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To this day, elucidating the charge transfer process in electrode material upon electrochemical cycling remains a challenge, primarily due to the complexity of chemical reactions at the electrode surfaces. Here we present an elegant and reliable method to probe bulk sensitive soft edges for elucidating anodic and cathodic charge compensation contribution via x-ray Raman scattering spectroscopy. By using a hard x-ray incident beam this technique circumvents surface limitations and is practically free of self- absorption due to its non-resonant nature. In addition, it does not require complex sample preparation or experimental setups, making it an ideal tool for potential in situ analysis of the electronic structure of electrode materials. In this study we monitored for the first time bulk soft edges of both oxygen and transition metal (iron) of the cathode material Li2FeSiO4 during one complete electrochemical cycle concurrently. Our results reveal that the redox mechanism relies primarily on the iron (cat...

Bulk-Sensitive Soft X-ray Edge Probing for Elucidation of Charge Compensation in Battery Electrodes