad range of fundamental studies in the research labs of Prof. John Berry at the University of Wisconsin – Madison. The overall goals of this research are to identify and explore promising new fundamental chemistry of metal-metal bonded coordination compounds in catalysis, with a particular focus on exploring the technologies needed for the transition to a nitrogen economy. We focus on two key technologies for this overall goal: Electrochemical synthesis of ammonia from nitrogen and water, and Electrochemical ammonia oxidation to produce nitrogen. Ammonia is the most hydrogen-rich material known aside from hydrogen itself, and is therefore an ideal fuel unit. Currently, ammonia synthesis uses significant fossil fuel inputs, has a large carbon footprint, and is performed in large, centralized facilities, mandating the exploration of carbon-neutral approaches that can be done in a distributable manner so that ammonia transportation does not pose a bottleneck. Our work towards these goals is organized as follows: Goal 1: Synthesis and characterization of new catalysts and N2RR intermediates; Goal 2: Thermodynamic investigations of all catalysts and intermediates; Goal 3: Exploration of the electrocatalytic N¬2RR using new catalysts. We additionally made progress toward a related Goal 4: Exploration of new types of catalysts with other, cheaper transition metals. We had a major setback in year 1 of the grant due to the student driving this project (Tristan Brown) contracting an incurable disease that made it impossible for him to perform lab work. Tristan transitioned to a computational chemistry project and was subsequently able to complete his PhD.

02 PETROLEUM↗

Synergistic catalysis by Mn promoted ceria for molecular oxygen assisted epoxidation

Mesoporous manganese doped cerium oxide catalysts were prepared by an inverse micelle method with different manganese loadings. These materials exhibited superior activity for epoxidation of alkenes with molecular oxygen. Highest active 10MnCe material showed an activity of 80 % conversion and >99 % selectivity for cyclooctene epoxidation. The fluorite crystal structure which facilitates the high oxygen mobility, low temperature reducibility, homogeneous distribution of manganese on ceria, nanoparticle nature, higher number of oxygen vacancies, low valent states of manganese and cerium, and the ability to generate reactive oxygen species of the manganese doped cerium oxide could be correlated to the high catalytic activity. The reaction followed first order kinetics with a rate constant of 0.31 h –1 at 100 °C, and the activation energy turned out to be 10.5 kJ/mol. In conclusion, the mechanistic study revealed that the reaction proceeds via a unique mechanism which involves in situ generated superoxide and singlet oxygen species..

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A bifunctional zeolitic porous liquid with incompatible Lewis pairs for antagonistic cascade catalysis

The emergence of porous liquids (PLs) opened opportunities to form unique antagonistic systems capable of fulfilling cascade reactions promoted by incompatible active sites in one pot, which is a long-term challenging subject in catalysis. Herein, unique bifunctional type III PL-based systems were facilely fabricated via assembly of zeolite nanosheets with ionic liquids. Rational structural design afforded PLs that feature high zeolite concentration, stable dispersion after 2 years, abundant cavity distribution, and involvement of antagonistic groups (acid and base sites) in separated and active form via steric hindrance control and electronic repulsion regulation. These unique properties worked cooperatively to fulfill the cascade deacetalization-Knoevenagel/Aldol condensation in one pot with superior catalytic efficiency outperforming the traditional systems. The key to success lies in the formation of bifunctional composites, transformation of zeolite from heterogeneous to homogeneous via surface modification, as well as rapid mass transfer ensured by the rigid porous architecture.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Design of Efficient Molecular Electrocatalysts for Water and Carbon Dioxide Reduction Using Predictive Models of Thermodynamic Properties

