Silica nanoparticles were surface-functionalized with diazonium groups. The reaction steps leading to the formation of the diazonium functionality were followed with IR and XPS, and the structure of the diazonium-functionalized nanoparticle was confirmed with solid state NMR. Nanoparticle size distribution was determined with DLS, SEM, and TEM. The nanoparticles were then covalently bonded to gold and iron surfaces. Their spatial distribution over the metal surface was analyzed by SEM. Diazonium modification of nanoparticles represents a new method for the covalent attachment of nanoparticles to metal surfaces.