Versatile electrochemical cell for Li/Na-ion batteries and high-throughput setup for combined operando X-ray diffraction and absorption spectroscopy

A fundamental understanding of de/intercalation processes (single phase versus multi-phase), structural stability and voltage–composition profiles is pivotal for optimization of electrode materials for rechargeable non-aqueous batteries. A fully operational setup (electrochemical cells, sample changer and interfacing software) that enables combined quasi-simultaneous operando X-ray diffraction (XRD) and absorption (XANES and EXAFS) measurements coupled with electrochemical characterization is presented. Combined XRD, XANES and EXAFS analysis provides a deep insight into the working mechanisms of electrode materials, as shown for the high-voltage Li insertion cathode material LiMn_1.5Ni_0.5O₄ and the high-capacity sodium conversion anode material Bi₂S₃. It is also demonstrated that the cell design can be used for in-house XRD characterization. Long-term cycling experiments on both Li and Na electrode materials prove the hermeticity and chemical stability of the design as a versatile operando electrochemical cell.