SummaryThe deposition of Ni nanoparticles into porous supports is very important in catalysis. In this paper, we explore the use of supercritical CO 2 (scCO 2 ) as a green solvent to deposit Ni nanoparticles on mesoporous SiO 2 SBA-15 and a carbon xerogel. The good transport properties of scCO 2 allowed the efficient penetration of metal precursors dissolved in scCO 2 within the pores of the support without damaging its structure. O were tried as precursors. Different methodologies were used: impregnation in scCO 2 and reduction in H 2 /N 2 at 400 ºC and low pressure, reactive deposition using H 2 at 200-250 ºC in scCO 2 and reactive deposition using EtOH at 150-200 ºC in scCO 2 . The effect of precursor and methodology on the nickel particle size and the material homogeneity (on the different substrates) was analyzed. This technology offers many opportunities in the preparation of metalnanostructured materials.