ACS Appl Mater Interfaces. 2022 Dec 1. doi: 10.1021/acsami.2c17962. Online ahead of print.
Since its discovery, atomic force microscopy (AFM) has become widely used for surface characterization, evolving from a tool for probing surface topography to a versatile method for characterizing mechanical, electrical, chemical, magnetic, and electro-optical properties of surfaces at the nanoscale. Developments of several AFM-based techniques have enabled even subsurface imaging, which is routinely being carried out at the qualitative level of feature detection for localized subsurface inhomogeneities. We surmise, however, that a quantitative three-dimensional (3D) subsurface characterization can emerge from the AFM mechanical response of flat buried interfaces, and present here a methodology for determining the depth of a film and its mechanical properties. Using load-dependent contact resonance atomic force microscopy (CR-AFM) and accurate modeling of the contact between the AFM tip and a layered sample, we determine the relationship between the measured resonance frequency of the AFM probe and the contact stiffness. Our subsequent statistical analysis reveals an intrinsic and sample-specific interdependence between the depth and modulus sensitivities of CR-AFM. This interdependence prevents the simultaneous accurate determination of both depth and modulus from measurements on a single-layered sample. If the elastic moduli of the sample components are predetermined from separate investigations of bulk samples (or otherwise known), then this methodology accurately yields the location of the interface between the layers of the sample; as such, it can serve as a nondestructive and robust technique for probing layer thickness, subsurface features, and elastic properties of materials used in semiconductor electronics, additive manufacturing, or biomaterials.