Ultrathin metal materials exhibit quantum size and surface effects that give rise to unique catalytic properties. In this paper, we report a facile liquid synthesis method for polyvinylpyrrolidone (PVP, K30) capped ultrathin Ni(OH) 2 nanosheets with lamellar structure. The as-prepared ultrathin Ni(OH) 2 nanosheets coupled with CdS nanorods exhibit excellent activity in hydrogen generation from water splitting under visible light. The H 2 evolution rate of Ni(OH) 2 /CdS, 40.18 mmol h -1 g Cat. -1 with a quantum efficiency of 66.1% at 420 nm, is ca. 1.5 times that of Pt/CdS with an optimal loading amount (1.25 wt%) under the same reaction conditions. Considering the cost of photocatalysts, the ultrathin Ni(OH) 2 nanosheet coupled CdS photocatalyst may have a promising commercial application in photocatalytic hydrogen production.