We report the synthesis of a new monomer, 9,9-diethylfluoren-2-yl methyl methacrylate (FMMA) and its controlled reversible addition-fragmentation chain transfer (RAFT) homopolymerization to give PFMMA with narrow polydispersity indices (PDIs). The corresponding copolymerization with 2-(N,N-dimethylamino)ethyl methacrylate (DMAEMA) also gave well-defined block and random copolymers with controlled molecular weights and narrow PDIs. Their thermal behavior. UV-Vis absorption, and photoluminescent properties were studied. The PDMAEMA-b-PFMMA amphiphilic block copolymers showed self-assembly into aqueous spherical micellar nanoparticles with uniform size. The PFMMA core showed photoluminescence when carrying dichloromethane "guest" molecules and its emission was shown to be quenched after the release of the guest. (C) 2012 Elsevier Inc. All rights reserved.