The continuous tunability of iron oxide nanoparticle dimensions is demonstrated using the pH controlled loading of ferric nitrate from aqueous solution into polystyrene–block–polyacrylic acid reverse micelles deposited on a silicon substrate. Quasi-hexagonally ordered two-dimensional arrays of iron oxide nanoparticles with a systematic tunability of particle heights in the sub-10 nm regime and a constant periodicity are obtained and characterized with atomic force microscopy and x-ray photoelectron spectroscopy.