Objectives: 1) To design and synthesize water soluble transition metal complexes that function as electrocatalysts for the reduction of water to hydrogen or carbon dioxide to formate 2) To experimentally measure thermochemical properties, such as hydride donor ability, and use these quantities to optimize catalyst performance in solutions of varying pH 3) To incorporate results from detailed mechanistic and kinetic studies to direct improvements in catalyst design 4) To use thermochemical data from objective 2 to generate predictive models for the properties of new complexes to apply to the development of catalysts for other reductive reactions, with an emphasis on carbon dioxide reduction to methanol Description: Wide-spread implementation of renewable but intermittent energy sources, such as solar, requires the development of efficient methods for energy storage. The high energy density of chemical bonds makes chemical fuels an ideal solution for energy storage. Hydrogen and reduced carbon compounds have been proposed as ideal candidates for chemical fuels. However, the generation of chemical fuels from electricity requires competent electrocatalysts. The proposed research focuses on developing electrocatalysts for the reduction of water to hydrogen, and carbon dioxide to formate. Both products can be used directly as an energy carrier in fuel cells, or as a reductant for more saturated chemical fuels. Hydrogen is the most common fuel used in current commercial fuel cells. Additionally, there is interest in formic acid as a liquid carrier for hydrogen because of its increased storage density and ease of dehydrogenation. Formate is also an intermediate in the sequential reduction of CO 2 to methanol, another potential chemical fuel with high energy storage density. Despite the utility of formate as a chemical fuel or precursor, there are very few examples of electrocatalysts for its production from CO 2 , and even fewer demonstrate high product selectivity. In heterogeneous catalysis, the Sabatier principle is used to generate volcano curves that describe optimal thermochemical properties for key intermediates that result in peak catalytic activity. In most cases, such as hydrogen production and oxidation, the most favorable metals (Pt, Re, Rh, and Ir) are rare and expensive. Molecular inorganic complexes provide an opportunity to use electronic and steric ligand effects to tune the critical thermodynamic parameters of abundant metals to values comparable to key surface intermediates on precious metals. This principle will be applied to the design of aqueous homogeneous catalysts for the reduction of H 2 O and CO 2 optimized to function at specific pH ranges. The critical intermediate in both of these reactions is a metal hydride. The strength of this bond, or hydricity (ΔGH - ) dictates the overall thermodynamics of the reduction of H + to H 2 and the sequential reduction of C1 substrates, such as CO 2 , CO, and H 2 CO (the latter to CH 3 OH). ΔGH - will be systematically measured for a series of first row metal complexes to form predictive models for metal and ligand electronic effects. Benefits and Outcomes: This approach addresses thermodynamic requirements essential for energy-efficient catalyst design and transition state barrier considerations for faster catalysis. The advancements made from this research will include the discovery of efficient, stable, and fast catalysts for hydrogen and formate generation from electricity. The ability to store energy efficiently is critical to the widespread use of renewable energy schemes. This provides a viable solution to produce high energy density fuels for stationary and mobile energy applications. The fundamental research conducted is also directly applicable to the design of catalysts for the generation of further reduced products such as methanol.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Economizing on Precious Metals in Three-Way Catalysts: Thermally Stable and Highly Active Single-Atom Rhodium on Cera for NO Abatement under Dry and Industrially Relevant Conditions

We show for the first time that atomically dispersed Rh cations on ceria, prepared via high-temperature atom trapping synthesis, are the active species for (CO+NO) reaction. This provides a direct link with the organometallic homogeneous Rh(I) complexes capable of catalyzing dry (CO+NO) reaction but without the stability concern. In particular, thermally stable Rh cations in 0.1wt% Rh1/CeO2 achieve full NO conversion with a TOF of ~ 330 hr-1 per Rh atom at 120 °C. Under dry conditions, the main product above 100 °C is N2 with N2O being the minor product. The presence of water promotes low-temperature activity of 0.1wt% Rh1/CeO2 starting at 50 °C with full NO conversion at ~120 °C. In the case with the wet stream, however, ammonia and nitrogen are the main products with only minor N2O amounts. NH3 formation at such low temperatures is attractive because of the potential to use this as a passive SCR system. Because of the uniformity of Rh ions on the support, we are able to observe the intermediates of (CO+NO) reaction via infrared measurements on Rh cations on zeolite and ceria. Furthermore, we show that ammonia formation correlates with the WGS activity of the material and thus, rhodium hydride Rh-H species are involved in this reaction: we detect Rh(CO)Hx species on ceria using isotopic IR measurements. These findings provide new mechanistic understanding for the catalytically active species in TWC catalysis and open up a new avenue for the synthesis of novel emissions control catalysts with 100% atom economy of ultra-expensive precious metals such as Rh.

Khivantsev, Konstantin↗

Single-Site Metal Organic Complexes on Oxide Supports for Selective Alkane Functionalization

High levels of reaction selectivity for heterogeneous catalysis are generally difficult to achieve with traditional metal nanoparticle catalysts, due to the variety of metal binding sites available. In this project, we have developed a metal-ligand coordination strategy to form transition metal single-sites on high surface area supports as heterogeneous single-site catalysts. Metal centers can be atomically dispersed in the binding pockets of organic ligands on oxide supports. The systems have to be carefully designed so that tendencies for metal cluster formation or binding to surface defect sites are overcome by the attractive coordination environment provided by the organic ligand. This was confirmed by a comprehensive set of characterization methods, including XAS, XPS, XRD, TEM, and CO adsorption. Design and tuning of metal-support and support-ligand interactions were crucial for high structural uniformity. We demonstrate that supported metal-ligand SSCs are effective, recyclable catalysts for alkene hydrosilylation reactions. Compared with commercial homogeneous catalysts, they exhibit improved yield and selectivity, less metal aggregation and side reactions, and stronger tolerance with functionalized substrates. These results give some preliminary indication that coordination with organic ligands can improve activity and selectivity in metal/oxide heterogeneous catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Role of Silica Support in Phosphoric Acid Catalyzed Production of p -Xylene from 2,5-Dimethylfuran and Ethylene

