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At least 883 records · Page 49

A crossed molecular beams and computational study on the unusual reactivity of banana bonds of cyclopropane (c-C 3 H 6 ; X 1 A$^{'}_{1}$ ) through insertion by ground state carbon atoms (C( 3 P j ))

The mechanism and chemical dynamics of the reaction of ground electronic state atomic carbon C( 3 P j ) with cyclopropane c-C 3 H 6 (X 1 A$^{'}_{1}$) have been explored by combining crossed molecular beams experiments with electronic structure calculations of the pertinent triplet C 4 H 6 potential energy surface and statistical computations of product branching ratios under single-collision conditions. The experimental findings suggest that the reaction proceeds via indirect scattering dynamics through triplet C 4 H 6 reaction intermediate(s) leading to C 4 H 5 product(s) plus atomic hydrogen via a tight exit transition state, with the overall reaction exoergicity evaluated as 231 ± 52 kJ mol –1 . The calculations indicate that C( 3 P j ) can easily insert into one of the three equivalent C–C ‘banana’ bonds of cyclopropane overcoming a low barrier of only 2 kJ mol –1 following the formation of a van der Waals reactant complex stabilized by 15 kJ mol –1 . The carbon atom insertion into one of the six C–H bonds is also feasible via a slightly higher barrier of 5 kJ mol –1 . Here, these results highlight an unusual reactivity of cyclopropane's banana C–C bonds, which behave more like unsaturated C–C bonds with a π-character than saturated σ C–C bonds, which are known to be generally unreactive toward the ground electronic state atomic carbon such as in ethane (C 2 H 6 ). The statistical theory predicts the overall product branching ratios at the experimental collision energy as 50% for 1-butyn-4-yl, 33% for 1,3-butadien-2-yl, i-C 4 H 5 , and 11% for 1,3-butadien-1-yl, n-C 4 H 5 , with i-C 4 H 5 (230 kJ mol –1 below the reactants) favored by the C–C insertion providing the best match with the experimentally observed reaction exoergicity. The C( 3 P j ) + c-C 3 H 6 reaction is predicted to be a source of C 4 H 5 radicals under the conditions where its low entrance barriers can be overcome, such as in planetary atmospheres or in circumstellar envelopes but not in cold molecular clouds. Both i- and n-C 4 H 5 can further react with acetylene eventually producing the first aromatic ring and hence, the reaction of the atomic carbon with c-C 3 H 6 can be considered as an initial step toward the formation of benzene.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Interlayer spacing in pillared and grafted MCM-22 type silicas: density functional theory analysis versus experiment

Pillaring of synthetic layered crystalline silicates and aluminosilicates provides a strategy to enhance their adsorption and separation performance, and can facilitate the understanding of such behavior in more complex natural clays. In this study, we perform the first-principles density functional theory calculations for the pillaring of the pure silica polymorph of an MCM-22 type molecular sieve. Starting with a precursor material MCM-22P with fully hydroxylated layers, a pillaring agent, (EtO) 3 SiR, can react with hydroxyl groups (–OH) on adjacent internal surfaces, 2(–OH) + (EtO) 3 SiR + H 2 O → (–O) 2 SiOHR + 3EtOH, to form a pillar bridging these surfaces, or with a single hydroxyl, –OH + (EtO) 3 SiR + 2H 2 O → (–O)Si(OH) 2 R + 3EtOH, grafting to one surface. For computational efficiency, we replace the experimental organic ligand, R, by a methyl group. We find that the interlayer spacing in MCM-22 is reduced by 2.66 Å relative to weakly bound layers in the precursor MCM-22P. Including (–O) 2 SiR bridges for 50% (100%) of the hydroxyl sites in MCM-22P increases the interlayer spacing relative to MCM-22 by 2.52 Å (2.46 Å). For comparison, we also analyze the system where all –OH groups in MCM-22P are replaced by non-bridging grafted (–O)Si(OH) 2 R which results in a smaller interlayer spacing expansion of 2.17 Å relative to MCM-22. Our results for the interlayer spacing in the pillared materials are compatible with experimental observations for a similar MCM-22 type material with low Al content (Si : Al = 51 : 1) of an expansion relative to MCM-22 of roughly 2.8 Å and 2.5 Å from our x-ray diffraction and scanning transmission electron microscopy analyses, respectively. The latter analysis reveals significant variation in individual layer spacings.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The coordination chemistry of oxide and nanocarbon materials

