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Inducing an inversion layer in organic semiconductors is a highly nontrivial, but critical, achievement for producing organic field-effect transistor (OFET) devices, which rely on the generation of inversion, accumulation, and depletion regimes for successful operation. In recent years, a major milestone was reached: an OFET was made to successfully operate in the inversion-mode for the first time. Here, we develop a pulsed bias technique to characterize the dopant type of any organic material system, without prior knowledge or characterization of the material in question. We use this technique on a pentacene/PTCDI heterostructure and thus deduce that pentacene is n-doped by impurities. Additionally, through tip-induced band-bending, we generate inversion, depletion, and accumulation regimes over a 20~nm radius, three monolayer thick n-doped pentacene island. Our findings demonstrate that nanometer-scale lateral extent and thickness are sufficient for an OFET device to operate in the inversion regime., Updated manuscript with additional data and findings

The nonlinear optical response of a material is a sensitive probe of electronic and structural dynamics under strong light fields. The induced microscopic polarizations are usually detected via their far-field light emission, thus limiting spatial resolution. Several powerful near-field techniques circumvent this limitation by employing local nanoscale scatterers; however, their signal strength scales unfavorably as the probe volume decreases. Here, we demonstrate that time-resolved atomic force microscopy is capable of temporally and spatially resolving the microscopic, electrostatic forces arising from a nonlinear optical polarization in an insulating dielectric driven by femtosecond optical fields. The measured forces can be qualitatively explained by a second-order nonlinear interaction in the sample. The force resulting from this nonlinear interaction has frequency components below the mechanical resonance frequency of the cantilever and is thus detectable by regular atomic force microscopy methods. The capability to measure a nonlinear polarization through its electrostatic force is a powerful means to revisit nonlinear optical effects at the nanoscale, without the need for emitted photons or electrons from the surface. © 2020 National Academy of Sciences. All rights reserved., Proceedings of the National Academy of Sciences of the United States of America, 117 (33), ISSN:0027-8424, ISSN:1091-6490

Long-range electron transfer is a ubiquitous process that plays an important role in electrochemistry, biochemistry, organic electronics, and single molecule electronics. Fundamentally, quantum mechanical processes, at their core, manifest through both electron tunneling and the associated transition between quantized nuclear vibronic states (intramolecular vibrational relaxation) mediated by electron-nuclear coupling. Here, we report on measurements of long-range electron transfer at the interface between a single ferrocene molecule and a gold substrate separated by a hexadecanethiol quantum tunneling barrier. These redox measurements exhibit quantized nuclear transitions mediated by electron-nuclear coupling at 4.7 K in vacuum. By detecting the electric force associated with redox events by atomic force microscopy (AFM), with increasing AFM oscillation amplitude, the intensity of the observed cantilever resonance frequency shift peak increases and then exhibits a series of discrete steps that are indicative of quantized nuclear transitions. The observed peak shapes agree well with a single-electron tunneling model with quantized nuclear state transitions associated with the conversion of the molecule between oxidized and reduced electronic states. This technique opens the door to simultaneously investigating quantized electron and nuclear dynamics in a diverse range of systems.

Recently, there have been a number of variations of electrostatic force microscopy (EFM) that allow for the measurement of time-varying forces arising from phenomena such as ion transport in battery materials or charge separation in photovoltaic systems. These forces reveal information about dynamic processes happening over nanometer length scales due to the nanometer-sized probe tips used in atomic force microscopy. Here, we review in detail several time-resolved EFM techniques based on non-contact atomic force microscopy, elaborating on their specific limitations and challenges. We also introduce a new experimental technique that can resolve time-varying signals well below the oscillation period of the cantilever and compare and contrast it with those previously established.

Solid-state nanopores are powerful tools for sensing of single biomolecules in solution. Fabrication of solid-state nanopores is still challenging, however; in particular, new methods are needed to facilitate the integration of pores with larger nanofluidic and electronic device architectures. We have developed the tip-controlled local breakdown (TCLB) approach, in which an atomic force microscope (AFM) tip is brought into contact with a silicon nitride membrane that is placed onto an electrolyte reservoir. The application of a voltage bias at the AFM tip induces a dielectric breakdown that leads to the formation of a nanopore at the tip position. In this work, we report on the details of the apparatus used to fabricate nanopores using the TCLB method, and we demonstrate the formation of nanopores with smaller, more controlled diameters using a current limiting circuit that zeroes the voltage upon pore formation. Additionally, we demonstrate the capability of TCLB to fabricate pores aligned to embedded topographical features on the membranes.

