The network formation employing hydrophobically modified poly(ethylene oxide) (HM-PEO) with dissimilar terminal groups poly(ethylene oxide) (PB) and poly(perfluoropropylene oxide) (PFPO) was explored. A BOF triblock terpolymers was able to self-assemble into a compartmentalized network, in which fluorocarbon disks with 14 nm diameter and 5nm thickness are distributed within thin PB sheets. To prepare an aqueous dispersion of BOF, a film of the desired amount of polymer was hydrated, and the resulting mixture was stirred at 65°C for 24 h. Mixtures of water and heavy water with compositions varying according to the desired contrast match, were used for SANS experiments. Three different contrast matching H 2O/D 2O mixtures but with same polymer concentration were prepared for SANS experiments. A bicontinuous structure results from the arrangement of strongly hydrophobic end blocks (PB and PFPO) into space-spanning sheets with nonpreferential curvature, while the PEO chains apparently shield the hydrophobes from water.