Understanding how a ligand affects the steric and electronic properties of a metal is the cornerstone of the inorganic chemistry enterprise. What happens when the ligand is an extended surface? This question is central to the design and implementation of state-of-the-art functional materials containing transition metals. Here, this perspective will describe how these two very different sets of extended surfaces can form well-defined coordination complexes with metals. In the Green formalism, functionalities on oxide surfaces react with inorganics to form species that contain X-type or LX-type interactions between the metal and the oxide. Carbon surfaces are neutral L-type ligands; this perspective focuses on carbons that donate six electrons to a metal. The nature of this interaction depends on the curvature, and thereby orbital overlap, between the metal and the extended π-system from the nanocarbon.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Probing borafluorene B–C bond insertion with gold acetylide and azide

In this study, the reaction of Ph 3 PAuN 3 with 9-Ph-9-borafluorene resulted in complexation of the azide to boron while a gold acetylide reacted with 9-Ph-9-borafluorene to insert the acetylide carbon to access a six-membered boracycle with an exocyclic double bond.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The mechanism for acetate formation in electrochemical CO (2) reduction on Cu: selectivity with potential, pH, and nanostructuring

Nanostructured Cu catalysts have increased the selectivities and geometric activities for high value C–C coupled (C 2 ) products (ethylene, ethanol, and acetate) in the electrochemical CO (2) reduction reaction (CO (2) RR). The selectivity among the high-value C 2 products is also altered, where for instance the yield of acetate increases with alkalinity and is dependent on the catalyst morphology. The reaction mechanisms behind the selectivity towards acetate vs. other C 2 products remain controversial. In this work, we elucidate the reaction mechanism for acetate formation by using ab initio simulations, a coupled kinetic-transport model, and loading dependent experiments. We find that trends in acetate selectivity can be rationalized from variations in electrolyte pH and the local mass transport properties of the catalyst and not from changes in Cu's intrinsic activity. The selectivity mechanism originates from the transport of ketene, a stable (closed shell) intermediate, away from the catalyst surface into solution where it reacts to form acetate. While this type of mechanism has not yet been discussed in the CO (2) RR, variants of it may explain similar selectivity fluctuations observed for other stable intermediates like CO and acetaldehyde. Our proposed mechanism suggests that acetate selectivity increases with increasing pH, decreasing catalyst roughness and significantly varies with the applied potential.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Metal (hydr)oxide surface precipitates and their effects on potassium sorption

Surface precipitation has been shown to occur on rapid time scales in clay and metal oxide mineral systems. The formation of surface precipitates is hypothesized to present new potential sorption sites for potassium (K), where K can become incorporated into newly formed interlayer spaces (e.g., between tetrahedral–octahedral–tetrahedral stacked sheets). The objective of this study is to determine the effects of newly formed mineral surface precipitates on K sorption. Potassium adsorption experiments were conducted by utilizing Al 2 O 3 and SiO 2 sorbents in the presence of various cations (magnesium, zinc, and nickel) that helped to catalyze the formation of surface precipitates. Dissolved concentrations of elements were monitored via inductively coupled plasma optical emission spectrometry (ICP-OES). Solids were characterized via X-ray diffraction (XRD), and K surface complexation was analyzed via X-ray absorption near edge structure (XANES) spectroscopy. X-ray diffraction analysis indicated bayerite, layered double hydroxides (LDH), and silicated LDH were formed as reaction products, thus creating new surface sites for potential K adsorption. The presence of Si increased K adsorption perhaps due to its role in the formation of LDH surface precipitates. When the differences between observed and theoretical surface area normalized K sorption densities were averaged, a 31% increase in K adsorption was observed in the presence of Si. XANES analysis indicated that the binding mechanism of K to Si is different than that of K to Al, perhaps due to the presence of inner-sphere complexation of K to Al-oxide. Samples reacted for one month versus one week yielded more intense XANES post-edge peaks which indicated that the K sorption complex changes over time. Altogether, our findings provide novel insights into the mechanisms of K fixation in soil and has high implication in providing improved K fertilizer recommendation to growers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Molecular speciation controls arsenic and lead bioaccessibility in fugitive dusts from sulfidic mine tailings

