Designing high performance Pt monolayer core-shell electrocatalysts for fuel cells
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99 GENERAL AND MISCELLANEOUS↗
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Identifying electrochemical processes by distribution of relaxation times in proton exchange membrane electrolyzers
Distribution of relaxation time (DRT) is used to interpret electrochemical impedance spectroscopy (EIS) for proton exchange membrane (PEM) water electrolyzers, with an attempt to separate overlapped relaxation processes in Nyquist plots. By varying operating conditions and catalyst loadings, four main relaxation peaks arising from EIS can be identified and successfully separated from low to high frequencies as (P1) mass transport, (P2) oxygen evolution reaction kinetics, (P3) reaction kinetics (with faster time constant than P2), and (P4) ionic transport. Here, the shape, height, and frequency of the DRT peaks change with different membrane electrode assembly (MEA) configurations. Electron microscopy reveals distinct features from the cross-sectioned MEAs which verify critical DRT results in that increasing the iridium (Ir)-anode loading from 0.2 mgIr/cm 2 to 1.5 mgIr/cm 2 reduces kinetic losses due to higher site-access; a thick and compacted anode, however, also triggers higher ohmic resistances from membrane/catalyst layer hydration and increases transport losses due to longer ionomer pathways. DRT provides higher resolution to EIS for deconvoluting processes with different relaxation times and the quantification of DRT peaks improves the accounting of total losses from each process.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Modifying redox properties and local bonding of Co 3 O 4 by CeO 2 enhances oxygen evolution catalysis in acid
Developing efficient and stable earth-abundant electrocatalysts for acidic oxygen evolution reaction is the bottleneck for water splitting using proton exchange membrane electrolyzers. Here, we show that nanocrystalline CeO 2 in a Co 3 O 4 /CeO 2 nanocomposite can modify the redox properties of Co 3 O 4 and enhances its intrinsic oxygen evolution reaction activity, and combine electrochemical and structural characterizations including kinetic isotope effect, pH- and temperature-dependence, in situ Raman and ex situ X-ray absorption spectroscopy analyses to understand the origin. The local bonding environment of Co 3 O 4 can be modified after the introduction of nanocrystalline CeO 2 , which allows the CoIII species to be easily oxidized into catalytically active CoIV species, bypassing the potential-determining surface reconstruction process. Co 3 O 4 /CeO 2 displays a comparable stability to Co 3 O 4 thus breaks the activity/stability tradeoff. This work not only establishes an efficient earth-abundant catalysts for acidic oxygen evolution reaction, but also provides strategies for designing more active catalysts for other reactions.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Boosting the performance of reversible solid oxide electrochemical cells with a novel hybrid oxygen electrode, Pr 1.39 Ba 0.14 Sr 0.53 Co 1.48 Fe 0.76 O 6- δ -Ba 0.66 Sr 0.34 CoO 3- δ
Solid oxide electrochemical cells (SOECs) stand out as a highly promising clean energy technology that offers several benefits, showing significant potential to play a pivotal role in the transition towards a sustainable and low-carbon energy future. SOECs can efficiently convert the chemical energy stored in fuels to electricity in fuel cell mode, and produce various chemicals from abundant feedstocks (e.g., CO 2 , H 2 O) and intermittent solar/wind-based renewable electricity. Despite extensive efforts that have been devoted to designing novel materials and optimizing SOEC manufacturing processes, aiming to achieve enhanced energy efficiency, the current SOECs still suffer from poor performance, which is mainly due to the sluggish oxygen reduction reaction (ORR) and oxygen evolution reaction (OER) kinetics. To address this challenge, in this work, we have successfully designed an in situ formed hybrid oxygen electrode material (Pr 1.39 Ba 0.14 Sr 0.53 Co 1.48 Fe 0.76 O 6- δ -Ba 0.66 Sr 0.34 CoO 3- δ ), which significantly improves the surface oxygen exchange coefficient and bulk oxygen-ion diffusion coefficient, enhancing the OER and ORR electrocatalytic activities. Further, the SOECs equipped with this newly developed oxygen electrode achieved exceptional performance for power generation using both hydrogen and propane as the fuels. At 750 °C, a peak power density of 2.4 W cm -2 was obtained with H 2 as the fuel. Additionally, the SOECs attain unprecedented performance in steam electrolysis mode. A current density of 4.4 A cm -2 was achieved at 1.3 V and 750 °C, which represents the highest performance among all yttria-stabilized zirconia (YSZ) electrolyte-based SOECs. The SOECs also deliver remarkable stability during the accelerated stability testing, highlighting the great potential of Pr 1.39 Ba 0.14 Sr 0.53 Co 1.48 Fe 0.76 O 6- δ -Ba 0.66 Sr 0.34 CoO 3- δ as a high-performance oxygen electrode for next generation SOECs.
08 HYDROGEN↗
Spin-dependent electron transfer in electrochemically transparent van der Waals heterostructures for oxygen evolution reaction
Spin selective catalysis is an emerging approach for improving the thermodynamics and kinetics of reactions. The role of electron spins has been scarcely studied in catalytic reactions. One exception is the oxygen evolution reaction (OER) where strongly correlated metals and oxides are used as catalysts. In OER, spin alignment facilitates the transition of singlet state of the reactant to the triplet state of O 2 . However, the influence of strong correlations on spin exchange mechanism and spin selective thermodynamics of most catalytic reactions remain unclear. Here we decouple the strongly correlated catalyst from the electrolyte to study spin exchange in two-dimensional (2D) magnetic iron germanium telluride (FGT) heterostructure. We demonstrate that transmission of spin and electrochemical information between the catalyst and the reactant can occur through quantum exchange interaction despite the catalyst of FGT being completely encapsulated by graphene or hexagonal boron nitride (hBN). The strong correlations in FGT that lead to enhanced spin exchange in OER are observed in graphene or hBN layers with thicknesses of up to 6 nm. We demonstrate that spin alignment in FGT leads to a lowering of thermodynamic barrier for adsorption of hydroxide ion and electron transfer to the catalyst. This results in up to fivefold enhancement in OER performance and improved kinetics. Our results provide clear evidence that transmission of both quantum mechanical and electrochemical information through quantum spin exchange interaction in FGT leads to an enhancement in catalytic performance.
2D materials↗
Vacancy‐Enabled O3 Phase Stabilization for Manganese‐Rich Layered Sodium Cathodes
Abstract Manganese‐rich layered oxide materials hold great potential as low‐cost and high‐capacity cathodes for Na‐ion batteries. However, they usually form a P2 phase and suffer from fast capacity fade. In this work, an O3 phase sodium cathode has been developed out of a Li and Mn‐rich layered material by leveraging the creation of transition metal (TM) and oxygen vacancies and the electrochemical exchange of Na and Li. The Mn‐rich layered cathode material remains primarily O3 phase during sodiation/desodiation and can have a full sodiation capacity of ca. 220 mAh g −1 . It delivers ca. 160 mAh g −1 specific capacity between 2–3.8 V with >86 % retention over 250 cycles. The TM and oxygen vacancies pre‐formed in the sodiated material enables a reversible migration of TMs from the TM layer to the tetrahedral sites in the Na layer upon de‐sodiation and sodiation. The migration creates metastable states, leading to increased kinetic barrier that prohibits a complete O3‐P3 phase transition.
Xiao, Biwei↗
An Unbalanced Battle in Excellence: Revealing Effect of Ni/Co Occupancy on Water Splitting and Oxygen Reduction Reactions in Triple–Conducting Oxides for Protonic Ceramic Electrochemical Cells
Porous electrodes that conduct electrons, protons, and oxygen ions with dramatically expanded catalytic active sites can replace conventional electrodes with sluggish kinetics in protonic ceramic electrochemical cells. In this work, a strategy is utilized to promote triple conduction by facilitating proton conduction in praseodymium cobaltite perovskite through engineering non-equivalent B-site Ni/Co occupancy. Surface infrared spectroscopy is used to study the dehydration behavior, which proves the existence of protons in the perovskite lattice. The proton mobility and proton stability are investigated by hydrogen/deuterium (H/D) isotope exchange and temperature-programmed desorption. It is observed that the increased nickel replacement on the B-site has a positive impact on proton defect stability, catalytic activity, and electrochemical performance. This doping strategy is demonstrated to be a promising pathway to increase catalytic activity toward the oxygen reduction and water splitting reactions. The chosen PrNi 0.7 Co 0.3 O 3–δ oxygen electrode demonstrates excellent full-cell performance with high electrolysis current density of –1.48 A cm –2 at 1.3 V and a peak fuel-cell power density of 0.95 W cm –2 at 600 °C and also enables lower-temperature operations down to 350 °C, and superior long-term durability.
