Surface-functionalized polymeric nanoparticles were prepared by: a) self-assembly of poly(4-vinyl-benzocyclobutene-b-butadiene) diblock copolymer (PVBCB-b-PB) to form spherical micelles (diameter: 15-48 nm) in decane, a selective solvent for PB, b) crosslinking of the PVBCB core through thermal dimerization at 200-240 degrees C, and c) cleavage of the PB corona via ozonolysis and addition of dimethyl sulfide to afford aldehyde-functionalized nanoparticles (diameter: similar to 16-20 nm), along with agglomerated nanoparticles ranging from similar to 30 to similar to 100 nm in diameter. The characterization of the diblock copolymer precursors, the intermediate micelles and the final surface-functionalized crosslinked nanoparticles was carried out by a combination of size exclusion chromatography, static and dynamic light scattering, viscometry, thermogravimetric analysis, H-1 NMR and FTIR spectroscopy and transmission electron rnicroscopy. Published by Elsevier Ltd.