NiTi-Layered double hydroxides (LDH) nanosheets with lateral dimensions in the range 30–60 nm have been prepared using a reverse microemulsion method. These materials exhibit excellent photocatalytic activity (∼2148 μmol g⁻¹ h⁻¹) for oxygen evolution from water using visible light. The quantum yield was found to be 65.0% and 20.0% using monochromatic irradiation at 400 and 650 nm respectively.