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At least 1,387 records · Page 77

Binary Atomically Dispersed Metal-Site Catalysts with Core–Shell Nanostructures for O 2 and CO 2 Reduction Reactions

Engineering atomically dispersed metal site catalysts with controlled local coordination environments and 3D nanostructures effectively improves the catalytic performance for the oxygen reduction reaction (ORR) and the carbon dioxide reduction reaction (CO 2 RR), which are critical for clean energy conversion and chemical production. Herein, an innovative approach for preparing core-shell nanostructured catalysts with different single-metal sites in the core and the shell, respectively, is developed. In particular, as the shell precursors, covalent organic polymers with a thin layered structure that is polymerized in situ and coated on a metal-doped ZIF-derived carbon core are used, followed by a controlled thermal activation. The selective combination and construction of different metal sites increase active site density in the surface layers, promote structural robustness, facilitate mass/charge transfer, and yield a possible synergy of active sites in the core and the shell. The p-FeNC(shell)@CoNC(core), consisting of a polymerized FeTPPCl-derived carbon layer (p-FeNC) on a Co-doped ZIF-derived carbon (CoNC), exhibits remarkable ORR activity and stability in acidic media along with encouraging durability in H 2 –air fuel cells. Likewise, a p-FeNC(shell)@NiNC(core) catalyst demonstrates outstanding CO 2 RR activity and stability. Hence, integrating two appropriate single-metal sites in core and shell precursors, respectively, can modulate morphological and catalytic properties for a possible synergy toward different electrocatalysis processes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

High-Throughput Microfluidics Platform for Intracellular Delivery and Sampling of Biomolecules from Live Cells

Nondestructive cell membrane permeabilization systems enable the intracellular delivery of exogenous biomolecules for cell engineering tasks as well as the temporal sampling of cytosolic contents from live cells for the analysis of dynamic processes. Here, in this paper, we report a microwell array format live-cell analysis device (LCAD) that can perform localized-electroporation induced membrane permeabilization, for cellular delivery or sampling, and directly interfaces with surface-based biosensors for analyzing the extracted contents. We demonstrate the capabilities of the LCAD via an automated high-throughput workflow for multimodal analysis of live-cell dynamics, consisting of quantitative measurements of enzyme activity using self-assembled monolayers for MALDI mass spectrometry (SAMDI) and deep-learning enhanced imaging and analysis. By combining a fabrication protocol that enables robust assembly and operation of multilayer devices with embedded gold electrodes and an automated imaging workflow, we successfully deliver functional molecules (plasmid and siRNA) into live cells at multiple time-points and track their effect on gene expression and cell morphology temporally. Furthermore, we report sampling performance enhancements, achieving saturation levels of protein tyrosine phosphatase activity measured from as few as 60 cells, and demonstrate control over the amount of sampled contents by optimization of electroporation parameters using a lumped model. Lastly, we investigate the implications of cell morphology on electroporation-induced sampling of fluorescent molecules using a deep-learning enhanced image analysis workflow.

59 BASIC BIOLOGICAL SCIENCES↗

Electrodeposited Mo x S y O z /Ni Tribological Coatings

Deposition of molybdenum disulfide (MoS 2 ) coatings using physical vapor deposition (PVD) and mechanical burnishing has been widely assessed for solid lubricants in space applications but still suffers from line-of-sight constraints on complex geometries. Here, we highlight one of the first demonstrations of electrodeposited Mo x S y O z and Mo x S y O z /Ni thin-film coatings from aqueous solutions of ammonium tetrathiomolybdate for solid lubricant applications and their remarkable ability to provide low coefficients of friction and high wear resistance. Characterization of the coating morphology shows amorphous microstructures with a high oxygen content and cracking upon drying. Even so, electrodeposited Mo x S y O z can achieve low steady-state coefficients of friction (μ ∼ 0.05–0.06) and wear rates (2.6 × 10 –7 mm 3 /(N m)) approaching those of physical vapor deposited coatings (2.3 × 10 –7 mm 3 /(N m)). Additionally, we show that adding dopants such as nickel increased the wear rate (7.5 × 10 –7 mm 3 /(N m)) and initial coefficient of friction (μ i = 0.23) due to compositional modifications such as dramatic sub-stoichiometry (S/Mo ∼ 1) and expression of a NiO x surface layer, although doping did reduce the degree of cracking upon drying.

