Two-dimensional carbide MXenes (Ti 3C 2T x and V 2CT x ) were prepared by exfoliating MAX phases (Ti 3AlC 2 and V 2AlC) powders in the solution of sodium fluoride (NaF) and hydrochloric acid (HCl). The specific surface area (SSA) of as-prepared Ti 3C 2T x was 21 m 2/g, and that of V 2CT x was 9 m 2/g. After intercalation with dimethylsulfoxide, the SSA of Ti 3C 2T x was increased to 66 m 2/g; that of V 2CT x was increased to 19 m 2/g. Their adsorption properties on carbon dioxide (CO 2) were investigated under 0–4 MPa at room temperature (298 K). Intercalated Ti 3C 2T x had the adsorption capacity of 5.79 mmol/g, which is close to the capacity of many common sorbents. The theoretical capacity of Ti 3C 2T x with the SSA of 496 m 2/g was up to 44.2 mmol/g. Additionally, due to high pack density, MXenes had very high volume-uptake capacity. The capacity of intercalated Ti 3C 2T x measured in this paper was 502 V·v –1. This value is already higher than volume capacity of most known sorbents. These results suggest that MXenes have some advantage features to be researched as novel CO 2 capture materials.