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The current focus in Autonomous Experimentation (AE) is on developing robust workflows to conduct the AE effectively. This entails the need for well-defined approaches to guide the AE process, including strategies for hyperparameter tuning and high-level human interventions within the workflow loop. This paper presents a comprehensive analysis of the influence of initial experimental conditions and in-loop interventions on the learning dynamics of Deep Kernel Learning (DKL) within the realm of AE in scanning probe microscopy. We explore the concept of the "seed effect," where the initial experiment setup has a substantial impact on the subsequent learning trajectory. Additionally, we introduce an approach of the seed point interventions in AE allowing the operator to influence the exploration process. Using a dataset from Piezoresponse Force Microscopy on PbTiO3 thin films, we illustrate the impact of the "seed effect" and in-loop seed interventions on the effectiveness of DKL in predicting material properties. The study highlights the importance of initial choices and adaptive interventions in optimizing learning rates and enhancing the efficiency of automated material characterization. This work offers valuable insights into designing more robust and effective AE workflows in microscopy with potential applications across various characterization techniques. [ABSTRACT FROM AUTHOR]

An advanced scanning probe microscopy system enhanced with artificial intelligence (AI‐SPM) designed for self‐driving atomic‐scale measurements is presented. This system expertly identifies and manipulates atomic positions with high precision, autonomously performing tasks such as spectroscopic data acquisition and atomic adjustment. An outstanding feature of AI‐SPM is its ability to detect and adapt to surface defects, targeting or avoiding them as necessary. It is also designed to overcome typical challenges such as positional drift and tip apex atomic variations due to the thermal effects, ensuring accurate, site‐specific surface analysis. The tests under the demanding conditions of room temperature have demonstrated the robustness of the system, successfully navigating thermal drift and tip fluctuations. During these tests on the Si(111)‐(7 × 7) surface, AI‐SPM autonomously identified defect‐free regions and performed a large number of current–voltage spectroscopy measurements at different adatom sites, while autonomously compensating for thermal drift and monitoring probe health. These experiments produce extensive data sets that are critical for reliable materials characterization and demonstrate the potential of AI‐SPM to significantly improve data acquisition. The integration of AI into SPM technologies represents a step toward more effective, precise and reliable atomic‐level surface analysis, revolutionizing materials characterization methods. [ABSTRACT FROM AUTHOR]

Atomic-scale imaging using scanning probe microscopy is a pivotal method for investigating the morphology and physico-chemical properties of nanostructured surfaces. Time resolution represents a significant limitation of this technique, as typical image acquisition times are on the order of several seconds or even a few minutes, while dynamic processes—such as surface restructuring or particle sintering, to be observed upon external stimuli such as changes in gas atmosphere or electrochemical potential—often occur within timescales shorter than a second. In this article, we present a fully redesigned field programmable gate array (FPGA)-based instrument that can be integrated into most commercially available standard scanning probe microscopes. This instrument not only significantly accelerates the acquisition of atomic-scale images by orders of magnitude but also enables the tracking of moving features such as adatoms, vacancies, or clusters across the surface ("atom tracking") due to the parallel execution of sophisticated control and acquisition algorithms and the fast exchange of data with an external processor. Each of these measurement modes requires a complex series of operations within the FPGA that are explained in detail. [ABSTRACT FROM AUTHOR]

Epoxyamine matrix-based composites containing 15 wt% of Fe nanoparticles and 1.5 or 2 wt% of carbon nanotubes, as well as composites containing only Fe particles, have been studied using microwave methods and various scanning probe microscopy techniques, such as scanning capacitance microscopy and scanning Kelvin probe force microscopy. The composites were prepared using technological methods that improve their homogeneity. Probe current dependences investigated by applying different voltages to the probe in the Kelvin probe force microscopy mode have shown that the falling regions of the dependences at both positive and negative values of the bias voltage are found only for the sample containing both the Fe particles and the CNT in the "soft epoxy" matrix. Microwave measurements of the transmission and reflection coefficients were performed in the frequency range from 26 to 38 GHz. The field dependences of the microwave power dissipation have been plotted. The ferromagnetic resonance in the composites has been investigated. Frequency dependences of the complex dielectric permittivity of the composites have been determined. Microwave properties of the CNT-containing and CNT-free composites have been compared. [ABSTRACT FROM AUTHOR]