Babuska, Tomas F.↗

Bioenergy sorghum’s deep roots: A key to sustainable biomass production on annual cropland

Abstract Bioenergy sorghum has high biomass yield potential, drought resilience, good nitrogen use efficiency, and a root system that contributes to the accumulation of soil organic carbon. In this study, field grown bioenergy sorghum root systems were analyzed during the growing season to characterize their depth, biomass, morphology, anatomy, and gene expression profiles. Bioenergy sorghum roots grew continuously during a 155‐day growing season producing ~175 nodal roots, accumulating ~7 Mg of dry biomass per hectare, and reaching >2 m deep in the soil profile. Nodal roots within 20 cm of the stem were 1–5 mm in diameter, whereas roots deeper in soil profiles were enriched in lateral roots with small diameters (~30–500 µm) enabling growth through soil macropores. In older field‐grown plants, roots with intact endodermal, vascular and inner root tissues were surrounded by degraded or aerenchyma‐filled epidermal and cortical cell layers. Transcriptome analysis of nodal, surface, and deep roots identified >2,500 differentially expressed genes involved in root growth, transport, adaptation, defense, and AMF–root interaction. Deep roots (180–240 cm) differentially expressed genes that regulate lateral root growth. Surface roots (0–20 cm) located mid‐row differentially expressed genes involved in nitrate transport, whereas ammonium transport genes were expressed in surface and deep roots and genes involved in phosphate transport were expressed in nodal, surface, and deep roots. Overall, bioenergy sorghum's long growing season enables root systems to grow deeper and accumulate more biomass than annual grain crops such as maize, attributes that could help restore annual cropland soil organic carbon levels and improve soil productivity. Deep roots active in nutrient transport are positioned to take‐up fertilizer leached deep into soil profiles mitigating potential nutrient run‐off. Bioenergy sorghum's large and deep root system is a key to sustainable production of biofuels, biopower, and bioproducts on annual cropland.

59 BASIC BIOLOGICAL SCIENCES↗

Oxygen and Proton Transport in Flooded Graphene Pores with N-Dopants and Defects

Reactant transport is an important consideration in the design of ideal electrode structures. For the oxygen reduction reaction catalyzed by Pt/C in proton exchange membrane fuel cell cathodes, O 2 and H + delivery to Pt surfaces and H 2 O transport away are required. Some Pt nanoparticles may only be accessible via micropores that are too small for ionomer molecules to enter, possibly requiring flooding for H + transport. Here, to test if these “buried” Pt particles can play a role in activity through this proposed transport mechanism, we have performed atomic-scale simulations based on reactive force field molecular dynamics with an emphasis on confinement below 20 Å. Diffusion coefficients as a function of the molar concentration and local environment have been evaluated in water domains confined in two-dimensional graphene nanochannels of various channel heights representing a morphological model for micropores in proton exchange fuel cell cathodes. Our study shows that local atomic-scale structures can strongly modify H + , O 2 , and H 2 O transport rates in flooded micropores less than 20 Å in size. We find that there is a critical crossover in diffusion behavior around the 20 Å spacing with larger pores having bulk-like diffusion properties and confinement below 20 Å monotonically decreases diffusion rates. As pore size decreases, we observe locally dispersed water regions that ultimately strand reactants from long-distance transport. These findings suggest that flooded micropores may in fact be viable transport pathways for relevant reactants and products if the pore walls on opposite sides remain separated by ≥10 Å separation. Furthermore, the confinement effect is so strong that N-doping and C-vacancy defects in the C pore wall have only a minimal impact on diffusion rates and their effects are counterintuitively more apparent at larger spacings. These findings provide valuable insight regarding cathode performance and the role “stranded” catalyst particles may play in fuel cell cathodes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Reconsidering tympanal-acoustic interactions leads to an improved model of auditory acuity in a parasitoid fly

