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At least 109 records · Page 6

Pseudocapacitive Charge Storage in Electrochromic Transition-Metal Oxide Thin Films

Electrochromic pseudocapacitive transition-metal oxide materials, such as tungsten oxide, which combine fast response, high energy density, and optical effects, can play a significant role as energy storage materials. Here we investigate the electrochemical kinetics of thin films of tungsten oxide, which turn transparent to sky-blue color in the lithiated state due to the reduction of W 6+ to W 5+ . In this study, we investigated the charge density, charge transfer, ion diffusion, and interfacial behavior upon Li + insertion/de-insertion in WO 3 . The electrochromic thin film's pseudocapacitive and electrical double layer mechanism was differentiated based on the power-law. Faradaic diffusion-controlled process dominates over the surface capacitive behavior at scan rates below 40 mV s –1 . These films exhibit an areal charge density of around 100 mC cm –2 and a capacitance of 80 mF cm –2 , superior to most comparable electrochromic materials and supercapacitors. This work combines electrochromics and energy storage properties and provides a fundamental understanding of pseudocapacitive and electrochromic mechanisms in WO 3 .

25 ENERGY STORAGE↗

Oxygen evolution electrocatalysis using mixed metal oxides under acidic conditions: Challenges and opportunities

Shaping the energy landscape through development of more efficient electrochemical energy conversion and storage devices requires significant advancements in the catalysis of key electrochemical processes involving oxygen. This is especially the case for the oxygen evolution reaction (OER), which is largely challenged by the cost-ineffectiveness of the best performing electrocatalysts (i.e., Ru, Ir), along with their limited stability under acidic conditions. This presents a roadblock in the development of robust acid-based polymer exchange membrane electrochemical systems, currently the most advanced technologies for electrochemical energy conversion. Approaches such as dilution of Ru/Ir into flexible mixed metal oxide frameworks have been used as alternative strategies in designing robust OER electrocatalysts. Herein, we discuss the state of research in this area and detail the effect of the composition and structure of mixed metal oxides on their acidic OER activity and stability. Future directions for developing mixed metal oxide electrocatalysts suitable for acidic electrochemical environments are devised.

36 MATERIALS SCIENCE↗

Prediction of O and OH Adsorption on Transition Metal Oxide Surfaces from Bulk Descriptors

In the search for stable and active catalysts, density functional theory and machine learning (ML) based models can accelerate the screening of materials. While stability is conveniently addressed on the bulk level of computation, the modelling of catalytic activity requires expensive surface simulations. Here, in this work, we develop models for the surface adsorption energy of O and OH intermediates across a consistent and extensive dataset of pure transition metal oxide surfaces. We show that adsorption energies across metal oxidation states of +2 to +6 are well captured from the metal-oxygen bond strength extracted from the bulk level calculation. Specifically, we calculate the integrated crystal orbital Hamiltonian population (ICOHP) of the metal-oxygen bond in the bulk oxide and employ a simple normalization scheme to obtain a strong correlation with adsorption energetics. By combining our ICOHP descriptor with non DFT features in a Gaussian Process regression (GPR) model, we achieve high model accuracy with mean absolute errors of 0.166 and 0.219 eV for OH and O adsorption, respectively. By targeting the O-OH adsorption energy difference with our GPR model, we predict the the oxygen evolution reaction (OER) activity from bulk descriptors only. Furthermore, we utilize the strong correlation between the COHP and metal oxygen bond lengths to rapidly predict adsorption energetics and catalytic activity from the optimized bulk geometry. Our approach can enable an efficient search for active catalysts by eliminating the need for surface calculations in the initial screening phase.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Comprehensive Characterization of Mixed Metal Oxide Catalysts for Enhanced Catalyst Lifetime During Bio-Based C2-C6 Oxygenates to Olefins Processes (CRADA CRD-18-00728 Final Report)

