Oxidizing Role of Cu Cocatalysts in Unassisted Photocatalytic CO 2 Reduction Using p-GaN/Al 2 O 3 /Au/Cu Heterostructures
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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
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Fe-carbide/Fe-oxide-based nanocomposites synthesized as magnetic nanomaterials via laser ablation synthesis in solution (LASiS)
Magnetic nanostructured materials (MNMs) have gained prominence in materials technology developments owing to their potential biomedical applications for hyperthermia cancer treatment, and transplant organ cryopreservation. Herein, we report the facile and cost-effective synthesis of Fe-based composite MNMs, comprising both Fe@Fe 2 O 3 and Fe 3 C@C core-shell nanoparticles (NPs), via Laser Ablation Synthesis in Solution (LASiS) using Fe targets ablated under acetone and toluene. Detailed materials characterizations using electron microscopy-based imaging, diffraction studies, and spectroscopic analyses - including Raman and Mössbauer spectroscopy - relate the structure-composition properties for different Fe-oxide/carbide phases in the aforesaid MNMs to their respective magnetic responses. Specifically, we confirm the presence of ultra-small (2–10 nm) amorphous Fe-oxide NPs, as well as Fe@Fe 2 O 3 core-shell NPs (20–40 nm) in the samples synthesized by ablating Fe under acetone. In contrast, samples synthesized under toluene indicate a higher concentration of Fe 3 C@C core-shell NPs (20–40 nm) with a relatively low concentration of Fe 2 O 3 NPs (2–10 nm). Furthermore, the crystallinity of the metallic phases and carbonaceous shell coatings are systematically increased by carrying out LASiS under heated toluene (up to ~95 °C). Importantly, mössbauer spectroscopy results indicate that the elevation in toluene temperature leads to an increase in the concentrations of Fe 3 C@C NPs from ~40 % to ~53 % (at.).
36 MATERIALS SCIENCE↗
Memory-dictated dynamics of single-atom Pt on CeO2 for CO oxidation
Abstract Single atoms of platinum group metals on CeO 2 represent a potential approach to lower precious metal requirements for automobile exhaust treatment catalysts. Here we show the dynamic evolution of two types of single-atom Pt (Pt 1 ) on CeO 2 , i.e., adsorbed Pt 1 in Pt/CeO 2 and square planar Pt 1 in Pt AT CeO 2 , fabricated at 500 °C and by atom-trapping method at 800 °C, respectively. Adsorbed Pt 1 in Pt/CeO 2 is mobile with the in situ formation of few-atom Pt clusters during CO oxidation, contributing to high reactivity with near-zero reaction order in CO. In contrast, square planar Pt 1 in Pt AT CeO 2 is strongly anchored to the support during CO oxidation leading to relatively low reactivity with a positive reaction order in CO. Reduction of both Pt/CeO 2 and Pt AT CeO 2 in CO transforms Pt 1 to Pt nanoparticles. However, both catalysts retain the memory of their initial Pt 1 state after reoxidative treatments, which illustrates the importance of the initial single-atom structure in practical applications.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Conversion of Formic Acid on Single- and Nano-Crystalline Anatase TiO 2 (101)
Understanding thermochemical transformations of formic acid (FA) on metal oxide surfaces is important for many catalytical reactions. Here we study thermally induced reactions of FA on a single-crystalline and nanocrystalline anatase TiO 2 (101). We employ a combination of scanning tunneling microscopy (STM), temperature-programmed desorption (TPD), infrared reflection absorption spectroscopy (IRAS), diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), and density functional theory (DFT) to follow the FA surface intermediates and reaction products above room temperature. We find that the primary reaction products desorbing at about 300, 480, and 515 K are molecular water, carbon monoxide, and formaldehyde, respectively. Bidentate (BD) formate and bridging hydroxyl (HO b ) are identified as central intermediates in the FA transformations. Bridging oxygen vacancies (V O ) are also likely participants despite their low stability at the surface. In conclusion, the parallel studies on single crystals and faceted TiO 2 (101) nanoparticles reveal the spectroscopic commonalities of surface species and of the thermal conversion of molecular and deprotonated forms of FA.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Biosynthesis of Zinc Oxide Nanoparticles using Fungal Filtrates
