LiCoO
2 films were prepared on polycrystalline Al
2O
3 substrates by metal organic chemical vapor deposition (MOCVD), and the effect of the Li to Co source vapor ratio (
RLi/Co) and substrate temperature (
Tsub) on the phases, orientation, morphology, and deposition rates were investigated. At
RLi/Co > 2.0, Li
2CO
3, Li
xCo
1−xO, and a LiCoO
2–CoO solid solution were co-deposited with LiCoO
2, whereas Co
3O
4 was co-deposited with LiCoO
2 at
RLi/Co < 0.7. Single-phase LiCoO
2 films were obtained in the
RLi/Co range of 0.7–2.0 at
Tsub > 873 K. Rutherford backscattering spectrometry revealed that single-phase LiCoO
2 film had uniform and stoichiometric composition. The orientation of single-phase LiCoO
2 films changed from (003) to (104) and (012) with increasing
Tsub at
RLi/Co ~ 1.0. LiCoO
2 film co-deposited with Co
3O
4 at
RLi/Co = 0.4 showed significant (101) orientation. The (003)-oriented LiCoO
2 had a flat surface with hexagonal faceted texture, whereas the (101)- and (104)-oriented LiCoO
2 had platelet grains in which the plate faces were tilted relative to the substrate surface. The highest deposition rate of single-phase LiCoO
2 film was 10–20 µm h
−1, which was 100 times greater than that reported in the literature.
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