Participant has developed mixed metal oxide (MMO) catalysts to selectively convert biomass-derived C2-C6 oxygenates to olefins and then hydrocarbon fuels to meet DOE 2022 fuel targets. Selective conversion ethanol to isobutylene with MMO catalysts (ZnOZrOx) requires low ethanol feeds to maintain performance. Increasing the feed results in rapid catalyst deactivation. Participant has increased catalyst stability by adding additional metal oxides. However, variations in performance based on the level and type of additive and catalytic conditions have been observed. This project will use advanced catalyst characterization methods through the ChemCatBio Advanced Catalyst Synthesis and Characterization (ACSC) project to gain insight into key catalyst features and deactivation modes with the goal of tailoring catalyst composition to improve performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Unraveling Electronic Trends in O* and OH* Surface Adsorption in the MO 2 Transition-Metal Oxide Series

Understanding the bond strength of O* and OH* intermediates to metal-oxide surfaces is key to predicting the catalytic activity in oxygen-based electrochemistry. Here, we uncover highly non-linear trends in O* and OH* adsorption energies across the 3d, 4d, and 5d series of MO 2 transition-metal (TM) oxide surfaces computed within Hubbard- U corrected density functional theory (DFT + U ). Investigating the electronic structure with crystal orbital Hamiltonian populations (COHP) of the relevant metal–oxygen bonds reveals that the spin-dependent coupling strength between metal-d and oxygen-2p atomic orbitals together with the extent of filling of bonding and anti-bonding orbitals are the primary contributors to the adsorption energy. Importantly, we show that the integrated COHP obtained purely from bulk calculations is a highly accurate descriptor for surface adsorption energetics that captures trends across the group 5–12 TM oxide series within 0.19–0.36 eV. Our results suggest a pathway to prediction of adsorption energies for an arbitrary metal–ligand catalyst system.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Nucleation and growth of molybdenum disulfide grown by thermal atomic layer deposition on metal oxides

To enable greater control over thermal atomic layer deposition (ALD) of molybdenum disulfide (MoS 2 ), here we report studies of the reactions of molybdenum hexafluoride (MoF 6 ) and hydrogen sulfide (H 2 S) with metal oxide substrates from nucleation to few-layer films. In situ quartz crystal microbalance experiments performed at 150, 200, and 250 °C revealed temperature-dependent nucleation behavior of the MoF 6 precursor, which is attributed to variations in surface hydroxyl concentration with temperature. In situ Fourier transform infrared spectroscopy coupled with ex situ x-ray photoelectron spectroscopy (XPS) indicated the presence of molybdenum oxide and molybdenum oxyfluoride species during nucleation. Density functional theory calculations additionally support the formation of these species as well as predicted metal oxide to fluoride conversion. Residual gas analysis revealed reaction by-products, and the combined experimental and computational results provided insights into proposed nucleation surface reactions. With additional ALD cycles, Fourier transform infrared spectroscopy indicated steady film growth after ~13 cycles at 200 °C. XPS revealed that higher deposition temperatures resulted in a higher fraction of MoS 2 within the films. Deposition temperature was found to play an important role in film morphology with amorphous films obtained at 200 °C and below, while layered films with vertical platelets were observed at 250 °C. Finally, these results provide an improved understanding of MoS 2 nucleation, which can guide surface preparation for the deposition of few-layer films and advance MoS 2 toward integration into device manufacturing.

36 MATERIALS SCIENCE↗

Ultrathin Amorphous Silica Membrane Enhances Proton Transfer across Solid-to-Solid Interfaces of Stacked Metal Oxide Nanolayers while Blocking Oxygen

A large jump of proton transfer rates across solid-to-solid interfaces by inserting an ultrathin amorphous silica layer into stacked metal oxide nanolayers is discovered using electrochemical impedance spectroscopy and Fourier-transform infrared reflection absorption spectroscopy (FT-IRRAS). The triple stacked nanolayers of Co 3 O 4 , SiO 2 , and TiO 2 prepared by atomic layer deposition (ALD) enable a proton flux of 2400 ± 60 s -1 nm -2 (pH 4, room temperature), while a single TiO 2 (5 nm) layer exhibits a threefold lower flux of 830 s -1 nm -2 . Based on FT-IRRAS measurements, this remarkable enhancement is proposed to originate from the sandwiched silica layer forming interfacial SiOTi and SiOCo linkages to TiO 2 and Co 3 O 4 nanolayers, respectively, with the O bridges providing fast H + hopping pathways across the solid-to-solid interfaces. Finally, together with the complete O 2 impermeability of a 2 nm ALD-grown SiO 2 layer, the high flux for proton transport across multi-stack metal oxide layers opens up the integration of incompatible catalytic environments to form functional nanoscale assemblies such as artificial photosystems for CO 2 reduction by H 2 O.