Scanning probe microscopy (SPM) and advanced atomic force microscopy (AFM++) have become pivotal for nanoscale elucidation of the structural, optoelectronic and photovoltaic properties of halide perovskite single crystals and polycrystalline films, both under ex situ and in situ conditions. These techniques reveal detailed information about film topography, compositional mapping, charge distribution, near-field electrical behaviors, cation–lattice interactions, ion dynamics, piezoelectric characteristics, mechanical durability, thermal conductivity, and magnetic properties of doped perovskite lattices. This article outlines the advancements in SPM techniques that deepen our understanding of the optoelectronic and photovoltaic performances of halide perovskites. [ABSTRACT FROM AUTHOR]

The comparative analysis of the structural, morphological, and local electrical properties of CVD graphene films synthesized at atmospheric and low pressure CVD growth conditions was carried out. The use of electrical techniques of scanning probe microscopy, such as Kelvin probe force microscopy, scanning capacitance microscopy, electrostatic force microscopy, and conductive atomic-force microscopy for investigation of heterogeneous graphene coverage was discussed. A significant change in the surface potential values was observed indicating the formation of p-type multilayered graphene domains on single layer graphene at low pressure and n-type multilayered graphene films at atmospheric pressure CVD. The effect of Ar flow rate increasing during cooling stage in the temperature range of 700–200 °C causing graphite formation was described. The employment of surface potential spectroscopy allows to indicate the presence of nonlinear phenomena in heterogeneous graphene. [ABSTRACT FROM AUTHOR]

The dielectric gap between the scanning probe microscopy (SPM) tip and the surface of a ferroelectric using conductive atomic force microscopy and piezoresponse force microscopy (PFM) is investigated. While the gap functions as a dielectric layer, it also allows tunneling current to inject charges into the ferroelectric when a critical loading force between 10–20 µN is applied to a tip with a radius of 25 nm under a bias voltage of 0.5 V. It is observed that the permittivity of the dielectric gap determines the coercive voltage measured by the piezoresponse hysteresis loop. While such studies done in air often produce coercive voltages much larger than those studied for the same materials in capacitor‐based studies, the use of high permittivity media such as water (ɛr = 79) or silicone oil (ɛr = 2.1‐2.8) produces coercive fields that more closely match those measured in conventional capacitor‐based polarization hysteresis loop measurements. Furthermore, using water as a dielectric medium in PFM imaging enhances the accuracy in extracting the amplitude and phase data from periodically poled lithium niobate crystals. These findings provide insight into the nanoscale phenomena of polarization switching instigated by the SPM tip and provide a pathway to improved quantitative studies. [ABSTRACT FROM AUTHOR]

Cantilever-free scanning probe microscopy has enormous potential for high-throughput topography imaging using parallel probe arrays. However, the current imaging mechanism of the cantilever-free tip architecture hardly considers the efficiency of the detection method regarding precision and bandwidth, which could be a bottleneck to expanding the application of this measurement system. In this communication, we present a contact resistance-based cantilever-free imaging system using radio frequency (RF) reflectometry. RF reflectometry measurements provide sensitive detection of the contact resistance with a wide bandwidth, enabling sub-micrometer-scale topography imaging. We demonstrated our imaging system using a carbon black-polydimethylsiloxane composite tip with a custom-built RF reflectometry setup. The proof-of-concept system achieved a resolution of 230 nm and a bandwidth of the detection system of approximately 8.5 MHz, validating the feasibility of the imaging technique for potential high-throughput cantilever-free scanning probe microscopy. [ABSTRACT FROM AUTHOR]

