Atomic force microscopy measurements. The deposited layers were analysed by AFM to study their size and shape. Topography images in Fig. ) show flakes obtained from freshly prepared MnPS 3 @H 2 O, MnPS 3 @PVP and MnPS 3 @PEI suspensions. In all cases, the images present homogeneous high-quality flakes with larger areas and lower thicknesses than those previously reported using pure sonicated-assisted approach, without preliminary intercalation. Moreover, analysing the height profiles of the flakes in detail, we find ~1 nm thick MnPS 3 bare flakes from MnPS 3 @H 2 O suspension, what means that our exfoliation has arrived to the monolayer limit. However, in the case of MnPS 3 @PVP and MnPS 3 @PEI, higher thicknesses are observed. As the exfoliating procedure is the same for all the samples, this difference should be related to the organic component. In order to get a better interpretation of these results, we studied the height histograms extracted from the AFM pictures of each system Fig. and Fig. . This analysis clearly indicates that while bare MnPS 3 flakes only show maxima at 1 nm and multiples of 1 nm, this is not the case for MnPS 3 @PVP where we detect maxima at ~2.8 nm and their multiples. This periodicity is in full agreement with the new interlayer distance that appears in the PXRD pattern (see above), which dismisses the idea that 2.8 nm height is related to MnPS 3 trilayer stacked units homogenously obtained by the exfoliation procedure. From our point of view, this result can be better understood by picturing the exfoliated material as a hybrid system of single MnPS 3 flakes sandwiched in between tight a