Nanoporous carbide-derived carbon (CDC) was synthesized starting with Ti2AlC powders via chlorination in the 400−1200 °C temperature range. X-ray diffraction, Raman spectroscopy, and transmission electron microscopy (TEM) confirmed a structural dependence on chlorination temperature. At low chlorination temperatures, the CDC structure appeared primarily amorphous. Graphitic ribbons, as well as sharply bent graphitic structures, were observed at 800 °C. As the chlorination temperature was further increased to 1000 °C, the width of the graphitic ribbon increased. No significant increase in graphitization occurred between 1000 and 1200 °C. Sorption measurements determined the presence of micropores (0.40−2.0 nm) after chlorination at 400 °C; chlorination at 800 °C or higher resulted in both micro- and mesopores (0.35 to >7 nm).