Scanning Probe Microscopy Research Articles

Solution-Processed Robust Multifunctional Memristor of 2D Layered Material Thin Film.

Memristors have gained significant attention recently due to their unique ability to exhibit functionalities for brain-inspired neuromorphic computing. Here, we demonstrate a high-performance multifunctional memristor using a thin film of liquid-phase exfoliated (LPE) 2D MoS2 pinched between two electrodes. Nanoscale inspection of a solution-processed MoS2 thin film using scanning electron and scanning probe microscopies revealed the high-quality and defect-free nature. Systematic current-voltage (I-V) characterizations depict a facile, nonvolatile resistive switching behavior of our 2D MoS2 thin film device with a current On/Off ratio of 103 and energy cost of only a few picojoules. Excellent performance metrics, including at least 103 cycle endurance, 104 s retention, and switching speed down to a few nanoseconds, reflect robust high-performance data storage capability. Charge carriers trapping and detrapping at the sulfur vacancy defect sites in MoS2 nanosheets mainly display the resistive switching property, supported by the impedance analysis and theoretical fitting results. Multifunctionality is leveraged through implementing two-input logic gate operations, edge computation, and crucial adaptive learning via a Pavlov's dogs experiment. Overall, our solution-processed MoS2 memristor has the potential for tremendous future opportunities in integrated circuits and different computing paradigms, including energy-efficient neuromorphic computing hardware in artificial intelligence.

Direct Observation of Contact Electrification Effects at Nanoscale Using Scanning Probe Microscopy

AbstractIn 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 Effect of Nanowire Gap for Silicon Nanowire Transistor to the Current-Voltage (I-Vds)

One-dimensional structures are attracting a lot of attention for optimizing applications as one of the most sensitive devices. Among the fabricated devices, silicon nanowires (SiNW) and silicon nanowire transistors (SiNWT) are of particular importance for promising applications fabricated using bottom-up or top-down approaches to nanoscale devices. In this paper, the sensitivity of the current-voltage characteristic to the nanowire gap of a silicon nanowire transistor (SiNWT) was analyzed. SiNWTs with different nanowire gaps were fabricated using scanning probe microscopy by local anodic oxidation (LOA). Varies gaps can be occurring during the fabrication processes and its can be controlled by RASTER programming in LAO. These gaps can give different results of the sensitivity to the volt-ampere response. However, these gaps can be neglected depending on the subject of the studies and important to the other study, especially in nano particle sensors. In this experiment, the nanowires gaps were developed in the range of 100.5-435.6 nm and had been plotted the measurement data with the volt-ampere response. The data was analyzed using a semiconductor analyzer connected to a HP 4156C SPA series software analysis model from Desert Cryogenics. From the results had been measured the Current-Voltage (IV) increases proportionally with the nanowire gap distance in the SINWT device and this results will give significant effects to the application in nanoparticle sensors

Cholla cactus wood (Cylindropuntia imbricata): Hierarchical structure and micromechanical properties

The Cholla cactus is a species of cacti that survives in arid environments and produces a unique mesh-like porous wood. In this article, we present a comprehensive investigation on the hierarchical structure and micromechanical properties of the Cholla cactus wood. Multiple approaches consisting of X-ray tomography, scanning electron microscopy, scanning probe microscopy, nanoindentation, and finite element simulations were used to gain insight into the structure, property, and design principles of the Cholla cactus wood. The microstructure of the Cholla cactus wood consists of different components, including vessels, rays, and fibers. In the present study, we quantitatively describe the structure of each of these wood components and their likely functions, both from the perspective of biological and mechanical behavior. Nanoindentation experiments revealed for the first time that the cell walls of the fibers exhibit stiffness and hardness higher than those of rays. Furthermore, the idea of making porous, thin-walled cylinders was abstracted from the design of vessel elements, and the structures inspired by this principle were studied in tensile and torsional loading conditions using finite element simulations. Finite element simulations revealed that the utilization of a larger volume of material to carry the load leads to an increase in toughness of these structures, and thus suggested that the pores should be architected to maximize the distribution of load. Statement of significanceThe Cholla cactus wood possess a unique hierarchical structure that enables it to thrive in arid environments. Our correlative microscopy approach reveals incredible strategies that individual wood components exhibit to enable the survival of Cholla cactus in extreme environments. The present work quantifies the microstructure and mechanical properties of this very interesting natural system. We further investigate a design principle inspired by the vessel elements, one of the wood components of Cholla cactus, using finite element simulations. The study presented here advances our understanding of the structural significance of Cholla cactus and potentially other desert plants and will further help design architected structural materials.

