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Surface Free Energy (SFE) has become a relevant design parameter to produce materials and devices with controlled wettability. The non-destructive measurement of SFE in nanopatterned super-hydrophobic hard surfaces is a challenge in both research and industry since in most cases time-consuming contact angle measurements are not feasible. In this work, we present a novel nanoindentation based method for the measurement of pull-off adhesive forces by carefully controlling environmental and instrumentation issues. The method is found to measure SFE over five orders of magnitude, covering hydrophilic to super-hydrophobic surfaces, and has been validated with contact angle measurements. Its limitations and shortcomings are critically discussed, with a specific focus on the experimental issues that could affect the reliability and reproducibility of the results. Finally, the potential applications of the newly developed methodology include fast non-destructive mapping of SFE over heterogeneous surfaces with spatially controlled wettability. Graphic abstract

A novel nanoindentation protocol to characterize surface free energy of superhydrophobic nanopatterned materials