We introduce a new scanning probe microscopy (SPM) concept called reverse tip sample scanning probe microscopy (RTS SPM), where the tip and sample positions are reversed as compared to traditional SPM. The main benefit of RTS SPM over the standard SPM configuration is that it allows for simple and fast tip changes. This overcomes two major limitations of SPM which are slow data acquisition and a strong dependency of the data on the tip condition. A probe chip with thousands of sharp integrated tips is the basis of our concept. We have developed a nanofabrication protocol for Si based probe chips and their functionalization with metal and diamond coatings, evaluated our probe chips for various RTS SPM applications (multi-tip imaging, SPM tomography, and correlative SPM), and showed the high potential of the RTS SPM concept. [ABSTRACT FROM AUTHOR]

In contact mode scanning probe microscopy (SPM), the microcantilever probe's dynamics are governed by the (short-range) surface interaction forces, where the tip is "always-in-contact" with the sample. In intermittent contact modes such as "tapping" or bimodal SPM, on the other hand, these are governed by the frequency of the microcantilever's own external excitation. However, when contact mode is employed with high scan speeds (for "video-rate" SPM), we see intermittent transitions—within a single oscillation cycle—between the "always-in-contact" regime and another which is dominated by the microcantilever's inertia. We find—through experiments and physical modeling—that the fast in-plane motion of the sample relative to the probe results in a high surface excitation frequency v / λ (and its harmonics), which excite the microcantilever's out-of-plane eigenmodes and cause it to "break free" of the surface and "overshoot" and "parachute." The impacts of the tip that consequently occur upon the sample inject energy over a wide frequency band into the higher eigenmodes, especially when operating in a low dissipation ambient environment. The microcantilever, then, exhibits phenomena such as eigenmode switching, sidebands, and fractional and combination resonances; such behavior is not seen in, say, tapping mode SPM, since, there, energy is injected at an externally-determined temporal rate. This article investigates the transition from the dynamics of the microcantilever at low speeds to that exhibited at high speeds. The model for dynamic contact loss is validated against the experiments and can be used to propose mitigation of such dynamics in order to achieve high-resolution imaging. [ABSTRACT FROM AUTHOR]

Li[Ni0.885Co0.1V0.015]O2 (NCV), Li[Ni0.9Co0.1]O2 (NC), and Li[Ni0.885Co0.1Al0.015]O2 (NCA) nanoparticles are synthesized by means of oxalic acid co-precipitation with subsequent calcination. The evolution of Li-ion diffusion and deformation of both NCV and NCA under an external electric field are characterized by means of conductive atomic force microscopy and electrochemical strain microscopy. Macroscopic electrochemical characterization reveals that the Li-ion diffusivity in NCA is greater than that in NCV, and the undesirable irreversible H2–H3 phase transition occurs more readily in NCV than in NCA. The scanning probe microscopy results corroborate well with the macroscopic electrochemical measurements, which tell that vanadium and aluminum substitution can accelerate Li+ diffusion kinetics and enhance the reversibility of the H2–H3 phase transformation during the electrochemical process in varying degrees. [ABSTRACT FROM AUTHOR]

Atomic-scale imaging using scanning probe microscopy is a pivotal method for investigating the morphology and physico-chemical properties of nanostructured surfaces. Time resolution represents a significant limitation of this technique, as typical image acquisition times are on the order of several seconds or even a few minutes, while dynamic processes—such as surface restructuring or particle sintering, to be observed upon external stimuli such as changes in gas atmosphere or electrochemical potential—often occur within timescales shorter than a second. In this article, we present a fully redesigned field programmable gate array (FPGA)-based instrument that can be integrated into most commercially available standard scanning probe microscopes. This instrument not only significantly accelerates the acquisition of atomic-scale images by orders of magnitude but also enables the tracking of moving features such as adatoms, vacancies, or clusters across the surface (“atom tracking”) due to the parallel execution of sophisticated control and acquisition algorithms and the fast exchange of data with an external processor. Each of these measurement modes requires a complex series of operations within the FPGA that are explained in detail.

