We studied the surface reactions of a LiCoO<sub>2</sub>/Li cell under high-voltage conditions using X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XAS), and two-dimensional correlation spectroscopy (2D-COS). 2D XPS correlation spectra show that Li<sub>2</sub>CO<sub>3</sub> is formed first by decomposition of the organic solvents, and then polycarbonate, which is formed by polymerization of the electrolytes, is produced on the cathode surface of the LiCoO<sub>2</sub>/Li system under high-voltage conditions. XAS measurements also confirm that the solid electrolyte interface (SEI) layer is formed on the LiCoO<sub>2</sub> electrode by decomposition of the organic solvents. The thickness of the SEI layer is less than 100 Å.
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