Communities nearby mine wastes in arid and semi-arid regions are potentially exposed to high concentrations of toxic metal(loid)s from fugitive dusts deriving from impoundments. To assess the relation between potentially lofted particles and human health risk, we studied the relationship between pharmacokinetic bioaccessibility and metal(loid) molecular speciation for mine tailings dust particulate matter (PM), with elevated levels of arsenic and lead (up to 59 and 34 mmol kg -1 , respectively), by coupling in vitro bioassay (IVBA) with X-ray absorption spectroscopy (XAS). Mine tailing efflorescent salts (PM ES ) and PM from the surface crust (0–1 cm, PM SC ) and near surface (0–25 cm) were isolated to <10 μm and <150 μm effective spherical diameter (PM 10 and PM 150 ) and reacted with synthetic gastric and lung fluid for 30 s to 100 h to investigate toxic metal(loid) release kinetics. Bioaccessible (BAc) fractions of arsenic and lead were about 10 and 100 times greater in gastric than in lung fluid simulant, respectively, and 10–100% of the maximum gastric BAc from PM 10 and PM 150 occurred within 30 s, with parabolic dissolution of fine, highly-reactive particles followed by slower release from less soluble sources. Evaporite salts were almost completely solubilized in gastric-fluid simulants. Arsenate within jarosite and sorbed to ferrihydrite, and lead from anglesite, were identified by XAS as the principal contaminant sources in the near surface tailings. In the synthetic lung fluid, arsenic was released continuously to 100 h, suggesting that residence time in vivo must be considered for risk determination. Analysis of pre- and post-IVBA PM indicated the release of arsenic in lung fluid was principally from arsenic-substituted jarosite, whereas in synthetic gastric fluid arsenic complexed on ferrihydrite surfaces was preferentially released and subsequently repartitioned to jarosite-like coordination at extended exposures. Lead dissolved at 30 s was subsequently repartitioned back to the solid phase as pyromorphite in phosphate rich lung fluid. The bioaccessibility of lead in surface tailings PM was limited due to robust sequestration in plumbojarosite. Kinetic release of toxic elements in both synthetic biofluids indicated that a single IVBA interval may not adequately describe release dynamics.

63 RADIATION, THERMAL, AND OTHER ENVIRON. POLLUTAN↗

Nanoconfinement matters in humidified CO 2 interaction with metal silicates

With enigmatic observations of enhanced reactivity of wet CO 2 -rich fluids with metal silicates, the mechanistic understanding of molecular processes governing carbonation proves critical in designing secure geological carbon sequestration and economical carbonated concrete technologies. Here, we use the first principle and classical molecular simulations to probe the impact of nanoconfinement on physicochemical processes at the rock–water–CO 2 interface. We choose nanoporous calcium–silicate–hydrate (C–S–H) and forsterite (Mg 2 SiO 4 ) as model metal silicate surfaces that are of significance in cement chemistry and geochemistry communities, respectively. We show that while a nanometer-thick interfacial water film persists at unsaturated conditions consistent with in situ infrared spectroscopy, the phase behavior of the water–CO 2 mixture changes from its bulk counterpart depending on the surface chemistry and nanoconfinement. We also observe enhanced solubility at the interface of water and CO 2 phases, which could amplify the CO 2 speciation rate. Additionally, through free energy calculations, we show that CO 2 could be found in a metastable state near the C–S–H surface, which can potentially react with surface water and hydroxyl groups to form carbonic acid and bicarbonate. These findings support the explicit consideration of nanoconfinement effects in reactive and non-reactive pore-scale processes.

54 ENVIRONMENTAL SCIENCES↗

Dissociation-induced depletion of high-energy reactant molecules as a mechanism for pressure-dependent rate constants for bimolecular reactions

