Ilias Belharouak, Jeffrey S. Spangenberger, Bryant J. Polzin, Matthew A. Keyser, Emma Kendrick
{"title":"Special Issue: Challenges and Opportunities in Sustainable Battery Recycling","authors":"Ilias Belharouak, Jeffrey S. Spangenberger, Bryant J. Polzin, Matthew A. Keyser, Emma Kendrick","doi":"10.1002/aenm.202505320","DOIUrl":"https://doi.org/10.1002/aenm.202505320","url":null,"abstract":"<h2> Conflict of Interest</h2>\u0000<p>The authors declare no conflict of interest.</p>","PeriodicalId":111,"journal":{"name":"Advanced Energy Materials","volume":"44 1","pages":""},"PeriodicalIF":27.8,"publicationDate":"2025-10-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145209429","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":1,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Muhammad Mominur Rahman, Anuj Bisht, Ruhul Amin, Ali Abouimrane, Chol-Bum M Kweon, Ilias Belharouak
{"title":"Thermal Dynamics and Lithium Plating Detection in High-Power Li-Ion Batteries for eVTOL Applications","authors":"Muhammad Mominur Rahman, Anuj Bisht, Ruhul Amin, Ali Abouimrane, Chol-Bum M Kweon, Ilias Belharouak","doi":"10.1002/aenm.202503292","DOIUrl":"https://doi.org/10.1002/aenm.202503292","url":null,"abstract":"The rapid electrification of aerial transportation is driving the need for high-performance Li-ion batteries that can operate reliably under stringent thermal and safety constraints. The unique mission profile of electric Vertical Take-off and Landing (eVTOL) aircraft necessitates a focused investigation into the thermal behavior and safety characteristics of these batteries. In this study, operando isothermal microcalorimetry is employed to examine the thermal evolution of Li-ion batteries under cycling conditions representative of eVTOL operations. These findings reveal that high-power discharge events—such as those during take-off and landing—shift the thermal response toward exothermic behavior, in contrast to the typically endothermic response expected under near-equilibrium cycling conditions. Additionally, the results suggest that advanced electrolyte formulations may help suppress excess heat generation, thereby improving battery safety. Notably, the calorimetric results exhibit a distinct thermal signature associated with lithium plating, offering a potential diagnostic for detecting Li plating during eVTOL operation. Overall, this study demonstrates the utility of isothermal microcalorimetry as a valuable tool for assessing thermal risks in Li-ion batteries for eVTOL applications, and highlights the importance of targeted design strategies to mitigate safety hazards during high-power demand scenarios.","PeriodicalId":111,"journal":{"name":"Advanced Energy Materials","volume":"120 1","pages":""},"PeriodicalIF":27.8,"publicationDate":"2025-10-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145209383","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":1,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Cong Zhong, Siheng Niu, Yixin Li, Suting Weng, Jiacheng Zhu, Zhaoxiang Wang, Lifan Wang, Ting Feng, Xiaoqi Han, Yejing Li, Shaofei Wang, Hong Li, Chun Zhan, Xuefeng Wang
{"title":"Interplay Between the Dissolved Mn2+ and Solid Electrolyte Interphases of Graphite Anode","authors":"Cong Zhong, Siheng Niu, Yixin Li, Suting Weng, Jiacheng Zhu, Zhaoxiang Wang, Lifan Wang, Ting Feng, Xiaoqi Han, Yejing Li, Shaofei Wang, Hong Li, Chun Zhan, Xuefeng Wang","doi":"10.1002/aenm.202503489","DOIUrl":"https://doi.org/10.1002/aenm.202503489","url":null,"abstract":"Transition metal (TM) dissolution and crosstalk are one of the main degradation mechanisms for the capacity fading of lithium‐ion batteries (LIBs). Although significant efforts have been devoted to elucidating the origins of TM dissolution, its crosstalk effect on the anode interface is unclear, especially for its specific chemical state and electrochemical behavior. Herein, the interplay between the dissolved Mn<jats:sup>2+</jats:sup> and the solid electrolyte interphases (SEI) on graphite anode is revealed by different characterization techniques, such as Raman spectroscopy, cryogenic transmission electron microscopy, electron energy loss spectroscopy, and time‐of‐flight secondary ion mass spectrometry. The results demonstrate that Mn<jats:sup>2+</jats:sup> is inclined