Carbonaceous templates with nanopores <10 nm in diameter have been produced using low molecular weight diblock copolymers of poly(styrene-b-acrylonitrile). PS-b-PAN was synthesized using sequential living and controlled polymerization approaches, where the first block was anionically synthesized while the second block was added using atom transfer radical polymerization (ATRP). Polystyrene with a hydroxy end group was synthesized anionically and then reacted with 2-bromoisobutyryl bromide to create the ATRP macroinitiator. Acrylonitrile was polymerized using ATRP procedures. Polymer microphase separation, stabilization, and subsequent pyrolysis were characterized by small-angle X-ray scattering (SAXS) and transmission electron microscopy (TEM).