The experimental data of studies of layered organic-inorganic nanocomposites ((𝛽)-Zn(OH)2+DS) and (Cu2(OH)3+DS) which were produced in the result ablation of zinc and copper in aqueous solutions of surfactants—dodecyl sodium sulfate (SDS) and sodium bis-ethylhexyl succinate (AOT)—are presented. Dependence of the formation dynamics of these composites on an exposure time of radiation and on an aging time of colloids was studied by the absorption spectroscopy, by X-ray diffraction, by scanning electron (SEM), and atomic force microscopy (AFM). Composite (Cu2(OH)3+DS) with bilayered structure was produced by method of laser ablation of the copper metal target in liquid for the first time.