In 1922, Lindemann proposed the now-well-known mechanism for pressure-dependent rate constants for unimolecular reactions: reactant molecules with sufficiently high energies dissociate more quickly than collisions can reestablish the Boltzmann distribution of the internal energies of the molecule during its dissociation at low pressures – yielding pressure-dependent rate constants for unimolecular reactions due to the preferential depletion of the high energy states capable of dissociation. In the last century, incredible progress has been made in achieving a far greater understanding of and quantitative predictions for unimolecular and association reactions. In the modern era, pressure-dependent phenomenological rate constants are now nearly universally used to describe the rates of unimolecular and associative reactions in phenomenological kinetic modeling. However, there is a second, more indirect, implication of Lindemann’s mechanism that relates to how these dissociation-induced non-equilibrium distributions impact bimolecular reactions, including non-associative bimolecular reactions – which are generally not considered to have pressure-dependent rate constants. Yet, as we show herein, the same high energy states depleted due to dissociation would otherwise react most rapidly in high-activation-energy bimolecular reactions – yielding a mechanism for pressure-dependent rate constants for bimolecular reactions (including non-associative reactions). Here, we present results from a case study for CH 2 O dissociation, isomerization, and bimolecular reaction with O2 to explore this question. Results from our master equation calculations indicate that the effect of dissociation-induced non-equilibrium distributions on bimolecular reactions can be substantial – even when chemical timescales are well separated from internal energy relaxational timescales (i.e. when the traditional rate constant description would be thought to apply). This effect is found to be more pronounced – and more complex – for bimolecular reactions involving molecular entities whose chemical timescales are merged with the internal energy relaxational timescales. Lastly, we present some ideas for discussion regarding what should be considered as “chemical species” in phenomenological kinetic models.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

How additives for tin halide perovskites influence the Sn 4+ concentration

Tin halide perovskite (Sn-HPs) photovoltaics could potentially equal or exceed the performance of their more toxic Pb-based analogues if defect state densities, particularly originating from the presence of Sn 4+ , can be significantly decreased. Numerous additives are incorporated into Sn-HPs to minimize the amount of Sn 4+ , including SnF 2 , reducing agents such as hydrazine derivatives, and various antioxidants. However, despite the frequent use of additives to reduce Sn 4+ content, there is limited understanding of how they function and consequently limited guidance for the development of new additives. Herein, we use cyclic voltammetry to probe the redox behavior of SnI 2 , SnI 4 , Sn-HP precursor solutions, and 18 different additives. Through 119 Sn NMR measurements we show that hydrochloride containing additives undergo halide exchange with SnI 4 to form SnI x Cl y , which results in decreased Sn 4+ concentrations and less p-type character in the Sn-HP films. We find that the most effective additive at lowering the Sn 4+ content in FASnI 3 is not capable of reducing SnI 4 or forming SnI x Cl y , but rather it acts as a sacrificial and coordinating antioxidant. In general, when selecting additives for Sn-HPs it is important to account for the redox potential, coordination with Sn species, ability to react with oxygen, and the potential for halide exchange.

36 MATERIALS SCIENCE↗

Optical detection of alcohols with a Cu($\tiny{I}$)HETPHEN complex by reversible aldehyde to hemiacetal conversion

A heteroleptic copper(I) bis(phenanthroline) complex with aldehyde groups at the 4,7 positions of the phenanthroline ligand was synthesized. Here, the complex is responsive to alcohol, resulting in a distinct colour change caused by the facile reaction of the aldehyde group with alcohol, forming a hemiacetal product. The aldehyde species can be regenerated after heating the intermediate at 80 °C for 10 minutes, demonstrating the reusability of the complex for alcohol detection. This work presents a new strategy for applying transition metal complexes in small molecule sensing by installing functional groups in the secondary coordination sphere which reversibly react with analytes.

36 MATERIALS SCIENCE↗

Reducing delamination of an electron-transporting polymer from a metal oxide for electrochemical applications

Delamination of the electron-transporting polymer N2200 from indium tin oxide (ITO) in aqueous electrolytes is mitigated by modifying ITO with an azide-functionalized phosphonic acid (PA) which, upon UV irradiation, reacts with the polymer. Here, the optical, electrochemical, and spectroelectrochemical properties of N2200 thin films are retained in aqueous and non-aqueous media.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

XANES analysis of phosphate glasses melted with Tb 4 O 7 and SnO: evaluating the impact of valence states on structural, thermal, and luminescent properties

Barium phosphate glasses were prepared with 0.5 mol% Tb 4 O 7 added alongside SnO up to 5 mol% with the purpose of evaluating the resulting terbium and tin oxidation states and their impact on glass structural, thermal, and luminescent properties. In this work, following material synthesis by melt-quenching, the composition-structure–property investigation was pursued encompassing measurements by X-ray diffraction (XRD), X-ray absorption near-edge spectroscopy (XANES), Raman spectroscopy, differential scanning calorimetry (DSC), dilatometry, and photoluminescence (PL) spectroscopy. While XRD confirmed the amorphous nature of the glasses, results from XANES indicated that terbium occurs as terbium(III) with a predisposition for tin to exist as tin(IV) which decreased at high SnO content. The structural as well as the thermal properties appeared to be mostly impacted by the presence of tin(IV). Specifically, glass depolymerization was indicated to be induced by Sn 4+ ions, and their concentration was observed to correlate with glass transition and softening temperatures. On the other hand, the tin(II) remnants were observed to exert an impact on the luminescent properties shifting light emission from the green towards the blue-green (cyan). It is indicated that Tb 4 O 7 reacting to produce Tb 2 O 3 supports the oxidation of tin(II) to tin(IV) which in turn dominates the physical properties. However, this was somewhat circumvented at the highest SnO content wherein tin(IV) appeared to be lower.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Trimethyltriazacyclohexane coordination chemistry of simple rare-earth metal salts