to coordinate with ethylene carbonate (EC), which is easily decomposed and generates organic‐Mn<jats:sup>2+</jats:sup> species and gaseous byproducts. These gases disrupt the SEI structure, facilitate electrolyte infiltration, and induce continuous growth of the SEI layer. This study deepens the understanding of TM crosstalk on SEI properties and LIB performance, offering potential strategies for enhancing battery durability and performance.","PeriodicalId":111,"journal":{"name":"Advanced Energy Materials","volume":"1 1","pages":""},"PeriodicalIF":27.8,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145195100","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":1,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Jun Su Kim, Uddhav Kulkarni, Jeong Hee Park, Won‐Jang Cho, Won Il Kim, Jin Suk Byun, You Kyung Jeong, Kyungho Ahn, Chul Haeng Lee, Gi‐Ra Yi, Ho Seok Park
{"title":"Eutectic Transition and Interfacial Modulation of Multifunctional Ionic Liquid Additives for Subzero‐Temperature Lithium‐Ion Batteries","authors":"Jun Su Kim, Uddhav Kulkarni, Jeong Hee Park, Won‐Jang Cho, Won Il Kim, Jin Suk Byun, You Kyung Jeong, Kyungho Ahn, Chul Haeng Lee, Gi‐Ra Yi, Ho Seok Park","doi":"10.1002/aenm.202503900","DOIUrl":"https://doi.org/10.1002/aenm.202503900","url":null,"abstract":"Commercial lithium‐ion batteries (LIBs) suffer substantial performance degradation at subzero temperatures due to the increased viscosity of ethylene carbonate (EC)‐based electrolytes and a high energy barrier for lithium‐ion (Li⁺) desolvation at the graphite anode interface, posing critical challenges for applications in cold climates and extreme environments. To overcome this, a phosphonium‐based ionic liquid, allyl trimethyl phosphonium bis(trifluoromethane)sulfonimide (APT), is introduced as a multifunctional electrolyte additive. APT forms a eutectic mixture with EC, effectively lowering the freezing point and viscosity while enhancing ionic conductivity at low temperatures. Furthermore, APT weakens the Li⁺–EC interaction, facilitating more efficient Li⁺ desolvation at the graphite interface, and promotes the formation of a thin, uniform, LiF‐rich solid electrolyte interphase on the graphite anode, leading to the fast interfacial Li⁺ transfer kinetics. Pouch cells with high‐mass‐loading electrodes (NCM811||graphite, 4.9 mAh cm<jats:sup>−2</jats:sup>) and lean electrolyte (3 g Ah<jats:sup>−1</jats:sup>) containing 1 wt.% of APT retained 87.56% of their capacity after 100 cycles at −20 °C, significantly outperforming cells without the additive (64.60% retention). Therefore, this work provides a rational design strategy for multifunctional electrolyte additives that simultaneously optimize bulk transport properties and interfacial stability for reliable LIB operation under subzero conditions.","PeriodicalId":111,"journal":{"name":"Advanced Energy Materials","volume":"17 1","pages":""},"PeriodicalIF":27.8,"publicationDate":"2025-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145194942","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":1,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Rational Electrostatic Iodine Regulation for Photothermally Stable Perovskite Solar Cells","authors":"Xiaotian Zhu, Xingxing Jiang, Sheng Fu, Qiang Weng, Yunfei Li, Nannan Sun, Jiaying Liu, Bo Feng, Wenxiao Zhang, Xiaohui Liu, Xiaodong Li, Andrey S. Vasenko, Junfeng Fang","doi":"10.1002/aenm.202503666","DOIUrl":"https://doi.org/10.1002/aenm.202503666","url":null,"abstract":"Perovskite solar cells (PSCs), as a promising photovoltaic technology, have achieved remarkable progress in efficiency. However, perovskite with soft‐lattice nature inherently suffers from severe iodine losses under photothermal operation, leading to the irreversible degradation in their photovoltaic performance, thereby remaining a great challenge to achieving durable PSCs. Here, electrostatic iodine regulation is reported by rational design on amine cations for photothermally stable PSCs. Theoretical simulations uncover that more alkyl chains binding on the nitrogen atom can not only strengthen the electrostatic interaction between amine cation and triiodine anions (I<jats:sub>3</jats:sub><jats:sup>−</jats:sup>), and the quaternary amine cation can also inhibit the amine cation from