Stable Catalyst Research Articles

Hierarchical Carbon-Based Electrocatalyst with Functional Separation Properties for Efficient pH Universal Nitrate Reduction.

The electrocatalytic reduction of nitrate (eNO3 -RR) to ammonia (NH3) across varying pH is of great significance for the treatment of practical wastewater containing nitrate. However, developing highly active and stable catalysts that function effectively in a wide pH range remains a formidable challenge. Herein, a hierarchical carbon-based metal-free electrocatalyst (C-MFEC) of winged carbon coaxial nanocables (W-CCNs, in situ generated graphene nanosheets and outside carbon layer with abundant topological defects from pristine carbon nanotubes, CNTs), is prepared through moderate oxidation of CNTs and the subsequent introduction of topological defects. The W-CCNs feature functional separation properties, with an inner core of pristine CNTs that facilitates efficient charge transfer, while the outer shell is composed of in situ generated graphene nanosheets and carbon layers enriched with topological defects characterized by distinct carbon atom configurations, which play a crucial role in promoting the adsorption of NO3 -, the dissociation of water, and the N─H bond formation. This innovative design enables the C-MFEC to exhibit outstanding performance for eNO3 -RR, operating efficiently with the NH3 yield rates of 49.5, 75.3, and 88.1g h-1 gcat. -1 in acidic, neutral, and alkaline media, respectively. Such performance metrics not only outshine C-MFECs but also rival or surpass those of certain metal-based catalysts.

Delineating Catalyst Deactivation Mechanisms in Electrocatalytic Glycerol Oxidation toward Biodiesel Wastewater/CO2 Co-valorization.

Biodiesel plays a key role in achieving economy-wide decarbonization but its production discharges significant amounts of CO2 and glycerol-laden wastewater. Given the increasing abundance of biodiesel wastewater and low redox potential of glycerol, coupling the glycerol oxidation reaction (GOR) with CO2 electrolysis has emerged as an attractive strategy to achieve sustainable wastewater management, CO2 utilization, and green chemical synthesis in a single unit process. Despite the need for highly stable catalysts, few studies have examined electrocatalyst deactivation in environmental waste streams. Here, we present a first-of-a-kind diagnostic study that investigates nickel (Ni) catalyst stability during the GOR in synthetic biodiesel wastewaters. A current decline of 99.7% was observed within 24 h of operation. This coincided with an 80% decrease in surface active Ni(II)/Ni(III) concentrations, 190-fold increases in interfacial impedance, and the appearance of electrode C-bonds that suggested surface coverage by GOR reactants and intermediates was likely a main contributor to loss in catalytic activity. Analyses in more complex electrolytes containing methanol and oleate suggested the emergence of distinct deactivation mechanisms through restricted NiOOH formation. Altogether, this study details several previously unreported catalyst deactivation mechanisms. These findings can ultimately help inform future catalyst design toward more practical and sustainable waste valorization.

Advances in CO2 assisted oxidative dehydrogenation of light alkanes to light alkenes.

The CO2-assisted oxidative dehydrogenation of light alkanes offers a promising route for converting underutilized resources into valuable chemical feedstocks while addressing environmental challenges associated with CO2 emissions. CO2 plays a dual role in ODH by acting as a mild oxidant that enhances product selectivity and catalyst stability while preventing carbon deposition through RWGSand Boudouard reactions. The review has elucidated a variety of catalyst design and optimization strategies that may guide the future development of novel CO2-assisted ODH catalysts with improved alkane conversion, superior alkene selectivity, and long-term stability.It provides a comprehensive analysis of the structural characteristics, catalytic performances, and reaction mechanisms of typical catalysts. Special attention is given to the structure-performance relationship of these catalysts, emphasizing how changes in promoters, supports, and morphology affect critical properties such as redox behavior, acidity-basicity balance, dispersion of active components, and catalyst-support interactions. Finally, future research directions and perspectives for the CO2-assisted ODH of ethane and propane are proposed, with a focus on advancing catalyst design and optimization strategies. This review aims to serve as a comprehensive reference for researchers exploring the potential of CO2-assisted ODH in promoting sustainable production of light alkenes.

Three Polyoxovanadoborates Constructed from "Sandwich"-Type {V10B24}, {V10B28}, and {V12B32} Clusters.

