Liquid-liquid interface of water-hexane provides a unique reaction environment in which CdS nanoparticles capped with mercaptoethylamine could be linked together to form a homodimer with a divalent acid chloride, sebacoyl chloride. Prior to the reaction, mercaptoethylamine-capped CdS in aqueous solution was purified by dialysis and freeze-drying. The observation with a transmission electron microscope suggested the formation of a homodimer of CdS nanoparticles.