Thin films of LiCoO2 prepared by RF magnetron sputtering on Si/SiO2/Ti/Au substrates are investigated microstructural and electrochemical properties. The as deposited film shown layered with (003) preferred orientation. After annealing at 923 K in presence of O2 ambient (5×10−2mbar), HT hexagonal phase LiCoO2 is obtained for the films deposited at O2 to Ar ratio 1:9 and at substrate temperature 523 K. LiCoO2 deposit is unambiguously shown two Raman bands at 465 and 545 cm−1 confirming layered hexagonal structure. Also, studied the performance of the LiCoO2 as positive electrode in aqueous (Pt// LiCoO2) and non‐aqueous (Li// LiCoO2) Li‐ion rechargeable batteries.

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