Fungi produce and excrete various proteins, enzymes, and polysaccharides, which may be used for the synthesis of nanoparticles. This study investigated the effect an anion species on the synthesis of ceramic nanoparticles using fungal filtrates. In this work, ceramic zinc oxide (ZnO) nanoparticles ranging between 1 nm and 1000 nm were successfully synthesized using three different filamentous fungi: Aspergillus sp., Penicillium sp., and Paecilomyces variotti. Each fungus was cultured, and the filtrate was extracted and individually exposed to zinc nitrate, zinc sulfate, or zinc chloride. The formation of nanoparticles was characterized using UV-visible spectrophotometry (UV-Vis), fluorescence microscopy, and with transmission electron microscopy (TEM) analyses. UV-Vis spectra exhibited broad increases in the absorption across the range of 200 nm - 800 nm, which corresponded to the formation of ZnO nanoparticles under various conditions. Nanoparticle formation was confirmed with fluorescence microscopy and TEM analysis and determined to form particles with an irregular spherical shape. To date, our work demonstrates that the ability of fungi to synthesize ZnO nanoparticles is not genus/species-specific but is dependent on the starting composition of a given metal salt.
59 BASIC BIOLOGICAL SCIENCES↗
Solid State Fluorination on the Minute Scale: Synthesis of WO[subscript 3;#8722;x]F[subscript x] with Photocatalytic Activity
Abstract not provided
Lange, Martin Alexander↗
Electrocatalytic Hydrogen Evolution at Full Atomic Utilization over ITO-Supported Sub-nano-Pt n Clusters: High, Size-Dependent Activity Controlled by Fluxional Pt Hydride Species
A combination of density functional theory (DFT) and experiments with atomically size-selected Pt n clusters deposited on indium-tin oxide (ITO) electrodes was used to examine the effects of applied potential and Pt n size on the electrocatalytic activity of Pt n (n = 1, 4, 7, 8) for the hydrogen evolution reaction (HER). Activity is found to be negligible for isolated Pt atoms on ITO, increasing rapidly with Pt n size, such that Pt 7 /ITO and Pt 8 /ITO have roughly double the activity per Pt atom compared to atoms in the surface layer of polycrystalline Pt. Both DFT and experiment find that hydrogen under-potential deposition (H upd ) results in Pt n /ITO (n = 4, 7, 8) adsorbing ~2 H atoms/Pt atom at the HER threshold potential, equal to ca. double the Hupd observed for Pt bulk or nanoparticles. Here, the cluster catalysts under electrocatalytic conditions are hence best described as a Pt hydride compound, significantly departing from a metallic Pt cluster. The exception is Pt 1 /ITO, where H adsorption at the HER threshold potential is energetically unfavorable. Theory combines global optimization with grand canonical approaches for the influence of potential, uncovering that several metastable structures contribute to HER, changing with the applied potential. It is hence critical to include reactions of the ensemble of energetically accessible Pt n H x /ITO structures to correctly predict the activity vs. Pt n size and applied potential. For the small clusters, spillover of H ads from the clusters to the ITO support is significant, resulting in a competing channel for loss of H ads , particularly at slow potential scan rates.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Infiltrated electrodes for metal supported solid oxide electrolysis cells
Metal-supported solid oxide cells (MSOCs) are an alternative to conventional solid oxide cells (SOCs) based on ceramic cermets, offering lower material costs and higher operational flexibility. In this study symmetric MSOCs with infiltrated electrodes are explored for steam electrolysis operation to understand the underlying operation and degradation principles and suggest a direction for future MSOCs development. Two different fuel electrode backbones are used: an electronically-conductive lanthanum strontium co-doped iron nickel titanate (LSFNT) infiltrated with cerium-gadolinium oxide (CGO), or an ionic conductive zirconia based backbone (10ScYSZ) infiltrated with Ni:CGO. At the oxygen side, the backbone is 10ScYSZ, which is infiltrated with lanthanum-strontium co-doped cobalt oxide (LSC), or praseodymium oxide as cobalt-free alternative for comparison. This study suggests that the backbone electronic conductivity is key for good electrochemical performance as well as for boosting cell durability. Highly electronically conductive nanoparticles, especially nickel, were observed to irreversibly agglomerate driven by thermal conditions, whereas CGO proved to be a very stable electrocatalyst. At the fuel side, CGO (LSFNT) electrode showed lower ASR and degradation rate than Ni:CGO(ScYSZ) configuration with measured values of 0.50 Ω cm2 and 11 %/1000 h (at 0.60 A/cm2), and 0.70 Ω cm2 and 26 %/1000 h (at 0.50 A/cm2) at 1.30 V, respectively (700 °C, 50 % steam in hydrogen at the fuel side and air at the oxygen electrode side, LSC(ScYSZ) oxygen electrode).
