A simple atomic force microscope-based method for quantifying wear of sliding probes.

Sliding wear is particularly problematic for micro- and nano-scale devices and applications, and is often studied at the small scale to develop practical and fundamental insights. While many methods exist to measure and quantify the wear of a sliding atomic force microscope (AFM) probe, many of these rely on specialized equipment and/or assumptions from continuum mechanics. Here we present a methodology that enables simple, purely AFM-based measurement of wear, in cases where the AFM probe wears to a flat plateau. The rate of volume removal is recast into a form that depends primarily on the time-varying contact area. This contact area is determined using images of sharp spikes, which are analyzed with a simple thresholding technique, rather than requiring sophisticated computer algorithms or continuum mechanics assumptions. This approach enables the rapid determination of volume lost, rate of material removal, normal stress, and interfacial shear stress at various points throughout the wear experiment. The method is demonstrated using silicon probes sliding on an aluminum oxide substrate. As a validation for the present method, direct imaging in the transmission electron microscope is used to verify the method's parameters and results. Overall, it is envisioned that this purely AFM-based methodology will enable higher-throughput wear experiments and direct hypothesis-based investigation into the science of wear and its dependence on different variables.

Towards easy and reliable AFM tip shape determination using blind tip reconstruction.

Quantitative determination of the geometry of an atomic force microscope (AFM) probe tip is critical for robust measurements of the nanoscale properties of surfaces, including accurate measurement of sample features and quantification of tribological characteristics. Blind tip reconstruction, which determines tip shape from an AFM image scan without knowledge of tip or sample shape, was established most notably by Villarrubia [J. Res. Natl. Inst. Stand. Tech. 102 (1997)] and has been further developed since that time. Nevertheless, the implementation of blind tip reconstruction for the general user to produce reliable and consistent estimates of tip shape has been hindered due to ambiguity about how to choose the key input parameters, such as tip matrix size and threshold value, which strongly impact the results of the tip reconstruction. These key parameters are investigated here via Villarrubia's blind tip reconstruction algorithms in which we have added the capability for users to systematically vary the key tip reconstruction parameters, evaluate the set of possible tip reconstructions, and determine the optimal tip reconstruction for a given sample. We demonstrate the capabilities of these algorithms through analysis of a set of simulated AFM images and provide practical guidelines for users of the blind tip reconstruction method. We present a reliable method to choose the threshold parameter corresponding to an optimal reconstructed tip shape for a given image. Specifically, we show that the trend in how the reconstructed tip shape varies with threshold number is so regular that the optimal, or Goldilocks, threshold value corresponds with the peak in the derivative of the RMS difference with respect to the zero threshold curve vs. threshold number.

Nanotribology of octadecyltrichlorosilane monolayers and silicon: self-mated versus unmated interfaces and local packing density effects.

We use atomic force microscopy (AFM) to determine the frictional properties of nanoscale single-asperity contacts involving octadecyltrichlorosilane (OTS) monolayers and silicon. Quantitative AFM measurements in the wearless regime are performed using both uncoated and OTS-coated silicon AFM tips in contact with both uncoated and OTS-coated silicon surfaces, providing four pairs of either self-mated or unmated interfaces. Striking differences in the frictional responses of the four pairs of interfaces are found. First, lower friction occurs with OTS present on either the tip or substrate, and friction is yet lower when OTS is present on both. Second, the shape of the friction versus load plot strongly depends on whether the substrate is coated with OTS, regardless of whether the tip is coated. Uncoated substrates exhibit the common sublinear dependence, consistent with friction being directly proportional to the area of contact. However, coated substrates exhibit an unusual superlinear dependence. These results can be explained qualitatively by invoking molecular plowing as a significant contribution to the frictional behavior of OTS. Direct in situ comparison of two intrinsic OTS structural phases on the substrate is also performed. We observe frictional contrast for different local molecular packing densities of the otherwise identical molecules. The phase with lower packing density exhibits higher friction, in agreement with related previous work, but decisively observed here in single, continuous images involving the same molecules. Lateral stiffness measurements show no distinction between the two OTS structural phases, demonstrating that the difference in friction is not due to divergent stiffnesses of the two phases. Therefore, the packing density directly affects the interface's intrinsic resistance to friction, that is, the interfacial shear strength.