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An electrochemical cell was designed to enable in situ atomic force microscopy (AFM) measurements. The finite-element method was implemented using COMSOL Multiphysics to simulate the electrical field within the cell and to find the current and potential distribution. A comparative three-dimensional simulation study was made to compare two different designs and to elucidate the importance of the geometry on the electrical field distribution. The design was optimized to reduce the uncertainty in the measurement of the electrochemical impedance. Then, an in situ, simultaneous electrochemical and time-resolved AFM experiments were conducted to study the surface evolution of the aluminum alloy AA2024-T3 exposed to 0.5 M NaCl. The temporal change of the surface topography was recorded during the application of chrono-amperometric pulses using a newly designed electrochemical cell. Electrochemical impedance spectroscopy was conducted on the sample to confirm the recorded topographical change. The newly developed cell made it possible to monitor the surface change and the growth of the oxyhydroxide layer on the AA2024-T3 with the simultaneous application of electrochemical methods.
We are proposing a novel fabrication method for single crystal diamond scanning probes for atomic force microscopy (AFM), exploiting Faraday cage angled etching (FCAE). Common, oxygen-based, inductively coupled plasma (ICP) dry etching processes for diamond are limited with respect to the achievable geometries. The fabrication of freestanding micro- and nanostructures is therefore challenging. This is a major disadvantage for several application fields e.g., for realizing scanning magnetometry probes based on nitrogen vacancy (NV) centres and capable of measuring magnetic fields at the nanoscale. Combining a planar design with FCAE and state-of-the-art electron beam lithography (EBL) yields a reduction of process complexity and cost compared to the established fabrication technology of micro-opto-mechanical diamond devices. Here, we report on the direct comparison of both approaches and present first proof-of-concept planar-FCAE-prototypes for scanning probe applications.
Single crystal gold clusters (10 nm in size) have been collectively manipulated on mono- and bi-layered MoS2 islands (up to 20 µm) grown on SiO2 using AFM. On the monolayer the clusters tend to move in a direction corresponding to the zigzag alignment of the Mo and S atoms, and assemble into long striation patterns parallel to the scan direction. The distance between consecutive stripes is inversely proportional to the cluster concentration and size. A more detailed observation based on SEM shows that within each stripe the clusters remain separated by gaps of few nm in width possibly caused by electrostatic repulsion and/or the roughness of the SiO2 substrate (~2 nm). The stripes also proved to be thermally stable, preserving their superstructures up to 823 K. On the bilayer gold clusters are much less prone to move and assemble into stripes. These results suggest that the formation of nanostructures resulting from collective manipulation of metal clusters can be oriented by a properly chosen scan path in a rather straightforward way (as compared to one-by-one displacement of single clusters). The goal of forming µm-long but nm-thin wires with a geometrically defined shape could be easily reached with the use of smoother substrates or TMD materials with lesser charge transfer to metals adsorbed on them.
Atomic force microscopy (AFM) is used in a wide range
of applications for imaging sub-nanometer resolution
topography, as well as for analysis of physical
characteristics (such as surface stiffness and
electromagnetic properties). While surface imaging
and characterization on the nanoscale is of great
value and is widely used across all fields of
science, correlation with other types of microscopy
can greatly enhance the value of those measurements.
Here, we discuss a new approach that uses a small,
ultra-thin AFM, which allows it to be integrated
with standard light microscopes. The authors believe
the design will allow for a new paradigm in
microscopy, by enabling all the advantages of AFM to
be combined with the advanced imaging capabilities
of research-grade light microscopes.
High-density storage technology beyond hard disk drives and flash memory is required. Efforts are underway to develop new high-density storage technology based on scanning probe-based data storage. One of the candidates for scanning probe-type storage is thermomechanical data storage (also known as millipede, developed by IBM Zürich), and another is ferroelectric data storage. In this article, probe data-storage technologies are overviewed. Thermomechanical data storage and ferroelectric data storage are described in detail for next-generation high-density data-storage technology based on scanning probe microscopy. Ferroelectric data storage and scanning nonlinear dielectric microscopy-based and field-effect transistor-type probe-based probe data storage are also described.
