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Activated carbon was prepared from cellulose-based aerogel (aerocellulose) monoliths by carbonization and subsequent CO₂ activation. The monolithic structure of the as-synthesized aerocellulose was retained during the carbonization and activation processes. The as-synthesized aerocellulose monolith was mainly mesoporous with well-developed surface area, large total pore volume, with only moderate CO₂ uptake. In order to enhance CO₂ adsorption, microporosity of carbonized aerocellulose was increased upon CO₂ activation. The resulting activated carbon showed an enhanced specific surface area of ~750 m² g⁻¹, total pore volume of 0.43 cm³ g⁻¹, and volume of micropores (pore widths <2 nm) of ~0.27 cm³ g⁻¹. Activation of carbonized aerocellulose resulted in about five-fold increase in the specific surface area and over 27-fold increase in the volume of micropores as compared to the as …