We have demonstrated that hybrid multiblock nanorods (MBNs) consisting of gold, nickel, and polypyrrole were prepared by electrochemical deposition method using anodized aluminum oxide as a template. Thiol substituted poly(fluorene) was synthesized through Ni(0)-mediated polymerization. Thiol substituted poly(fluorene) was used for the surface modification of MBNs. The as-synthesized thiol substituted poly(fluorene) and surface modified MBNs were characterized by NMR, SEM, AFM, TEM, TGA, XRD, GPC and XPS. Optical properties of the prepared materials were investigated via UV–vis Spectroscopy and photoluminescence spectroscopy. The poly(fluorene) and surface modified MBNs were showing fluorescence decay life time of 3.47 and 2.77ns, respectively.