The data experimental synthesis and studies of layered organic-inorganic nanocomposites [Cu 2 (OH) 3 + DS], resulting from ablation of copper in aqueous solutions of surfactantdodecyl sodium sulfate (SDS) are presented. By the methods of absorption spectroscopy of colloidal solutions, X-ray diffraction, scanning electron (SEM) and atomic force microscopy (AFM) of solid phase colloids was traced the formation dynamics of these composites, depending on the exposure duration of copper vapor laser radiation on the target of copper as well as the aging time of the colloid. Bilayered structures of composite [Cu 2 (OH) 3 + DS] fabricated by method of laser ablation copper metal target in liquid are demonstrated for the first time.