25 ENERGY STORAGE↗
Pt Catalysts Modified with Manganese Oxide through Atomic Layer Deposition for CO Oxidation: Establishing a Coating Layer above or below Pt
The effect of atomic layer deposition (ALD) of manganese oxide on CO oxidation over Pt/Al2O3 is investigated. Two types of catalysts with a thin MnOx layer coated on or under the Pt nanoparticles (NPs) are prepared, and a pristine Pt/Al2O3 catalyst is used as a reference sample. The addition of the ALD layers improves the catalyst durability and both catalysts with MnOx exhibit greater stability after thermal aging at 1073-K. Besides, MnOx promotes CO oxidation through active Pt-MnOx interfacial sites, showing a reaction rate up to 35-fold faster than that of unmodified Pt. Interestingly, the CO adsorption ability of the Pt catalysts with MnOx overcoats is greatly suppressed after the high-temperature calcination; however, the reaction rate of CO oxidation is still excellent. This phenomenon is because the uniformly covered MnOx with two atomic layers diminishes the exposed Pt surface, but the reaction near the Pt-MnOx interfacial site still occurs. Our results guide the effective use of ALD, which is actively applied to heterogeneous catalysis, and provide a novel direction to control metal-assisted interactions.
36 MATERIALS SCIENCE↗
Phosphate adsorption kinetics and equilibria on natural iron and manganese oxide composites
We report that it is well known that phosphate retention in soils and sediments is strongly influenced by binding to secondary iron oxides, there have been relatively few studies examining its adsorption/desorption behavior on multicomponent particles of realistic natural complexity. In this study, natural Mn-rich limonite (LM), was used to prepare naturally complex Fe- and Mn-oxide composite materials to examine phosphate adsorption/desorption. To clarify the role of the Mn-oxides, results for the LM sample were compared to those for an acid treated version (LAT), in which the acid-extractable Mn-oxide fraction has been selectively eliminated while leaving the Fe-oxide fraction intact. The saturated adsorption capacity on LAT was almost double that on LM, suggesting that phosphate adsorption to the iron oxides is strongly occluded by the Mn-oxide fraction. This result is reinforced by the comparing the pH dependence and fits to adsorption isotherms, and by desorption experiments and STEM-EDS mapping showing that phosphate loading on Mn-oxides was limited. Hence, although the collective results confirm that phosphate uptake and strong binding is selectively controlled by the Fe-oxide fraction, our study reveals that the Mn-oxide fraction strongly interferes with this process. Therefore, phosphate uptake behavior on metal oxides cannot be predicted solely on the basis of the Fe-oxide fraction present, but instead must take into account the deleterious impacts of other intimately associated phases. For co-diagenetic Fe/Mn-oxide composites in particular, Mn-oxides appear to severely limit phosphate uptake on the Fe-oxide fraction, either by hindering access to binding sites on the Fe-oxide or by lowering their affinity for P.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Enhancing Acidic Oxygen Evolution Activity by Supporting Iridium Electrocatalysts on Tantalum Carbide
For a high-performance proton exchange membrane water electrolyzer (PEMWE), acidic oxygen evolution reaction (OER) electrocatalysts require highly dispersed iridium oxide (IrO x ) nanoparticles. Although carbon-based materials have been explored as promising supports for IrO x nanoparticles, their limited stability under harsh oxidative and acidic PEMWE conditions remains a significant challenge. Here, in this study, we report the synthesis and in situ characterization of active and durable IrOx electrocatalysts supported on electrochemically stable and electrically conducting tantalum carbide (TaC). When applied in a PEMWE, the IrO x /TaC electrocatalyst achieves a cell voltage of 1.71 V at 1.0 A cm –2 , outperforming the commercial IrO 2 catalyst (1.82 V at 1.0 A cm –2 ). Furthermore, the IrO x /TaC catalyst maintains a stable operation for 200 h at 0.5 A cm –2 with a low degradation rate of 36 μV h –1 . Density functional theory calculations further confirm that Ir–O–Ta bond formation at the IrO x /TaC interface reduces the overpotential of the OER compared to IrO 2 . This study underscores the pivotal role of supporting IrO x over stable and conducting metal carbides, providing guidance for the design of advanced acidic OER catalysts.