Although most binaural organisms locate sound sources using neurological structures to amplify the sounds they hear, some animals use mechanically coupled hearing organs instead. One of these animals, the parasitoid fly Ormia ochracea (O. ochracea), has astoundingly accurate sound localization abilities. It can locate objects in the azimuthal plane with a precision of 2°, equal to that of humans, despite an intertympanal distance of only 0.5 mm, which is less than 1/100th of the wavelength of the sound emitted by the crickets that it parasitizes. O. ochracea accomplishes this feat via mechanically coupled tympana that interact with incoming acoustic pressure waves to amplify differences in the signals received at the two ears. In 1995, Miles et al developed a model of hearing mechanics in O. ochracea that represents the tympana as flat, front-facing prosternal membranes, though they lie on a convex surface at an angle from the flies' frontal and transverse planes. The model works well for incoming sound angles less than ±30° but suffers from reduced accuracy (up to 60% error) at higher angles compared to response data acquired from O. ochracea specimens. Despite this limitation, it has been the basis for bio-inspired microphone designs for decades. Here, we present critical improvements to this classic hearing model based on information from three-dimensional reconstructions of O. ochracea's tympanal organ. We identified the orientation of the tympana with respect to a frontal plane and the azimuthal angle segment between the tympana as morphological features essential to the flies' auditory acuity, and hypothesized a differentiated mechanical response to incoming sound on the ipsi- and contralateral sides that depend on these features. We incorporated spatially-varying model coefficients representing this asymmetric response, making a new quasi-two-dimensional (q2D) model. The q2D model has high accuracy (average errors of under 10%) for all incoming sound angles. This improved biomechanical model may inform the design of new microscale directional microphones and other small-scale acoustic sensor systems.

36 MATERIALS SCIENCE↗

Spontaneous and field-induced crystallographic reorientation of metal electrodeposits at battery anodes

The propensity of metal anodes of contemporary interest (e.g., Li, Al, Na, and Zn) to form non-planar, dendritic morphologies during battery charging is a fundamental barrier to achievement of full reversibility. We experimentally investigate the origins of dendritic electrodeposition of Zn, Cu, and Li in a three-electrode electrochemical cell bounded at one end by a rotating disc electrode. We find that the classical picture of ion depletion–induced growth of dendrites is valid in dilute electrolytes but is essentially irrelevant in the concentrated (≥1 M) electrolytes typically used in rechargeable batteries. Using Zn as an example, we find that ion depletion at the mass transport limit may be overcome by spontaneous reorientation of Zn crystallites from orientations parallel to the electrode surface to dominantly homeotropic orientations, which appear to facilitate contact with cations outside the depletion layer. This chemotaxis-like process causes obvious texturing and increases the porosity of metal electrodeposits.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Enhancing Cycling Stability and Capacity Retention of NMC811 Cathodes by Reengineering Interfaces via Electrochemical Fluorination

High-capacity cathodes (LiNi 0.8 Mn 0.1 Co 0.1 O 2 ) that can boost the energy density of lithium-ion batteries are promising candidates for vehicle electrification. However, several factors specific to high energy density materials entailing electrode reactions inhibit their application. Fluorination has shown a promising ability to combat the detrimental electrochemical performances of cathode materials, however, it remains difficult to achieve the desired functionality. In this work, a novel electrochemical fluorination (ECF) that demonstrates a promising electrochemical performance enhancement via stabilization of the cathode–electrolyte-interphase (CEI) by forming conformal LiF is proposed. Besides LiF surface layer formation, ECF reduces the degree of fluorination-induced Ni/Li disordering and enhances the layered structural stability as probed by X-ray diffraction. Because of the robust CEI, ECF-NMC811 cathodes deliver 203.0 mAh g -1 first discharge capacity at the current rate of C/10, with ≈98% capacity retention up to 100 cycles. Similarly, it delivers ≈180 mAh g -1 capacity at a 1 C rate with 86.4% capacity retention up to 200 cycles with average coulombic efficiency of > 99.5%. Comprehensive characterization with a multitude of probes reveals that ECF enhances the cycling stability of the electrode without altering bulk structure and morphology.