Reactions of 1,3,5-trimethyl-triazacyclohexane (Me 3 tach) with common rare-earth metal iodide, chloride, and triflate salts were examined to determine the capacity of this inexpensive chelate to provide alternative precursors for THF-free reactions. The reaction of LaI 3 (THF) 4 and CeI 3 (THF) 4 with 1,3,5-trimethyl-triazacyclohexane in THF generated toluene soluble (Me 3 tach) 2 LnI 3 , 1-Ln , in which the Ln center has a tri-capped trigonal prismatic geometry with two eclipsed Me 3 tach rings. Reaction with NdI 3 (THF) 3.5 forms the analogous 1-Nd , but a different structure with one outer sphere iodide, [(Me 3 tach) 2 NdI 2 ][I], 2-Nd , is also accessible and has a structure reminiscent of bent metallocenes. The reaction of LaCl 3 and Me 3 tach forms the less soluble (Me 3 tach) 2 LaCl 3 , which has a structure analogous to 1-Ln with eclipsed Me 3 tach rings. The mono-ring yttrium complex, (Me 3 tach)YCl 3 (THF) 2 , could be isolated from the reaction of YCl 3 with Me 3 tach. Reactions of La(OTf) 3 with Me 3 tach were sensitive to the presence of residual proton sources as exemplified by the isolation of {[(Me 3 tach)La(μ-OH)(μ-OTf)] 2 (μ-OTf) 2 } 2 , 5-La , and [HMe 3 tach][(Me 3 tach) 2 La-(OTf) 4 ], 6-La . SmI 2 reacts with Me 3 tach to produce the Sm( II ) complex, (Me 3 tach) 2 SmI 2 (THF), 7-Sm , but 2-Sm can also form in this reaction. Complexes of the larger 1,4,7-trimethyltriazacyclononane (Me 3 tacn) ligand, namely (Me 3 tacn)LaI 3 (THF), (Me 3 tacn)YCl 3 , and (Me 3 tacn)SmI 2 (THF) were synthesized for comparison. Several examples of the protonated ligands with simple counteranions, [HMe 3 tach][X] (X = Cl, Br, I) and [HMe 3 tacn][OTf], were identified in the course of these studies.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Formation and transformation of iron oxy-hydroxide precursor clusters to ferrihydrite

Iron (Fe) oxy-hydroxide minerals such as ferrihydrite (Fh) are ubiquitous in Earth-surface environments and important in biogeochemical element cycling. Recent research has suggested that their formation is preceded by the precipitation of ultrasmall (~1 nm) Keggin-like Fe oxy-hydroxide clusters. However, relatively little is understood about the structure of the precursor clusters and the impacts of pH and time on their growth and transformation to more stable phases. Here, we used a new method that involves mixed flow reactors (MFR) to synthesize these Fe oxy-hydroxide precursor clusters at pH 1.0, 1.5, 2.5, and 4.5. In situ and ex situ synchrotron scattering measurements and laboratory small-angle X-ray scattering (SAXS) were used to study the structure and size of Fe oxy-hydroxide clusters and their transformation products, respectively. Results show that with increasing pH, the particle size and structural order of samples increase, forming solids that resemble 2-line Fh at pH 4.5. The experimental data were compared with X-ray pair distribution functions (PDF) calculated for a range of Fe(III) oxyhydroxide clusters, including Fe 13 Keggin isomers computed previously using density functional theory (DFT), which yielded at best only partial agreement at short range (<5 Å). Aging of the clusters synthesized at pH 1.5 and 2.5 results in growth and transformation via Ostwald ripening to mixtures of goethite (Gt) and lepidocrocite (Lp). This process was inhibited by immediately reacting the early-formed clusters with phosphate (PO 4 3– ), suggesting that oxyanion surface complexes can stabilize the initial clusters by preventing growth and crystallization to more stable phases.