58 GEOSCIENCES↗
Atomic Layer Deposition for Improved Biomass Conversion Catalysts
Heterogeneous catalysts are a key enabler of the transition towards a sustainable, bio-based economy for fuels and chemicals. However, the harsh conditions in many biomass conversion processes lead to nanoparticle sintering, support collapse, and metal leaching in conventional PGM catalysts. Next-generation catalysts must be developed to address these stability challenges. This presentation will discuss ongoing work between the Catalytic Carbon Transformation and Scale-Up Center at NREL and various industrial partners to develop scalable and cost-effective atomic layer deposition (ALD) coatings for improving the performance of biomass conversion catalysts. The substantial focus will be devoted to the benefits of TiO2 ALD coatings on supported Pd hydrogenation catalysts. Ten cycles of TiO2 ALD were found to dramatically improve the activity of a conventional Pd/Al2O3 catalyst towards aromatic hydrogenation, despite partial coverage of the Pd sites by the ALD layer. Subsequent advanced characterization and atomic-scale computational modeling revealed that the ALD coating weakened the adsorption strength of hydrogenation surface intermediates, leading to higher reaction rates. Reaction testing after exposure to sulfur impurities, high temperature oxidation, and hydrothermal treatment demonstrated the improved stability of the ALD-coated catalyst. Additionally, the ALD synthesis process was found to be scalable over two orders of magnitude with minimal deviation in synthesized catalyst properties. These results were contextualized with cost models of industrial ALD coating and aromatic hydrogenation processes to further refine the value proposition of ALD coatings. Given the demonstrated improvements in hydrogenation, TiO2 ALD coatings have also been applied to supported Pt catalysts for use in other biomass conversion reactions, such as hydrodeoxygenation for the production of sustainable aviation fuel (SAF) and the oxidation of glucose to bio-derived gluconic acid.
29 ENERGY PLANNING, POLICY, AND ECONOMY↗
Atomic Layer Deposition for Improved Biomass Conversion Catalysts
Heterogeneous catalysts are a key enabler of the transition towards a sustainable, bio-based economy for fuels and chemicals. However, the harsh conditions in many biomass conversion processes lead to nanoparticle sintering, support collapse, and metal leaching in conventional PGM catalysts. Next-generation catalysts must be developed to address these stability challenges. This presentation will discuss ongoing work between the Catalytic Carbon Transformation & Scale-Up Center at NREL and various industrial partners to develop scalable, cost-effective atomic layer deposition (ALD) coatings for improving the performance of biomass conversion catalysts. Substantial focus will be devoted to the benefits of TiO2 ALD coatings on supported Pd hydrogenation catalysts. Ten cycles of TiO2 ALD were found to dramatically improve the activity of a conventional Pd/Al2O3 catalyst towards aromatic hydrogenation, despite partial coverage of the Pd sites by the ALD layer. Subsequent advanced characterization and atomic-scale computational modeling revealed that the ALD coating influenced the adsorption strength of hydrogenation surface intermediates in unexpected ways, leading to higher reaction rates. Reaction testing after exposure to sulfur impurities, high temperature oxidation, and hydrothermal treatment demonstrated the improved stability of the ALD-coated catalyst. Additionally, the ALD synthesis process was found to be scalable over two orders of magnitude with minimal deviation in synthesized catalyst properties. These results were contextualized with cost models of industrial ALD coating and aromatic hydrogenation processes to further refine the value proposition of ALD coatings. Given the demonstrated improvements in hydrogenation, TiO2 ALD coatings have also been applied to supported Pt catalysts for use in other biomass conversion reactions, such as hydrodeoxygenation for production of sustainable aviation fuel (SAF) and the oxidation of glucose for bio-derived gluconic acid. Recent findings from these experimental campaigns will also be shared. ALD technology holds great potential in the development of next-generation catalysts for biofuels and bioproducts and this work constitutes an important examination of the impact of ALD coatings in a variety of reaction environments.
