Superwettability involving water affinity has demonstrated prominent
advantages in oil−water separation. However, superwetting surfaces in nonpolar
liquid−polar liquid systems are rarely explored for the separation of organic liquids.
In this work, a protocol of elaborately controlling surface chemistry is presented to
construct dual superlyophobic surfaces for polar or nonpolar liquids in opposite
organic media. On two kinds of silver-roughened copper coatings, a polar hydroxyl
group is subtly integrated with nonpolar perfluoroalkyl chain at the nanoscale.
Prewetted by one organic liquid, the obtained dual superlyophobic mesh can
selectively intercept other immiscible organic liquids, realizing high-efficiency on-
demand separation. In theory, the dual superlyophobic surfaces in organic media are
strongly dependent on their affinity toward polar liquids and the surface roughness.
The discovery may promote the development of organic liquid-related interfacial
materials.