Abstract In the last decade, contact electrification has gained attention for its potential in energy harvesting, addressing fundamental physics. Scanning probe microscopy (SPM) has evolved as a powerful platform, enabling the in situ characterization/manipulation of a sample's tribological/electrical properties at nanoscale. However, although both the sliding and tapping modes are available in the energy harvesting, the lateral sliding using contact mode SPM has predominantly been employed in triboelectric study. In this work, contact electrification on polydimethylsiloxane is investigated, using peak force tapping atomic force microscopy (PF‐AFM). As PF‐AFM quasi‐discretely offers vertical tapping motions of the probe with a regulated force amplitude, resembling a vertical‐type triboelectric nanogenerator, while minimizing lateral forces. The subsequent surface potential measurements reveal that the generated tribocharge is influenced by both the effective work function difference and energy dissipation at the interface. Furthermore, the accumulation of transferred charges is explored by measuring tip‐sample current during the PF‐AFM operation, showing the comparable results with the surface potential measurement. The results can be attributed to the contact potential difference assisted by the energy dissipation at the interface. This study offers an advanced opportunity to understand and study charge generation behavior based on surface properties without damaging the sample.

The impact of Artificial Intelligence (AI) is rapidly expanding, revolutionizing both science and society. It is applied to practically all areas of life, science, and technology, including materials science, which continuously requires novel tools for effective materials characterization. One of the widely used techniques is scanning probe microscopy (SPM). SPM has fundamentally changed materials engineering, biology, and chemistry by providing tools for atomic-precision surface mapping. Despite its many advantages, it also has some drawbacks, such as long scanning times or the possibility of damaging soft-surface materials. In this paper, we focus on the potential for supporting SPM-based measurements, with an emphasis on the application of AI-based algorithms, especially Machine Learning-based algorithms, as well as quantum computing (QC). It has been found that AI can be helpful in automating experimental processes in routine operations, algorithmically searching for optimal sample regions, and elucidating structure-property relationships. Thus, it contributes to increasing the efficiency and accuracy of optical nanoscopy scanning probes. Moreover, the combination of AI-based algorithms and QC may have enormous potential to enhance the practical application of SPM. The limitations of the AI-QC-based approach were also discussed. Finally, we outline a research path for improving AI-QC-powered SPM. RESEARCH HIGHLIGHTS: Artificial intelligence and quantum computing as support for scanning probe microscopy. The analysis indicates a research gap in the field of scanning probe microscopy. The research aims to shed light into ai-qc-powered scanning probe microscopy., (© 2024 Wiley Periodicals LLC.)

Carbon black (CB) has wide range of industrial applications, including in the manufacturing of automobile tires, rubber products, inks, and plastics. To improve the properties of the target products and establish recycling systems, it must be fully characterized. However, characterization of CB is challenging owing to its structural complexity and the limitation of conventionally used experimental techniques, especially for surface structures at the nanoscale. In this study, we characterized the surface structures of two commercial CB via atomic force and scanning tunneling microscopy. Analysis of well-dispersed aggregates on atomically flat solid surfaces revealed primary particles of diverse sizes. The particle surfaces lacked edges, grooves, and steps that should be observed between stacked graphene sheets, which contradicts the widely accepted crystallite model. Observed images suggest that the graphene sheets exhibit a size distribution, inferring that multiple non-uniformly sized small graphene sheets are stacked turbostratically, with each sheet displaying a localized curvature rather than the ideal planar form. Varying size of sheets and curvature indicate the presence of a decent number of edges terminated with hydrogen and oxygen-containing functional groups. This interpretation was corroborated by conventional spectroscopic techniques: Raman spectroscopy, X-ray photoelectron spectroscopy, temperature-programmed desorption, and infrared absorption spectroscopy.