36 MATERIALS SCIENCE↗

Surface Oxygen Depletion of Layered Transition Metal Oxides in Li-Ion Batteries Studied by Operando Ambient Pressure X-ray Photoelectron Spectroscopy

A new operando spectro-electrochemical setup was developed to study oxygen depletion from the surface of layered transition metal oxide particles at high degrees of delithiation. An NCM111 working electrode was paired with a chemically delithiated LiFePO 4 counter electrode in a fuel cell-inspired membrane electrode assembly (MEA). A propylene carbonate-soaked Li-ion conducting ionomer served as an electrolyte, providing both good electrochemical performance and direct probing of the NCM111 particles during cycling by ambient pressure X-ray photoelectron spectroscopy. The irreversible emergence of an oxygen-depleted phase in the O 1s spectra of the layered oxide particles was observed upon the first delithiation to high state-of-charge, which is in excellent agreement with oxygen release analysis via mass spectrometry analysis of such MEAs. By comparing the metal oxide-based O 1s spectral features to the Ni 2p 3/2 intensity, we can calculate the transition metal-to-oxygen ratio of the metal oxide close to the particle surface, which shows good agreement with the formation of a spinel-like stoichiometry as an oxygen-depleted phase. This new setup enables a deeper understanding of interfacial changes of layered oxide-based cathode active materials for Li-ion batteries upon cycling.

25 ENERGY STORAGE↗

Data-driven approach to parameterize SCAN + U for an accurate description of 3 d transition metal oxide thermochemistry

Semilocal density-functional theory (DFT) methods exhibit significant errors for the phase diagrams of transition-metal oxides that are caused by an incorrect description of molecular oxygen and the large self-interaction error in materials with strongly localized electronic orbitals. Empirical and semiempirical corrections based on the DFT + U method can reduce these errors, but the parameterization and validation of the correction terms remains an on-going challenge. Here we develop a systematic methodology to determine the parameters and to statistically assess the results by considering interlinked thermochemical data across a set of transition metal compounds. We consider three interconnected levels of correction terms: (1) a constant oxygen binding correction, (2) Hubbard-U correction, and (3) DFT/DFT + U compatibility correction. The parameterization is expressed as a unified optimization problem. We demonstrate this approach for 3d transition metal oxides, considering a target set of binary and ternary oxides. With a total of 37 measured formation enthalpies taken from the literature, the dataset is augmented by the reaction energies of 1710 unique reactions that were derived from the formation energies by systematic enumeration. To ensure a balanced dataset across the available data, the reactions were grouped by their similarity using clustering and suitably weighted. The parameterization is validated using leave-one-out cross validation (CV), a standard technique for the validation of statistical models. We apply the methodology to the strongly constrained and appropriately normed (SCAN) density functional. Based on the CV score, the error of binary (ternary) oxide formation energies is reduced by 40% (75%) to 0.10 (0.03) eV/atom. A simplified correction scheme that does not involve SCAN/SCAN + U compatibility terms still achieves an error reduction of 30% (25%). The method and tools demonstrated here can be applied to other classes of materials or to parameterize the corrections to optimize DFT + U performance for other target physical properties.