deprotonation, yielding much more effective iodine confinement than widely‐used van der Waals interactions. After incorporating tetrabutylammonium iodide (TBAI), substantial enhancements on photothermal tolerances are detected on perovskite films with effectively suppressed iodine losses and metal electrode erosions. Additionally, TBAI also promotes the crystallization and passivate defect, resulting in reduced undesirable recombination within perovskite. Consequently, the targeted PSCs realize a champion efficiency of 26.23%. Moreover, the device features superior operational stability and maintains 92.5% of initial efficiency after 1000 h maximum power point (MPP) tracking at 85 °C.","PeriodicalId":111,"journal":{"name":"Advanced Energy Materials","volume":"70 1","pages":""},"PeriodicalIF":27.8,"publicationDate":"2025-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145194945","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":1,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Low‐Reactivity Electrolytes Achieve Safe and Durable Energy‐Dense NCM955|SiC Pouch Cells","authors":"Junxian Hou, Liqi Zhao, Xuning Feng, Yurui Hao, Dongdong Zheng, Yukun Sun, Qinyu Shi, Chen Cao, Huafeng Li, Li Wang, Languang Lu, Xiangming He, Guohua Ma, Chengshan Xu, Xuebing Han, Cheng Bao, Minggao Ouyang","doi":"10.1002/aenm.202504009","DOIUrl":"https://doi.org/10.1002/aenm.202504009","url":null,"abstract":"Solvent coordination in conventional electrolytes demonstrates poor thermal compatibility with energy‐dense lithium‐ion batteries, resulting in significant reactivity and the potential for thermal failure. Herein, a low‐reactivity electrolyte (LRE) engineered through anionic coordination is developed to regulate thermally‐driven interfacial and crosstalk reactions, achieving inherent safety in 300 Wh kg<jats:sup>−1</jats:sup> LiNi<jats:sub>0.9</jats:sub>Mn<jats:sub>0.05</jats:sub>Co <jats:sub>0.05</jats:sub>O<jats:sub>2</jats:sub>|Graphite@10%SiO (NCM955|SiC) pouch cells. The anionic coordination complexes demonstrate exceptional thermal stability when interfacing with the lithiated anode, effectively suppressing both exothermic reactions and flammable gas evolution. In situ temperature‐dependent X ‐ ray diffraction confirms that LRE stabilizes the lithiated anode phase up to 184 °C, a 51 °C improvement over conventional electrolytes, thereby retarding exothermic electrolyte reduction. Notably, a subsequent 27.3% decrease in reductive gases mitigates crosstalk‐induced cathode degradation while reducing combustion risks in pouch cells when employing LRE. Practical evaluation in 2.4 Ah NCM955|SiC pouch cells reveals that LRE sustains exceptional stability up to 255.0 °C under heating, significantly outperforming conventional cells that failed at 165.6 °C with violent combustion. Furthermore, the 2.4Ah pouch cell maintains an impressive 84.5% capacity retention after 800 cycles, indicating enhanced electrochemical stability and longevity. This work highlights the potential of coordination chemistry in developing safe and durable energy‐dense batteries.","PeriodicalId":111,"journal":{"name":"Advanced Energy Materials","volume":"71 1","pages":""},"PeriodicalIF":27.8,"publicationDate":"2025-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145194946","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":1,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Chunsheng Ding, Qiwen Su, Xiaowen Ruan, Dongxu Jiao, Hao Cai, Minghua Xu, Wei Zhang, Hongwei Huang, Sai Kishore Ravi, Xiaoqiang Cui
{"title":"Polydopamine‐Modified BiOX with Interfacial p‐Orbital Coupling Enhances Superoxide Conversion for Efficient Piezocatalytic H2O2 Production","authors":"Chunsheng Ding, Qiwen Su, Xiaowen Ruan, Dongxu Jiao, Hao Cai, Minghua Xu, Wei Zhang, Hongwei Huang, Sai Kishore Ravi, Xiaoqiang Cui","doi":"10.1002/aenm.202503493","DOIUrl":"https://doi.org/10.1002/aenm.202503493","url":null,"abstract":"Hydrogen peroxide (H<jats:sub>2</jats:sub>O<jats:sub>2</jats:sub>) production via piezocatalysis offers a sustainable route to convert mechanical energy into chemical oxidants using water and oxygen. However, its efficiency is limited by sluggish surface redox kinetics, particularly the conversion of key radical intermediates (•O<jats:sub>2</jats:sub><jats:sup>−</jats:sup> and •OH), and by the kinetic mismatch between charge carrier transfer and proton availability. Here, a polydopamine‐modified bismuth oxide halide (BiOX, X = Cl, Br, I) catalyst is reported that achieves a high piezocatalytic H<jats:sub>2</jats:sub>O<jats:sub>2</jats:sub> production rate of 3083 µmol g<jats:sup>−1</jats:sup> h<jats:sup>−1</jats:sup> and maintains stable activity across a broad pH range (3–9). Spectroscopic analyses and density functional theory calculations reveal that the polydopamine layer introduces interfacial p‐orbital interactions between carbon (from polydopamine) and bismuth sites, which enhance O<jats:sub>2</jats:sub> adsorption, lower the energy barrier for •O<jats:sub>2</jats:sub><jats:sup>−</jats:sup> to •OOH conversion, and accelerate water oxidation for proton supply. This synergistic modulation of radical reaction pathways enables efficient and selective H<jats:sub>2</jats:sub>O<jats:sub>2</jats:sub> generation. The as‐produced H<jats:sub>2</jats:sub>O<jats:sub>2</jats:sub> demonstrates practical utility in pollutant degradation and antimicrobial applications. These findings establish a rational strategy for designing piezocatalysts by engineering interfacial orbital coupling to control reaction intermediate dynamics.","PeriodicalId":111,"journal":{"name":"Advanced Energy Materials","volume":"102 1","pages":""},"PeriodicalIF":27.8,"publicationDate":"2025-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145194963","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":1,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Tingting Liang, Jiangnan Lv, Lanfang Wang, Qianwen Yang, Jianlei Shen, Xiaoting Sun, Wanting Rong, Qiqi Dai, Fang Wang, Yang Liu
{"title":"Unveiling the Role of Topological Surface States in Boosting Electrocatalytic Nitrate Reduction to Ammonia","authors":"Tingting Liang, Jiangnan Lv, Lanfang Wang, Qianwen Yang, Jianlei Shen, Xiaoting Sun, Wanting Rong, Qiqi Dai, Fang Wang, Yang Liu","doi":"10.1002/aenm.202503473","DOIUrl":"https://doi.org/10.1002/aenm.202503473","url":null,"abstract":"Designing efficient catalysts for nitrate reduction reaction (NO<jats:sub>3</jats:sub><jats:sup>−</jats:sup>RR) poses a challenge in advancing the selectivity and yield of ammonia (NH<jats:sub>3</jats:sub>). Unlike conventional catalytic descriptors, topological surface states (TSSs) represent an orthogonal avenue for tailoring catalytic properties, while its role in NO<jats:sub>3</jats:sub><jats:sup>−</jats:sup>RR remains unknown. Here, the semimetallic character of Co<jats:sub>3</jats:sub>Sn<jats:sub>2</jats:sub>S<jats:sub>2</jats:sub>, endowed with robust TSSs is leveraged and enhances charge transport characteristics, to establish this system as a prototypical platform for decoding surface state‐governed NO<jats:sub>3</jats:sub><jats:sup>−</jats:sup>RR mechanism. The catalyst exhibits exceptional NO<jats:sub>3</jats:sub><jats:sup>−</jats:sup>RR performance, achieving a maximum NH<jats:sub>3</jats:sub> Faradaic efficiency of 91.6% at −0.5 V<jats:sub>RHE</jats:sub> and a high NH<jats:sub>3</jats:sub> yield of 22.4 mg h<jats:sup>−1</jats:sup> cm<jats:sup>−2</jats:sup> at −0.6 V<jats:sub>RHE</jats:sub>, while maintaining excellent stability over 200 h in a membrane–electrode assembly electrolyzer, outperforming its semiconductor counterparts. In situ experiments and density functional theory calculations reveal that the TSSs accelerate charge transfer kinetics as well as alleviate the energy barrier for the *NOH → *N step. This work highlights the critical role of TSSs in governing electrocatalytic mechanisms and advances the rational design of high‐performance topological NO<jats:sub>3</jats:sub><jats:sup>−</jats:sup>RR catalysts.","PeriodicalId":111,"journal":{"name":"Advanced Energy Materials","volume":"71 1","pages":""},"PeriodicalIF":27.8,"publicationDate":"2025-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145195101","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":1,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Dongfeng Du, Yumeng Han, Peixuan Liu, Linxiao Wu, Bin Shao, Jingshan Luo