Ice nucleation microphysical processes are identified to be of high importance in forecasting the magnitude of the Earth’s climate change. The environmental conditions often influence the ice nucleation processes in the Earth’s atmosphere. We herein study the impact of various environmental conditions on FeHg (maghemite–Hg2Cl2 composite), a highly efficient ice nucleating particle with similar freezing point to the best inorganic ice nuclei, AgI. FeHg is formed from FeCl2·4H2O and HgCl2, which are observed in the environment, in contrast to AgI, which is rarely found. The ice nucleation efficacy remained unchanged for FeHg under ambient conditions for a long duration. To mimic the atmosphere, we performed a series of experiments using a suite of complementary techniques, at various levels of radiation intensity, temperature, and pH for FeHg. Experiments were also performed in the presence of atmospheric pollutants, such as ozone (in the presence or absence of light), as well as nine emerging metal oxides ...

With recent advances in scanning probe microscopy (SPM), it is now routine to determine the atomic structure of surfaces and molecules while quantifying the local tip-sample interaction potentials. Such quantitative experiments are based on the accurate measurement of the resonance frequency shift due to the tip-sample interaction. Here, we experimentally show that the resonance frequency of oscillating probes used for SPM experiments change systematically as a function of oscillation amplitude under typical operating conditions. This change in resonance frequency is not due to tip-sample interactions, but rather due to the cantilever strain or geometric effects and thus the resonance frequency being a function of the oscillation amplitude. Our numerical calculations demonstrate that the amplitude dependence of the resonance frequency is an additional yet overlooked systematic error source that can result nonnegligible errors in measured interaction potentials and forces. Our experimental results and complementary numerical calculations reveal that the frequency shift due to this amplitude dependence needs to be corrected even for experiments with active oscillation amplitude control to be able to quantify the tip-sample interaction potentials and forces with milli-electron volt and pico-Newton resolutions., 18 pages, 3 Figures, 1 table, and supplemental material

Reliable operation of frequency modulation mode atomic force microscopy (FM-AFM) depends on a clean resonance of an AFM cantilever. It is recognized that the spurious mechanical resonances which originate from various mechanical components in the microscope body are excited by a piezoelectric element that is intended for exciting the AFM cantilever oscillation and these spurious resonance modes cause the serious undesirable signal artifacts in both frequency shift and dissipation signals. We present an experimental setup to excite only the oscillation of the AFM cantilever in a fiber-optic interferometer system using optical excitation force. While the optical excitation force is provided by a separate laser light source with a different wavelength (excitation laser : {\lambda} = 1310 nm), the excitation laser light is still guided through the same single-mode optical fiber that guides the laser light (detection laser : {\lambda} = 1550 nm) used for the interferometric detection of the cantilever deflection. We present the details of the instrumentation and its performance. This setup allows us to eliminate the problems associated with the spurious mechanical resonances such as the apparent dissipation signal and the inaccuracy in the resonance frequency measurement., Comment: 11 pages, 10 figures

A common use of atomic force microscopy is quantifying local forces through tip-sample interactions between the probe tip and a sample surface. The accuracy of these measurements depends on the accuracy to which the cantilever spring constant is known. Recent work has demonstrated that the measured spring constant of a cantilever can vary up to a factor of five, even for the exact same cantilever measured by different users on different microscopes. Here, we demonstrate that a standard method for calibrating the spring constant (using oscillations due to thermal energy) is susceptible to ambient acoustic noise, which can alter the result significantly. We demonstrate a step-by-step method to measure the spring constant by actively driving the cantilever to measure the resonance frequency and the quality factor, giving results that are unaffected by acoustic noise. Our method can be performed rapidly on any atomic force microscope without any expensive additional hardware.A common use of atomic force microscopy is quantifying local forces through tip-sample interactions between the probe tip and a sample surface. The accuracy of these measurements depends on the accuracy to which the cantilever spring constant is known. Recent work has demonstrated that the measured spring constant of a cantilever can vary up to a factor of five, even for the exact same cantilever measured by different users on different microscopes. Here, we demonstrate that a standard method for calibrating the spring constant (using oscillations due to thermal energy) is susceptible to ambient acoustic noise, which can alter the result significantly. We demonstrate a step-by-step method to measure the spring constant by actively driving the cantilever to measure the resonance frequency and the quality factor, giving results that are unaffected by acoustic noise. Our method can be performed rapidly on any atomic force microscope without any expensive additional hardware.

