Block molecules consisting of crystalline and amorphous blocks recently gained interest towards application in novel nanomaterials. This is due to the unique properties derived from their highly ordered nanoscale structures, such as unprecedented morphologies or small domain spacings. This project explores the synthesis, characterization, and morphology of block molecules containing oligodimethylsiloxane (oDMS), end capped with small Kevlar strands, in an attempt to create a library of block molecules that vary in molecular weight. The methods approach allowed the coupling reactions of polymers to be specific in order to ensure a customized molar mass. Thus, allowing the properties and phase behavior to be studied using small-angle X-ray scattering, and DSC while having molecular mass as a variable.