Metallic nanoparticles of palladium and silver ranging in size from 1 to 15 nm were produced entirely within carbon dioxide by spraying a carbon dioxide carrier solution containing CO2-soluble metal precursors into a CO2 receiving solution containing a reducing agent (NaBH(OAc)(3) or 112) and fluorocarbon thiol stabilizing ligands. The process uses the benign solvent CO2 while also allowing for the production of nanoparticles with a limited number of chemical components. Particles were characterized by transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS).