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  1. Abstract Copper (Cu) is the most attractive electrocatalyst for CO2reduction to multi‐carbon (C2+) products with high economic value in considerable amounts. However, the rational design of a structurally stable Cu‐based catalyst that can achieve high activity and stability towards C2+products remain a grand challenge. Here, a highly stable nickel oxygenate/Cu electrocatalyst is developed with abundant NiOOH/Cu interfaces by in situ electrochemical reconstruction. The nickel oxygenate/Cu electrocatalyst achieves a superior Faradaic efficiency of 86.3 ± 3.0% and a record partial current density of 2085 A g−1for C2+products with long‐term stability. In situ experimental and theoretical studies demonstrates that the exceptional performance in generating C2+products is attributed to the presence of the NiOOH/Cu interfaces which increase *CO coverage, lower energy barrier for *CO coupling and stabilize *OCCO simultaneously. This work provides new insights into the rational design of electrocatalysts to achieve stable and efficient electrocatalytic CO2reduction capabilities. 
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  2. Abstract High‐efficiency and low‐cost catalysts for oxygen evolution reaction (OER) are critical for electrochemical water splitting to generate hydrogen, which is a clean fuel for sustainable energy conversion and storage. Among the emerging OER catalysts, transition metal dichalcogenides have exhibited superior activity compared to commercial standards such as RuO2, but inferior stability due to uncontrolled restructuring with OER. In this study, we create bimetallic sulfide catalysts by adapting the atomic ratio of Ni and Co in CoxNi1‐xSyelectrocatalysts to investigate the intricate restructuring processes. Surface‐sensitive X‐ray photoelectron spectroscopy and bulk‐sensitive X‐ray absorption spectroscopy confirmed the favorable restructuring of transition metal sulfide material following OER processes. Our results indicate that a small amount of Ni substitution can reshape the Co local electronic structure, which regulates the restructuring process to optimize the balance between OER activity and stability. This work represents a significant advancement in the development of efficient and noble metal‐free OER electrocatalysts through a doping‐regulated restructuring approach. 
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  3. Abstract Designing cost‐efffective electrocatalysts for the oxygen evolution reaction (OER) holds significant importance in the progression of clean energy generation and efficient energy storage technologies, such as water splitting and rechargeable metal–air batteries. In this work, an OER electrocatalyst is developed using Ni and Fe precursors in combination with different proportions of graphene oxide. The catalyst synthesis involved a rapid reduction process, facilitated by adding sodium borohydride, which successfully formed NiFe nanoparticle nests on graphene support (NiFe NNG). The incorporation of graphene support enhances the catalytic activity, electron transferability, and electrical conductivity of the NiFe‐based catalyst. The NiFe NNG catalyst exhibits outstanding performance, characterized by a low overpotential of 292.3 mV and a Tafel slope of 48 mV dec−1, achieved at a current density of 10 mA cm2. Moreover, the catalyst exhibits remarkable stability over extended durations. The OER performance of NiFe NNG is on par with that of commercial IrO2in alkaline media. Such superb OER catalytic performance can be attributed to the synergistic effect between the NiFe nanoparticle nests and graphene, which arises from their large surface area and outstanding intrinsic catalytic activity. The excellent electrochemical properties of NiFe NNG hold great promise for further applications in energy storage and conversion devices. 
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  4. Abstract Fe–N–C single‐atom catalysts (SACs) exhibit excellent peroxidase (POD)‐like catalytic activity, owing to their well‐defined isolated iron active sites on the carbon substrate, which effectively mimic the structure of natural peroxidase's active center. To further meet the requirements of diverse biosensing applications, SAC POD‐like activity still needs to be continuously enhanced. Herein, a phosphorus (P) heteroatom is introduced to boost the POD‐like activity of Fe–N–C SACs. A 1D carbon nanowire (FeNCP/NW) catalyst with enriched Fe–N4active sites is designed and synthesized, and P atoms are doped in the carbon matrix to affect the Fe center through long‐range interaction. The experimental results show that the P‐doping process can boost the POD‐like activity more than the non‐P‐doped one, with excellent selectivity and stability. The mechanism analysis results show that the introduction of P into SAC can greatly enhance POD‐like activity initially, but its effect becomes insignificant with increasing amount of P. As a proof of concept, FeNCP/NW is employed in an enzyme cascade platform for highly sensitive colorimetric detection of the neurotransmitter acetylcholine. 