bioenergy↗
Atomic Layer Deposition for Improved Biomass Conversion Catalysts
Heterogeneous catalysts are a key enabler of the transition towards a sustainable, bio-based economy for fuels and chemicals. However, the harsh conditions in many biomass conversion processes lead to nanoparticle sintering, support collapse, and metal leaching in conventional PGM catalysts. Next-generation catalysts must be developed to address these stability challenges. This presentation will discuss ongoing work between the Catalytic Carbon Transformation and Scale-Up Center at NREL and various industrial partners to develop scalable and cost-effective atomic layer deposition (ALD) coatings for improving the performance of biomass conversion catalysts. The substantial focus will be devoted to the benefits of TiO2 ALD coatings on supported Pd hydrogenation catalysts. Ten cycles of TiO2 ALD were found to dramatically improve the activity of a conventional Pd/Al2O3 catalyst towards aromatic hydrogenation, despite partial coverage of the Pd sites by the ALD layer. Subsequent advanced characterization and atomic-scale computational modeling revealed that the ALD coating weakened the adsorption strength of hydrogenation surface intermediates, leading to higher reaction rates. Reaction testing after exposure to sulfur impurities, high temperature oxidation, and hydrothermal treatment demonstrated the improved stability of the ALD-coated catalyst. Additionally, the ALD synthesis process was found to be scalable over two orders of magnitude with minimal deviation in synthesized catalyst properties. These results were contextualized with cost models of industrial ALD coating and aromatic hydrogenation processes to further refine the value proposition of ALD coatings. Given the demonstrated improvements in hydrogenation, TiO2 ALD coatings have also been applied to supported Pt catalysts for use in other biomass conversion reactions, such as hydrodeoxygenation for the production of sustainable aviation fuel (SAF) and the oxidation of glucose to bio-derived gluconic acid. Recent findings from these experimental campaigns will also be shared. ALD technology holds great potential in the development of next-generation catalysts for biofuels and bioproducts, and this work constitutes an important examination of the impact of ALD coatings in a variety of reaction environments.
atomic layer deposition↗
Alcohol-Induced Low-Temperature Blockage of Supported-Metal Catalysts for Enhanced Catalysis
The partial or complete blockage of active sites of metal nanoparticles (NPs) on supported-metal catalysts has been of interest for tuning the stability, selectivity, and rate of reactions. In this study, we show that Au-sites in Au/TiO 2 surprisingly become blocked upon treatment in common alcohols (2-propanol and methanol), with 2-propanol causing a greater extent of blockage. Nearly 95% of Au-sites are covered after treatment in 2-propanol at room temperature, followed by desorption at 150 °C. Infrared spectroscopy of CO adsorption unambiguously confirms the occurrence of this phenomenon. Electron energy loss spectroscopy (EELS), temperature-programmed desorption (TPD), Raman spectroscopy, and DFT simulations suggest that the formation of carbon deposits from 2-propanol decomposition and/or the migration of a TiO x layer over the supported NPs may be responsible for the blockage of Au-sites. Nearly full coverage of Au NPs after treatment in 2-propanol led to negligible activity for catalytic CO oxidation, whereas partial retraction of the overlayer led to enhanced activity with time-on-stream, suggesting a self-activating catalytic performance.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Integrated in situ spectroscopic studies on syngas production from partial oxidation of methane catalyzed by atomically dispersed rhodium cations on ceria