36 MATERIALS SCIENCE↗

A machine learning approach for determining temperature-dependent bandgap of metal oxides utilizing Allen–Heine–Cardona theory and O’Donnell model parameterization

To evaluate the high temperature sensing properties of metal oxide and perovskite materials suitable for use in combustion environments, it is necessary to understand the temperature dependence of their bandgaps. Although such temperature-driven changes can be calculated via the Allen–Heine–Cardona (AHC) theory, which assesses electron–phonon coupling for the bandgap correction at given temperatures, this approach is computationally demanding. Another approach to predict bandgap temperature-dependence is the O’Donnell model, which uses analytical expressions with multiple fitting parameters that require bandgap information at 0 K. This work employs data-driven Gaussian process regression (GPR) to predict the parameters employed in the O’Donnell model from a set of physical features. We use a sample of 54 metal oxides for which density functional theory has been performed to calculate the bandgap at 0 K, and the AHC calculations have been carried out to determine the shift in the bandgap at non-zero temperatures. As the AHC calculations are impractical for high-throughput screening of materials, the developed GPR model attempts to alleviate this issue by predicting the O'Donnell parameters purely from physical features. To mitigate the reliability issues arising from the very small size of the dataset, we apply a Bayesian technique to improve the generalizability of the data-driven models as well as quantify the uncertainty associated with the predictions. The method captures well the overall trend of the O’Donnell parameters with respect to a reduced feature set obtained by transforming the available physical features. Quantifying the associated uncertainty helps us understand the reliability of the predictions of the O’Donnell parameters and, therefore, the bandgap as a function of temperature for any novel material.

36 MATERIALS SCIENCE↗

Multiphase layered transition metal oxide positive electrodes for sodium ion batteries

Abstract Multiphase layered transition metal oxides (LTMOs) for sodium ion battery (SIB) positive electrodes with phase interfaces across multiple length scales are a promising avenue toward practical, high‐performance SIBs. Combinations of phases can complement each other's strengths and mitigate their weaknesses if their interfaces are carefully controlled. Intra‐ and interparticle phase interactions from nanoscale to macroscale must be carefully tuned to generate distinct effects on properties and performance. An informed design strategy must be paired with relevant synthesis techniques and complemented by spatially resolved characterization tools to manipulate different length scales and interfaces. This review examines the design, synthesis, and characterization strategies that have been demonstrated for the preparation of heterogeneous, multiphasic LTMOs with phase interfaces across varied length scales.

25 ENERGY STORAGE↗

Photoelectron Spectroscopic Determination of the Interfacial Energetics of Metal Oxide Protection Layers on p-InP Photocathodes

The interfacial energetics between p-type InP and a series of metal oxides, including TiO 2 , Nb 2 O 5 , Ta 2 O 5 , and HfO 2 , were evaluated using X-ray photoelectron spectroscopy (XPS), ultraviolet photoelectron spectroscopy (UPS), and optical absorption spectroscopy. The energy of the conduction-band minimum ( E cb ) of TiO 2 and Nb 2 O 5 was more negative (i.e., further from the vacuum level) than the conduction-band minimum at the surface of InP ( E cb,s ), whereas E cb for Ta 2 O 5 and HfO 2 was more positive than E cb,s for InP. The data are consistent with the electrochemical behavior of p-InP coated with various metal oxide candidate protection layers, with TiO 2 and Nb 2 O 5 facilitating interfacial transfer of photogenerated minority-carrier electrons in p-InP photocathodes, and Ta 2 O 5 and HfO 2 blocking photogenerated electrons in p-InP from readily transferring across the oxide-coated photocathodes. The energy of the valence-band maximum ( E vb ) for all of the oxides was much more negative than E vb,s for InP, consistent with observations that these protection layers effectively block hole transport and consequently suppress oxidative degradation of the underlying p-InP photocathodes.