Single-molecule electron spin resonance by means of atomic force microscopy

Understanding and controlling decoherence in open quantum systems is of fundamental interest in science, whereas achieving long coherence times is critical for quantum information processing1. Although great progress was made for individual systems, and electron spin resonance (ESR) of single spins with nanoscale resolution has been demonstrated2–4, the understanding of decoherence in many complex solid-state quantum systems requires ultimately controlling the environment down to atomic scales, as potentially enabled by scanning probe microscopy with its atomic and molecular characterization and manipulation capabilities. Consequently, the recent implementation of ESR in scanning tunnelling microscopy5–8 represents a milestone towards this goal and was quickly followed by the demonstration of coherent oscillations9,10 and access to nuclear spins11 with real-space atomic resolution. Atomic manipulation even fuelled the ambition to realize the first artificial atomic-scale quantum devices12. However, the current-based sensing inherent to this method limits coherence times12,13. Here we demonstrate pump–probe ESR atomic force microscopy (AFM) detection of electron spin transitions between non-equilibrium triplet states of individual pentacene molecules. Spectra of these transitions exhibit sub-nanoelectronvolt spectral resolution, allowing local discrimination of molecules that only differ in their isotopic configuration. Furthermore, the electron spins can be coherently manipulated over tens of microseconds. We anticipate that single-molecule ESR-AFM can be combined with atomic manipulation and characterization and thereby paves the way to learn about the atomistic origins of decoherence in atomically well-defined quantum elements and for fundamental quantum-sensing experiments.

Scanning Probe Microscopy Techniques for Studying the Cell Glycocalyx.

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.

Coupled mechanical oscillator enables precise detection of nanowire flexural vibrations

The field of nanowire (NW) technology represents an exciting and steadily growing research area with applications in ultra-sensitive mass and force sensing. Existing detection methods for NW deflection and oscillation include optical and field emission approaches. However, they are challenging for detecting small diameter NWs because of the heating produced by the laser beam and the impact of the high electric field. Alternatively, the deflection of a NW can be detected indirectly by co-resonantly coupling the NW to a cantilever and measuring it using a scanning probe microscope. Here, we prove experimentally that co-resonantly coupled devices are sensitive to small force derivatives similar to standalone NWs. We detect force derivatives as small as 10−9 N/m with a bandwidth of 1 Hz at room temperature. Furthermore, the measured hybrid vibration modes show clear signatures of avoided crossing. The detection technique presented in this work verifies a major step in boosting NW-based force and mass sensing.

Impact of grain-dependent boron uptake on the nano-electrical and local optical properties of polycrystalline boron doped CVD diamond

Boron-doped diamond (BDD) films grown by chemical vapor deposition (CVD) exhibit unique electrical and optical properties owing to the non-uniform uptake of boron dopants across grains. This study utilizes scanning probe microscopy and confocal micro- spectroscopy techniques to elucidate the influence of grain-dependent boron incorporation on the nano-electrical and local optical characteristics of polycrystalline BDD. The CVD- grown BDD film contained crystallites up to tens of microns, while the surface comprised 200…800 nm grains. Scanning spreading resistance microscopy (SSRM) revealed significant nanoscale resistance variations among individual grains, attributable to differential boron distributions. No distinct grain boundary features were discernible in SSRM data, likely due to the high boron doping of ~ 3·10 19 cm –3 . SSRM of the Au surface of a BDD/Ti/Pd/Au contact indicated a comparable granular morphology but three orders lower resistance. A network of more resistive grain boundaries was evident, modulated by underlying BDD grain clusters. Photoluminescence spectroscopy showed characteristic bands of nitrogen-vacancy centers and donor-acceptor pairs. Confocal Raman and photoluminescence mapping elucidated substantial spatial heterogeneity in micrometer- scale grains regarding crystal quality, boron and nitrogen concentrations, related to preferential incorporation. The observed peculiarities in BDD’s structural and nano- electrical characteristics stem from inherent growth inhomogeneities and grain-dependent boron uptake influenced by defects and strain fields modifying local chemical potentials. This multifaceted nanoscale examination provides critical insights into optimizing electrical and optical properties of BDD films by controlling synthesis conditions and minimizing defects for tailored performance in electronic, electrochemical, and quantum applications.

Identification of Ultrastructural Details of the Astrocyte Process System in Nervous Tissue of the Brain Using Correlative Scanning Probe and Transmission Electron Microscopy.

Nanoscale morphological features of branched processes of glial cells may be of decisive importance for neuron-astrocyte interactions in health and disease. The paper presents the results of a correlation analysis of images of thin processes of astrocytes in nervous tissue of the mouse brain, which were obtained by scanning probe microscopy (SPM) and transmission electron microscopy (TEM) with high spatial resolution. Samples were prepared and imaged using a unique hardware combination of ultramicrotomy and SPM. Astrocyte details with a thickness of several tens of nanometers were identifiable in the images, making it possible to reconstruct the three-dimensional structure of astrocytic processes by integrating a series of sequential images of ultrathin sections of nervous tissue in the future.

Machine learning-enabled autonomous operation for atomic force microscopes.

The use of scientific instruments generally requires prior knowledge and skill on the part of operators, and thus, the obtained results often vary with different operators. The autonomous operation of instruments producing reproducible and reliable results with little or no operator-to-operator variation could be of considerable benefit. Here, we demonstrate the autonomous operation of an atomic force microscope using a machine learning-based object detection technique. The developed atomic force microscope was able to autonomously perform instrument initialization, surface imaging, and image analysis. Two cameras were employed, and a machine-learning algorithm of region-based convolutional neural networks was implemented, to detect and recognize objects of interest and to perform self-calibration, alignment, and operation of each part of the instrument, as well as the analysis of obtained images. Our machine learning-based approach could be generalized to apply to various types of scanning probe microscopes and other scientific instruments.

Generating smooth potential landscapes with thermal scanning-probe lithography

Scanning probe microscopy (SPM) uses a sharp tip to interrogate surfaces with atomic precision. Inputs such as mechanical, electrical, or thermal energy can activate highly localized interactions, providing a powerful class of instruments for manipulating materials on small length scales. Thermal scanning-probe lithography (tSPL) is an advanced SPM variant that uses a silicon tip on a heated cantilever to locally sublimate polymer resist, acting as a high-resolution lithography tool and a scanning probe microscope simultaneously. The main advantage of tSPL is the ability to electrically control the temperature and applied force of the tip, which can produce smooth topographical surfaces that are unattainable with conventional nanofabrication techniques. Recent investigations have exploited these surfaces to generate potential landscapes for enhanced control of photons, electrons, excitons, and nanoparticles, demonstrating a broad range of experimental possibilities. This paper outlines the principles, procedures, and limitations of tSPL for generating smooth potentials and discusses the prospective impact in photonics, electronics, and nanomaterials science.