Catalytic reforming of methane to produce syngas is an important strategy for producing value-added chemicals. The conventional reforming catalyst relies on supported nickel nanoparticles. Here, in this work, we investigated singly dispersed Rh cations anchored on a CeO 2 catalyst (Rh 1 /CeO 2 ) for high activity and selectivity towards the production of syngas via partial oxidation of methane (POM) in the temperature range of 600–700 °C. The yields of H 2 and CO at 700 °C are 83% and 91%, respectively. The anchored Rh 1 atoms on CeO 2 of Rh 1 /CeO 2 are in the cationic state, and on an average each Rh 1 atom coordinates with 4–5 surface lattice oxygen atoms of CeO 2 . Compared to inert CeO 2 for POM, via the incorporation of single-atom sites, Rh 1 modifies the electronic state of oxygen atoms proximal to the Rh 1 atoms and thus triggers the catalytic activity of CeO 2 . The high activity of single-atom catalyst Rh 1 /CeO 2 suggests that the incorporation of single atoms of transition metals to the surface of a reducible oxide can modulate the electronic state of proximal anions of the oxide support toward forming an electronic state favorable for the selective formation of ideal products.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Unraveling Spatio-Temporal Chemistry Evolution in Laser Ablation Plumes and Its Relation to Initial Plasma Conditions
The chemistry evolution in a laser ablation plume depends strongly on its initial physical conditions. In this article, we investigate the impact of plasma generation conditions on the interrelated phenomena of expansion dynamics, plasma chemistry, and physical conditions. Plasmas are produced from a uranium metal target in air using nanosecond, femtosecond, and femtosecond filament-assisted laser ablation. Time-resolved two-dimensional spectral imaging was performed for evaluating the spatio-temporal evolu-tion of atoms, diatoms, polyatomic molecules, and nanoparticles in situ. Emission spectral features reveal that molecular formation occurs at early times in both femtosecond and filament ablation plumes, although with different temporal decay. In contrast, mo-lecular formation is found to occur at much later times in nanosecond plasma evolution. Spectral modeling is used to infer tem-poral behavior of plasma excitation temperature, and results highlighted that nanosecond plume temperatures decay rapidly while plumes generated by filament ablation show slowest decay. In this work, we find U atoms and UO molecules co-exist in ultrafast laser produced plasmas even at early times after plasma onset owing to favorable temperatures for molecular formation. Regardless of irradiation conditions, plume emission features showed presence of higher oxides (i.e. UxOy), although with different temporal histories. Our study provides insight into the impact of plasma generation conditions on chemistry evolution in plasmas produced from traditional focused femtosecond, nanosecond, and filament-assisted laser ablation.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
High current density electroreduction of CO 2 into formate with tin oxide nanospheres
In this study, we demonstrate three-dimensional (3D) hollow nanosphere electrocatalysts for CO 2 conversion into formate with excellent H-Cell performance and industrially-relevant current density in a 25 cm 2 membrane electrode assembly electrolyzer device. Varying calcination temperature maximized formate production via optimizing the crystallinity and particle size of the constituent SnO 2 nanoparticles. The best performing SnO 2 nanosphere catalysts contained ~ 7.5 nm nanocrystals and produced 71–81% formate Faradaic efficiency (FE) between -0.9 V and -1.3 V vs. the reversible hydrogen electrode (RHE) at a maximum formate partial current density of 73 ± 2 mA cm geo -2 at -1.3 V vs. RHE. The higher performance of nanosphere catalysts over SnO 2 nanoparticles and commercially-available catalyst could be ascribed to their initial structure providing higher electrochemical surface area and preventing extensive nanocrystal growth during CO 2 reduction. Our results are among the highest performance reported for SnO 2 electrocatalysts in aqueous H-cells. We observed an average 68 ± 8% FE over 35 h of operation with multiple on/off cycles. In situ Raman and time-dependent X-ray diffraction measurements identified metallic Sn as electrocatalytic active sites during long-term operation. Further evaluation in a 25 cm 2 electrolyzer cell demonstrated impressive performance with a sustained current density of 500 mA cm geo -2 and an average 75 ± 6% formate FE over 24 h of operation. Our results provide additional design concepts for boosting the performance of formate-producing catalysts.
36 MATERIALS SCIENCE↗