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Instruments / Technical Area	Publication Details	Published	Actions
B18-Core EXAFS	Beyond activity: a perspective on diagnosing instability of reversible O₂ catalysts for metal-air batteries Ricardo P. M. Duarte , Reshma R. Rao , Mary P. Ryan , Trung Dung Tran , Veronica Celorrio , Jonathan Sharman , Alejandro Martinez-Bonastre , Ifan E. I. Stephens Ees Catalysis DOI: 10.1039/D5EY00236B Diamond Proposal Number(s): [27861] Open Access Show Abstract ▼ Abstract: Zinc–air redox flow batteries have high potential to penetrate the stationary energy storage market, due to the abundancy, and low cost of active species – oxygen and zinc. However, their technological fruition is limited by the development of reversible O2 electrodes operating at potentials between 0.6 VRHE to 1.7 VRHE, under which no catalyst material has been shown to be stable over long durations. Despite heavy research on the topic of reversible O2 catalysis, little is known about the parameters controlling the stability of the bifunctional catalyst. Several research accounts assess the activity of reversible O2 catalysts, but only a small portion cover degradation mechanism over such a large potential window. In this perspective, we summarize our current understanding of material challenges for Zn–air batteries, reversible O2 catalyst integration strategies, and electrochemical behaviour, with a particular focus on catalyst stability. Nickel cobalt oxide (NiCo2O4), a promising yet understudied system, is used as an example material for investigations at potentials of both the O2 reduction (ORR) and evolution (OER) reactions. We also report original data employing ex situ X-ray diffraction, electron energy loss spectroscopy, and X-ray photoelectron spectroscopy, as well as electrochemical measurements to study the activity of NiCo2O4. Furthermore, electrochemical accelerated stress tests are coupled with post-mortem transmission electron microscopy, inductively coupled plasma, and X-ray photoelectron spectroscopy to study the dissolution, compositional changes and amorphization of the top surface 5 nm of the catalyst surface. In situ X-ray absorption spectroscopy revealed irreversible oxidation of Co centres in NiCo2O4 during OER, which explains the reduction in activity of the ORR after the catalyst was exposed to anodic OER potentials. This methodology provides a broader method to screen reversible O2 catalyst stability and enables us to summarize future strategies to improve the activity and stability of reversible O2 catalysts and electrodes.	Sep 2025
B18-Core EXAFS E01-JEM ARM 200CF	Understanding the mechanochemical synthesis of the perovskite LaMnO 3 and its catalytic behaviour Rachel H. Blackmore , Maria Elena Rivas , Tugce Eralp Erden , Trung Dung Tran , Huw R. Marchbank , Dogan Ozkaya , Martha Briceno De Gutierrez , Alison Wagland , Paul Collier , Peter P. Wells Dalton Transactions 23 DOI: 10.1039/C9DT03590G Diamond Proposal Number(s): [15151] Open Access Show Abstract ▼ Abstract: Mechanochemistry offers a solventless, ‘waste free’ route to preparing metal oxide catalysts, however, there is limited information on the chemical steps involved. In this work, the perovskite LaMnO3 has been successfully synthesized via mechanochemistry from metal oxide powders, La2O3 and Mn2O3, at room temperature, using a planetary ball mill. Separate ex situ ‘time slices’ were taken during the milling procedure to provide insights into the underlying chemistry. The crystalline material was assessed using XRD, which identified 100% perovskite phase after 3 h of milling. Conversely, characterization by X-ray absorption spectroscopy (XAS) at both the Mn K-edge and La L3-edge provides a very different picture. The XAS data shows that there are significant structural alterations as early as 30 min of milling, with the La precursor dispersed over Mn2O3. Increasing milling time then allows for mechanical activation of both precursors and the formation of powdered LaMnO3, with no calcination step required. The XAS highlights that there is a significant amount of amorphous, oxygen deficient, content even when XRD has identified 100% perovskite phase. The samples were tested for the decomposition of the environmental pollutant N2O; at a milling time of 3 h, the LaMnO3 catalyst displays a much early onset production of N2 compared to a traditional sol–gel synthesized LaMnO3, resulting from increased oxygen deficiency at the surface, confirmed by XPS and STEM-EELS. This is an encouraging sign that mechanochemical routes can be harnessed to provide a sustainable route to preparing mixed metal oxide catalysts with enhanced catalytic performance.	Dec 2019

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