Epitaxial Growth of 1D Te/2D MoSe2 Mixed‐Dimensional Heterostructures for High‐Efficient Self‐Powered Photodetector

AbstractMixed‐dimensional heterostructures provide additional freedom to construct diverse functional electronic and optoelectronic devices, gaining significant interest. Herein, highly‐aligned pseudo‐1D tellurium is epitaxially grown on 2D monolayer transition metal dichalcogenides (TMDs), including MoSe2, MoS2, and WS2. A one‐pot chemical vapor deposition (CVD) technique eliminates the normally required transfer steps, thereby producing mixed‐dimensional heterostructures with an ultraclean interface. The controllable epitaxial growth of Te/TMD heterostructures are verified by Raman, scanning probe microscopy (SPM), and transmission electron microscopy (TEM) observation. The photoluminescence results indicate that the emission from TMDs is quenched in the heterostructure, confirming the efficient transfer of photogenerated carriers from TMDs to Te. Additionally, the mixed‐dimensional p‐n Te/MoSe2 heterojunction photodetector presents self‐driven behavior with high responsivity (328 mA W−1), external quantum efficiency (79%), and specific detectivity (8.2 × 109 Jones). The modified facile synthesis strategy and proposed growth mechanism in this study shed light on synthesizing mixed‐dimensional heterojunctions. This opens avenues for fabricating functional devices with reduced sizes and high densities, further enabling miniaturization and integration opportunities.

Measurement of the Adhesion Force of a Living Sessile Organism on Antifouling Coating Surfaces Prepared with Polysulfobetaine-Grafted Particles.

An antifouling polymer brush-like structure was fabricated by a simple and versatile dip-coating method of sulfobetaine containing copolymer-grafted silica nanoparticles (SiNPs) and alkyl diiodide cross-linkers. Surface-initiated atom transfer radical copolymerization of 3-(N-2-methacryloyloxyethyl-N,N-dimethyl)ammonatopropanesulfonate (MAPS) and N,N-dimethylaminoethyl methacrylate (DMAEMA) was carried out from initiator-immobilized SiNPs to give poly(MAPS-co-DMAEMA)-grafted SiNPs (MAPS/DMAEMA = 9/1, mol/mol) with diameters of 150-170 nm. The SiNP-g-copolymer/2,2,2-trifluoroethanol solution was dip-coated on silicon and glass substrates. Successive treatment with 1,4-diiodobutane in methanol gave a hydrophilic cross-linked coating film for the SiNP-g-copolymer. The cross-linked particle brushes did not peel off from the substrate even after washing with water in an ultrasonic cleaner despite the simple physical absorption of the SiNP-g-copolymer on the substrate surface. The adhesion force of the tentacle of a living barnacle cyprid on a glass surface covered with the cross-linked SiNP-g-copolymer was directly measured by scanning probe microscopy in seawater. The coating film exhibited extremely low adhesion to the cypris larva in the seawater, expecting this to be an effective antifouling property.

Evaluation of improved corrosion resistance of Zn alloy as electrode material by Co3O4 coatings

This work uses the sonochemical method to represent synthesized cobalt oxide nanoparticles (Co3O4) and analysed using different techniques. The X-ray diffraction analysis (XRD) and Fourier-transform infrared spectroscopy (FTIR) examinations of the synthesized nanoparticles confirmed their cubic structure and average crystallite size of 21.3 nm. The spherical surface shape and presence of components with a particle size of 25.3 nm were revealed. Scanning probe microscopy (SPM) methods analysed the Co3O4 coated plates' surface characteristics, including roughness and topographical ideas. An aqueous electrolyte medium (6 M KOH) was used to investigate the electrochemical corrosion behaviour of Co3O4-coated plates. According to the Tafel plot, coating Zn plates with a high surface area and mesoporous Co3O4 in KOH electrolytes greatly reduced the corrosion of the plates. The coated plates are thermally treated up to 600℃. The temperature-dependent anticorrosive properties of Co3O4 NPs are evaluated.
 KEY WORDS: Co3O4, Zn plate, Tafel plot, Linear sweep voltammetry, Anti-corrosive performance, Nanoindentation
 Bull. Chem. Soc. Ethiop. 2024, 38(1), 241-253. DOI: https://dx.doi.org/10.4314/bcse.v38i1.18

