Solution-processed nanomaterials can be assembled by a range of interfacial techniques, including as stabilizers in Pickering emulsions. Two-dimensional (2D) materials present a promising route toward nanosheet-stabilized emulsions for functional segregated networks, while also facilitating surface energy studies. Here, we demonstrate emulsions stabilized by the 2D materials including the transition metal carbide MXene, titanium carbide (Ti3C2T x ), and develop an approach for in situ measurement of nanosheet surface energy based on emulsion inversion. This approach is applied to determine the influence of pH and nanosheet size on surface energy for MXene, graphene oxide, pristine graphene, and molybdenum disulfide. The surface energy values of hydrophilic Ti3C2T x and graphene oxide decrease significantly upon protonation of usually dissociated functional groups, facilitating emulsion stabilization. Similarly, pristine graphene and molybdenum disulfide increase in surface energy when their surface functional groups are deprotonated under basic conditions. In addition, the surface energies of these pristine materials are correlated with nanosheet size, which allows for the calculation of the basal plane and edge surface energies of pristine nanosheets. This understanding of surface energies and control of emulsion inversion will allow design of emulsion-templated structures and surface energy studies of a wide range of solution-processable nanomaterials.