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Abstract Pressure‐induced swelling has been reported earlier for several hydrophilic layered materials. MXene Ti3C2Tx is also a hydrophilic layered material composed by 2D sheets but so far pressure‐induced swelling is reported for this material only under conditions of shear stress at MPa pressures. Here, high‐pressure experiments are performed with MXenes prepared by two methods known to provide “clay‐like” materials. MXene synthesized by etching MAX phase with HCl+LiF demonstrates the effect of pressure‐induced swelling at 0.2 GPa with the insertion of additional water layer. The transition is incomplete with two swollen phases (ambient with d(001) = 16.7Å and pressure‐induced with d(001) = 19.2Å at 0.2 GPa) co‐existing up to the pressure point of water solidification. Therefore, the swelling transition corresponds to change from two‐layer water intercalation (2L‐phase) to a never previously observed three‐layer water intercalation (3L‐phase) of MXene. Experiments with MXene prepared by LiCl+HF etching have not revealed pressure‐induced swelling in liquid water. Both MXenes also show no anomalous compressibility in liquid methanol. The presence of pressure‐induced swelling only in one of the MXenes indicates that the HCl+LiF synthesis method is likely to result in higher abundance of hydrophilic functional groups terminating 2D titanium carbide.

Pressure‐induced swelling has been reported earlier for several hydrophilic layered materials. MXene Ti3C2Tx is also a hydrophilic layered material composed by 2D sheets but so far pressure‐induced swelling is reported for this material only under conditions of shear stress at MPa pressures. Here, high‐pressure experiments are performed with MXenes prepared by two methods known to provide "clay‐like" materials. MXene synthesized by etching MAX phase with HCl+LiF demonstrates the effect of pressure‐induced swelling at 0.2 GPa with the insertion of additional water layer. The transition is incomplete with two swollen phases (ambient with d(001) = 16.7Å and pressure‐induced with d(001) = 19.2Å at 0.2 GPa) co‐existing up to the pressure point of water solidification. Therefore, the swelling transition corresponds to change from two‐layer water intercalation (2L‐phase) to a never previously observed three‐layer water intercalation (3L‐phase) of MXene. Experiments with MXene prepared by LiCl+HF etching have not revealed pressure‐induced swelling in liquid water. Both MXenes also show no anomalous compressibility in liquid methanol. The presence of pressure‐induced swelling only in one of the MXenes indicates that the HCl+LiF synthesis method is likely to result in higher abundance of hydrophilic functional groups terminating 2D titanium carbide. [ABSTRACT FROM AUTHOR]