Mechanical properties of neurons represent a key factor that determines the functionality of neuronal cells and the formation of neural networks. The main source of mechanical stability for the cell is a biopolymer network of microtubules and actin filaments that form the main components of the cellular cytoskeleton. This biopolymer network is responsible for the growth of neuronal cells as they extend neurites to connect with other neurons, forming the nervous system. Here we present experimental results that combine atomic force microscopy (AFM) and fluorescence microscopy to produce systematic, high-resolution elasticity and fluorescence maps of cortical neurons. This approach allows us to apply external forces to neurons, and to monitor the dynamics of the cell cytoskeleton. We measure how the elastic modulus of neurons changes upon changing the ambient temperature, and identify the cytoskeletal components responsible for these changes. These results demonstrate the importance of taking into account the effect of ambient temperature when measuring the mechanical properties of cells.
Despite being one of the oldest phenomena known to mankind and its vast use, there still are open questions about the frictional process between two surfaces, especially at the nanometer scale, such as the energy dissipation mechanism, the influence of the crystallographic orientation and the correlation between macroscopic and microscopic scales. In this work, we analyze the interaction between a sharp tip and graphene by friction force microscopy. The graphene surface roughness and adhesion forces with the microscope tip were measured. Neither roughness nor adhesion were observed to influence the friction forces. The scanning velocity dependence of friction was also measured for a different number of layers. The friction forces were observed to increase with the scanning velocity until a critical velocity is achieved by which we have estimated the effective interaction potential between the tip and the graphene surface.
The main functions of the dynamic cantilever calibrator (DCC), which are related to characterization of AFM probes and instruments, are demonstrated on a variety of probes. The resonant frequency, Q-factor and spring constant of the rectangular and V-shaped probes were evaluated by thermal tune method. The inverse optical sensitivity and optical beam deflection noise, which define performance of AFM microscopes, were extracted from DCC data. Peculiarities of thermal tune studies and the use of DCC for advanced applications are discussed.
Temperature-dependent variations in electric switching and transverse resistance of phase-change [(GeTe)2(Sb2Te3)]n (n=4 and 8) chalcogenide superlattice (CSL) films were studied using conductive scanning probe microscopy (SPM). Three temperature regions with different electric transport properties were recognized in point current-voltage (I-V) spectra and the surface potential maps measured with tantalum and platinum-coated SPM cantilevers. At around 80°C the switching voltage decreased abruptly from ∼2 V to 0.5 V and the thermal coefficient of resistance changes its sign, indicating different carrier transport mechanisms. The observed changes correlated with decrease in the surface potential by ∼150 meV from 25 to 150°C. The results were ascribed to an opening of the CSL electronic band gap near the Fermi energy caused by thermal stress, which led to the transition from a Dirac-like semimetal to a narrow-gap semiconductor.
Atomic force microscopy (AFM) and nanoindentation were used to characterize poly (methyl methacrylate) (PMMA) films with a wide distribution of pores. Pores with diameters ranging from tens of nanometers to few micrometers were measured by AFM and cross-section scanning electron microscopy (SEM). Atomic force acoustic microscopy (AFAM) mapping of the elastic modulus were correlated with the samples topography and pore distribution. The elastic moduli of the samples were additionally measured by nanoindentation.
