Comparison of test methods estimating the stiffness of ultrathin coatings

A key engineering parameter of thin coatings is their stiffness. Stiffness characterization of ultrathin coatings with a nanometer scale thickness is experimentally challenging. In this work, three feasible methods have been used to estimate the Young’s modulus of metal coatings on polymer films. The methods are: (1) nanoindentation, (2) strain-induced elastic buckling and (3) peak-force measurements integrated in atomic force microscopy. The samples were prepared by atomic layer deposition of TiO₂ (6 and 20 nm thick) and mixed oxides of TiO₂ and Al₂O₃ (4 and 20 nm thick). The differences in estimated Young’s modulus are interpreted in terms of the underlying assumptions and test conditions. Their specific advantages and drawbacks are also compared and discussed. In particular, the nanoindentation necessitates a sufficiently sharp indenter tip to make localized measurements dominated by the coating. The strain-induced elastic buckling method is simple in practice, but showed a large scatter due to variation in local coating thickness and irregular deformation patterns. The stiffness characterization using atomic force microscopy gave the most consistent results, due to a sharp tip with a radius comparable to the thinnest coating thickness. All methods gave a higher Young’s modulus for the TiO₂ coating than for the mixed oxide coating, with a variation within one order of magnitude between the methods.