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The layered P2‐Na  x  MO 2  (M: transition metal) system has been widely recognized as electronic or mixed conductor. Here, we demonstrate that Co vacancies in P2‐Na  x  CoO 2  created by hydrogen reductive elimination lead to an ionic conductivity of 0.045 S cm −1  at 25 °C. Using in situ synchrotron X‐ray powder diffraction and Raman spectroscopy, the composition of the superionic conduction phase is evaluated to be Na 0.61 (H 3 O) 0.18 Co 0.93 O 2 . Electromotive force measurements as well as molecular dynamics simulations indicate that the ion conducting species is proton rather than hydroxide ion. The fact that the Co‐stoichiometric compound Na  x  (H 3 O)  y  CoO 2  does not exhibit any significant ionic conductivity proves that Co vacancies are essential for the occurrence of superionic conductivity.

Superionic Conduction in Co‐Vacant P2‐Na x CoO 2 Created by Hydrogen Reductive Elimination