The morphological features of the tin-dichalcogenides SnS2, Sn(S0,5Se0,5)2, and SnSe2 samples diluted in water and isopropanol, followed by natural drying at RT or by IR, and annealed at 300 °C and diluted in water and isopropanol, followed by drying at RT are respectively shown from Fig. to Fig. . The SEM images reveal an overall tendency to form aggregated microparticles, along with some nanometric structures. The red, cyan and green arrows highlight regions with cracks, step-like grains, as well as platelet-like structures, respectively. The last two are typical of lamellar crystal structures, although they do not represent the sample morphology on large scale. It is well known that the high-energy mechanical milling process is based on a continuous cycle of cold welding, fracturing, and resoldering of the powder mixture. It favors the formation of defective aggregates without a well-defined geometry, and regions with high mechanical stress . In this context, the deformed and defective morphology of these samples is very reactive, causing an exothermic relaxation in the DSC measurements .