Despite considerable research efforts, the influence of contact line tension during wetting at the nanoscale and its experimental determination remain challenging tasks. So far, molecular dynamics simulations and atomic force microscope measurements have contributed to the understanding of these phenomena. However, a direct measurement of the size dependence of the contact angle and the magnitude of the apparent line tension has not been realized so far. Here, we show that the contact angle is indeed dependent on the drop size for small drop diameters and determine the magnitude of the apparent line tension via liquid-metal based measurements of advancing and receding contact angle inside a scanning electron microscope. For this purpose, a robotic setup inside an electron microscope chamber and oxide-free Galinstan droplets—produced via an electromigration-based and focused ion beam irradiation-assisted process—are employed. Using the first-order correction of Young’s equation, we find an apparent line tension value of 4.02 × 10⁻⁷ J/m for Galinstan© on stainless steel.

Van der Waals forces, electrostatic interactions, and capillary forces are the dominant force interactions at the micro- and nanoscale. This complex ensemble of surface forces is oftentimes summarized as adhesion and is important for various applications and research fields. So far, numerous measurement techniques have evolved in this field. However, there is still a lack of experimental insight into the complex interplay of van der Waals, electrostatic, and capillary forces for small force ranges below 10 nN, as this is the order of magnitude of the latter, which can shadow other interactions in ambient and even inert gas environments. To exclude capillary forces and thus to turn the van der Waals and electrostatic forces into the most significant interactions, we develop an interferometric force spectroscopy setup based on a scanning probe technique, featuring a sub-nanonewton resolution, and integrate it into the vacuum chamber of a scanning electron microscope. In this work, we describe the setup integration, show the long-term drift behavior and resolution capabilities, and conduct first measurements of adhesion energies between a silica colloidal probe and a silicon substrate. The presented setup shows its capability to reliably measure adhesive interactions in vacuum and an ambient environment with a sub-nanonewton resolution proving its potential to allow for the investigation of the separate contribution of capillary, van der Waals, and electrostatic interactions to adhesion and for a systematic experimental validation of the established adhesion theories and approximations on the micro- and nanoscale.

Fabrication of tailored photonic structures with sufficient precision is a major topic in photonics since decades. However, until now, the assembly of photonic structures in order to control light propagation in all three spatial dimensions remains challenging. This paper presents a reliable approach for fabricating three-dimensional structures consisting of individually stacked colloidal particles. The combination of a robotic dual-probe setup inside a scanning electron microscope and the purposeful use of ion beam based etching and deposition techniques allows to fabricate on-demand three-dimensional photonic structures with cubic geometry. The advantages and limits of this technique are highlighted with respect to further application scenarios.

Scanning electron microscope is not only a versatile visualization and characterization tool for nanomaterials, but it is also widely used for visual feedback during assembly and manipulation of micro- and nanoparticles, novel devices based on 2D and 1D materials, and microrobots. Due to increase in the surface-to-volume ratio, adhesion forces play a significant role in micro- and nanorobotic applications. We investigate the quantitative effect of electron beam irradiation on nanoscale adhesive interactions between different end effector types and plain substrates. For this purpose, we use an interferometry-based force measurement setup integrated into the chamber of a scanning electron microscope capable of a subnano Newton force resolution. We provide quantitative results for the influence of the electron beam on the adhesion forces depending on the exposure dose, geometrical configuration in which it is applied, as well as on the material of the end effector. Simulation results, atomic force microscope adhesion measurements, and measurements with piezoresistive cantilevers serve as references. Our findings indicate that the electron beam influences the adhesive interaction not only in the case of insulating probes but also for well-grounded conducting and semiconducting probes. Its influence can range from several 10% to several 100% in comparison to the adhesion values measured with an atomic force microscope in an ambient atmosphere and no charged particle beam is applied. Moreover, it is shown that the influence of a charged particle beam is a multidimensional phenomenon that depends on several factors such as end effector and substrate material, geometry and aspect ratio of the end effector, geometrical configuration between particle beam and probe–sample arrangement, as well as exposure dose and field of view. We provide recommendations for handling and characterization of micro- and nano-objects using end effectors under the influence of charged particle beams: not to rely on adhesion values acquired in different environmental and exposure conditions, not to expect the application of conductive materials and grounding to completely avoid the effect of charged particle beams, and to be aware that charged particle beams can lower or increase the adhesion force in vacuum depending on material properties, among others.

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