Sodium (de)intercalation in the Na 4 MnV-(PO 4 ) 3 NASICON-type cathode has been studied with operando synchrotron X-ray powder diffraction and galvanostatic cycling up to 3.8 and 4.0 V cutoff voltages. Symmetry reduction from rhombohedral to monoclinic was observed immediately after the start of the electrochemical desodiation, with restoring of the rhombohedral phase at 3.8 V. Cycling within the 2.5−3.8 V potential range proceeds through both solid-solution and two-phase processes. An additional voltage plateau at ∼3.9 V is observed, associated with "unlocking" of the Na1 site in the rhombohedral phase. Reverse insertion of Na + cations proceeds via the entire solid-solution region. The experimentally observed discharge capacity increases by ≈14% after raising cutoff voltage. KEYWORDS: sodium-ion battery, NASICON, Na 4 MnV(PO 4 ) 3 , phase transitions, operando XRD

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Switching between solid solution and two-phase regimes in the cathode materials during lithium (de)insertion : combined PITT, in situ XRPD and electron diffraction tomography study Electrochimica acta -

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