Emergent properties of magnetic ions and nanoparticles in micellar solutions of surfactants: Use in fine technologies

Objectives. To establish expected emergent (unexpected) properties of magnetic materials when obtained in aqueous micellar solutions of surfactants (aqueous quantum materials), and their use in fine technologies.Methods. Chemical synthesis of magnetic nanoparticles in aqueous micellar solutions of surfactants of various nature. Characterization of magnetic solutions and nanoparticles by magnetic measurements, spectroscopy, diffractometry, small-angle X-ray diffraction, scanning probe microscopy, and others.Results. The term “water quantum material” refers to materials (micellar solutions) whose properties are mainly determined by the nuclear quantum effect on macroscopic scales (emergent property). Micellar solutions exhibit phenomena and functionality not always consistent with the classical theory of micellization. The article presents in detail the experimental results that suggest the manifestation of the emergent properties of magnetic materials obtained in aqueous micellar solutions of surfactants. In particular, Gd3+ ions in an aqueous micellar solution of sodium dodecyl sulfate exhibit paramagnetic properties, possibly indicating their random arrangement in solution contrary to the classical theory of micellization with an ordered adsorption layer on micelles. Hybrid Pt–Gd nanoparticles are formed in a quantum material with cetylpyridinium chloride as a matrix, although Gd3+ ions must be repelled by CP+ ions on micelles. Nanosized powders of cobalt ferrite and nickel ferrite obtained in a micellar solution of sodium dodecyl sulfate have superparamagnetic properties, although the presence of their precursor ions in the adsorption layer in classical micelles should lead to ferromagnetic properties.Conclusions. The synthesis of nanoparticles in a quantum material opens up the possibility of reducing ions of different signs in one stage during the processing of metallurgy waste, in order to obtain nanoparticles of various metals and their composites. Magnetic nanoparticles obtained in a quantum surfactant material self-assemble on various substrates, enabling the creation of materials whose residual magnetization and coercive field can be controlled at room temperatures.

A multi-resistance wide-range calibration sample for conductive probe atomic force microscopy measurements.

Measuring resistances at the nanoscale has attracted recent attention for developing microelectronic components, memory devices, molecular electronics, and two-dimensional materials. Despite the decisive contribution of scanning probe microscopy in imaging resistance and current variations, measurements have remained restricted to qualitative comparisons. Reference resistance calibration samples are key to advancing the research-to-manufacturing process of nanoscale devices and materials through calibrated, reliable, and comparable measurements. No such calibration reference samples have been proposed so far. In this work, we demonstrate the development of a multi-resistance reference sample for calibrating resistance measurements in conductive probe atomic force microscopy (C-AFM) covering the range from 100 Ω to 100 GΩ. We present a comprehensive protocol for in situ calibration of the whole measurement circuit encompassing the tip, the current sensing device, and the system controller. Furthermore, we show that our developed resistance reference enables the calibration of C-AFM with a combined relative uncertainty (given at one standard deviation) lower than 2.5% over an extended range from 10 kΩ to 100 GΩ and lower than 1% for a reduced range from 1 MΩ to 50 GΩ. Our findings break through the long-standing bottleneck in C-AFM measurements, providing a universal means for adopting calibrated resistance measurements at the nanoscale in the industrial and academic research and development sectors.

Spin-Stabilization by Coulomb Blockade in a Vanadium Dimer in WSe2.