25 ENERGY STORAGE↗

Probing the Li 4 Ti 5 O 12 Interface Upon Lithium Uptake by Operando Small Angle Neutron Scattering

The formation of a solid–electrolyte interphase (SEI) on the surface of Li 4 Ti 5 O 12 (LTO) has become a highly controversial topic, with arguments for it and against it. However, prior studies supporting the formation of an SEI layer have typically suggested that a layer forms upon cycling of a cell, although the layer is probed after disassembling. In this study, cubic mesostructured LTO is synthesized with crystallite domain sizes between 3 and 4 nm and uniform pores with diameters ≤8 nm. The mean pore size is controlled between 4–8 nm through the use of a triblock amphipathic copolymer with a tunable hydrophobic block as template and by thermal treatment. The LTO morphology obtained is spherical and evolves upon heat treatment. We report these materials show excellent electrochemical performance, including high rate capability and capacity retention. The LTO material is subjected to operando small-angle neutron scattering and X-ray photoelectron spectroscopy experiments, which reveal that the highly debated SEI forms at potentials as high as 2.2 V, first as a LiF-rich layer and subsequently by the growth of a carbonaceous layer. These SEI products form first on the smaller pores before forming on the mesopores.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A perspective on single-crystal layered oxide cathodes for lithium-ion batteries

As the demand for lithium-ion batteries grows exponentially to feed the nascent electric-vehicle and grid-storage markets, the need for higher energy density and longer cycle life becomes more apparent. Increasing the nickel content in the layered-oxide cathodes has been a dominant strategy to increase energy density, but this has exacerbated the surface reactivity concerns. Furthermore, the high states of charge associated with increased capacity lead to cracking of the polycrystalline cathode particles, which exposes fresh surfaces and accelerates capacity fade. Single-crystal cathode particles with low susceptibility to cracking have recently taken on intense interest due to their remarkable cyclability. Many different approaches to single-crystal synthesis have been explored, but there has been no systematic analysis of the different techniques to date. Additionally, many reports have taken on a trial-and-error approach, ignoring well established literature on grain growth outside the battery field. This perspective reviews the literature on single-crystal cathode synthesis through the lens of classic grain growth theories, providing insight and hopefully accelerating the adoption of the promising single-crystal cathode morphology.

25 ENERGY STORAGE↗

Synthesis, Characterization, and Utilization of a Lignin-Based Adsorbent for Effective Removal of Azo Dye from Aqueous Solution

How to effectively remove toxic dyes from the industrial wastewater using a green low-cost lignocellulose-based adsorbent, such as lignin, has become a topic of great interest but remains quite challenging. In this study, cosolvent-enhanced lignocellulosic fractionation (CELF) pretreatment and Mannich reaction were combined to generate an aminated CELF lignin which is subsequently applied for removal of methylene blue and direct blue (DB) 1 dye from aqueous solution. 31P NMR was used to track the degree of amination, and an orthogonal design was applied to determine the relationship between the extent of amination and reaction parameters. The physicochemical, morphological, and thermal properties of the aminated CELF lignin were characterized to confirm the successful grafting of diethylenetriamine onto the lignin. The aminated CELF lignin proved to be an effective azo dye-adsorbent, demonstrating considerably enhanced dye decolorization, especially toward DB 1 dye (>90%). It had a maximum adsorption capacity of DB 1 dye of 502.7 mg/g, and the kinetic study suggested the adsorption process conformed to a pseudo-second-order kinetic model. The isotherm results also showed that the modified lignin-based adsorbent exhibited monolayer adsorption. The adsorbent properties were mainly attributed to the incorporated amine functionalities as well as the increased specific surface area of the aminated CELF lignin.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Local halide heterogeneity drives surface wrinkling in mixed-halide wide-bandgap perovskites

