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Wear is one of the main factors that hinders the performance of probes for atomic force microscopy (AFM), including for the widely used amplitude modulation (AM-AFM) mode. Unfortunately, a comprehensive scientific understanding of nanoscale wear is lacking. We have developed a protocol for conducting consistent and quantitative AM-AFM wear experiments. The protocol involves controlling the tip-sample interaction regime during AM-AFM scanning, determining the tip-sample contact geometry, calculating the peak repulsive force and normal stress over the course of the wear test, and quantifying the wear volume using high-resolution transmission electron microscopy imaging. The peak repulsive tip-sample interaction force is estimated from a closed-form equation accompanied by an effective tip radius measurement procedure, which combines transmission electron microscopy and blind tip reconstruction. The contact stress is estimated by applying Derjaguin-Müller-Toporov contact mechanics model and also numerically solving a general contact mechanics model recently developed for the adhesive contact of arbitrary axisymmetric punch shapes. We discuss the important role that the assumed tip shape geometry plays in calculating both the interaction forces and the contact stresses. Contact stresses are significantly affected by the tip geometry while the peak repulsive force is mainly determined by experimentally controlled parameters, specifically, the free oscillation amplitude and amplitude ratio. The applicability of this protocol is demonstrated experimentally by assessing the performance of diamond-like carbon-coated and silicon-nitride-coated silicon probes scanned over ultrananocrystalline diamond substrates in repulsive mode AM-AFM. There is no sign of fracture or plastic deformation in the case of diamond-like carbon; wear could be characterized as a gradual atom-by-atom process. In contrast, silicon nitride wears through removal of the cluster of atoms and plastic deformation.

We report a wear-resistant ultrananocrystalline (UNCD) diamond tip integrated onto a heated atomic force microscope (AFM) cantilever and UNCD tips integrated into arrays of heated AFM cantilevers. The UNCD tips are batch-fabricated and have apex radii of approximately 10 nm and heights up to 7 μm. The solid-state heater can reach temperatures above 600 °C and is also a resistive temperature sensor. The tips were shown to be wear resistant throughout 1.2 m of scanning on a single-crystal silicon grating at a force of 200 nN and a speed of 10 μm s(-1). Under the same conditions, a silicon tip was completely blunted. We demonstrate the use of these heated cantilevers for thermal imaging in both contact mode and intermittent contact mode, with a vertical imaging resolution of 1.9 nm. The potential application to nanolithography was also demonstrated, as the tip wrote hundreds of polyethylene nanostructures.

We report exceptional nanoscale wear and fouling resistance of ultrananocrystalline diamond (UNCD) tips integrated with doped silicon atomic force microscope (AFM) cantilevers. The resistively heated probe can reach temperatures above 600 degrees C. The batch fabrication process produces UNCD tips with radii as small as 15 nm, with average radius 50 nm across the entire wafer. Wear tests were performed on substrates of quartz, silicon carbide, silicon, or UNCD. Tips were scanned for more than 1 m at a scan speed of 25 mum s(-1) at temperatures ranging from 25 to 400 degrees C under loads up to 200 nN. Under these conditions, silicon tips are partially or completely destroyed, while the UNCD tips exhibit little or no wear, no signs of delamination, and exceptional fouling resistance. We demonstrate nanomanufacturing of more than 5000 polymer nanostructures with no deterioration in the tip.