Imaging of nanoscale structures buried in a covering material is an extremely challenging task, but is also considered extremely important in a wide variety of fields. From fundamental research into the way living cells are built up to process control in semiconductor manufacturing would all benefit from the capability to image nanoscale structures through arbitrary covering layers. Combining Atomic Force Microscopy (AFM) with ultrasound has been shown a promising technology to enable such imaging in various configurations. Here we report the development of an alternative method of combining AFM with ultrasound which we call SubSurface Ultrasonic Resonance Force Microscopy (SSURFM) and which is based on a combination of the two most common variants described in literature, which each have their specific strong points: Ultrasonic Force Microscopy (UFM) and Contact Resonance AFM (CR-AFM). We show the excellent performance of this combination on a number of samples designed specifically to mimic relevant conditions for the application as a metrology technique in the semiconductor manufacturing process. We also discuss the physics of the image contrast mechanism which is based on sensing local changes in visco-elastic properties of the sample bygenerating large indentations in the surface.
Structural analysis on interfaces between ionic liquids (ILs) and solid substrates is an important study for not only the basic fundamental aspects but also many technological processes. In the present work, we utilized frequency modulation atomic force microscopy (FM-AFM) based on a quartz tuning fork sensor to elucidate the structure of interface between 1-butyl-3-methylimidazolium hexafluorophosphate (BMI-PF6) IL and highly ordered pyrolytic graphite (HOPG) surface. It was observed that this IL form solvation layers at their interface, with ∼0.5-0.57 nm thickness of each layer. We have compared our experimental results with previously reported results from molecular dynamics simulation study, and combination of classical molecular dynamics and density functional theory calculations in order to understand the IL/HOPG interface.
BiFeO3 (BFO) is the most studied room temperature multiferroic compound. In this work we demonstrate a template assisted growth process through which the growth strain is controlled to achieve required phase of BFO. Growth of (∼20nm) fully strained tetragonal (T), rhombohedral (R) and mixed phase of T and R of Bismuth ferrite (BiFeO3) was achieved by varying the thickness of the template layer. The different phases were confirmed by using high resolution x-ray diffractions studies. The conductivity map of all the three phases were carried out using an atomic force microscope operating in conductive mode. Tip induced surface defect migration within a given grain was observed in pure phases and the conductivity map confirmed the same. The room temperature resistivity is found to be decreasing systematically from 1.1×106 Ωm , 935×105 Ωm and 1.16×104 Ωm respectively for tetragonal, mixed phase and rhombohedral phase BFO. In the case of mixed phase both the nano- scale and macroscopic leakage current studies show low conductivity, which could be due to the increased pinning sites that increases the energy barrier for the defect migration. The local nano-scale measurements and conductivity mapping corroborates well with the macroscopic studies.
Environmental atomic force microscopy (AFM) study of brush macromolecules, polymer blends and bitumen was performed with regular and Quick Scan imaging. Condensation of different vapors on sample surface has induced swelling of hydrophilic domains that helps recognizing the components of heterogeneous compounds. High-resolution imaging of brush macromolecules was achieved in ethyl acetate vapor. Fast monitoring of aggregation/spreading of brush macromolecules revealed dynamics of conformational changes and molecular motion.
Fast imaging in Atomic Force Microscopy enhances the capability of studying phase transitions and surface properties of materials at variable temperatures. This is demonstrated by measurements of several polymers [poly(diethylsiloxane), low-density polyethylene and ethylene-octene copolymer] and bitumen at low (down to -20°C) and high (up to +150°C) temperatures. Monitoring of structural transitions was performed at small and large (up to 40 μm) areas with 1-5°C/min cooling/heating rates. Novel data about dynamics and structural transitions of mesomorphic transitions and crystallization were obtained.
Scanning tunneling microscopy (STM) is an excellent technique to image the surfaces of materials with extreme spatial resolution. However, it is difficult to maintain its imaging quality when applying the technique under the conditions used in many practical processes, such as chemical vapor deposition and catalysis. In this article, we describe two special classes of STM instruments that are capable of maintaining good imaging quality under “difficult” conditions, namely, one for high and variable temperatures and the other for the combination of high temperatures and high gas pressures. In both cases, we discuss the special design features that make these instruments robust with respect to the challenging imaging conditions and provide examples to illustrate how they are applied.
