The qualitative observations of particle size from SEM are quantitatively confirmed by dynamic light scattering (DLS), indicating a reduction in mean secondary particle diameter from approximately 30 to 5 µm (Fig. ). Argon sorption measurements reveal type III isotherms according to IUPAC classification for both bulk-and nano-TiS2, with negligible hysteresis loops between adsorption and desorption branches (Fig. ), revealing a nonporous or macroporous character for both materials. With the Brunauer-Emmett-Teller (BET) analysis a roughly doubled specific surface area is determined after ball-milling, increasing from ca. 12 to 24 m 2 /g. X-ray diffractograms of both materials indicate identical phases of trigonal 1T-TiS2 (space group space group P3̅ m1), with no significant broadening of the (001) interlayer spacing signal for nano-TiS2 (Fig. ). Furthermore, secondary phases were not observed. Raman spectroscopy shows typical signals of E1g, A1g, and Sh (Fig. ), further validating the absence of impurities in both samples. Overall, the combination of structural characterization methods indicates that (1) no chemical changes occur and phase-pure TiS2 is maintained after mechanical treatment, and (2) no significant/preferential exfoliation is caused by the mechanical treatment. This suggests that the main mode of particle size reduction during ballmilling is breaking of basal planes.