PXRD measurement (Figure ) performed on a drop-casted sample on a low background silicon sample holder confirms the existence of the two phases. Although oscillations in the low angles can be due to a variety of reasons, they can be a characteristic of stacking of lamellar materials. However, in this case, as the distances between the peaks are not the same, they are not only simple stacks of monolayers. The peak at 14° corresponds to the 2H (002) plane reflection, and confirms the formation of 2H-WS2 multilayers. In the inset, the area between 30° and 40° is magnified to better illustrate the presence of the 1T' and 2H phases. The peak at 31.8° corresponds to the reflection from (2-20) of 1T'-WS2 and the peak at 32.8° corresponds to the reflection from (100) of 2H-WS2. This confirms that the WS2 nanosheets synthesized using this pure OAm protocol are a mixture of 1T' and 2H-WS2. In contrast with the previous study, where the 2H-WS2 formed as aggregated nanoflowers, TEM observation shows that this polymorphic WS2 is formed as nanosheet multilayers (Figure ), with a mean diameter of (82 ± 12) nm. The diversity of contrast between different nanosheets confirms that nanosheets are of different thicknesses, partially aggregated or formed of multilayers. Furthermore, the size dispersion of the produced nanosheets is large (see Figure ).