63 RADIATION, THERMAL, AND OTHER ENVIRON. POLLUTAN↗

Controlling Heterogeneous Catalysis with Organic Monolayers on Metal Oxides

A key theme of heterogeneous catalysis research is achieving control of the environment surrounding the active site to precisely steer the reactivity toward desired reaction products. One method toward this goal has been the use of organic ligands or self-assembled monolayers (SAMs) on metal nanoparticles. Metal-bound SAMs are typically employed to improve catalyst selectivity but often decrease the reaction rate as a result of site blocking from the ligands. Recently, the use of metal oxide-bound organic modifiers such as organophosphonic acid (PA) SAMs has shown promise as an additional method for tuning reactions on metal oxide surfaces as well as modifying oxide-supported metal catalysts. In this Account, we summarize recent approaches to enhance catalyst performance with oxide-bound monolayers. These approaches include (1) modification of metal oxide catalysts to tune surface reactions, (2) formation of SAMs on the oxide component of supported metal catalysts to modify sites at the metal–support interface, and (3) enhancement of catalyst performance (e.g., stability) through modification of sites remote from the active sites. Further, both the headgroups and organic tail groups of PA SAMs or other ligands can influence reactions on metal oxide surfaces. Binding of the headgroup can selectively poison certain active sites, altering the selectivity in a manner analogous to metal-bound ligands (at the expense of active site quantity). Moreover, tail groups can be functionalized to interact favorably with reactants and intermediates, for instance through dipole–dipole interactions. On supported metal catalysts like Pt/Al 2 O 3 , PA SAMs can selectively form on the oxide support. This selective deposition allows for modification of the metal–support interface with minimal blockage of metal sites. PA headgroups were shown to provide tunable acid sites at the interface, dramatically improving hydrodeoxygenation rates of various alcohols. Additionally, organic tail functionality was used to activate or stabilize specific reactants at the interface, such as with the use of amine-functionalized PAs to stabilize chemisorption of CO 2 during the reverse water gas shift reaction. PAs have also been found to affect the electronic properties of bulk metal sites through long-range electron withdrawal via the oxide, providing an additional avenue to tune catalytic behavior. Finally, organic modifiers were shown to enhance catalytic performance without directly modifying the active site. For instance, in biphasic liquid environments the modification of catalyst particles with hydrophobic or hydrophilic SAMs shifts the selectivity of multipath reactions on the basis of the hydrophobicities of different intermediates and products. As another “long-range” effect, the deposition of ligands on oxide supports improved catalyst stability through both improved resistance to sintering and suppression of active site poisoning. The recent contributions discussed in this Account demonstrate the versatility and significant potential for the approach of modifying catalysts with oxide-bound organic monolayers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Deciphering phase evolution in complex metal oxide thin films via high-throughput materials synthesis and characterization

Discovery of structure-property relationships in thin film alloys of complex metal oxides enabled by high-throughput materials synthesis and characterization facilities is demonstrated here with a case-study. In this study, thin films of binary transition metal oxides (Ti–Zn) are prepared by pulsed laser deposition with continuously varying Ti:Zn ratio, creating combinatorial samples for exploration of the properties of this material family. The atomic structure and electronic properties are probed by spatially resolved techniques including x-ray absorption near edge structures (XANES) and x-ray fluorescence (XRF) at the Ti and Zn K-edge, x-ray diffraction, and spectroscopic ellipsometry. The observed properties as a function of Ti:Zn ratio are resolved into mixtures of five distinguishable phases by deploying multivariate curve resolution analysis on the XANES spectral series, under constraints set by results from the other characterization techniques. First-principles computations based on density function theory connect the observed properties of each distinct phase with structural and spectral characteristics of crystalline polymorphs of Ti–Zn oxide. Continuous tuning of the optical absorption edge as a function of Ti:Zn ratio, including the unusual observation of negative optical bowing, exemplifies a functional property of the film correlated to the phase evolution.

36 MATERIALS SCIENCE↗

Single-Atom Metal Oxide Sites as Traps for Charge Separation in the Zirconium-Based Metal–Organic Framework NDC–NU-1000

Solvothermal deposition in metal–organic frameworks (MOFs) can be utilized to mount single-metal-atom catalytic species at chemically reactive sites on hexa-Zr(IV)-oxy(oxo,hydroxo,aqua) nodes in nanoscale crystallites of the MOF NDC-NU-1000 in a self-limiting fashion. Upon photoexcitation of the 1,3,6,8-tetrakis( p -benzoato)pyrene chromophores of the parent framework, charge transfer may occur between the chromophores and the installed heterometal sites. Extended X-ray absorption fine structure studies revealed the single-atom nature of the installed species. A combination of steady-state and ultrafast optical spectroscopy was utilized to uncover evidence of a charge-separated (CS) state arising in the metalated samples. The relevant dynamics were characterized with transient photoluminescence and femtosecond transient absorption spectroscopy. Here, we find that a titanium-oxy single atom site gives rise to the longest-lived CS species compared to cobalt and nickel in a similar arrangement. This study provides guidance in designing MOF-based catalytic systems for photocatalysis and solar-fuel production.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Intrinsic Kinetic Limitations in Substituted Lithium-Layered Transition-Metal Oxide Electrodes

