Fig. 3: Characterization of electrochemical exfoliation process.

a Discharge curve of the fabricated half-cell with multi-layered Ti₃C₂Cl₂ pellet as work electrode, Li metal as counter electrode and 1 M LiTFSI in PC as electrolyte. Stage 1, 2, and 3 represents the voltage window of open-circuit voltage (OCV) to 0.86 V, 0.86 V to 0.50 V, and 0.50 V to 0.01 V in the discharging process, respectively. b In-situ XRD patterns for Ti₃C₂Cl₂ upon electrochemical intercalation process, including 45 data sets at various cut-off potentials. c In-situ XRD curves at specific cut-off potentials, including OCV, 1.73 V, 0.86 V, 0.77 V, 0.50 V, and 0.01 V. d In-situ differential electrochemical mass spectrometry (DEMS) analysis of gaseous products in the half-cell. e Ex-situ FT-IR spectra of the pristine Ti₃C₂Cl₂ and intercalated compounds at various cut-off potentials. The red shaded bars represent Li₂CO₃. Source data are provided as a Source Data file.