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NaBH4 is an attractive candidate for closed-loop hydrogen generation in small practical applications owing to its ambient condition hydrogen release mechanism, non-toxic byproduct, ability to regenerate, and stability at ambient conditions. The hydrolysis of NaBH4 requires a catalyst to accelerate the hydrogen generation process and cobalt oxide is one such promising catalyst in this reaction. The surface species and crystalline phases of cobalt oxide catalysts play an important role in determining the hydrogen generation rate and overall hydrolysis process. In this study, cobalt oxide nanoparticles are synthesized by a thermal plasma route. The two crystalline phases, namely c-CoO and Co3O4, are tuned using thermal plasma operating conditions. The catalysts so obtained have been thoroughly characterized using analytical techniques like XRD, XPS, HR-TEM, etc. Furthermore, the catalyst was used for hydrogen production in the hydrolysis process of NaBH4. The ex situ X-ray photoelectron spectra recorded at different stages of the hydrolysis process have been extensively used to understand surface modifications occurring at the surface of the catalyst. The Co+3/Co+2 ratio and attachment of other species during hydrolysis analyzed using XPS are correlated with the overall hydrolysis reaction before and after catalysis. It was concluded that the presence of the c-CoO (i.e. initial Co+2 species presence) phase brings stability to hydrogen production in that cycle. [ABSTRACT FROM AUTHOR]