In this study, we have focused on the water-splitting reaction using lithium cobalt oxide LiCoO
2 as a hydrogen generation technique. LiCoO
2 is known as positive electrode of lithium ion battery. The valence fluctuation of Co and diffusivity of Li are also attractive for the water-splitting. To understand the reaction process, the hydrolysis and regeneration of LiCoO
2 are separately investigated and analyzed by using X-ray diffraction measurement, X-ray photoelectron spectroscopy (XPS). XPS spectra of the products after the hydrolysis reaction indicated that LiOH is formed at 300 °C, although the reaction yield is very low. LiCoO
2 is synthesized by the reaction between LiOH and Co
3O
4 at 500 °C. From the results, a possible reaction process of water-splitting by LiCoO
2 is proposed.
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