The microphase structure of a series of poly(styrene-b-methylphenylsiloxane) (PS-b-PMPS)-diblock copolymers with various compositions and molecular weights has been studied by small-angle X-ray scattering, electron spectroscopic imaging and solid-state nuclear magnetic resonance spectroscopy. This diblock copolymer system is miscible within a distinct range of temperature and molecular weight exhibiting an upper critical solution temperature. The three chosen methods which complement each other can be applied to the chemically un modified model system. The results of the various measurements correlate to describe the microphase structure, the domain size and the interphase.