To improve the efficiency of water splitting systems for hydrogen production, the high overvoltages of electrochemical reactions caused by catalysts in the oxygen evolution reaction (OER, Oxygen Evolution Reaction) must be reduced. Among them, LDH (Layered Double Hydroxide) compounds containing transition metal such as Ni, are attracting attention as catalyst materials that can replace precious metals such as platinum that are currently used. In this study, nickel foam, an inexpensive metallic porous material, was used as a support, and NiCo LDH (Layered Double Hydroxide) nanocrystals were synthesized through a hydrothermal synthesis process. In addition, changes in the shape, crystal structure, and water decomposition characteristics of the Mo-doped NiCo LDH nanocrystal samples synthesized by doping Mo to improve OER properties were observed.