A novel strategy to synthesize amphiphilic surface-compartmentalized nanopa
rticles based on linear ABC triblock copolymers is presented. These so-call
ed Janus micelles consist of a cross-linked core and a corona with a "north
ern" and a "southern" hemisphere. Selectively cross-linking spherical domai
ns of the polybutadiene middle block in a well-ordered bulk morphology of a
polystyrene-block-polybutadiene-block-poly( methyl methacrylate) triblock
copolymer (SBM) leads to the conservation of the compartmentalization of th
e outer blocks after dissolution of the material. Multi-angle laser light s
cattering gel permeation chromatography, fluorescence correlation spectrosc
opy, small-angle neutron scattering, and static and dynamic light scatterin
g, as well as scanning force microscopy, indicate the existence of an equil
ibrium between molecularly dissolved Janus micelles (unimers) and aggregate
s (multimers), so-called supermicelles.