Mechanical Mapping of Nanoblisters Confined by Two-Dimensional Materials Reveals Complex Ridge Patterns.

Understanding the mechanics of blisters confined by two-dimensional (2D) materials is of great importance for either fundamental studies or for their practical applications. In this work, we investigate the mechanical properties of nanoscale 2D material blisters using contact-resonance atomic force microscopy (CR-AFM). From the measurement results at the blister centers, the blisters' internal pressures are characterized, which are shown to be inversely proportional to the blisters' sizes. Our measurements agree considerably well with values predicted by theoretical mechanic analyses of the blisters. In addition, high-resolution mechanical mapping with CR-AFM reveals fine, complex ridge patterns of the blisters' confining membranes, which can hardly be distinguished from their topographies. The pattern complexity of a blister system is shown to increase with an increase in its bendability.

Time-Dependent Pinning of Nanoblisters Confined by Two-Dimensional Sheets. Part 1: Scaling Law and Hydrostatic Pressure.

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 two-part 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.

Time-Dependent Pinning of Nanoblisters Confined by Two-Dimensional Sheets. Part 2: Contact Line Pinning.

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.

Subsurface imaging of flexible circuits via contact resonance atomic force microscopy.

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.

Stress stiffened silicon nitride micro bridges array as substrate with tunable stiffness for cell culture.

Recently, interactions between one-dimensional structural stiffness of physical micro environments and cell biological process have been widely studied. However in previous studies, the influence of structural stiffness on biological process was coupled with the influence of micro fiber curvature. Therefore decoupling the influences of fiber curvature and structural stiffness on cell biological process is of prime importance. In this study, we proposed a novel cell culture substrate comprised of silicon nitride bridges whose structure stiffness can be regulated by altering the axial residual stress without changing material and geometry properties. Both theoretical calculations and finite element simulations were performed to study the influence of residual stress on structure stiffness of bridges. Then multi-positions AFM bending tests were implemented to measure local stiffness of a single micro bridge so as to verify our predictions. NIH/3T3 mouse fibroblast cells were cultured on our substrates to examine the feasibility of the substrate application for investigating cellular response to microenvironment with variable stiffness. The results showed that cells on the edge region near bridge ends were more spread, elongated and better aligned along the bridge axial direction than those on the bridge center region. The results suggest that cells can sense and respond to the differences of stiffness and stiffness gradient between the edge and the center region of the bridges, which makes this kind of substrates can be applied in some biomedical fields, such as cell migration and wound healing.

Visualizing subsurface defects in graphite by acoustic atomic force microscopy.

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.

16 nm-resolution lithography using ultra-small-gap bowtie apertures.

Photolithography has long been a critical technology for nanoscale manufacturing, especially in the semiconductor industry. However, the diffractive nature of light has limited the continuous advance of optical lithography resolution. To overcome this obstacle, near-field scanning optical lithography (NSOL) is an alternative low-cost technique, whose resolution is determined by the near-field localization that can be achieved. Here, we apply the newly-developed backside milling method to fabricate bowtie apertures with a sub-15 nm gap, which can substantially improve the resolution of NSOL.  A highly confined electric near field is produced by localized surface plasmon excitation and nanofocusing of the closely-tapered gap. We show contact lithography results with a record 16 nm resolution (FWHM). This photolithography scheme promises potential applications in data storage, high-speed computation, energy harvesting, and other nanotechnology areas.

Effects of temperature and humidity on atomic force microscopy dimensional measurement.

The influence of environmental factors on dimensional measurements of atomic force microscopy (AFM) was investigated experimentally. Measurements were taken with environmental control over a whole AFM chamber and a local sample chamber to highlight the influence of working conditions on the instrument itself. Both temperature and humidity were found to have a significant impact on pitch measurements of a two-dimensional grating. The effect of temperature on the behavior of the microscope itself is generally larger than the thermal expansion or contraction of the sample. The effect of humidity was further determined to be relevant to the scan direction and velocity. For precise AFM dimensional measurements, the possible influences of temperature and humidity must be carefully considered.

Atomic force microscopy force-distance curves with small amplitude ultrasonic modulation.

Force-distance curves were acquired on a highly oriented pyrolytic graphite (HOPG) specimen and a gold film specimen under ultrasonic modulation in atomic force microscopy (AFM). Measurements demonstrated that small amplitude ultrasonic oscillation of either the cantilever or the sample has significant impacts on the characteristics of force-distance curves. With the increase of excitation amplitude, the apparent pull-off force decreased gradually and the hysteresis between the approach and retraction curves reduced significantly. Furthermore, the decrease of the pull-off force was determined to be also relevant to the excitation frequency. With the assistance of contact resonance spectra, the pull-off force was verified to have a near-linear relationship with the cantilever contact oscillation amplitude. Theoretical analysis and subsequent numerical simulations well interpreted the experimental results. The emergence of large oscillating contact forces under ultrasonic modulation altered the force-distance curves, and such a mechanism was ascertained by further ultrasonic AFM imaging.

Spectral analysis of irregular roughness artifacts measured by atomic force microscopy and laser scanning microscopy.

Atomic force microscopy (AFM) and laser scanning microscopy (LSM) measurements on a series of specially designed roughness artifacts were performed and the results characterized by spectral analysis. As demonstrated by comparisons, both AFM and LSM can image the complex structures with high resolution and fidelity. When the surface autocorrelation length increases from 200 to 500 nm, the cumulative power spectral density spectra of the design, AFM and LSM data reach a better agreement with each other. The critical wavelength of AFM characterization is smaller than that of LSM, and the gap between the measured and designed critical wavelengths is reduced with an increase in the surface autocorrelation length. Topography measurements of surfaces with a near zero or negatively skewed height distribution were determined to be accurate. However, obvious discrepancies were found for surfaces with a positive skewness owing to more severe dilations of either the solid tip of the AFM or the laser tip of the LSM. Further surface parameter evaluation and template matching analysis verified that the main distortions in AFM measurements are tip dilations while those in LSM are generally larger and more complex.