Atomic force microscopy (AFM) is an analytical surface characterization tool which can reveal a sample's topography with high spatial resolution while simultaneously probing tip-sample interactions. Local measurement of chemical properties with high-resolution has gained much popularity in recent years with advances in dynamic AFM methodologies. A calibration factor is required to convert the electrical readout to a mechanical oscillation amplitude in order to extract quantitative information about the surface. We propose a new calibration technique for the oscillation amplitude of electrically driven probes, which is based on measuring the electrical energy input to maintain the oscillation amplitude constant. We demonstrate the application of the new technique with quartz tuning fork including the qPlus configuration, while the same principle can be applied to other piezoelectric resonators such as length extension resonators, or piezoelectric cantilevers. The calibration factor obtained by this technique is found to be in agreement with using thermal noise spectrum method for capsulated, decapsulated tuning forks and tuning forks in the qPlus configuration., Comment: Main Text 10 pages (3 Figures and 1 Table), Supplemental Information (7 pages)

We review a new experimental implementation of Kelvin probe force microscopy (KPFM) in which the dissipation signal of frequency modulation atomic force microscopy (FM-AFM) is used for dc bias voltage feedback (D-KPFM). The dissipation arises from an oscillating electrostatic force that is coherent with the tip oscillation, which is caused by applying the ac voltage between the tip and sample. The magnitude of the externally induced dissipation is found to be proportional to the effective dc bias voltage, which is the difference between the applied dc voltage and the contact potential difference. Two different implementations of D-KPFM are presented. In the first implementation, the frequency of the applied ac voltage, \(f_\mathrm {el}\), is chosen to be the same as the tip oscillation (\(f_\mathrm {el} = f_\mathrm {m}\): \(1\omega \)D-KPFM). In the second one, the ac voltage frequency, \(f_\mathrm {el}\), is chosen to be twice the tip oscillation frequency (\(f_\mathrm {el}= 2 f_\mathrm {m}\): \(2\omega \)D-KPFM). In \(1\omega \)D-KPFM, the dissipation is proportional to the electrostatic force, which enables the use of a small ac voltage amplitude even down to \({\approx }10\) mV. In \(2\omega \)D-KPFM, the dissipation is proportional to the electrostatic force gradient, which results in the same potential contrast as that obtained by FM-KPFM. D-KPFM features a simple implementation with no lock-in amplifier and faster scanning as it requires no low frequency modulation. The use of a small ac voltage amplitude in \(1\omega \)D-KPFM is of great importance in characterizing of technically relevant materials in which their electrical properties can be disturbed by the applied electric field. \(2\omega \)D-KPFM is useful when more accurate potential measurement is required. The operations in \(1\omega \) and \(2\omega \)D-KPFM can be switched easily to take advantage of both features at the same location on a sample.

One of the main challenges in improving fast charging lithium-ion batteries is the development of suitable active materials for cathodes and anodes. Many materials suffer from unacceptable structural changes under high currents and/or low intrinsic conductivities. Experimental measurements are required to optimize these properties, but few techniques are able to spatially resolve ionic transport properties at small length scales. Here we demonstrate an atomic force microscope (AFM)-based technique to measure local ionic transport on LiFePO4 to correlate with the structural and compositional analysis of the same region. By comparing the measured values with density functional theory (DFT) calculations, we demonstrate that Coulomb interactions between ions give rise to a collective activation energy for ionic transport that is dominated by large phase boundary hopping barriers. We successfully measure both the collective activation energy and the smaller single-ion bulk hopping barrier and obtain excellent ...