Three distinct polyoxovanadoborates modified by transition metals, specifically {V10B26Cd8(phen)12} (1, phen = 1,10-phenanthroline), {V10B32Zn6} (2), and {V12B32Cu2} (3), have been synthesized under hydrothermal conditions. Compounds 1-3 feature three unique sandwich-type clusters, namely, {V10B24}, {V10B28}, and {V12B32}, each characterized by toroidal (O═VO2)n (n = 10, 12) rings. In the structure of 1, two pairs of {Cd(phen)} and {Cd(phen)2} units are grafted on the {B13} rings from the top and bottom of the {V10B24} cluster, respectively. Compound 2 is a 1D polymeric chain consisting of the bridging ligand {ZnO6} unit linked to {V10B28}, which accommodates the {Zn4B4O8} unit. The {V12B32} cluster in 3 is interconnected with [Cu(en)2]2+ (en = ethylenediamine) to create the sql layer, which is further stacked in an ABAB sequence to form a 3D supramolecular framework. Additionally, sulfide catalytic oxidation experiments revealed that compound 2 is an efficient and stable sulfide oxidation catalyst.

Enhancing OER Activity Through Water Treatment-Induced Surface Reconstruction of Metal Surfaces.

This research introduces a simple and effective method to enhance oxygen evolution reaction (OER) performance through surface reconstruction of metal substrates via hydration. A water treatment technique is employed to form a nanometer-thick hydroxide layer on Ni foam, which significantly improved OER activity compared to pristine Ni. To further explore catalyst performance on hydrated substrates, NiFe layered double hydroxide (LDH) is deposited, resulting in NiFe LDH@hydrated Ni foam achieving superior performance and exceptional stability, maintaining 1 Acm-2 for 1000 h. In contrast, NiFe LDH@pristine Ni foam showed rapid degradation. Interestingly, while the hydrated hydroxide layer demonstrated remarkable OER activity, it is ineffective for hydrogen evolution reaction (HER). Density functional theory (DFT) calculations revealed the differing roles of hydroxides in OER and HER, providing insights into their electrochemical pathways. These findings highlight that simple hydration enhances the activity and long-term stability of LDH catalysts, addressing a key limitation in their practical use. This study demonstrates a promising and scalable strategy for improving OER performance and catalyst durability, offering valuable insights into the role of surface hydroxides in electrode reactions for energy applications.

Insights into Segregation and Aggregation in Dilute Atom Alloy Catalysts using DFT and Machine Learning

Dilute atom alloys (DAAs) are an important class of heterogeneous catalysts due to their ability to precisely tune the activity and selectivity of reactions. DAA catalysts typically consist of a small quantity of metal solute in a metal host. Key considerations in the stability of DAA catalysts are the segregation and aggregation energy. In this work, we report a systematic theoretical study of segregation and aggregation energies of DAA catalysts composed of 3d, 4d, and 5d transition metals. To investigate the nature of DAAs, we analyzed both Bader charge and density of states, as well as formation energies to identify the most stable DAA configuration for a given alloy. We further applied regression‐based, tree‐based, and neural network machine learning (ML) models to gain physics‐based insights in predicting segregation and aggregation energies based on readily available atomic and bulk features. We found that the d‐band filling of the solute and host, nearest neighbor distance of the host and d‐band width of the solute determine the segregation energy while the Pauling electronegativity of the host and solute, nearest neighbor distance of the host, and cohesive energy of host determine aggregation energy. Our findings provide crucial insights for DAA catalyst design.

Bi Dendrites Succeed Under Challenging Flue Gas Conditions for CO2RR

AbstractThe electrochemical reduction of carbon dioxide (ERC) from flue gas is a promising solution to mitigate CO2 emissions and importantly has the ability for direct industrial application. However, components such as N2, O2, SOx, NOx, and H2O in flue gas can hinder ERC efficiency, affecting catalyst stability and selectivity. This study systematically investigates the effect of these flue gas components on a metallic Bi dendrite catalyst. The catalyst shows remarkable stability (over 6 days are observed with constant current generation) surpassing other monometallic Bi catalysts. The active state of the catalyst has been demonstrated with operando XANES (X‐ray Absorption Near Edge Structure) analysis which has confirmed the metallic state of bismuth and notably, the catalyst performance remains unaffected despite the presence of other flue gas components such as N2, O2, SOx, and NOx. This research aims to fill a critical gap, demonstrating how flue gas components influence ERC activity and pave the way for future advancements in catalyst optimization.

