Small aminosilica nanoparticles (NPs, 12 nm SiO2 core) were covered with ferrocenyl (Fc) and pentamethylferrocenyl (Fc*) groups by reactions with metallocenyl carbonyl chlorides. Cyclic voltammetry in methanol/acetonitrile showed a single fully chemically- and electrochemically-reversible wave with a diffusion-controlled current; colorimetric titrations with [FcCOMe][BF4] of the Fc-SiO2 and Fc*-SiO2 NPs indicated a coverage of the aminosilica NPs of 335 ± 50 Fc or 240 ± 40 Fc* groups.