08 HYDROGEN↗
Optimization of La 2 NiO 4+δ Electrolysis Cell Oxygen Electrode through Surfactant-Enabled LaCoO 3±δ Nanocatalyst Deposition
Lanthanum nickelate (LNO) has shown promise as a Cr-resistant air electrode material for SOECs but has suboptimal surface oxygen exchange properties. Nanocoating of the LNO surface with lanthanum cobaltite (LCO) was chosen to improve cell performance as a surface oxygen conductor. The work focused on the implementation of a two-step nano-LCO film deposition utilizing catechol molecules in a porous LNO electrode. The subgoals of the work were to maintain nanosized LCO particles/ grains to increase active surface area and to control the regularity/ homogeneity of the coating across the microstructure. To achieve these goals, a novel surfactant-enhanced liquid infiltration method was utilized, where nucleation sites were spread across the electrode structure to control the location and size of LCO particles. Various catechol surfactant compositions were evaluated for their ability to control the kinetics of nanoparticle deposition and the homogeneity of the coating. Chelated LCO was characterized by X-ray diffraction (XRD), which found a substantial improvement in LCO formation with surfactant addition and determined polymerized norepinephrine to be the best-performing surfactant, with 88.4% pure LCO formed at low temperature. X-ray photoelectron spectroscopy (XPS) confirmed LCO nanostructures formed by the two-step infiltration process, showing no impurities and a stable perovskite structure. Deposition kinetics were analyzed using atomic force microscopy (AFM), correlating infiltration times and solution molarity to nanoparticle size and distribution, the results of which were confirmed in symmetrical cell samples by scanning electron microscopy (SEM). Electrochemical impedance spectroscopy (EIS) testing demonstrated substantial improvements in polarization resistance, where the nanocoating reduced the resistance by ∼55% to 0.152 Ω·cm 2 at 700 °C and 0.039 Ω·cm 2 at 800 °C. Electrical conductivity relaxation (ECR) at this temperature confirmed an improved surface oxygen exchange coefficient of the LCO + LNO heterostructure predicted by the Bode data from EIS, alongside a reduction in activation energy by about 30%.
Deposition↗
Engineered Catalyst Support with Improved Durability at Higher Weight Percentage of Platinum
Proton Exchange Membrane (PEM) fuel cells are a suitable electrochemical power source for heavy duty vehicle (HDV) applications due to their high efficiency and durability. The cathode of the fuel cell uses a higher geometric loading of platinum (∼0.2 to 0.4 mg Pt /cm 2 ) for the electrocatalysis of the kinetically sluggish Oxygen Reduction Reaction (ORR) which requires higher weight percent loading of the metal (∼50%) on the carbon support to decrease the catalyst layer thickness and hence, the reactant transport losses. The conventionally used supports for platinum catalyst, such as the KetjenBlack TM type high surface area carbon (HSC) features limited mesopore area for the dispersion of Pt nanoparticles leading to increased aggregation and poor durability. Here, we show a new class of carbon materials known as the Engineered Catalyst Support (ECS) developed by Pajarito Powder with higher mesopore fraction for the dispersion of higher weight percentage of Pt nanoparticles. ECS materials can disperse up to 50% Pt by weight of the catalyst thereby enabling lower catalyst layer thickness with higher performance retained after durability test. A comprehensive set of physico-chemical and electrochemical studies in membrane electrode assembly (MEA) are reported to understand the performance and durability of Pt/ECS catalysts.
