Freeze Fracture Approach to Directly Visualize Wetting Transitions on Nanopatterned Superhydrophobic Silicon Surfaces: More than a Proof of Principle

Freeze fracturing is applied to make the wetting behavior of artificially nanopatterned Si surfaces directly visible. For this purpose, almost hexagonally arranged nanopillars of fixed areal density (127 μm–2) and diameters (35 nm) but varying heights (40–150 nm) were fabricated on silicon. Measurement of contact angles (CAs) including hysteresis allowed to distinguish between the Wenzel (W) and the Cassie–Baxter (CB) states with droplets completely wetting the pillars or residing on top of them, respectively. Providing additional depth contrast by evaporating the ice replica with thin carbon and (typically 3 nm) platinum layers under 45° allowed resolving 3D features of 5 nm within the ice replica. In this way, laterally sharp transitions from CB- to W-states could be revealed, indicating the formation of zero-curvature water surfaces even on the nanoscale.