Nylon-6,6 was synthesized in cetyltrimethylammonium chloride reverse micelles adsorbed on silica surfaces to study the feasibility of preparing a surface modified with grafted polyamide brushes using the immobilized reverse micelle as a microreactor. The nylon-modified silica gel preparation procedure involved: (1) adsorption of the CTAC reverse micelles containing 1,6-hexanediamine and sodium hydroxide onto silica gel surfaces, (2) in situ polymerization of 1,6-hexanediamine and adipoyl dichloride at the reversed micellar interfaces, and (3) the removal of residual components such as CTAC or reverse micelles. The nylon produced on silica surface was characterized in detail. The principal interaction in the immobilization of nylon on silica surface may be hydrogen bonding between the terminal amine groups of nylon and the surface silanol groups. Atomic force microscopy images of the nylon monolayers attached to glass plate surfaces showed the formation of grafted polymer brushes or nanoclusters on the surfaces. To characterize the prepared surface of the silica gel, the modified silica gel particles were successfully employed in chromatographic analysis as a stationary phase for the separation of o-, m-, and p-nitroanisoles using cyclohexane as a mobile phase.