08 HYDROGEN↗
Tandem bulk oxygen diffusion and surface reactions in reducible metal oxides control redox cycle dynamics
The interplay between bulk oxygen diffusion and surface reactions in reducible metal oxides is key in heterogeneous catalysts, but direct measurements of oxygen mobility, transient kinetics, and in situ spectroscopies have been lacking. Here, we reveal complex dynamic behavior of ceria-zirconia by H 2 using transient kinetics via mass spectrometry and in situ Raman and near-ambient pressure x-ray photoelectron spectroscopies. Molecular dynamics simulations with a machine learning potential delineate competitive oxygen diffusion mechanisms, with an optimal mobility at intermediate reductions. We expose a compensation between vacancy availability and lattice distortion at intermediate to high reductions and Frenkel defects at low reductions, underscoring a potential deficiency of 16 O/ 18 O exchange experiments in deducing oxygen mobility. Vacancies in proximity require electron localization on Ce atoms further away. The continuous replenishment of surface oxygen results in a varying reduction rate, with H 2 dissociation being the rate-limiting step. Multiscale transient simulations, consistent with experiments, indicate catalysts of potentially spatially varying oxidation states. The approach is broadly applicable to reducible oxide materials.
36 MATERIALS SCIENCE↗
Molecular structure and catalytic promotional effect of Mn on supported Na 2 WO 4 /SiO 2 catalysts for oxidative coupling of methane (OCM) reaction
The structure and promotional effect of Mn in supported Mn-Na 2 WO 4 /SiO 2 catalysts for the oxidative coupling of methane (OCM) reaction has been debated for a longtime in the literature. In the current investigation, with the aid of multiple in-situ characterization studies, we show that the freshly calcined supported 1.2Mn-5Na 2 WO 4 /SiO 2 catalyst possesses crystalline Na 2 WO 4 , Mn 2 O 3 and SiO 2 (cristobalite phase) along with surface MnO x and Na-WO x sites at low temperature and oxidizing environments. Under the OCM reaction environment (T>800°C), the crystalline Na 2 WO 4 phase melts and Mn 2 O 3 phase reduces. In contrast, the surface MnO x and Na-WO x sites exhibit excellent thermal and chemical stability. Exposure of the 1.2Mn-5Na 2 WO 4 /SiO 2 catalyst to the OCM reaction environment redisperses the molten Na 2 WO 4 phase on the SiO 2 support to form new surface WO x sites. Interestingly, the stable MnO x species interacts with both molten Na 2 WO 4 phase and surface Na-WO x sites during OCM reaction. Controlled transient kinetic experiments in TAP and detailed steady state OCM fixed-bed reaction studies reveal the role and promotional effect of Mn in the 1.2Mn-5Na 2 WO 4 /SiO 2 catalyst. The W-oxides (both molten Na 2 WO 4 and surface Na-WO x sites) are the active sites for the catalytic OCM reaction and the MnO x species only function as promoters. The promotion of MnO x strongly depends on the gas phase O 2 partial pressure and the MnO x species act as mediators for oxygen exchange between the gas phase molecular O 2 and catalyst lattice oxygen. In conclusion, the temperature dependent MnO x promotion reveals that the MnO x species selectively promote the molten Na 2 WO 4 phase at lower reaction temperature and the surface Na-WO x sites at higher temperature.
36 MATERIALS SCIENCE↗
Elucidating effects of catalyst loadings and porous transport layer morphologies on operation of proton exchange membrane water electrolyzers
Producing green hydrogen efficiently via proton exchange membrane water electrolysis (PEMWE) is the key for achieving decarbonization targets. Iridium catalyst is expensive, and it is important to minimize its use and to optimize interface between Ir and ionomer or water for higher utilization of catalyst in oxygen evolution reaction. In this work, x-ray computed tomography along with electrochemical and modeling techniques are used to characterize the interface for two different porous transport layers (PTLs) and catalyst layers at various loadings. We show that low porosity sintered PTLs exhibit higher interfacial contact with the catalyst and the membrane that results in improved kinetics. Radiography and modeling results indicate that oxygen taking multiple transport pathways through the PTL results in slug flow through the channels that reduces mass transport overpotential. Based on the results, we suggest design guidelines for high efficiency and durable PEMWE and their components.
