The self-assembly of amphiphilic metallo-supramolecular A-b-B-b-A triblock copolymers containing a B block formed from a bisfunctional terpyridine monomer and an A block based on a monofunctional terpyridine polymer is described. these polymers have been prepared by a polycondensation approach, based on metal-ligand complexation, in which the molecular weight of the central B block has been controlled by the addition of a monofunctional chain-stopper A. Details for the preparation of the A-b-B-b-A triblock copolymers based on the tpy(2)Ni(II), tpy(2)Fe(II), and tpy(2)Co(II) connectivity are given. The influence of the different binding strength of Ni(II), Fe(II), and Co(II) metal ions with terpyridine ligands on the metallo-polycondensation reaction and on the micellization behavior of those materials was studied. Micelles of the obtained block copolymers were prepared and studied by DLS and cryo-TEM.