Engineering active sites in ternary CeO2-CuO-Mn3O4 heterointerface embedded in reduced graphene oxide for boosting water splitting activity

The rational design of highly efficient and stable bifunctional catalysts for overall water splitting is vitally important. In this study, to increase the active catalytic sites of CeO2 for electrochemical water splitting, a ternary CeO2-CuO-Mn3O4 heterostructure, synthesized by coprecipitation method, is loaded on reduced graphene oxide (rGO) nanosheets in different amounts to produce CeO2-CuO-Mn3O4@rGO nanocomposites. It is found that CeO2-CuO-Mn3O4@rGO nanocomposites show higher electrocatalytic activity than unsupported samples, and the best activity is observed when the wieght ratio of CeO2-CuO-Mn3O4 is three times that of rGO. The CeO2-CuO-Mn3O4@rGO(3:1) requires low overpotentials of 130 and 270 mV for hydrogen and oxygen evolution reactions (HER and OER) at a current density of 10 mA cm−2. Furthermore, this material demonstrates a large electrochemically active surface area, low charge transfer resistance, suitable kintics, and high long-term stability for both OER and HER. Additionally, when CeO2-CuO-Mn3O4@rGO(3:1) is used as self-supported electrodes for the overall water splitting reaction, a low cell voltage of 1.68 V is obtained. This superior performance is due to: (i) active multi-metal sites that produce strong synergistic effects; (ii) the high conductivity of rGO, which faciliate favorable electron transfer; and (iii) the homogenous anchoring of CeO2-CuO-Mn3O4 on rGO, which increases the number of active sites available on the catalyst surface.

Atomically Dispersed Metal Catalysts for Oxygen Reduction Reaction: Two‐Electron vs. Four‐Electron Pathways

Developing eco‐friendly electrochemical devices for electrosynthesis, fuel cells (FCs), and metal‐air batteries (MABs) requires precisely designing the electronic pathway in the oxygen reduction reaction (ORR) process. Understanding the principle of designing low‐cost, highly active, and stable catalysts helps to reduce the usage of noble metals in ORR. Atomically dispersed metal catalysts (ADMCs) emerge as promising alternatives to replace commercial noble metals due to their high utilization of active metal atoms, high intrinsic activity, and controllable coordination environments. In this review, the research tendency and reaction mechanisms in ORR are first summarized. The basic principles concerning the geometric size of the catalysts for both two‐electron ORR (2e ORR) and four‐electron ORR (4e ORR) were then discussed, aiming to outline the material design differences for 2e ORR and 4e ORR. Subsequently, the recent advances concentrated on the ADMCs, including coordination numbers, light heteroatom doping, dual‐metal atoms‐based coordination, and interaction between nanoparticle (NPs)/nanoclusters (NCs) and ADMs are documented. Finally, the key challenges and opportunities in the future design of ADMCs for the ORR are highlighted.

Atomically Dispersed Metal Catalysts for Oxygen Reduction Reaction: Two-Electron vs. Four-Electron Pathways.

Developing eco-friendly electrochemical devices for electrosynthesis, fuel cells (FCs), and metal-air batteries (MABs) requires precisely designing the electronic pathway in the oxygen reduction reaction (ORR) process. Understanding the principle of designing low-cost, highly active, and stable catalysts helps to reduce the usage of noble metals in ORR. Atomically dispersed metal catalysts (ADMCs) emerge as promising alternatives to replace commercial noble metals due to their high utilization of active metal atoms, high intrinsic activity, and controllable coordination environments. In this review, the research tendency and reaction mechanisms in ORR are first summarized. The basic principles concerning the geometric size of the catalysts for both two-electron ORR (2e ORR) and four-electron ORR (4e ORR) were then discussed, aiming to outline the material design differences for 2e ORR and 4e ORR. Subsequently, the recent advances concentrated on the ADMCs, including coordination numbers, light heteroatom doping, dual-metal atoms-based coordination, and interaction between nanoparticle (NPs)/nanoclusters (NCs) and ADMs are documented. Finally, the key challenges and opportunities in the future design of ADMCs for the ORR are highlighted.

Enhanced electrocatalytic performance of LCO-NiFe-C3N4 composite material for highly efficient overall water splitting.

