A Single‐Source Co/Li/O Organometallic Precursor for Nanocrystalline LiCoO 2 – Synthesis, Formation Pathway, and Electrochemical Performance

A single‐source precursor route to phase‐pure LiCoO 2 by employing the organometallic precursor [(COD) 2 CoLi(thf) 2 ] ( 1 ) to introduce a Co/Li/O 1:1:2 stoichiometry is described for the first time. Compound 1 undergoes decomposition in the presence of oxygen, forming nanoscaled, electrochemically active LiCoO 2 starting at a temperature as low as 200 °C. Its temperature‐dependent formation pathway was studied by various spectroscopic and microscopic techniques. The transition temperature for the evolution of layered LiCoO 2 is above 400 °C. Electrochemical studies indicate that the low‐temperature modification of LiCoO 2 can be obtained at 500 °C, showing moderate electrochemical battery performance.