Nanosheets of cobalt and nickel hydroxides nanosheets were prepared by delamination of layered compounds, CoII(OH)1.73(DBS)0.27·0.87H2O (Co-DBS, DBS = dodecylbenzene sulfonate) and NiII(OH)1.63(DBS)0.37·1.24H2O (Ni-DBS), respectively. Powder X-ray diffraction analyses of the layered compounds revealed lattice parameters of a0 = 3.07 Å and c0 = 30 Å (Co-DBS) and a0 = 3.09 Å and c0 = 30 Å (Ni-DBS) in the hexagonal system. Dispersions of Co-DBS and Ni-DBS in 1-butanol produced colloidal solutions of nanosheets, [Co-DBS]delam and [Ni-DBS]delam, respectively. Poly(vinylpyrrolidone) (PVP) was dissolved in [Co-DBS]delam and [Ni-DBS]delam and the mixtures were dried to yield Co-PVP and Ni-PVP, respectively. These nanosheets measured 150-500 nm for [Co-DBS]delam and 135-400 nm for [Ni-DBS]delam by means of dynamic light scattering. Atomic force microscopy images showed lateral dimensions of 100-500 nm for [Co-DBS]delam and 50-100 nm for [Ni-DBS]delam. In the former image, the cobalt hydroxide nanosheets had a fairly flat terrace structure with thickness of 3.1-3.6 nm and with aspect ratios of 30-150, whereas in the latter image dome-like nanosheets of nickel hydroxide with height of 2.2-2.3 nm were confirmed. These nanosheets were regarded as monolayer. Magnetization experiments at 1.8 K showed hysteresis loops for Co-DBS, Co-PVP, Ni-DBS, and Ni-PVP.