{"title":"Simultaneous Glycolate and Hydrogen Generation Enabled by Unassisted Photocathode-Anode Cells","authors":"Dongfeng Du, Yumeng Han, Peixuan Liu, Linxiao Wu, Bin Shao, Jingshan Luo","doi":"10.1002/aenm.202504721","DOIUrl":"https://doi.org/10.1002/aenm.202504721","url":null,"abstract":"Photoelectrochemical (PEC) water splitting has emerged as a highly promising solar-driven technology for sustainable chemical synthesis. However, this photosynthesis-inspired approach is limited by slow oxygen evolution kinetics. Herein, a bias-free, energy-saving PEC system for simultaneous glycolate and hydrogen production is reported. A highly efficient PdAu catalyst on Ni foam is developed for the upgrading of ethylene glycol (EG) derived from polyethylene terephthalate (PET) plastics, which shows a high performance for electrochemical glycolate production with a low onset potential of 0.25 V vs the reversible hydrogen electrode (RHE) and a high Faradaic efficiency (FE) of 95.6% at 100 mA cm<sup>−2</sup>. When coupled with a cuprous oxide (Cu<sub>2</sub>O) photocathode, the constructed solar-driven PEC-HER//EGOR device achieves a photocurrent density of up to 5.6 mA cm<sup>−2</sup> at zero applied bias, owing to the lower potential requirement of EG oxidation than oxygen evolution reaction. Moreover, it has nearly unity hydrogen FE and 94.8% glycolate FE at 1 h of unbiased operation, showing great potential in continuous and simultaneous hydrogen production and PET-derived EG valorization without any additional bias or expensive chemicals. This work demonstrates a straightforward, energy-efficient, and environmentally benign solar-to-chemical conversion approach for integrating environmental remediation and PEC synthesis.","PeriodicalId":111,"journal":{"name":"Advanced Energy Materials","volume":"118 1","pages":""},"PeriodicalIF":27.8,"publicationDate":"2025-09-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145183239","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":1,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Iain Malone, Seçil Ünsal, R. S. Young, Matthew P. Jones, Francesco Spanu, Shashidhara Marathe, Rhodri Jervis, Hugh G.C. Hamilton, Christopher M. Zalitis, Thomas S. Miller, Alexander J.E. Rettie
{"title":"Deconvoluting Degradation Mechanisms in Anion Exchange Membrane Water Electrolysis Using Operando X-ray Microtomography","authors":"Iain Malone, Seçil Ünsal, R. S. Young, Matthew P. Jones, Francesco Spanu, Shashidhara Marathe, Rhodri Jervis, Hugh G.C. Hamilton, Christopher M. Zalitis, Thomas S. Miller, Alexander J.E. Rettie","doi":"10.1002/aenm.202501339","DOIUrl":"https://doi.org/10.1002/aenm.202501339","url":null,"abstract":"Anion exchange membrane water electrolysers are held back by the low durability of the ionomer in the membrane and catalyst layers. Studying ionomer degradation in these systems is challenging because the main mechanisms - which result in catalyst detachment, membrane thinning, and loss of cationic functionality - have opposing effects on the cell potential. Electrochemical measurements alone are therefore insufficient for elucidating the underlying causes of degradation. To address this, a bespoke miniature-electrolyser-cell is developed for X-ray microtomography imaging of membrane electrode assemblies at 1.6 µm resolution. This setup enables the study of the entire active volume of the electrolyser under static and operando conditions and is validated against standard 5 cm<sup>2</sup> laboratory cells. An operando investigation of degradation in Fumasep-based catalyst-coated membranes reveals both significant membrane thinning and loss of membrane ionic conductivity during stability testing, leading to increased ohmic resistance and cell potential. In contrast, a Selemion membrane shows minimal changes in thickness and conductivity and is significantly more stable compared to Fumasep when exposed to synchrotron radiation. This platform has relevance for operando studies of electrochemical materials and devices generally, including proton exchange membrane electrolysers, fuel cells, and CO<sub>2</sub> electrolysers using both lab-based and synchrotron X-ray sources.","PeriodicalId":111,"journal":{"name":"Advanced Energy Materials","volume":"77 1","pages":""},"PeriodicalIF":27.8,"publicationDate":"2025-09-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145153840","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":1,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}