In this paper, we prepared nickel nanoparticles for the non oxidative methane activation. A nickel acetate solution was impregnated on silica support and then reduced with NaBH 4 (NiB/SiO 2) exhibiting only small metallic Ni 0 particles of the order of 15 nm. Part of this solid was then oxidized under mild conditions, where Ni ions were re-structured and redistributed as a Ni-O x /SiO 2 oxide solid that after reduction with hydrogen favored the formation of smaller Ni particles. XPS spectra of the Ni-O x /SiO 2 sample before the reduction showed that NiO is the predominant species at the surface and after reduction it indicates the presence of small metallic nickel particles at the surface interacting with the SiO 2 support. XRD and DRIFTS results confirm the structural interaction of metal-support after the mild oxidation and TEM images indicate small particles of the order of 3.5 nm and surface defects. The non oxidative methane activation evidenced significant formation of methane coupling products over the Ni-O x /SiO 2 catalyst during methane chemisorption. Chemisorption of methane on the NiB/SiO 2 showed ethane formation only. The temperature programmed surface hydrogenation (TPSH) results suggested the formation of carbidic species at lower temperatures of adsorption.