The rising global energy demand & environmental crisis spur exploration of traditional fuel alternatives. Hydrogen, with high energy density & pollution-free potential, is seen as a promising energy carrier. The development of efficient and durable electrocatalysts for both oxygen evolution reaction (OER) and hydrogen evolution reaction (HER) is of paramount importance for renewable energy conversion and storage systems. Developing efficient and stable catalysts is crucial for improving OER performance, but the scarcity, high cost, and stability issues of precious metal oxide catalysts hinder their industrial application. Herein, the composite material was synthesized using a combination of sol-gel and one-step hydrothermal methods, followed by an annealing process. The inherent electrocatalytic activity of LaCoO3, a perovskite oxide, towards both OER and HER was harnessed. In an alkaline electrolyte, the LCO-NiFe-C3N4 demonstrated remarkable electrocatalytic performance with overpotentials of 251.4mV for OER and 186.7mV for HER at a current density of 10mA cm-2. The Tafel slopes were 60.8mV dec-1 for OER and 138.53mV dec-1 for HER, suggesting that the LCO-NiFe-C3N4 composite material is a promising candidate as a bifunctional catalyst. Theoretical calculations also confirm that doped elements can effectively regulate the electronic properties of active sites, thereby reducing the energy barrier of the rate-limiting step in the OER reaction and significantly enhancing the electrocatalytic activity of the catalyst. This study presents the synthesis and electrocatalytic performance evaluation of a novel (LCoO3-NiFe-C3N4) LCO-NiFe-C3N4 composite material, showcasing its potential as an effective bifunctional catalyst.

Thiol-Assisted Regulated Electronic Structure of Ultrafine Pd-based Catalyst for Superior Formic Acid Electrooxidation Performances

In order to further boost the electrocatalytic performances of small organic molecule oxidation and maintain the structure stability of Pd-based catalyst during long cycle, a new ligand compound (i.e. propanethiol) was introduced into the Pd/C anode catalyst to prepared Pd/C-SH catalyst by two main steps of propanethiol adsorbed on Vulcan XC-72 carbon (C-SH) by water bath impregnation method and Pd nanoparticles anchored on the functionalized C-SH support by improved liquid reduction method. Results showed that the Pd nanoparticles with high dispersion in Pd/C-SH catalyst were obtained and their particle size distribution was in the range of 1.6-4.8nm. Moreover, Pd particle size became smaller with the modification of propanethiol, indicating that propanethiol could facilitate the formation of smaller Pd. Electrochemical measurements showed that the mass activity of Pd/C-SH (1229mAmg-1) was 4.6 times that of Pd/C (267mAmg-1) towards formic acid oxidation. Higher stability (30 times higher than Pd/C) and more faster charge transfer kinetics of oxidation reaction were also recorded for Pd/C-SH catalyst. The enhancement of electrochemical performances of Pd/C-SH catalyst might be related to highly dispersed Pd with reduced particle size, adjusted electronic structure of Pd as well as maintained stable Pd structure and particle size.

Au@Snβ zeolite as stable and active catalyst for the conversion of glycerol to methyl lactate

Au@Snβ zeolite as stable and active catalyst for the conversion of glycerol to methyl lactate

Electronic interactions between neighboring functionalized guest Sb single atoms and Pt clusters enhance CO tolerance

Platinum-based (Pt) catalysts are notoriously susceptible to deactivation in industrial chemical processes due to carbon monoxide (CO) poisoning. Overcoming this poisoning deactivation of Pt-based catalysts while enhancing their catalytic activity, selectivity, and durability remains a major challenge. Herein, we propose a strategy to enhance the CO tolerance of Pt clusters (Ptn) by introducing neighboring functionalized guest single atoms (such as Fe, Co, Ni, Cu, Sb, and Bi). Among them, antimony (Sb) single atoms (SAs) exhibit significant performance enhancement, achieving 99% CO selectivity and 33.6% CO2 conversion at 450 °C. Experimental results and density functional theory (DFT) calculations indicate the optimization arises from the electronic interaction between neighboring functionalized Sb SAs and Pt clusters, leading to optimal 5d electron redistribution in Pt clusters compared to other functionalized guest single atoms. The redistribution of 5d electrons weaken both the σ donation and π backdonation interactions, resulting in a weakened bond strength with CO and enhancing catalyst activity and selectivity. The redistribution of 5d electrons weaken both the σ donation and π backdonation interactions, resulting in a weakened bond strength with CO. In situ environmental transmission electron microscopy (ETEM) further demonstrates the exception thermal stability of catalyst, even under H2 at 700 ℃. Notably, the functionalized Sb SAs also improve CO tolerance in various heterogenous catalysts, including Co/CeO2, Ni/CeO2, Pt/Al2O3, and Pt/CeO2-C. This finding provides an effective approach to overcome the primary challenge of CO poisoning in Pt-based catalysts, making their broader applications in various industrial catalysts.