Substituted Li-layered transition-metal oxide (LTMO) electrodes such as Li x Ni y Mn z Co 1-y-z O 2 (NMC) and Li x Ni y Co 1-y-z Al z O 2 (NCA) show reduced first cycle Coulombic efficiency (90-87% under standard cycling conditions) in comparison with the archetypal Li x CoO 2 (LCO; similar to 98% efficiency). Focusing on Li x Ni 0.8 Co 0.15 Al 0.0.5 O 2 as a model compound, we use operando synchrotron X-ray diffraction (XRD) and nuclear magnetic resonance (NMR) spectroscopy to demonstrate that the apparent first-cycle capacity loss is a kinetic effect linked to limited Li mobility at x > 0.88, with near full capacity recovered during a potentiostatic hold following the galvanostatic charge- discharge cycle. This kinetic capacity loss, unlike many capacity losses in LTMOs, is independent of the cutoff voltage during delithiation and it is a reversible process. The kinetic limitation manifests not only as the kinetic capacity loss during discharge but as a subtle bimodal compositional distribution early in charge and, also, a dramatic increase of the charge-discharge voltage hysteresis at x > 0.88. 7 Li NMR measurements indicate that the kinetic limitation reflects limited Li transport at x > 0.86. Electrochemical measurements on a wider range of LTMOs including Li x (Ni,Fe) y Co 1-y O 2 suggest that 5% substitution is sufficient to induce the kinetic limitation and that the effect is not limited to Ni substitution. In this paper, we outline how, in addition to a reduction in the number of Li vacancies and shrinkage of the Li-layer size, the intrinsic charge storage mechanism (two-phase vs solid-solution) and localization of charge give rise to additional kinetic barriers in NCA and nonmetallic LTMOs in general.

25 ENERGY STORAGE↗

In Situ Optical Quantification of Extracellular Electron Transfer Using Plasmonic Metal Oxide Nanocrystals**

Extracellular electron transfer (EET) is a critical form of microbial metabolism that enables respiration on a variety of inorganic substrates, including metal oxides. However, quantifying current generated by electroactive bacteria has been predominately limited to biofilms formed on electrodes. To address this, we developed a platform for quantifying EET flux from cell suspensions using aqueous dispersions of infrared plasmonic tin-doped indium oxide nanocrystals. Furthermore, tracking the change in optical extinction during electron transfer enabled quantification of current generated by planktonic Shewanella oneidensis cultures. Using this method, we differentiated between starved and actively respiring cells, cells of varying genotype, and cells engineered to differentially express a key EET gene using an inducible genetic circuit. Overall, our results validate the utility of colloidally stable plasmonic metal oxide nanocrystals as quantitative biosensors in aqueous environments and contribute to a fundamental understanding of planktonic S. oneidensis electrophysiology using simple in situ spectroscopy.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Nano-layer deposition of metal oxides via a condensed water film

Abstract Nanocoatings on solids can be achieved by various processes, including sol-gel and atomic layer deposition. However, challenges remain for achieving uniform nanocoatings on nanoscale substrates at a large scale. Here, we report a versatile and fundamentally different technique, termed condensed layer deposition, for depositing conformal metal oxide nanocoatings on nanoparticles and nanofibers. This approach involves water in liquid hydrocarbons condensing as a nanoscale water film on the substrate surface, enabled by interfacial tension between polar water and nonpolar liquid hydrocarbons. Chemical precursors are then added, which react with the condensed water film to form a metal oxide nanocoating. We demonstrate this for titania, alumina, and niobia on substrates including carbon nanotubes, iron oxide particles and carbon black. Condensed layer deposition can achieve oxide nanocoatings on a variety of substrates with tunable thickness, in one pass, at room temperature.

36 MATERIALS SCIENCE↗