58 GEOSCIENCES↗

ZeoNet: 3D convolutional neural networks for predicting adsorption in nanoporous zeolites

Zeolites are one of the most widely used materials in the chemical industry due to their nanometer-sized pores that can adsorb and react upon molecules selectively. With hundreds of known framework topologies and hundreds of thousands of computationally predicted structures, the ability to rapidly predict zeolite performance allows researchers to prioritize their efforts on the most promising structures for a given application. Although the accuracy of forcefield-based atomistic simulations has advanced significantly in the past two decades, these simulations can be computationally expensive, especially for long-chain, complex molecules. Here, we present ZeoNet, a representation learning framework using convolutional neural networks (ConvNets) and 3D volumetric representations for predicting adsorption in zeolites. ZeoNet was trained on the task of predicting Henry's constants for adsorption, k H , of n-octadecane in more than 330 000 known and predicted zeolite materials. Employing a 3D grid based on the distances to solvent-accessible surfaces, a volumetric representation that can be generated efficiently, the best-performing ZeoNet achieved a correlation coefficient r 2 = 0.977 and a mean-squared error MSE = 3.8 in ln k H , which corresponds to an error of 9.3 kJ mol -1 in adsorption free energy. In comparison, a model based on hand-designed geometric features has values of r 2 = 0.783 and MSE = 35.7. ZeoNet is also relatively efficient and can process ≈8 structures per second on an Nvidia RTX 2080TI GPU, orders of magnitude faster than forcefield-based simulations. A systematic analysis was conducted to investigate how the choice of ConvNet architectures, the linear dimension (L) and spatial resolution (Δd) of the distance grids, batch size, optimizer, and learning rate impact the model performance. We found that ConvNets based on the ResNet architecture offer the best tradeoff between expressiveness and efficiency. The performance for all models reaches a plateau at L = 30–45 Å and depends less sensitively on grid resolution, with a small benefit around Δd = 0.30–0.45 Å. Finally, saliency maps were visualized to identify which regions of the materials contributed the most to model predictions. It was found, interestingly, that the predictions are driven primarily by the accessible pore volume rather than the region occupied by the framework atoms.

36 MATERIALS SCIENCE↗

Proton surface exchange kinetics of perovskite triple conducting thin films for protonic ceramic electrolysis cells: BaPr 0.9 Y 0.1 O 3–δ (BPY) vs. Ba 1–x Co 0.4 Fe 0.4 Zr 0.1 Y 0.1 O 3–δ (BCFZY)

Protonic ceramic electrolysis cells (PCECs) are an attractive green H 2 production technology, given their intermediate-temperature operating range and ability to produce dry H 2 . However, PCECs will benefit from development of more efficient and durable “triple conducting” anodes where steam is split, H incorporated, and oxygen evolved. In this work, we evaluated the kinetics of the steam-splitting/H incorporation reaction on BaPr 0.9 Y 0.1 O 3–δ (BPY) in comparison to the benchmark Ba 1–x Co 0.4 Fe 0.4 Z r0.1 Y 0.1 O 3–δ (BCFZY) composition, replacing most of the transition metal elements (Co, Fe, Zr) with the lanthanide Pr. We prepared geometrically well-defined perovskite BPY and BCFZY thin films by pulsed laser deposition and performed simultaneous optical transmission relaxation and electrical conductivity relaxation measurements at 400–500 °C in 0.21 atm O 2 during switching of the steam partial pressure to isolate and compare their proton surface exchange coefficients (k). The k values of BPY were comparable to those of BCFZY and more stable over time. According to angle-resolved XPS and STEM-EDS mapping of FIB cross-sections, the surface of BPY exhibited Ba enrichment, Pr deficiency, and Si contamination. In contrast, BCFZY exhibited Ba deficiency throughout, no obvious surface segregation, and less Si contamination. The Ba segregation on the BPY film appears to have promoted steam splitting/H incorporation kinetics even though the more basic surface reacted with the acidic environmental SiO x H y . Faster kinetics observed on stoichiometric BCFZY vs. Ba-deficient BCFZY confirmed the benefit of a high A-site Ba concentration. This result contrasts with most work on perovskites applied in solid oxide electrolysis cell anodes, in which A-site segregation is considered deleterious for surface reaction kinetics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