Stabilization of surface supported fluid lipid multilayers for underwater characterization is an essential step in making them useful for scalable cell culture applications such as high throughput screening. To this end, we used tetraethyl orthosilicate (TEOS), recently shown to stabilize fluid lipid films while maintaining their fluidity and functionality under water, to stabilize lipid multilayer micropatterns of 1,2-dioleoyl-sn-glycero-3-phosphocholine (DOPC). The treated multilayers were immersed under water and successfully imaged by atomic force microscopy (AFM), a difficult feat to perform on fluid lipid multilayers without TEOS treatment. The treated lipid multilayer showed an average swelling of approximately 18% in water but remained stable during the imaging process. The TEOS-treated lipid multilayers also proved compatible with cell culture as HeLa, MDCK, and HEK cell types all adhered and grew in high numbers over the multilayers. The results obtained here open the door to the use of fluid lipid multilayers in biotechnology applications such as microarray based high throughput cell assays.
Lignocellulosic biofuels have been identified as a possible solution to contribute to the world’s demands in energy and environmental sustainability. However, the fundamental understanding of the physical and chemical traits hindering key reactions during biomass to biofuel conversion processes has been limited by the lack of suitable tools and by the large natural variability in such systems. Reaction wood constitutes a good model system to study variations of cellulose content, given the increase in cellulose content in the cell walls of the region under tension in the plant during growth. In this work, we use confocal Raman mapping and Pulsed Force Mode Atomic Force Microscopy (PFM) to explore the effect of variation in cellulose content on the structure and composition of the plant cell wall at the nanoscale. Using statistical analysis on Raman datasets, the characteristic peaks for cellulose and lignin are examined to reveal changes in peak positions across the different scanned regions of the cross section. PFM is used to study local mechanical properties of the different layers of the cell wall. Our approach facilitates the correlation of structure-composition traits of the plant cell wall for a more fundamental understanding of processes involved in biofuel research.
The rapid growth of scientific publications necessitates new methods to understand the direction of scientific research within fields of study, ascertain the importance of particular groups, authors, or institutions, compute metrics that can determine the importance (centrality) of particular seminal papers, and provide insight into the social (collaboration) networks that are present. We present one such method based on analysis of citation networks, using the freely available CiteSpace Program. We use citation network analysis on three examples, including a single material that has been widely explored in the last decade (BiFeO3), two small subfields with a minimal number of authors (flexoelectricity and Kitaev physics), and a much wider field with thousands of publications pertaining to a single technique (scanning tunneling microscopy). Interpretation of the analysis and key insights into the fields, such as whether the fields are experiencing resurgence or stagnation, are discussed, and author or collaboration networks that are prominent are determined. Such methods represent a paradigm shift in our way of dealing with the large volume of scientific publications and could change the way literature searches and reviews are conducted, as well as how the impact of specific work is assessed.
Nanodiamonds (NDs) represent a novel nanomaterial applicable from biomedicine to
spintronics. Here we study ability of air annealing to further decrease the
typical 5 nm NDs produced by detonation synthesis. We use atomic force
microscopy (AFM) with sub-nm resolution to directly measure individual
detonation nanodiamonds (DNDs) on a flat Si substrate. By means of particle
analysis we obtain their accurate and statistically relevant size distributions.
Using this approach, we characterize evolution of the size distribution as a
function of time and annealing temperature: i) at constant time (25 min) with
changing temperature (480, 490, 500°C) and ii) at constant temperature
(490°C) with changing time (10, 25, 50 min). We show that the mean size
of DNDs can be controllably reduced from 4.5 nm to 1.8 nm without noticeable
particle loss and down to 1.3 nm with 36% yield. By air annealing the size
distribution changes from Gaussian to lognormal with a steep edge around 1 nm,
indicating instability of DNDs below 1 nm.