We report a Kelvin probe force microscopy (KPFM) implementation using the dissipation signal of a frequency modulation atomic force microscopy that is capable of detecting the gradient of electrostatic force rather than electrostatic force. It features a simple implementation and faster scanning as it requires no low frequency modulation. We show that applying a coherent ac voltage with two times the cantilever oscillation frequency induces the dissipation signal proportional to the electrostatic force gradient which depends on the effective dc bias voltage including the contact potential difference. We demonstrate the KPFM images of a MoS$_2$ flake taken with the present method is in quantitative agreement with that taken with the frequency modulated Kelvin probe force microscopy technique., Comment: 4 pages, 4 figures, supplemental materials. arXiv admin note: text overlap with arXiv:1508.05866

Atoms transferred to W(111) and W(110) tip apices from the Au(111) surface during tunneling and approach to mechanical contact experiments in STM are characterized in FIM at room temperature and at 158 K. The different activation energies for diffusion on the (111) and (110) tip planes and the experiment temperature are shown to be important factors controlling the extent of changes to the atomic structure of the tip. W(111) tips are much better suited to scanning probe studies which require the characterization of an atomically defined tip and subsequent verification of its integrity in FIM. The statistics of the observed spikes in the tunneling current when the tips are approached to Au(111) are interpreted using a simple model of adatoms diffusing through the STM junction., 11 pages, 13 figures

We use atomic force microscopy to measure electron addition spectra of individual Au nanoparticles that exhibit Coulomb blockade at room temperature. The cantilever tip charges individual nanoparticles supported on an ultra-thin NaCl film via single-electron tunneling from the metal back electrode. The tunneling is detected by measuring frequency shift and damping of the oscillating cantilever. Finite element electrostatic calculations indicate that the total nanoparticle capacitance is dominated by mutual capacitance to the back electrode.

a b s t r a c t Ultra-thin MgO films grown reactively on the Fe(0 0 1) surface by evaporation of magnesium in an atmo- sphere of molecular oxygen have been investigated by low energy electron diffraction and non-contact atomic force microscopy. Preparation of structurally stable crystalline films requires a protocol that pre- vents an excessive interfacial reaction between oxygen and the Fe(0 0 1) surface, but at the same time provides a sufficient amount of oxygen in order to grow a stoichiometric MgO film. The proper ratio between the magnesium deposition rate and the oxygen pressure has been determined, as well as meas- ures to prevent initial interfacial oxidation of the substrate. The effect of both post-annealing and an increased substrate temperature during the growth has been studied. We demonstrate that the reactive deposition method, which gives full control over the gaseous species that reach the surface, can produce terraces that have an average size of 10 nm (on an 8 monolayer thick film), which is a significant improve- ment compared to other preparation methods, such as thermal or electron beam evaporation of MgO.

CNS injury may lead to permanent functional deficits because it is still not possible to regenerate axons over long distances and accurately reconnect them with an appropriate target. Using rat neurons, microtools, and nanotools, we show that new, functional neurites can be created and precisely positioned to directly (re)wire neuronal networks. We show that an adhesive contact made onto an axon or dendrite can be pulled to initiate a new neurite that can be mechanically guided to form new synapses at up to 0.8 mm distance in SIGNIFICANCE STATEMENTBrain and spinal cord injury may lead to permanent disability and death because it is still not possible to regenerate neurons over long distances and accurately reconnect them with an appropriate target. Using microtools and nanotools we have developed a new method to rapidly initiate, elongate, and precisely connect new functional neuronal circuits over long distances. The extension rates achieved are ≥60 times faster than previously reported. Our findings have direct implications for the development of new therapies and surgical techniques to achieve functional regeneration after trauma and in neurodegenerative diseases. It also opens the door for the direct wiring of robust brain–machine interfaces as well as for investigations of fundamental aspects of neuronal signal processing and neuronal function.

A mechanically formed electrical nanocontact between gold and tungsten is a prototypical junction between metals with dissimilar electronic structure. Through atomically characterized nanoindentation experiments and first-principles quantum transport calculations, we find that the ballistic conduction across this intermetallic interface is drastically reduced because of the fundamental mismatch between s wave-like modes of electron conduction in the gold and d wave-like modes in the tungsten. The mechanical formation of the junction introduces defects and disorder, which act as an additional source of conduction losses and increase junction resistance by up to an order of magnitude. These findings apply to nanoelectronics and semiconductor device design. The technique that we use is very broadly applicable to molecular electronics, nanoscale contact mechanics, and scanning tunneling microscopy.

