The stability of phosphorene is shown to be degraded by water. However, the presence of a small amount of water allows the synthesis of high‐quality material in liquid exfoliation of black phosphorus using dimethylsulfoxide as solvent. A phosphorus/water molar ratio between 1.5 and 14 maximizes the quality of the phosphorene flakes and their stability.

A new surface functionalization of exfoliated black phosphorus has been carried out with Ni nanoparticles. The nanohybrid catalyzed the semihydrogenation of phenylacetylene achieving high selectivity to styrene.