Triblock copolymer nanotubes bearing end-exposed poly(acrylic acid) or PAA core chains were prepared. The exposed PAA chains were reacted by amidization with a large excess of polystyrene spacer chains possessing amino end groups or amino-containing end blocks to graft the spacer chains. The amino groups at the other end of the spacer chains were then reacted with nanospheres bearing surface carboxyl groups to connect the nanotubes to nanospheres. The products from such a coupling reaction ranged from multiarm adduct to surfactant- and dumbbell-like objects. Product control using different strategies was explored. The products may have interesting properties and applications.