In this work, we explore Franck-Condon blockade in the "redox limit," where nuclear relaxation processes occur much faster than the rate of electron transfer. To this end, the quantized rate expressions for electron transfer are recast in terms of a quantized redox density of states (DOS) within a single phonon mode model. In the high temperature regime, this single-particle picture formulation of electron transfer is shown to agree well with the semi-classical rate and DOS expressions developed by Gerischer and Hopfield. Upon incorporation into a two electrode formulation, utilizing the master equation approach, the low temperature quantized conductance features of Franck-Condon blockade are reproduced. Moreover, at sufficiently large reorganization energies, it is argued that Franck-Condon blockade should also be observable in room temperature systems. In general, this work aims to further bridge descriptions of electron transfer and transport in the single-particle picture.

In this study we aim to create a scanning probe measurement device capable of studying the charging characteristics of battery materials. While Scanning Ion Conductance Microscopy (SICM) allows for local probing of conductance characteristics of materials, the poor spatial resolution of this technique limits its use to flat samples. By combining SICM with Atomic Force Microscopy we may overcome these issues and produce spatially resolved ionic conductance measurements in real time. This can be used to coordinate the charging characteristics of lithium iron phosphate battery materials with conformational changes which occur through charging events.

We report a new experimental technique for Kelvin probe force microscopy (KPFM) using the dissipation signal of frequency modulation atomic force microscopy for bias voltage feedback. It features a simple implementation and faster scanning as it requires no low frequency modulation. The dissipation is caused by the oscillating electrostatic force that is coherent with the tip oscillation, which is induced by a sinusoidally oscillating voltage applied between the tip and sample. We analyzed the effect of the phase of the oscillating force on the frequency shift and dissipation and found that the relative phase of 90$^\circ$ that causes only the dissipation is the most appropriate for KPFM measurements. The present technique requires a significantly smaller ac voltage amplitude by virtue of enhanced force detection due to the resonance enhancement and the use of fundamental flexural mode oscillation for electrostatic force detection. This feature will be of great importance in the electrical characterizations of technically relevant materials whose electrical properties are influenced by the externally applied electric field as is the case in semiconductor electronic devices., Comment: 6 pages, 4 figures

We present theoretical and experimental studies of the effect of the density of states of a quantum dot (QD) on the rate of single-electron tunneling that can be directly measured by electrostatic force microscopy (e-EFM) experiments. In e-EFM, the motion of a biased atomic force microscope cantilever tip modulates the charge state of a QD in the Coulomb blockade regime. The charge dynamics of the dot, which is detected through its back-action on the capacitavely coupled cantilever, depends on the tunneling rate of the QD to a back-electrode. The density of states of the QD can therefore be measured through its effect on the energy dependence of tunneling rate. We present experimental data on individual 5 nm colloidal gold nanoparticles that exhibit a near continuous density of state at 77 K. In contrast, our analysis of already published data on self-assembled InAs QDs at 4 K clearly reveals discrete degenerate energy levels.

A technique for highly reproducible deposition of nanoscale sized gold dots in an atomic force microscopy (AFM) configuration is described. This is achieved by precisely controlling the tip–sample separation, using feedback control enabled by the application of an external electrostatic servo force. Application of a voltage pulse of either polarity to a gold coated oscillating cantilever tip leads to the deposition of the Au dot. Dimensions for the fabricated dots are 6–100 nm in width, and

Bi 2 Te 3 and Sb 2 Te 3 semiconductors are layered crystals with rhombohedral structures, space group R 3 m ( ). The crystal lattice is formed by periodically ordered layers lying in the planes perpendicular to the C 3 symmetry axis. Each layer comprises five atomic planes (quintets) that form the sequence Te 1 ‐Bi‐Te 2 ‐ Bi‐Te 1 . Here, Te 1 and Te 2 are Te atoms in different sites. The atoms in separate layers are identical and form a planar hexagonal lattice. The atoms of each subsequent layer are situated above the centers of the triangles formed by the atoms of the preceding layer (close hexagonal packing); that is, the Te 1 and Bi atoms occupy octahedral sites in the tetradymite structure. The chemical bonds within the quintets are covalentionic. Between the quintets, the distance is comparatively long and bonds are van der Waals in nature and weak. This determines the anisotropy of the electrophysical properties of the single crystals [1].

