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Three-dimensional ceramic nanostructured films were produced from silicon-containing triblock copolymer films exhibiting the double gyroid and inverse double gyroid morphologies (space groupIa3d). A one-step room-temperature oxidation process that used ozonolysis and ultraviolet irradiation effected both the selective removal of the hydrocarbon block and the conversion of the silicon-containing block to a silicon oxycarbide ceramic stable to 400°C. Depending on the relative volume fraction of the hydrocarbon block to the silicon- containing block, either nanoporous or nanorelief structures were fabricated with calculated interfacial areas of ∼40 square meters per gram and pore or strut sizes of ∼20 nanometers.