Charged dopants in 2D transition metal dichalcogenides (TMDs) have been associated with the formation of hydrogenic bound states, defect-bound trions, and gate-controlled magnetism. Charge-transfer at the TMD-substrate interface and the proximity to other charged defects can be used to regulate the occupation of the dopant's energy levels. In this study, we examine vanadium-doped WSe2 monolayers on quasi-freestanding epitaxial graphene, by high-resolution scanning probe microscopy and ab initio calculations. Vanadium atoms substitute W atoms and adopt a negative charge state through charge donation from the graphene substrate. VW-1 dopants exhibit a series of occupied p-type defect states, accompanied by an intriguing electronic fine-structure that we attribute to hydrogenic states bound to the charged impurity. We systematically studied the hybridization in V dimers with different separations. For large dimer separations, the 2e- charge state prevails, and the magnetic moment is quenched. However, the Coulomb blockade in the nearest-neighbor dimer configuration stabilizes a 1e- charge state. The nearest-neighbor V-dimer exhibits an open-shell character for the frontier defect orbital, giving rise to a paramagnetic ground state. Our findings provide microscopic insights into the charge stabilization and many-body effects of single dopants and dopant pairs in a TMD host material.

Impact of high substrate temperature on pulsed laser deposited ZnO pillars: A technological route to investigate the structural, optical and superhydrophilic properties

The structural, optical, and superhydrophilic properties of zinc oxide (ZnO) pillars are reported by pulsed laser deposition (PLD) technique at a high substrate temperature of 700 °C. The X-ray diffraction (XRD) analysis reveals that the increased crystallite size in ZnO-700 (98.47 nm) plays an important role in promoting superhydrophilic behaviour than ADZnO-RT (57.19 nm). The root-mean-square surface roughness (Rr.m.s) from scanning probe microscope (SPM) analysis demonstrates the significant enhancement in ZnO-700 surfaces. The ZnO-700 based samples show improved light absorption in the ultra-violet (UV) and visible light absorption which can boost photocatalytic activity. The photoluminescence (PL) analysis shows the highest (zinc) Zn interstitial (Zni) and lowest oxygen vacancy (OV) concentration in ZnO-700. A static contact angle (CA) measurement was performed, where ZnO-700 sample displays a smaller static CA (98.60°) compared to ADZnO-RT (101.90°), indicating more superhydrophilic nature. The ZnO-700 based sample had a better sliding angle (α) of 61.65°, a maximum frictional force (Fmax) of 1.76 μN, a corresponding work of adhesion (Wadhesion) 61.01 mN/m, and a wettability conversion rate (WCR) of 7.20 × 10−5°−1/min indicating fast sliding phenomena and better superhydrophilic transition. The superhydrophilic properties of ZnO-700 make it a valuable asset for smart surfaces and microfluidic devices application.

Toward conformational identification of molecules in 2D and 3D self-assemblies on surfaces

The design of supramolecular networks based on organic molecules deposited on surfaces, is highly attractive for various applications. One of the remaining challenges is the expansion of monolayers to well-ordered multilayers in order to enhance the functionality and complexity of self-assemblies. In this study, we present an assessment of molecular conformation from 2D to 3D supramolecular networks adsorbed onto a HOPG surface under ambient conditions utilizing a combination of scanning probe microscopies and atomic force microscopy- infrared (AFM-IR). We have observed that the infrared (IR) spectra of the designed molecules vary from layer to layer due to the modifications in the dihedral angle between the C=O group and the neighboring phenyl ring, especially in the case of a 3D supramolecular network consisting of multiple layers of molecules.

Scanning probe microscopy in the age of machine learning

Scanning probe microscopy (SPM) has revolutionized our ability to explore the nanoscale world, enabling the imaging, manipulation, and characterization of materials at the atomic and molecular level. However, conventional SPM techniques suffer from limitations, such as slow data acquisition, low signal-to-noise ratio, and complex data analysis. In recent years, the field of machine learning (ML) has emerged as a powerful tool for analyzing complex datasets and extracting meaningful patterns and features in multiple fields. The combination of ML with SPM techniques has the potential to overcome many of the limitations of conventional SPM methods and unlock new opportunities for nanoscale research. In this review article, we will provide an overview of the recent developments in ML-based SPM, including its applications in topography imaging, surface characterization, and secondary imaging modes, such as electrical, spectroscopic, and mechanical datasets. We will also discuss the challenges and opportunities of integrating ML with SPM techniques and highlight the potential impact of this interdisciplinary field on various fields of science and engineering.