Molten Salt Assisted Self‐Assembly: Synthesis of Mesoporous LiCoO2 and LiMn2O4 Thin Films and Investigation of Electrocatalytic Water Oxidation Performance of Lithium Cobaltate

Mesoporous thin films of transition metal lithiates (TML) belong to an important group of materials for the advancement of electrochemical systems. This study demonstrates a simple one pot method to synthesize the first examples of mesoporous LiCoO2 and LiMn2O4 thin films. Molten salt assisted self‐assembly can be used to establish an easy route to produce mesoporous TML thin films. The salts (LiNO3 and [Co(H2O)6](NO3)2 or [Mn(H2O)4](NO3)2) and two surfactants (10‐lauryl ether and cethyltrimethylammonium bromide (CTAB) or cethyltrimethylammonium nitrate (CTAN)) form stable liquid crystalline mesophases. The charged surfactant is needed for the assembly of the necessary amount of salt in the hydrophilic domains of the mesophase, which produces stable metal lithiate pore‐walls upon calcination. The films have a large pore size with a high surface area that can be increased up to 82 m2 g−1. The method described can be adopted to synthesize other metal oxides and metal lithiates. The mesoporous thin films of LiCoO2 show promising performance as water oxidation catalysts under pH 7 and 14 conditions. The electrodes, prepared using CTAN as the cosurfactant, display the lowest overpotentials in the literature among other LiCoO2 systems, as low as 376 mV at 10 mA cm–2 and 282 mV at 1 mA cm–2. Mesoporous thin films of metal lithiates (LiCoO2 and LiMn2O4) can be prepared in one pot using a molten salt‐assisted self‐assembly approach. The salt species acts as a solvent in the assembly process and the metal ion precursors. Mesoporous LiCoO2 thin films display promising performance as a water oxidation electrocatalyst with a low overpotential.