Direct Measurement of Periodic Electric Forces in Liquids

The electric forces acting on an atomic force microscope tip in solution have been measured using a microelectrochemical cell formed by two periodically biased electrodes. The forces were measured as a function of lift height and bias amplitude and frequency, providing insight into electrostatic interactions in liquids. Real-space mapping of the vertical and lateral components of electrostatic forces acting on the tip from the deflection and torsion of the cantilever is demonstrated. This method enables direct probing of electrostatic and convective forces involved in electrophoretic and dielectroforetic self-assembly and electrical tweezer operation in liquid environments

The Band Excitation Method in Scanning Probe Microscopy for Rapid Mapping of Energy Dissipation on the Nanoscale

Mapping energy transformation pathways and dissipation on the nanoscale and understanding the role of local structure on dissipative behavior is a challenge for imaging in areas ranging from electronics and information technologies to efficient energy production. Here we develop a novel Scanning Probe Microscopy (SPM) technique in which the cantilever is excited and the response is recorded over a band of frequencies simultaneously rather than at a single frequency as in conventional SPMs. This band excitation (BE) SPM allows very rapid acquisition of the full frequency response at each point (i.e. transfer function) in an image and in particular enables the direct measurement of energy dissipation through the determination of the Q-factor of the cantilever-sample system. The BE method is demonstrated for force-distance and voltage spectroscopies and for magnetic dissipation imaging with sensitivity close to the thermomechanical limit. The applicability of BE for various SPMs is analyzed, and the method is expected to be universally applicable to all ambient and liquid SPMs.Comment: 32 pages, 9 figures, accepted for publication in Nanotechnolog

Fabrication, Dynamics, and Electrical Properties of Insulated SPM Probes for Electrical and Electromechanical Imaging in Liquids

Insulated cantilever probes with a high aspect ratio conducting apex have been fabricated and their dynamic and electrical properties analyzed. The cantilevers were coated with silicon dioxide and a via was fabricated through the oxide at the tip apex and backfilled with tungsten to create an insulated probe with a conducting tip. The stiffness and Q-factor of the cantilevers increased after the modifications and their resonances shifted to higher frequencies. The coupling strength between the cantilever and the coating are determined. The applications to conductive and electromechanical imaging of ferroelectric domains are illustrated, and a probe apex repair process is demonstrated.Comment: 3 fig

Theory-assisted determination of nano-rippling and impurities in atomic resolution images of angle-mismatched bilayer graphene

Ripples and impurity atoms are universally present in 2D materials, limiting carrier mobility, creating pseudo–magnetic fields, or affecting the electronic and magnetic properties. Scanning transmission electron microscopy (STEM) generally provides picometer-level precision in the determination of the location of atoms or atomic 'columns' in the in-image plane (xy plane). However, precise atomic positions in the z-direction as well as the presence of certain impurities are difficult to detect. Furthermore, images containing moiré patterns such as those in angle-mismatched bilayer graphene compound the problem by limiting the determination of atomic positions in the xy plane. Here, we introduce a reconstructive approach for the analysis of STEM images of twisted bilayers that combines the accessible xy coordinates of atomic positions in a STEM image with density-functional-theory calculations. The approach allows us to determine all three coordinates of all atomic positions in the bilayer and establishes the presence and identity of impurities. The deduced strain-induced rippling in a twisted bilayer graphene sample is consistent with the continuum model of elasticity. We also find that the moiré pattern induces undulations in the z direction that are approximately an order of magnitude smaller than the strain-induced rippling. A single substitutional impurity, identified as nitrogen, is detected. The present reconstructive approach can, therefore, distinguish between moiré and strain-induced effects and allows for the full reconstruction of 3D positions and atomic identities

Electronic Transport Imaging in a Multiwire SnO2 ChemFET Device

The electronic transport and the sensing performance of an individual SnO2 crossed nanowires device in a three-terminal field effect configuration were investigated using a combination of macroscopic transport measurements and Scanning Surface Potential Microscopy (SSPM). The structure of the device was determined using both Scanning Electron- and Atomic Force Microscopy data. The SSPM images of two crossed 1D nanostructures, simulating a prototypical nanowire network sensors, exhibit large dc potential drops at the crossed-wire junction and at the contacts, identifying them as the primary electroactive elements in the circuit. The gas sensitivity of this device was comparable to those of sensors formed by individual homogeneous nanostructures of similar dimensions. Under ambient conditions, the DC transport measurements were found to be strongly affected by field-induced surface charges on the nanostructure and the gate oxide. These charges result in a memory effect in transport measurements and charge dynamics which are visualized by SSPM. Finally, scanning probe microscopy is used to measure the current-voltage characteristics of individual active circuit elements, paving the way to a detailed understanding of chemical functionality at the level of an individual electroactive element in an individual nanowire.Comment: 30 pages, 8 figures, accepted to J. Appl. Phy