Compositional heterogeneity in wide-bandgap (1.8 - 2.1 eV) mixed-halide perovskites is a key bottleneck in the processing of high-quality solution-processed thin films and prevents their application in efficient multijunction solar cells. Notably, mixed-cation (formamidinium-methylammonium) wide-bandgap perovskite films are prone to form micrometer-scale wrinkles which can interfere with the smooth surfaces ideal for multijunction devices. Here, we study the formation dynamics of wrinkled mixed-halide perovskite films and its impact on the local composition and optoelectronic properties. We use in situ X-ray scattering during perovskite film formation to show that crystallization of bromide-rich perovskites precedes that of mixed-halide phases in wrinkled films cast using an antisolvent-based process. Using nanoscopic X­-ray fluorescence and hyperspectral photoluminescence imaging, we also demonstrate the formation of iodide- and bromide-rich phases in the wrinkled domains. This intrinsic spatial halide segregation results in an increased local bandgap variation and Urbach energy. Morphological disorder and compositional heterogeneity also aggravate the formation of sub-bandgap electronic defects, reducing photostability and accelerating light-induced segregation of iodide and bromide ions in thin films and solar cells.

36 MATERIALS SCIENCE↗

Synergistic effects of W–Ta alloys exposed to various ELM-like fusion events

Abstract Recently tungsten alloys have shown capabilities in suppressing morphological changes when exposed to harsh fusion conditions. Morphological changes due to He + and D + ions at high temperatures (1000–2000 K) can lead to easier erosion and sputtering of tungten (W) particles towards quenching the fusion plasma. This study investigated W–3Ta alloy as potential plasma facing materials (PFMs) exposed to different edge-localized mode (ELM)-like energies and ion loadings. Performance of W–3Ta has been tested as a function of ELM-like energies (0.6–1.5 GW m −2 ) and varying He + and D + ion concentrations (100% He + , 50% He + :50% D + ,10% He + :90% D + (similar ELM-like reactor condition), and 100% D + ions). Early-stage fuzz formation and surface pores were observed during 100% He + ion irradiation and mixed ion loadings but not observed during 100% D + ion loadings. Pores decreased in quantity and increased in size with increasing transient heat loading. Grain boundaries acted as trapping sites of helium and deuterium atoms during dual beam ion irradiations, as observed through increased pore size along the grain boundary. Qualitative erosion estimates were measured using witness plates. Increased erosion was observed with increasing D + ion concentration, which is attributed to D supersaturation in the near surface region affecting thermal and mechanical properties. More erosion was observed for W–3Ta samples compared to pure W, evident through large (>10 µ m) cracks on the surface, and an increase in W metal x-ray photoelectron spectroscopy peaks under similar loading conditions. The slight enhancement in erosion is attributed to the slightly decreased thermal properties, ∼10% thermal diffusivity drop, of W–3Ta at high temperatures. The damage threshold was impacted by ion loading, where distinct cracking was observed for 100% He + at a lower heat loading. This matrix study using reactor-like loading supports the need for extensive studies on future W alloy PFMs before selecting one as an alternative.

Physics↗

Understanding the morphology and chemical activity of model ZrO x /Au (111) catalysts for CO 2 hydrogenation

In this study, the growth of ZrO x on Au (111) was investigated using scanning tunneling microscopy (STM) and synchrotron-based ambient pressure X-ray photoelectron spectroscopy (AP-XPS). Nanostructures of ZrO x (x= 1,2) at the sub-monolayer (≤ 0.3 ML) level were prepared by vapor depositing Zr metal onto Au (111) followed by oxidation with O 2 or CO 2 . At low coverages of the admetal (< 0.05 ML), the formed ZrO x nanostructures were dispersed randomly on the terraces and steps of the Au(111) substrate. Strong oxide-metal interactions prevented the formation of islands of zirconia. The ZrO x nanostructures displayed a reactivity towards CO 2 and H 2 not seen for bulk zirconia. C 1 s AP-XPS results indicated that CO 2 molecules adsorbed on Zr/ZrO x /Au(111) surfaces could undergo partial decomposition on Zr (CO 2 , gas → CO gas + O ads ), or react with oxygen sites from ZrO x to yield carbonates (Zr-CO 3, ads ). Further, after exposing ZrO 2 /Au (111) surfaces to 1:3 mixtures of CO 2 :H 2 , the formation of HCOO, CO 3 , and CH 3 O was detected in AP-XP spectra. These chemical species decomposed at temperatures in the range of 400-600 K, making them possible reaction intermediates for methanol synthesis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Aqueous Polymer Modification of Cellulose Nanofibrils by Grafting‐Through a Reactive Methacrylate Group

