MXenes, a rapidly expanding family of two‐dimensional transition metal carbides and nitrides, have emerged as leading materials for wearable bioelectronics due to their metallic conductivity, termination‐rich surfaces, mechanical compliance, and tunable interlayer structures. However, wearable biosensor performance does not arise from conductivity alone, but from coupled interactions among surface termination chemistry, heterointerface engineering, hierarchical architecture, and device integration under dynamic physiological conditions. This review establishes a predictive structure‐interface‐device framework linking MXene chemistry to system‐level performance across electrochemical, mechanical, gas, optical, and energy‐storage modalities. We analyze how termination‐controlled adsorption governs charge transfer and selectivity, how heterojunction formation modulates carrier density and signal amplification, and how interlayer engineering and restacking suppression regulate ion transport, durability, and stability. Beyond materials design, we evaluate system‐level constraints including impedance stability, wireless communication, AI‐enabled analytics, and self‐powered operation. Key translational challenges, such as oxidation resistance, biocompatibility, scalable manufacturing, and reliable performance in complex biofluids, are assessed using quantitative benchmarks relevant to real‐world wearable deployment. By integrating nanoscale interfacial physics with device and systems engineering, this review defines generalizable design principles for durable, selective, and energy‐autonomous MXene‐enabled biosensors for intelligent, connected, and clinically translatable wearable platforms.

The development of synthetic methods that enable the conversion of readily accessible chemicals into highly valuable small organic molecules, especially those with potential pharmacological and medicinal applications, holds substantial importance in organic synthesis. In this regard, the synthesis of substituted azaindoles and their derivatives, given their structural diversity, presents a considerable synthetic challenge. Herein, we report the development of a novel electrochemical cascade methodology that unites amide bond formation and electro‐induced C–H halogenation of azaindoles in a single, atom‐economical, and environmentally benign process. This approach enables the direct and efficient preparation of halogenated N ‐acyl azaindole amides and carbamates, operating efficiently without the need for additives or supporting electrolytes. Taken together, these results underscore the power of the cascade strategy and its promise for broad application in the exploration of uncharted chemical space relevant to biomedical research.

Experimental high‐throughput electrochemistry (HTE) addresses fundamental limitations of classical electrochemical methods, which are often characterized by high manual effort, low experimental throughput, and limited reproducibility. By employing parallelized and automated experimental systems in combination with advanced data analysis techniques such as Bayesian optimization and machine learning, the development and optimization of electrochemical processes and materials can be significantly accelerated. Emphasis is placed on combinatorial approaches, automated laboratory platforms, and self‐driving systems. This review presents key technologies, application areas, and methodological advances in experimental HTE, including microelectrode arrays and robotics‐based platforms. The aim is to provide a comprehensive overview of the field, bridge existing knowledge gaps, contextualize current developments, and outline future innovation pathways for experimental electrochemical research. Although high‐throughput approaches have increasingly been applied across diverse areas such as battery research, electrocatalysis, and organic electrosynthesis, a coherent methodological overview of the underlying technologies, platform concepts, and levels of automation has been lacking. By consolidating previously scattered developments and systematically comparing different experimental strategies, this article provides a detailed picture of the current state of experimental HTE and identifies key directions for future research, particularly toward autonomous laboratory systems.

The reliable conversion and utilization of green hydrogen are often hindered by carbon monoxide (CO) impurities, which strongly poison conventional platinum catalysts in acidic media. To address this challenge, we developed PdPt alloys supported on reduced graphene oxide (PdPt/rGO) with controlled Pd:Pt ratios and investigated their activity toward the hydrogen oxidation (HOR) and hydrogen evolution reactions (HER). Structural analyses (PXRD, TEM, XPS, CO‐DRIFTS, H 2 ‐D 2 exchange) confirmed alloy formation, lattice strain, and electronic interactions between Pd and Pt, resulting in a downshifted d‐band center. These modifications weaken hydrogen and CO binding, leading to enhanced activity and CO tolerance. Among the series, Pd3Pt1/rGO showed the most balanced performance, delivering higher current densities and lower Tafel slopes than monometallic Pd/rGO and Pt/rGO, with activity comparable to commercial Pt/C. The results highlight that minimal Pt incorporation into Pd‐based catalysts effectively tunes the electronic structure, enabling reversible HOR/HER catalysis in acidic environments. This study provides a rational design approach for developing efficient, CO‐tolerant electrocatalysts to advance hydrogen energy technologies.