Phase transitions in two dimensions - the case of Sn adsorbed on Ge(111) surfaces

Accurate atomic coordinates of the room-temperature (root3xroot3)R30degree and low-temperature (3x3) phases of 1/3 ML Sn on Ge(111) have been established by grazing-incidence x-ray diffraction with synchrotron radiation. The Sn atoms are located solely at T4-sites in the (root3xroot3)R30degree structure. In the low temperature phase one of the three Sn atoms per (3x3) unit cell is displaced outwards by 0.26 +/- 0.04 A relative to the other two. This displacement is accompanied by an increase in the first to second double-layer spacing in the Ge substrate.Comment: RevTeX, 5 pages including 2 figure

Dynamic Behavior in Piezoresponse Force Microscopy

Frequency dependent dynamic behavior in Piezoresponse Force Microscopy (PFM) implemented on a beam-deflection atomic force microscope (AFM) is analyzed using a combination of modeling and experimental measurements. The PFM signal comprises contributions from local electrostatic forces acting on the tip, distributed forces acting on the cantilever, and three components of the electromechanical response vector. These interactions result in the bending and torsion of the cantilever, detected as vertical and lateral PFM signals. The relative magnitudes of these contributions depend on geometric parameters of the system, the stiffness and frictional forces of tip-surface junction, and operation frequencies. The dynamic signal formation mechanism in PFM is analyzed and conditions for optimal PFM imaging are formulated. The experimental approach for probing cantilever dynamics using frequency-bias spectroscopy and deconvolution of electromechanical and electrostatic contrast is implemented.Comment: 65 pages, 15 figures, high quality version available upon reques

Nanoelectromechanics of Polarization Switching in Piezoresponse Force Microscopy

Nanoscale polarization switching in ferroelectric materials by Piezoresponse Force Microscopy (PFM) in weak and strong indentation limits is analyzed using exact solutions for electrostatic and coupled electroelastic fields below the tip. It is proposed that the tip-induced domain switching can be mapped on the Landau theory of phase transitions with the domain size as an order parameter. For a point charge interacting with a ferroelectric surface, switching of both first and second order is possible depending on the charge-surface separation. For a realistic tip shape, the domain nucleation process is first order in charge magnitude and polarization switching occurs only above a critical tip bias. In pure ferroelectric or ferroelastic switching, the late stages of the switching process can be described using point charge/force model and arbitrarily large domains can be created; however, the description of the early stages of nucleation process when domain size is comparable with the tip radius of curvature requires exact field structure to be taken into account.Comment: 16 pages, 3 figures, expanded version of paper submitted to PR

Determination of the (3x3)-Sn/Ge(111) structure by photoelectron diffraction

At a coverage of about 1/3 monolayer, Sn deposited on Ge(111) below 550 forms a metastable (sqrt3 x sqrt3)R30 phase. This phase continuously and reversibly transforms into a (3x3) one, upon cooling below 200 K. The photoemission spectra of the Sn 4d electrons from the (3x3)-Sn/Ge(111) surface present two components which are attributed to inequivalent Sn atoms in T4 bonding sites. This structure has been explored by photoelectron diffraction experiments performed at the ALOISA beamline of the Elettra storage ring in Trieste (Italy). The modulation of the intensities of the two Sn components, caused by the backscattering of the underneath Ge atoms, has been measured as a function of the emission angle at fixed kinetic energies and viceversa. The bond angle between Sn and its nearest neighbour atoms in the first Ge layer (Sn-Ge1) has been measured by taking polar scans along the main symmetry directions and it was found almost equivalent for the two components. The corresponding bond lengths are also quite similar, as obtained by studying the dependence on the photoelectron kinetic energy, while keeping the photon polarization and the collection direction parallel to the Sn-Ge1 bond orientation (bond emission). A clear difference between the two bonding sites is observed when studying the energy dependence at normal emission, where the sensitivity to the Sn height above the Ge atom in the second layer is enhanced. This vertical distance is found to be 0.3 Angstroms larger for one Sn atom out of the three contained in the lattice unit cell. The (3x3)-Sn/Ge(111) is thus characterized by a structure where the Sn atom and its three nearest neighbour Ge atoms form a rather rigid unit that presents a strong vertical distortion with respect to the underneath atom of the second Ge layer.Comment: 10 pages with 9 figures, added reference