p-Xylene is a commodity chemical of industrial importance for terephthalic acid production, for which renewable sourcing from naturally abundant lignocellulosic biomass is highly desired. Previous work demonstrated that phosphoric acid stabilized on siliceous zeolite supports (e.g., P-BEA, P-SPP) exhibits high selectivity toward p-xylene (>97%) from 2,5-dimethylfuran (DMF) and ethylene. However, the effect of the support and the contribution of heterogeneous versus homogeneous phosphoric acid on the observed catalytic behavior in the solvated reaction system have not been addressed. Here, we determine the phosphoric acid catalytic activity for DMF conversion and its selectivity to p-xylene when it is supported on a silica support as well as in the absence of a support. Specifically, phosphoric acid catalysis was studied in three different scenarios: (1) phosphoric acid was added in the liquid reaction mixture in the absence of any solid support, (2) phosphoric acid was added in the liquid reaction mixture along with inert silica support including siliceous zeolite (i.e., allowing for phosphoric acid–support assembly to proceed in the reaction mixture), and (3) phosphoric acid was first impregnated on the siliceous zeolite support and then the preassembled supported phosphoric acid catalyst was added in the liquid reaction mixture. We found that the reaction rate and selectivity to p-xylene are different in the above scenarios reflecting the effect of the solid support on the catalytic performance of phosphoric acid. In scenario 1, a low concentration of phosphoric acid (1.7 mM) in the absence of any solid support exhibited high selectivity to p-xylene (80% selectivity to p-xylene at 60% conversion of DMF), which decreased with increasing acid concentration. The selectivity to p-xylene and activity of phosphoric acid significantly increased by adding a silica support into the reaction system (scenario 2). Furthermore, this improvement was attributed to phosphoric acid partial association with the surface of the silica support under the reaction conditions (in situ catalyst assembly). Phosphoric acid predeposited on siliceous zeolite supports (e.g., P-BEA, P-SPP) synthesized via impregnation prior to the reaction (scenario 3) catalyzed the reaction heterogeneously without noticeable leaching and exhibited the highest activity and selectivity to p-xylene, suggesting an important role of the silica support and the need to ensure that phosphoric acid acts as a heterogeneous catalyst in order to accomplish selective conversion of DMF to p-xylene.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Energizing Robust Sulfur/Lithium Electrochemistry via Nanoscale-Asymmetric-Size Synergism

Sluggish redox kinetics and dendrite growth perplex the fulfillment of efficient electrochemistry in lithium–sulfur (Li–S) batteries. The complicated sulfur phase transformation and sulfur/lithium diversity kinetics necessitate an all-inclusive approach in catalyst design. Herein, a compatible mediator with nanoscale-asymmetric-size configuration by integrating Co single atoms and defective CoTe 2–x (Co SA -CoTe 2–x @NHCF) is elaborately developed for regulating sulfur/lithium electrochemistry synchronously. Substantial electrochemistry and theoretical analyses reveal that CoTe 2–x exhibits higher catalytic activity in long-chain polysulfide transformation and Li 2 S decomposition, while monodispersed Co sites are more effective in boosting sulfur reduction kinetics to regulate Li 2 S deposition. Such cascade catalysis endows Co SA -CoTe 2–x @NHCF with the all-around service of “trapping-conversion-recuperation” for sulfur species during the whole redox reaction. Furthermore, it is demonstrated by in situ transmission electron microscopy that initially formed electronic-conductive Co and ionic-conductive Li 2 Te provide sufficient lithiophilic sites to regulate homogeneous Li plating and stripping with markedly suppressed dendrite growth. Consequently, by coupling the Co SA -CoTe 2–x @NHCF interlayer and Li@Co SA -CoTe 2–x @NHCF anode, the constructed Li–S full batteries deliver superior cycling stability and rate performance, and the flexible pouch cell exhibits stable cycling performance at 0.3 C. In conclusion, the gained insights into the synergistic effect of asymmetric-size structures pave the way for the integrated catalyst design in advanced Li–S systems.

36 MATERIALS SCIENCE↗