A new metavanadate inserted layered double hydroxide was prepared by a chimie douce method. This material was characterized by X-ray diffraction, infrared spectroscopy, chemical analysis and thermogravimetry. Its structure consists of a packing of Ni 0 . 7 0 Co 0 . 3 0 (OH) 2 slabs, with (VO 3 ) n - n metavanadate anionic chains intercalated within the interslab space. The influence of such chains on both the structural features and the exchange properties of the material was investigated. Heating this material to 190°C leads to a grafting of the VO 4 tetrahedra to the slabs coupled with a partial chain fragmentation.