Nitrogen-phosphorus codoped biochar prepared from tannic acid for degradation of trace antibiotics in wastewater.

This study was designed to develop a one-step pyrolysis process that could efficiently activate peroxymonosulfate (PMS) and degrade tetracycline hydrochloride (TCH) by producing N, and P codoped carbon materials (NPTC3-800). Furthermore, it exhibited a high specific surface area (658cm2g-1), a larger pore volume (0.3cm3g-1), and a certain content of heteroatoms (nitrogen and phosphorus). PMS-activated NPTC3-800 attained a TCH removal efficiency of over 90% within 40min, with an observed rate constant (kobs) of 0.0307 min-1. Similarly, the materials exhibited strong resistance to ionic interferences and showed broad applicability across various water bodies. Mobility experiments were conducted to further assess the stability of catalyst (92%, 40h). Non-radical oxidation pathways, particularly including the singlet oxygen (1O2), were evidenced to play dominant roles in TCH degradation, as demonstrated by electron paramagnetic resonance (EPR) observations and experiments with free radical quenching. Theoretical calculations demonstrated that the N and P codoped domains substantially improve TCH removal compared to pure biochar. Finally, the proposed degradation pathways for TCH were identified, and the resulting degradation products demonstrated reduced biological toxicity.

Novel MOF-derived hexagonal starfish-shaped hollow prismatic cone-loaded metal complexes for electrocatalytic water decomposition study

Exploring efficient and stable bifunctional electrocatalysts for oxygen evolution reaction/hydrogen evolution reaction (OER/HER) is an urgent need and challenge for sustainable energy. Non-noble metal-based catalysts have attracted more and more attention due to their low cost and high catalytic performance. The construction of heterostructures is considered to be one of the most promising strategies for revealing the efficient performance for OER and HER. As a result, we prepared a nanomaterial catalyst based on the combination of three non-precious metals, which were simultaneously used for efficient OER, HER and integral water splitting techniques. We first prepared a very novel hollow hexagram star-shaped metal-organic frameworks (MOFs) by a one-step hydrothermal method, then used it as the substrate material, introduced Mo6+ and Fe3+ through ion exchange reaction, and finally formed a composite system of Co3Fe7 and Mo2C through high-temperature calcination, and the product with hexagonal starfish morphology was named as hexagonal starfish-shaped hollow prismatic cone-loaded metal complexes (HSHP-Mo2C/Co3Fe7). Taking advantage of the synergistic effect of the Co3Fe7 site and the Mo2C site, HSHP-Mo2C/Co3Fe7 not only exhibit excellent OER and HER properties, but also exhibit good stability and durability. Specifically, the optimal catalyst HSHP-Mo2C/Co3Fe7-1 shows a Tafel slope of only 46mV dec-1 for OER and 99mV dec-1 fort HER, an overpotential of only 324 and 371mV and the stability is even up to 60h. This work provides a promising strategy for the development of cost-effective, efficient and stable catalysts for energy area.

Stability challenges of transition metal-modified cathodes for electro-Fenton process: A mini-review.

Electro-Fenton (EF) process with transition-metal (TM) modified cathode has been regarded as a green and promising technology for wastewater treatment. Recently, breakthroughs in boosting catalyst activity for both two-electron oxygen reduction reaction (2e- ORR) and Fenton's reaction have gained intensive attention. However, achieving long-term stability of catalysts remains challenging, but is decisive for large-scale applications. This minireview provides fundamental understanding on the activity-stability correlation and the deactivation mechanisms of TM-based catalysts in EF systems, focusing on physical and chemical evolution, metal dissolution, catalyst detachment and structure collapse during long-term electrolysis. Subsequently, ongoing efforts from catalyst design to electrode engineering to stabilize the metal active sites are highlighted. Finally, the challenges and future perspectives in developing active and durable TM-modified cathodes are discussed, serving as a roadmap towards the large-scale application of EF process for wastewater treatment.

