Publication date: 15th December 2025
Improving the performance of rechargeable batteries in terms of energy density, lifetime, and reliability is a central challenge for modern energy storage technologies. Achieving these improvements requires a detailed understanding of the processes that govern electrochemical behaviour at the atomic and electronic scales during operation. Battery performance is strongly determined by how charge is compensated within the electrode during cycling, through the interplay of transition-metal redox activity, anionic redox contributions, and associated structural rearrangements.
Understanding how different redox-active centres coevolve during battery operation is essential for disentangling complex charge-compensation mechanisms in layered cathode materials. In this work, we present a correlative operando analysis framework designed to track the coupled evolution of Mn and Ni redox processes using Multivariate Curve Resolution (MCR) applied to X-ray Absorption Spectroscopy (XAS) data.
Operando Mn and Ni K-edge XAS datasets acquired during electrochemical cycling are first decomposed independently using MCR to extract chemically meaningful spectral components and their concentration profiles. These component evolutions are then synchronized in time and analysed through direct correlation plots, enabling the identification of distinct regimes of coupled or decoupled Mn-Ni behaviour throughout the state of charge. By focusing on the relative coevolution of MCR-derived components rather than on absolute spectral changes, this approach provides a robust and intuitive representation of redox dynamics that is less sensitive to experimental noise or material-specific spectral features.
Applied to Li- and Na-based layered oxides, the methodology reveals recurring linear correlation regimes associated with different charge-compensation modes and highlights transitions that are not evident from single-edge or single-technique analyses. These results demonstrate how MCR-based correlative analysis can serve as an effective intermediate step between raw operando data and mechanistic interpretation, offering a transferable tool for comparative redox studies across battery materials.
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