Among the many materials with a 2D structure, the family of transition metal chalcogenophosphates (MPX 3 ; where M = V, Cr, Mn, Fe, Co, Ni, Cu, Zn and Cd and X = S, Se, Te) has recently attracted the growing attention of the research community. This interest arises from its extensive variety of electronic and magnetic properties. Thus, for example, these materials exhibit a wide bandgap (up to 3.5 eV) 4 that broaden their potential application in optoelectronics; In addition, these materials exhibit cooperative magnetic properties, in particular antiferromagnetism, which has been proven to persist even in the 2D limit. Interestingly, the reliance between structural, electronic and magnetic properties boosts their potential in spintronics. Furthermore, these materials have also been studied as promising candidates for electrocatalytic applications. Notice that most of the works focused on the fundamental characterization of ultrathin layers use dry approaches to obtain these layers, either top-down, using the scotch-tape method for exfoliating large crystals, 10 or bottom-up strategies for synthesizing nanosheets in a controlled way. These methods give rise to high quality single or few layers MPX 3 with a low degree of defects. However, for large-scale applications they suffer from an important lack of scalability. From a different point of view, we find methods in solution, like bottom-up chemical synthesis from thiohypophosphate (P 2 S 6 ) 4-anions and divalent metallic cations M 2+ , and the top-down liquid-phase exfoliation (LPE) approach. These strategies provide much higher versatility and processability, making them perfect candidates for developing 2D-crystal-based functional inks. Regarding LPE approach, it is a straightforward method but with a low degree of control over the quality of the layers. Even so, very few works have tried to exfoliate MPX 3 through sonication-assisted exfoliation. This method has permitted to improve, for example, the electrocatalytic activity of these nanosheets with respect to the bulk. Unfortunately, the thickness and the lateral dimension of the resulting flakes are not of the finest quality. In order to improve the quality of the flakes, we can benefit from the well-known capacity of MPX 3 family to chemically intercalate ions in between their layers 17 to expand them before the sonication step. This ability was first applied by to exfoliate MnPS 3 and CdPS 3 . However, full characterization of the resulting layers was not reported, and it was mandatory to use polyvinylpyrrolidone (PVP) as a capping agent to achieve the exfoliation of MnPS 3 .