Understanding the mechanics of blisters is important for studying two-dimensional (2D) materials, where nanoscale blisters appear frequently in their heterostructures. It also benefits the understanding of a novel partial wetting phenomenon known as elastic wetting, where droplets are confined by thin films. In this twopart work, we study the static mechanics of nanoscale blisters confined between a 2D elastic sheet and its substrate (part 1) as well as their pinning/depinning dynamics (part 2). Here, in part 1, we investigate the morphology characteristics and hydrostatic pressures of the blisters by using atomic force microscopy (AFM) measurements and theoretical analysis. The morphology characteristics of the blisters are shown to be the interplay results of the elasticity of the capping sheet, the adhesion between the capping sheet and the substrate, and the interfacial tensions. A universal scaling law is observed for the blisters in the experiments. Our analyses show that the hydrostatic pressures inside the blisters can be estimated from their morphology characteristics. The reliability of such an estimation is verified by AFM indentation measurements of the hydrostatic pressures of a variety of blisters.

To meet the surging demands for quantitative and nondestructive testing at the nanoscale in various fields, ultrasonic-based scanning probe microscopy techniques, such as contact-resonance atomic force microscopy (CR-AFM), have attracted increased attention. Despite considerable success in subsurface nanostructure or defect imaging, the detecting capabilities of CR-AFM have not been fully explored yet. In this paper, we present an analytical model of CR-AFM for detecting subsurface cavities by adopting a circular freestanding membrane structure as an equivalent cavity. The parameters describing the detection limits of CR-AFM for such structures include the detecting depth and the detectable area. These parameters are systematically studied for different cantilever eigenmodes for structures of different sizes and depths. The results show that the detecting depth depends on the structure size. The higher eigenmodes generally provide better detecting capabilities than the lower ones. For an experimental verification, samples were prepared by covering a polymethylmethacrylate (PMMA) substrate with open pores at its surface with HOPG flakes. CR-AFM imaging on the HOPG-covered area was carried out using different eigenmodes in order to detect the pores in the PMMA. In addition, the influence of the applied tip load is also discussed.

Subsurface metrology techniques are of significant importance at the nanoscale, for instance, for imaging buried defects in semiconductor devices and in intracellular structures. Recently, ultrasonic-based atomic force microscopy has attracted intense attention also for subsurface imaging. Despite many applications for measuring the real and imaginary part of the local surface modulus, the physical mechanism for subsurface imaging is not fully understood. This prevents accurate data interpretation and quantitative reconstruction of subsurface features and hinders the development of an optimized experimental and engineering setup. In this paper, we present quantitative depth-sensing of subsurface cavity structures using contact-resonance atomic force microscopy (CR-AFM) imaging and spectroscopy. Our results indicate that for imaging subsurface cavity structures using CR-AFM, the induced contact stiffness variations are the key contrast mechanism. The developed algorithm based on this mechanism allows one to precisely simulate the experimental image contrasts and give an accurate prediction of the detection depth. The results allow a better understanding of the imaging mechanism of ultrasonic-based AFM and pave the way for quantitative subsurface reconstruction.

As one of the fundamental sources of noise in atomic force microscopy (AFM), thermal fluctuations of the cantilever have been studied for the case of a free tip but not much for cantilevers in contact. In this paper, using the equipartition theorem, we calculated the thermal deflection amplitude for all normal modes of an elastically supported AFM cantilever, including the free cantilever as a special case. With increasing contact stiffness, the mean thermal fluctuation amplitude decreases for all cantilever modes when in the elastic contact. In addition, considering the optical lever detection scheme used in most AFMs, we calculated the corresponding output thermal noise amplitude. The experiments validated our theoretical calculations. Our investigation facilitates a more comprehensive understanding of the thermal noise in AFM. It provides guidance for thermally excited contact-resonance AFM, which is promising for quantitative viscoelastic measurements.

Imaging of subsurface features down to the nanometer scale is of great importance in various fields such as microelectronics, materials science, nanobiology, and nanomedicine. Since their invention 25 years ago, ultrasonic-based atomic force microscopy (AFM) techniques have attracted vast attention for their mechanical surface and subsurface sensing capability. In this Perspective article, we review the research on ultrasonic AFMs for subsurface imaging. We first describe the instrumentation setups and different detection schemes of ultrasonic AFMs. Then, attention is paid to the studies of the physical contrast mechanism, the evaluation of the detection capabilities, in particular, the detection depth limits, and the optimization approaches to enhance the contrast and to improve the detection depth. After that we present typical applications of using ultrasonic AFMs for detecting subsurface defects including dislocations, voids, and interfaces in functional materials and devices; visualizing embedded inclusions in composites; and imaging subcellular structures in biological materials. We conclude with an outlook of the challenges faced by ultrasonic AFMs toward fast, high resolution, and quantitative subsurface imaging.

We describe a versatile platform, which combines atomic force acoustic microscopy, ultrasonic atomic force microscopy and heterodyne force microscopy. The AFM system can enable in-situ switching among these operation modes flexibly and thus benefit the discrimination of differences in mechanical properties and buried subsurface nanostructures. We demonstrate the potential of this platform for visualizing the subsurface defects of graphite. Our results show that tiny topographic edges are enhanced in acoustic oscillation signals whilst embedded defects and inhomogeneous in mechanical properties are made clearly distinguishable. The possibility of detecting subsurface defects in few-layer graphene is further discussed with first-principles calculations. Microsc. Res. Tech. 80:66-74, 2017. © 2016 Wiley Periodicals, Inc.

Subsurface imaging of Au circuit structures embedded in poly(methyl methacrylate) (PMMA) thin films with a cover thickness ranging from 52 to 653 nm was carried out by using contact resonance atomic force microscopy (CR-AFM). The mechanical difference of the embedded metal layer leads to an obvious CR-AFM frequency shift and therefore its unambiguous differentiation from the polymer matrix. The contact stiffness contrast, determined from the tracked frequency images, was employed for quantitative evaluation. The influence of various parameter settings and sample properties was systematically investigated by combining experimental results with theoretical analysis from finite element simulations. The results show that imaging with a softer cantilever and a lower eigenmode will improve the subsurface contrast. The experimental results and theoretical calculations provide a guide to optimizing parameter settings for the nondestructive diagnosis of flexible circuits. Defect detection of the embedded circuit pattern was also carried out, which indicates the capability of imaging tiny subsurface structures smaller than 100 nm by using CR-AFM.

Pinning of droplets on solids is an omnipresent wetting phenomenon that attracts intense research interest. Unlike in classical wetting, pinning effects in a novel wetting problem where droplets are confined onto the substrates by elastic films have hardly been investigated. Here, following our study in an accompanying paper (part 1) on the static mechanics of nanoscale blisters confined between a two-dimensional elastic sheet and its substrate, we investigate in this part the pinning behaviors of such blisters by using atomic force microscopy. The blisters’ lateral retention forces are shown to scale almost linearly with their contact lines and to increase until saturation upon increasing their resting times. Our analysis reveals a mechanism of microdeformation of the substrate at the contact line. The creep of the microdeformation is found to cause the time-dependent pinning, which is evidenced by residual fine ridge structures left by blisters after their spread after long resting times.