A non-contact atomic force microscope (NC-AFM) based on a microfabricated piezoelectric cantilever is presented. A single piezoelectric lead zirconate titanate thin film layer on the cantilever serves as deflection sensing, cantilever oscillation and feedback actuation. Since such an AFM requires neither external oscillator nor external deflection sensor, considerably simple instrumentation becomes possible even for extreme environments such as low temperature or ultra-high vacuum. Also feedback control by the integrated actuator in the cantilever makes faster scanning possible. Images of atomic steps on annealed sapphire (0001) surfaces have been observed in air atmosphere in frequency modulation mode.

Atomic force microscopy (AFM) routinely achieves structural information in the sub-nm length scale. Measuring time resolved properties on this length scale to understand kinetics at the nm scale remains an elusive goal. We present a general analysis of the lower limit for time resolution in AFM. Our finding suggests that the time resolution in AFM is ultimately limited by the well-known thermal limit of AFM and not as often proposed by the mechanical response time of the force sensing cantilever. We demonstrate a general pump-probe approach using the cantilever as a detector responding to the averaged signal. This method can be applied to any excitation signal such as electrical, thermal, magnetic or optical. Experimental implementation of this method allows us to measure a photocarrier decay time of ∼1 ps in low temperature grown GaAs using a cantilever with a resonant frequency of 280 kHz.

Electric charge detection by atomic force microscopy (AFM) with single- electron resolution (e-EFM) is a promising way to investigate the electronic level structure of individual quantum dots (QD). The oscillating AFM tip modulates the energy of the QDs, causing single electrons to tunnel between QDs and an electrode. The resulting oscillating electrostatic force changes the resonant frequency and damping of the AFM cantilever, enabling electrometry with a single-electron sensitivity. Quantitative electronic level spectroscopy is possible by sweeping the bias voltage. Charge stability diagram can be obtained by scanning the AFM tip around the QD. e-EFM technique enables to investigate individual colloidal nanoparticles and self- assembled QDs without nanoscale electrodes. e-EFM is a quantum electromechanical system where the back-action of a tunneling electron is detected by AFM; it can also be considered as a mechanical analog of admittance spectroscopy with a radio frequency resonator, which is emerging as a promising tool for quantum state readout for quantum computing. In combination with the topography imaging capability of the AFM, e-EFM is a powerful tool for investigating new nanoscale material systems which can be used as quantum bits., 28 pages, 17 figures

Two coupled single wall carbon nanotube quantum dots in a multiple quantum dot system were characterized by using a low temperature scanning gate microscopy (SGM) technique, at a temperature of 170 mK. The locations of single wall carbon nanotube quantum dots were identified by taking the conductance images of a single wall carbon nanotube contacted by two metallic electrodes. The single electron transport through single wall carbon nanotube multiple quantum dots has been observed by varying either the position or voltage bias of a conductive atomic force microscopy tip. Clear hexagonal patterns were observed in the region of the conductance images where only two sets of overlapping conductance rings are visible. The values of coupling capacitance over the total capacitance of the two dots, C(m)/C(1(2)) have been extracted to be 0.21 ∼ 0.27 and 0.23 ∼ 0.28, respectively. In addition, the interdot coupling (conductance peak splitting) has also been confirmed in both conductance image measurement and current-voltage curves. The results show that a SGM technique enables spectroscopic investigation of coupled quantum dots even in the presence of unexpected multiple quantum dots.

The effect of doping with Hf atoms on the nearly commensurate (NC) charge-density-wave (CDW) structures of 1T-TaS2 was investigated using scanning tunnelling microscopy (STM) at room temperature, for levels of substitution of Hf for Ta up to 6.9%. It was found that the Hf atom introduces a point defect to the CDW superlattice at the CDW domain boundary for lower contents. For Hf contents higher than 1%, the CDW superlattice melted and a distorted structure was observed instead of the usual CDW superlattice. The change of the CDW structure observed by STM was compared with the change of the ρ-T characteristics.

Noncontact atomic force microscopy with frequency modulation detection is a promising technique for surface observation with true atomic resolution. The piezoelectric material itself can be an actuator and sensor of the oscillating probe simultaneously, without the need for additional electro-mechanical transducers or other measurement systems. A vertical resolution of 0.01 nm rms has been achieved using a microfabricated cantilever with lead zirconate titanate thin film in noncontact mode frequency modulation detection. The cantilever also has a sharpened pyramidal stylus with a radius of about 10 nm for noncontact atomic force microscopy.

