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Cobalt metal clusters were synthesized in interlayers of Layered Double Hydroxide (LDH) composed of magnesium and aluminum. Chelate type complex, which is Co-citrate, was used as a precursor of the cluster and intercalated into the interlayer of LDH by ion exchange method. A structural characterization using XRD, IR, TEM-STEM-EELS and nitrogen adsorption/desorption isotherm revealed that Co-citrate was successfully inserted and reduced in the interlayer. Co clusters smaller than 5 nm were formed and catalyzed a hydrolysis reaction of sodium borohydride, resulting in hydrogen generation.