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  5. Abstract The solid–solid electrode–electrolyte interface represents an important component in solid‐state batteries (SSBs), as ionic diffusion, reaction, transformation, and restructuring could all take place. As these processes strongly influence the battery performance, studying the evolution of the solid–solid interfaces, particularly in situ during battery operation, can provide insights to establish the structure–property relationship for SSBs. Synchrotron X‐ray techniques, owing to their unique penetration power and diverse approaches, are suitable to investigate the buried interfaces and examine structural, compositional, and morphological changes. In this review, we will discuss various surface‐sensitive synchrotron‐based scattering, spectroscopy, and imaging methods for the in situ characterization of solid–solid interfaces and how this information can be correlated to the electrochemical properties of SSBs. The goal is to overview the advantages and disadvantages of each technique by highlighting representative examples, so that similar strategies can be applied by battery researchers and beyond to study similar solid‐solid interface systems. 
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  6. Abstract Metal anode instability, including dendrite growth, metal corrosion, and hetero-ions interference, occurring at the electrolyte/electrode interface of aqueous batteries, are among the most critical issues hindering their widespread use in energy storage. Herein, a universal strategy is proposed to overcome the anode instability issues by rationally designing alloyed materials, using Zn-M alloys as model systems (M = Mn and other transition metals). An in-situ optical visualization coupled with finite element analysis is utilized to mimic actual electrochemical environments analogous to the actual aqueous batteries and analyze the complex electrochemical behaviors. The Zn-Mn alloy anodes achieved stability over thousands of cycles even under harsh electrochemical conditions, including testing in seawater-based aqueous electrolytes and using a high current density of 80 mA cm−2. The proposed design strategy and the in-situ visualization protocol for the observation of dendrite growth set up a new milestone in developing durable electrodes for aqueous batteries and beyond. 
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  7. Self-discharge and chemically induced mechanical effects degrade calendar and cycle life in intercalation-based electrochromic and electrochemical energy storage devices. In rechargeable lithium-ion batteries, self-discharge in cathodes causes voltage and capacity loss over time. The prevailing self-discharge model centers on the diffusion of lithium ions from the electrolyte into the cathode. We demonstrate an alternative pathway, where hydrogenation of layered transition metal oxide cathodes induces self-discharge through hydrogen transfer from carbonate solvents to delithiated oxides. In self-discharged cathodes, we further observe opposing proton and lithium ion concentration gradients, which contribute to chemical and structural heterogeneities within delithiated cathodes, accelerating degradation. Hydrogenation occurring in delithiated cathodes may affect the chemo-mechanical coupling of layered cathodes as well as the calendar life of lithium-ion batteries. 
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  8. This study explores the microreactor-assisted soft lithography (MASL) method for direct, one-step synthesis and patterning of additive-free antimony sulfide (Sb2S3) nanostructured thin films. 
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  9. Developing low platinum-group-metal (PGM) catalysts for the oxygen reduction reaction (ORR) in proton-exchange membrane fuel cells (PEMFCs) for heavy- duty vehicles (HDVs) remains a great challenge due to the highly demanded power density and long-term durability. This work explores the possible synergistic effect between single Mn site-rich carbon (MnSA-NC) and Pt nanoparticles, aiming to improve intrinsic activity and stability of PGM catalysts. Density functional theory (DFT) calculations predicted a strong coupling effect between Pt and MnN4 sites in the carbon support, strengthening their interactions to immobilize Pt nanoparticles during the ORR. The adjacent MnN4 sites weaken oxygen adsorption at Pt to enhance intrinsic activity. Well-dispersed Pt (2.1 nm) and ordered L12-Pt3Co nanoparticles (3.3 nm) were retained on the MnSA-NC support after indispensable high-temperature annealing up to 800 °C, suggesting enhanced thermal stability. Both PGM catalysts were thoroughly studied in membrane electrode assemblies (MEAs), showing compelling performance and durability. The Pt@MnSA-NC catalyst achieved a mass activity (MA) of 0.63 A mgPt−1 at 0.9 ViR‐free and maintained 78% of its initial performance after a 30,000-cycle accelerated stress test (AST). The L12-Pt3Co@MnSA-NC catalyst accomplished a much higher MA of 0.91 A mgPt−1 and a current density of 1.63 A cm−2 at 0.7 V under traditional light-duty vehicle (LDV) H2−air conditions (150 kPaabs and 0.10 mgPt cm−2). Furthermore, the same catalyst in an HDV MEA (250 kPaabs and 0.20 mgPt cm−2) delivered 1.75 A cm−2 at 0.7 V, only losing 18% performance after 90,000 cycles of the AST, demonstrating great potential to meet the DOE targets. 
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