Abstract Modifying the surface of cellulose nanofibrils (CNFs) produced by mechanical refinement with a variety of polymer functional groups in an entirely water‐based system is challenging because only surface hydroxyl groups are accessible. To address this limitation, an entirely water‐based, polymer modification scheme is developed. CNFs are functionalized with a reactive methacrylate functional group followed by subsequent grafting‐through polymerization. This modification worked with a variety of water‐soluble and water‐insoluble (meth)acrylates and (meth)acrylamides, grafting up to 45 wt% polymer on to the CNFs. The reaction conditions introducing the methacrylate functional group are adjusted to vary the degree of functionality. Soxhlet extraction of modified samples demonstrates that the reactive methacrylate group is necessary to facilitate polymer grafting. The degree of functionalization of the polymers is studied via quantitative transmission IR spectroscopy and the morphology of the resulting cellulose nanofibrils is studied via a combination of optical, scanning electron, and atomic force microscopy. High levels of polymer modification do not significantly affect the micrometer‐scale fibril morphology.

Kelly, Peter V.↗

Macroscale Control of Reactivity using 3D Printed Materials with Intrinsic Catalytic Properties

The morphology of heterogeneous catalysts can impact their performance. However, standard manufacturing methods like extrusion or pelleting offer little options for tailoring catalyst shape. Herein, stereolithographic 3D printing is used to produce catalysts with controlled topologies to enhance their performance. A series of magnetic stir-bar compartments (SBC) were 3D printed and tested as catalysts for sucrose hydrolysis. The SBC were printed using acrylic acid (AA) and 1,6-hexanediol diacrylate (HDDA) as acid sites and hydrophobic crosslinking domains, respectively. Variations in the number and tilt direction of the SBC blades produced significant changes in their apparent catalytic activities. These changes resulted from differences in the fraction of active surface effectively interacting with the reactants in solution, as revealed by computational fluid dynamics simulations. Moreover, varying HDDA:AA ratios in SBC regulated reactant-surface interactions to control catalytic activity. Overall, 3D printing catalysts enables quick performance optimization by simultaneously controlling macroscopic structure and molecular composition.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Impact of Grafting Density on the Assembly and Mechanical Properties of Self-Assembled Metal–Organic Framework Monolayers

Polymer-grafted metal–organic frameworks (MOFs) can be used to form free-standing self-assembled MOF monolayers (SAMMs). Polymer chains can be introduced onto MOF surfaces through either the ligands or metal nodes using both grafting-to and grafting-from approaches. However, controlling the grafting density of polymer-grafted MOFs has not yet been achieved, because a means to control the density of grafting sites on the MOF surface has not been developed. In this study, the grafting density of polymer-grafted UiO-66 (UiO = University of Oslo) was controlled by functionalizing a portion of the Zr(IV) secondary building units (SBUs) on a UiO-66 surface with a so-called blocking agent. The remaining sites on the UiO-66 SBUs were functionalized with polymerization initiation groups, and polymers were grown from these sites to obtain particles with variable grafting densities and chain lengths that form SAMMs at an air–water interface. Even under conditions of low grafting density, these materials retain the ability to form SAMMs and their free-standing ability. Changes in particle arrangement within the monolayers were investigated using SEM imaging, and the toughness of the monolayers was evaluated using a film-on-water (FOW) method. Furthermore, coarse-grained molecular dynamics simulations were carried out to elucidate the morphology and mechanical properties of the monolayers. Findings from both experiments and simulations indicate that the toughness of SAMMs is more heavily influenced by the chain length of the grafted polymers than by the overall polymer content in the composite.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