We report on transient adhesion and conductance phenomena associated with tip wetting in mechanical contacts produced by the indentation of a clean W(111) tip into a Au(111) surface. A combination of atomic force microscopy and scanning tunneling microscopy was used to carry out indentation and to image residual impressions in ultra-high vacuum. The ~7 nm radii tips used in these experiments were prepared and characterized by field ion microscopy in the same instrument. The very first indentations of the tungsten tips show larger conductance and pull-off adhesive forces than subsequent indentations. After ~30 indentations to a depth of ~1.7 nm, the maximum conductance and adhesion forces reach steady-state values approximately 12x and 6x smaller than their initial value. Indentation of W(111) tips into Cu(100) was also performed to investigate the universality of tip wetting phenomena with a different substrate. We propose a model from contact mechanics considerations which quantitatively reproduces the observed decay rate of the conductance and adhesion drops with a 1/e decay constant of 9-14 indentation cycles. The results show that the surface composition of an indenting tip plays an important role in defining the mechanical and electrical properties of indentation contacts., 8 pages, 7 figures

The formation of the smallest permanent indentation in a Au(111) surface is studied by scanning tunneling microscopy and atomic force microscopy in ultrahigh vacuum. The 9.5 nm radius W(111) indenter was characterized in situ by field ion microscopy. Elastic and plastic indentations are identified both in the residual impression image and by features in their force-displacement curves such as the sink-in depth, pop-ins, and hysteresis energy. Plasticity is best identified quantitatively in the force-displacement curves by the sink-in depth. The minimum of plastic damage producible in the substrate is associated with an energy budget of ∼70 eV.

Focused ion beam (FIB) milling is a common fabrication technique to make nanostencil masks which has the unintended consequence of gallium ion implantation surrounding milled features in silicon nitride membranes. We observe major changes in film structure, chemical composition, and magnetic behaviour of permalloy nanostructures deposited by electron beam evaporation using silicon nitride stencil masks made by a FIB as compared to stencil masks made by regular lithography techniques. We characterize the stenciled structures and both types of masks using transmission electron microscopy, electron energy loss spectroscopy, energy dispersive x-ray spectroscopy, magnetic force microscopy and kelvin probe force microscopy. All these techniques demonstrate distinct differences at a length scale of a 1-100 nm for the structures made using stencil mask fabricated using a FIB. The origin of these differences seems to be related to the presence of implanted ions, a detailed understanding of the mechanism however remains to be developed. © 2013 IOP Publishing Ltd.

The cow energy gap structure of TISQ has been observed by tunnelling specvoscopy and itE temperature dependence obtained for 77 K 6 T 6 295 K. In addition to the energy gap associated wilh the cow with T, = 201 K, a nmwer gap svucture was observed to persist at higher temperature, which explains lhc negative temperature coefficient of the p-T curve above Tc .

Measuring the structure function relation in photovoltaic materials has been a major drive for atomic force microscopy (AFM) and Kelvin probe force microscopy (KPFM). The local surface photovoltage (SPV) is measured as the change in contact potential difference (CPD) between the tip and sample upon illumination. The quantities of interest that one will like to correlate with the structure are the decay times of SPV and/or its wavelength dependence. KPFM depends on the tip and sample potential; therefore SPV is prone to tip changes rendering an accurate measurement of SPV challenging. We present a measurement technique which allows us to directly measure the difference in the CPD between illuminated and dark states and thus SPV as well as the capacitance derivative by using pulsed illumination. The variation of the measured SPV can be minimized due to the time domain measurement allowing accurate measurements of the SPV. The increased accuracy enables the systematic comparison of SPV across different measurement setups and excitation conditions (e.g. wavelength dependence and decay time of SPV).

Ultra-thin NaCl films epitaxially grown on an Fe(001)-p(1 × 1)O surface have been investigated in ultra-high vacuum by non-contact atomic force microscopy and low energy electron diffraction. It has been found that at temperatures below 145 °C NaCl initially grows as monoatomic thick islands on substrate terraces, while at temperatures above 175 °C biatomic thick islands are also formed at substrate step edges. Both types of islands have the same Fe(001)-O[100] [parallel] NaCl(001)[110] orientation, leading to a (4 × 4) superstructure, where the NaCl unit cell is oriented at 45° with respect to the substrate. Interestingly, no c(2 × 2) superstructure with the NaCl unit cell oriented at 0° has been observed. The oxygen on the iron surface promotes layer-by-layer growth, resulting in atomically flat films with 40-60 nm wide terraces at coverages ranging from 0.75 to 12 ML. Such NaCl films are of much higher quality than MgO films grown on Fe(001) and Fe(001)-p(1 × 1)O surfaces and represent a unique epitaxial system of an alkali halide on a pure metallic substrate. The reduced number of defects and the layer-by-layer mode of growth make this system very attractive for applications where an atomically defined tunnel barrier is required to control the properties of a device.

