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Polyion complex micelles (PICMs) arise from the spontaneous self-assembly of ionic polymers of opposite charges to form a condensate that is dispersed in aqueous media by a hydrophilic segment, usually poly(ethylene glycol) (PEG), present on at least one of the two ionic polymers. PICMs are used for many applications, especially drug delivery. This protocol paper describes the preparation by atom transfer radical polymerization (ATRP) of diblock copolymers of PEG bearing either positive or negative charges, both of which have been shown to form PICMs. Furthermore, methods of preparation and characterization of PICMs loaded with nucleic acid drugs are presented.