The cover image illustrates a modular workflow for electrode fabrication via 3D printing, electrocatalytic evaluation, and mechanistic analysis of reaction pathways and material properties. The resulting data enable machine-learning approaches to identify optimal reaction and manufacturing conditions and support further process automation. More information can be found in the Review by Dandan Gao and Jennifer Christina Schmidt (DOI: 10.1002/celc.202500397).

This paper discusses the ethanol oxidation reaction (EOR) on rough Pt electrodes prepared through electrodeposition. EOR on Pt surfaces is typically characterized by a hysteretic cyclic voltammogram in low ethanol concentrations, where anodic current drops due to the formation of surface‐poisoning species that hinder further reaction. In this study, we show that Pt electrodes with increased surface roughness ( R f ) exhibit a linear EOR response up to 1.4 V versus RHE, in contrast to the hysteretic behavior reported in the literature. We further show that comparable linearity can be induced by increasing the bulk ethanol concentration or decreasing the water content in the electrolyte. These systemic perturbations suggest that enhanced surface roughness promotes higher local coverage of ethanol and its intermediates at the electrode surface, thereby suppressing competitive adsorption of water/OH − species and shifting Pt surface poisoning to more positive potentials. Furthermore, we demonstrate that the antipoisoning effect associated with rough Pt electrode can be amplified by polymer co‐electrodeposition, which yields lower current decay rates and higher acetate formation rates compared to rough Pt without polymer. Together, these findings highlight the critical role of catalyst surface roughness in mitigating surface‐poisoning processes and promoting efficient electro‐oxidation of small organic molecules.

Electrochromic devices (ECDs) are promising as smart windows, as they provide dynamic control over light transmission and contribute to reducing energy costs in buildings. However, sluggish response times and low cycling stability highlight key barriers to their commercialization. One approach to tackle these is to optimize gel polymer electrolytes (GPEs) for ECDs, as they already balance high ionic conductivity and low risk of leakage. This study compares the GPE compositions with and without crosslinker poly(propylene glycol) diacrylate (PPGDA) in hybrid and inorganic ECDs. These include Fe(II) metal coordination polymer (Fe(II)‐MCP) with Prussian blue (PB) and WO 3 with NiO x . Some of the ECD performance parameters are not altered, like contrast ratio and coloration efficiencies, as they correspond to the electrochromic materials. By adding PPGDA to the GPE the charge density is lower for both cell types and the cyclability over 1000 switching cycles is demonstrated. Additionally, PPGDA reduces the bleaching time for the WO 3 /NiO x device, while the coloring time of the Fe(II)‐MCP/PB devices slightly increases. These results show the benefits of the crosslinker PPGDA in a GPE on response time and cycling stability of two various ECDs.

During aluminum (Al) electrolysis, large amounts of spent cathode carbon (SCC) are generated, often contaminated with hazardous substances such as fluorides and cyanides. As a result, SCC is classified as a dangerous solid waste posing long‐term risks to ecosystems and human health if untreated. This review comprehensively analyzes the chemical composition, formation mechanisms, and environmental hazards of SCC, and summarizes current physical and chemical remediation strategies. Unlike previous reviews, it integrates a comparative life cycle assessment (LCA) to evaluate the environmental performance of different SCC treatment routes, offering a holistic view of their sustainability. Additionally, it highlights opportunities for recovering valuable elements, particularly carbon (C), fluorine (F), and lithium (Li), and explores high‐value recycling pathways such as battery anodes, graphene, and SiC semiconductors. Although many studies focus on laboratory‐scale recovery efficiencies, environmental sustainability assessments remain scarce. Integrated processes including molten salt roasting, ultrasonic‐assisted leaching, and cryolite regeneration show promise for detoxification and resource recovery. However, challenges such as C passivation, fluoride stabilization, and high energy demands persist. By combining technological and environmental perspectives, this review provides a framework for developing scalable, low‐emission SCC recycling technologies aligned with circular economy principles.