08 HYDROGEN↗
Atomically dispersed metal–nitrogen–carbon catalysts for fuel cells: advances in catalyst design, electrode performance, and durability improvement
The urgent need to address the high-cost issue of proton-exchange membrane fuel cell (PEMFC) technologies, particularly for transportation applications, drives the development of simultaneously highly active and durable platinum group metal-free (PGM-free) catalysts and electrodes. The past decade has witnessed remarkable progress in exploring PGM-free cathode catalysts for the oxygen reduction reaction (ORR) to overcome sluggish kinetics and catalyst instability in acids. Among others, scientists have identified the newly emerging atomically dispersed transition metal (M: Fe, Co, or/and Mn) and nitrogen co-doped carbon (M–N–C) catalysts as the most promising alternative to PGM catalysts. Here, we provide a comprehensive review of significant breakthroughs, remaining challenges, and perspectives regarding the M–N–C catalysts in terms of catalyst activity, stability, and membrane electrode assembly (MEA) performance. A variety of novel synthetic strategies demonstrated effectiveness in improving intrinsic activity, increasing active site density, and attaining optimal porous structures of catalysts. Rationally designing and engineering the coordination environment of single metal MN x sites and their local structures are crucial for enhancing intrinsic activity. Increasing the site density relies on the innovative strategies of restricting the migration and agglomeration of single metal sites into metallic clusters. Relevant understandings provide the correlations among the nature of active sites, nanostructures, and catalytic activity of M–N–C catalysts at the atomic scale through a combination of experimentation and theory. Current knowledge of the transferring catalytic properties of M–N–C catalysts to MEA performance is limited. Rationally designing morphologic features of M–N–C catalysts play a vital role in boosting electrode performance through exposing more accessible active sites, realizing uniform ionomer distribution, and facilitating mass/proton transports. We outline future research directions concerning the comprehensive evaluation of M–N–C catalysts in MEAs. The most considerable challenge of current M–N–C catalysts is the unsatisfied stability and rapid performance degradation in MEAs. Therefore, we further discuss practical methods and strategies to mitigate catalyst and electrode degradation, which is fundamentally essential to make M–N–C catalysts viable in PEMFC technologies.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
From Fundamental Interfacial Reaction Kinetics to Macroscopic Current–Voltage Characteristics: Case Study of Solid Acid Fuel Cell Limitations and Possibilities
The unique properties of solid acid electrolytes, in particular CsH 2 PO 4 , are in many ways ideal for fuel cell operation. However, the technology is constrained by high cathode overpotentials. Here a simplified cathode geometry is employed to obtain the fundamental electrochemical parameters (exchange current density and charge transfer coefficient) describing the oxygen reduction reaction (ORR) at the CsH 2 PO 4 -Pt-gas interface. The parameters are incorporated into a 1D model of the voltage–current characteristics of realistic SAFC cathodes, which reproduced the measured polarization behavior of such cathodes without recourse to fitting adjustable parameters. Following this validation, the model is utilized to evaluate the impact of changes to cathode properties, microstructure, and operating conditions. Of these, the charge transfer coefficient, measured to have a value of ≈0.6 for ORR on Pt in the SAFC cathode environment, is found to have the greatest impact on power output. Nevertheless, even without material modifications, a combination of microstructural and operational modifications are identified with projected performance metrics meeting Department of Energy targets (0.8 V at 300 mA cm –2 , and peak power density of 1 W cm –2 ), albeit at high Pt loadings. However, the analysis indicates that truly meaningful advances will likely necessitate the discovery of alternative ORR catalysts.