The glycocalyx is a brush-like layer that covers the surfaces of the membranes of most cell types. It consists of a mixture of carbohydrates, mainly glycoproteins and proteoglycans. Due to its structure and sensitivity to environmental conditions, it represents a complicated object to investigate. Here, we review studies of the glycocalyx conducted using scanning probe microscopy approaches. This includes imaging techniques as well as the measurement of nanomechanical properties. The nanomechanics of the glycocalyx is particularly important since it is widely present on the surfaces of mechanosensitive cells such as endothelial cells. An overview of problems with the interpretation of indirect data via the use of analytical models is presented. Special insight is given into changes in glycocalyx properties during pathological processes. The biological background and alternative research methods are briefly covered. [ABSTRACT FROM AUTHOR]

We describe an approach to determine the in-plane crystallographic surface directions in scanning probe microscopy (SPM) images. This method is based on a one-time characterization of the SPM instrument with an appropriate test sample and is exemplified by the analysis of non-contact atomic force microscopy (NC-AFM) images on surfaces whose natural cleavage occurs along {111} planes. We introduce a two-dimensional rotation matrix relating the crystallographic surface directions known from an analysis of the macroscopic crystal to the directions in the NC-AFM images. The procedure takes into account rotations and mirror axes resulting from sample mounting, the SPM scanner rotation, the choice of scan direction, as well as data processing, storage, and display. We demonstrate the practicability of the approach by determining the [ 11 2 ̄ ] direction in topographic images of a CeO2(111) film grown on a Si(111) wafer and atomic resolution images of CaF2(111) with an instrument based on the beetle-type scanner. [ABSTRACT FROM AUTHOR]

Starting from the late 1980’s, scanning probe microscopy has progressively diffused in Italy until today. In this paper, we provide a brief account of the main historical events and a current picture of the distribution of the active groups. A survey was prepared by LimeSurvey, made of six sections asking for personal and institutional data, human resources, equipment available, fields of interest, research projects, educational/dissemination activities, and two relevant publications in the last six years. It turns out that the Italian community includes more than seventy groups and two companies. It is widely diffused, although mostly concentrated near large academic and research institutions, often in locations where prominent Italian researchers have operated. This community is active in many scientific fields and can produce research of high international quality. It shows a wide competence, as proven by the list of research works published in journals ranked within the top 20% class. The diffusion of SPM microscopes in industry is still sporadic, possibly due to extensive collaborations between the research institutions and industries themselves. The authors hope that this work might be useful to the community and beyond, and that it might stimulate the formation of a more structured network.

In the twenty-first century, scanning probe microscopy characterization techniques have seen significant progress and are capable of probing complex structures and devices for a variety of near-surface features and phenomena with nanometer scale resolution. With modest customization, we can deploy these techniques for industrial metrology purposes in a simultaneous and multimethod system capable of shedding light on device function and failure modes, as well as determining the most efficient methods for data collection. To demonstrate this concept with a current, complex industrial device under development, several scanning probe microscopy techniques advantageous to the progress of heat-assisted magnetic recording heads were selected. This work describes simultaneous and multimethod approaches for performing heat-assisted magnetic recording head characterization using atomic force microscopy with scattering scanning near-field optical microscopy simultaneously performed with magnetic force microscopy or photo-induced force microscopy that could be extended to applications of other complex nanoscale devices. We demonstrate that the optical and magnetic fields are overlapping for fabricated heads, which is necessary for performing heat-assisted magnetic recording. We also observed that the multimethod atomic force microscopy methods show strong agreement between the measured optical and magnetic fields and the locale of their associated parts on the head. [ABSTRACT FROM AUTHOR]

Shear-force acoustic near-field microscopy (SANM) is employed to monitor stochastic formation and post dynamic response of a water meniscus that bridges a tapered gold probe (undergoing lateral oscillations of a few nanometers amplitude at constant frequency) and a flat (gold or silicon oxide) substrate. As the probe further approaches the substrate, its amplitude decreases. Shear forces (of yet unknown precise origin) are typically invoked to explain the apparently pure damping effects affecting the probe's motion. Herein, SANM measurements underscore instead the role of near-field acoustic emission from the water meniscus as an elastic energy dissipation channel involved in shear interactions. A simplified thermodynamic argument is provided to justify the formation of a water meniscus between the probe and the sample once they are at sufficient separation distance. The reported measurements focus on the role played by the tip's geometry (by using probes of slender and chubby apex termination). The results shed some light on the potential origin of the so-called shear forces, invoked in many scanning probe microscopy applications, but not yet well understood. [ABSTRACT FROM AUTHOR]