Unlocking Peak Efficiency in Anion-Exchange Membrane Electrolysis with Iridium-Infused Ni/Ni2P Heterojunction Electrocatalysts.

Developing cost-effective, highly efficient, and durable bifunctional electrocatalysts for water electrolysis remains a significant challenge. Nickel-based materials have shown promise as catalysts, but their efficiency in alkaline electrolytes is still lacking. Fascinatingly, Mott-Schottky catalysts can fine-tune electron density at interfaces, boosting intermediate adsorption and facilitating desorption to reduce the energy barrier. In this study, iridium-implanted Mott-Schottky Ni/Ni2P nanosheets (IrSA-Ni/Ni2P) is introduced, which are delivered from the metal-organic framework and employ them as the bifunctional catalysts for water electrolysis devices. This catalyst requires a small 54mV overpotential for hydrogen evolution reaction (HER) and 192mV for oxygen evolution reaction (OER) to reach 10 mA·cm-2 in a 1.0m KOH electrolyte. Density functional theory (DFT) calculations reveal that the incorporation of Ir atoms with enriched interfaces between Ni and Ni2P can promote the active sites and be favorable for the HER and OER. This discovery highlights the most likely reactive sites and offers a valuable blueprint for designing highly efficient and stable catalysts tailored for industrial-scale electrolysis. The IrSA-Ni/Ni2P electrode exhibits exceptional current density and outstanding stability in a single-cell anion-exchange membrane electrolyzer.

Metal-organic frameworks-derived CaO/ZnO composites as stable catalysts for biodiesel production from soybean oil at room temperature

Biodiesel presents a sustainable alternative to fossil fuels, yet traditional homogeneous catalysts like sodium and potassium hydroxide face challenges with separation and reuse. Calcium oxide (CaO) is an effective heterogeneous catalyst for biodiesel production, but its chemical instability under reaction conditions restricts its long-term performance. This study introduces MOF-mediated synthesis (MOFMS) of heterogeneous catalysts, specifically CaO@ZnO and ZnO@CaO nanocomposites, from inexpensive and non-toxic metal salts and linkers in water. Comprehensive characterization techniques, including XRD, FT-IR, BET, FE-SEM, ICP, and CO2-TPD, were employed to analyze these catalysts. When applied to biodiesel production from soybean oil at ambient temperature and pressure, CaO@ZnO and ZnO@CaO achieved impressive biodiesel conversion rates of 99% and 92%, respectively, within 25 min. Both catalysts maintained their activity over six utilization cycles, with Ca²⁺ leaching remaining below 4% (2% for CaO@ZnO and 4% for ZnO@CaO) after the sixth run. These results provide valuable insights into catalyst preparation and leaching control, enhancing reusability in biodiesel production. Future research should aim to improve the long-term stability and reusability of these catalysts, investigate their performance with various feedstocks, and evaluate the feasibility for industrial applications.

Monitoring the Fate of Zn in the Cu/ZnO/ZrO2 Catalyst during CO2-to-Methanol Synthesis at High Conversions by Operando Spectroscopy.

In the frame of developing a sustainable chemical industry, heterogeneously catalyzed CO2 hydrogenation to methanol has attracted considerable interest. However, the Cu-Zn based catalyst system employed in this process is very dynamic, especially in the presence of the products methanol and water. Deactivation needs to be prevented, but its origin and mechanism are hardly investigated at high conversion where product condensation is possible. Here, we report on the structural dynamics of a Cu/ZnO/ZrO2 catalyst at 90 bar and 40% CO2 conversion (at equilibrium conditions), investigated in a dedicated metal-based spectroscopic cell specially fabricated using additive manufacturing. This particular reactor configuration aims to mimic the high CO2 conversion part of the catalyst bed and can induce product condensation, which is monitored by operando X-ray absorption spectroscopy. While Cu remained mostly stable throughout the experiment, Zn underwent strong restructuring. The chosen reaction conditions, including the use of CO2 as carbon source and in situ product condensation, were selected to provide insights under industrial conditions. This work highlights the importance of spectroscopic investigations at high conversion levels, offering insights into chemical transformations during deactivation, extending the concept of spatially resolved studies, and thus providing guidance for the design of more stable catalysts.