36 MATERIALS SCIENCE↗
Thermodynamic modeling of countercurrent chemical looping reverse water gas shift process for redox material screening
The reverse water gas shift (RWGS) reaction is a key pathway for CO 2 utilization, particularly within Power-to-X process chains aimed at sustainable fuel and chemical production. Countercurrent chemical looping (CL-RWGS) using non-stoichiometric oxides can overcome equilibrium limitations of conventional RWGS reactors, enabling significantly higher CO 2 conversions. However, modeling the limiting performance of such systems is challenging due to their multiphase nature and coupled spatial and temporal variation in chemical composition. In this work, we present a discretized batch equilibrium model that simulates CL-RWGS reactors as a series of localized equilibrium exchanges between gas and solid elements. The model is numerically stable, computationally efficient, and free of kinetic source terms, making it well-suited for parametric studies and system-level integration. It is validated against established convection–diffusion models and shown to predict reasonable upper bounds on experimental results. Application of the model to a range of oxygen carrier materials identifies cerium–zirconium solid solutions, particularly Ce 0.80 Zr 0.20 O 2 , as a promising class offering superior oxygen storage characteristics compared to state-of-the-art La 0.6 Sr 0.4 FeO 3 . This framework provides a robust platform for materials screening, reactor sizing, and performance optimization in chemical looping systems. The model implementation is available as open-source software to support further research and development.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
The Impact of Catalyst Layer Composition and Structure on Performance and Durability of PEMWE Anodes
A study of various compositions of anodes for proton exchange membrane water electrolysis aimed at reducing precious metal content and system costs without compromising performance and durability is presented. A key challenge in current water electrolysis technologies is the reliance on high iridium loadings to ensure sufficient catalytic activity, electronic conductivity, and durability for the oxygen evolution reaction. To address this, catalyst layers based on the stable but kinetically limited rutile phase of iridium oxide are combined with platinum nanoparticles and carbon-based additives to improve structural properties and ink processability. By systematically varying the volume ratios of carbon to precious metals and ionomer to solids, compositional trends have been identified, and significant performance improvements have been achieved. Structural and elemental analysis confirms improved dispersion of platinum and iridium can be achieved, as well as electronic conductivity improvements within the catalyst layer. Polarization curve analysis has shown the ability of added Pt and C to significantly increase catalytic activity. These results highlight the potential positive impact of Pt and C on anode structure, composition, and cell performance.
36 MATERIALS SCIENCE↗
Tuning Catalyst Activation and Utilization Via Controlled Electrode Patterning for Low-Loading and High-Efficiency Water Electrolyzers
An anode electrode concept of thin catalyst-coated liquid/gas diffusion layers (CCLGDLs), by integrating Ir catalysts with Ti thin tunable LGDLs with facile electroplating in proton exchange membrane electrolyzer cells (PEMECs), is proposed. The CCLGDL design with only 0.08 mg Ir cm -2 can achieve comparative cell performances to the conventional commercial electrode design, saving ~97% Ir catalyst and augmenting a catalyst utilization to ~24 times. CCLGDLs with regulated patterns enable insight into how pattern morphology impacts reaction kinetics and catalyst utilization in PEMECs. A specially designed two-sided transparent reaction-visible cell assists the in situ visualization of the PEM/electrode reaction interface for the first time. Oxygen gas is observed accumulating at the reaction interface, limiting the active area and increasing the cell impedances. In this work, it is demonstrated that mass transport in PEMECs can be modified by tuning CCLGDL patterns, thus improving the catalyst activation and utilization. The CCLGDL concept promises a future electrode design strategy with a simplified fabrication process and enhanced catalyst utilization. Furthermore, the CCLGDL concept also shows great potential in being a powerful tool for in situ reaction interface research in PEMECs and other energy conversion devices with solid polymer electrolytes.
08 HYDROGEN↗
Stabilizing Single-Atom Iron Electrocatalysts for Oxygen Reduction via Ceria Confining and Trapping
Atomically dispersed Fe-N-C materials recently hold great interest in costly Pt substitution for the cathodic oxygen reduction reaction of fuel cells. However, the heat treatment involved in the materials preparation excites Fe aggregating into low activity of nanosized species rather than high activity of single-atom Fe sites. Herein we proposed a new "ceria-assisted" strategy to preferentially generate the active single-atom Fe sites in Fe-N-C materials, which involves oxidative polymerization of pyrrole, Ce 3+ and Fe 3+ adsorption, and subsequent heat treatment. Owing to its spatial confinement and strong trapping for Fe atoms, ceria can effectively suppress agglomeration of isolated Fe atoms and stabilize the Fe atoms by bonding to O in the lattice during the heat treatment, leading to a high content of atomically dispersed Fe (4.6 wt.%). Accordingly, the final catalyst showed ultrahigh ORR activity with a half-wave potential of 0.915 V and kinetic current density of 7.15 mA cm -2 at 0.9 V. When it was as assembled an anion exchange membrane fuel cell, a large maximum power density of 496 mW cm -2 was achieved.
25 ENERGY STORAGE↗