It is well known that the low-Q regime in dynamic atomic force microscopy is afflicted by instrumental artifacts (known as "the forest of peaks") caused by piezoacoustic excitation of the cantilever. In this article, we unveil additional issues associated with piezoacoustic excitation that become apparent and problematic at low Q values. We present the design of a photothermal excitation system that resolves these issues, and demonstrate its performance on force spectroscopy at the interface of gold and an ionic liquid with an overdamped cantilever (Q < 0.5). Finally, challenges in the interpretation of low-Q dynamic AFM measurements are discussed.

Having reached the quantum and thermodynamic limits of detection, atomic force microscopy (AFM) experiments are routinely being performed at the fundamental limit of signal to noise. A critical understanding of the statistical properties of noise leads to more accurate interpretation of data, optimization of experimental protocols, advancements in instrumentation, and new measurement techniques. Furthermore, accurate simulation of cantilever dynamics requires knowledge of stochastic behavior of the system, as stochastic noise may exceed the deterministic signals of interest, and even dominate the outcome of an experiment. In this article, the power spectral density (PSD), used to quantify stationary stochastic processes, is introduced in the context of a thorough noise analysis of the light source used to detect cantilever deflections. The statistical properties of PSDs are then outlined for various stationary, nonstationary, and deterministic noise sources in the context of AFM experiments. Following these developments, a method for integrating PSDs to provide an accurate standard deviation of linear measurements is described. Lastly, a method for simulating stochastic Gaussian noise from any arbitrary power spectral density is presented. The result demonstrates that mechanical vibrations of the AFM can cause a logarithmic velocity dependence of friction and induce multiple slip events in the atomic stick-slip process, as well as predicts an artifactual temperature dependence of friction measured by AFM.

We present a new charge sensing technique for the excited-state spectroscopy of individual quantum dots, which requires no patterned electrodes. An oscillating atomic force microscope cantilever is used as a movable charge sensor as well as gate to measure the single-electron tunneling between an individual self-assembled InAs quantum dot and back electrode. A set of cantilever dissipation versus bias voltage curves measured at different cantilever oscillation amplitudes forms a diagram analogous to the Coulomb diamond usually measured with transport measurements. The excited-state levels as well as the electron addition spectrum can be obtained from the diagram. In addition, a signature which can result from inelastic tunneling by phonon emission or a peak in the density of states of the electrode is also observed, which demonstrates the versatility of the technique.

A modification of the common electrochemical etching setup is presented. The described method reproducibly yields sharp tungsten tips for usage in the scanning tunneling microscope and tuning fork atomic force microscope. In situ treatment under ultrahigh vacuum (p ≤10(-10) mbar) conditions for cleaning and fine sharpening with minimal blunting is described. The structure of the microscopic apex of these tips is atomically resolved with field ion microscopy and cross checked with field emission.

The deposition of gold ions from atomic force microscope cantilever tips onto bulk insulating substrates with nearby surface electrodes is discussed. Numerical models of the potential distribution are used to estimate potential barriers for the desorption process. These models indicate deposition height thresholds of 7–10 nm with the tip 20–25 nm from the metallic electrode edge over a KBr surface but greater than 20 nm high for InP/GaAs/InP substrates with a two-dimensional electron gas (2DEG) as the back electrode. Experimental results for the deposition of gold clusters over KBr surfaces near metal electrodes in ultra-high vacuum (UHV) are presented and show promising agreement with calculations of the deposition threshold heights. Deposition of clusters over InP is discussed for comparison and indicates similar trends.

The electrostatic potential profile is of great importance in nanoscale electronic devices. The effect of the random potential caused by dopants or other defects becomes an increasingly more important problem as device size continues to shrink and as devices exploiting quantum effects emerge. We review the past studies on the potential profile in semiconductor heterostructures by Kelvin probe force microscopy (KPFM) and electrostatic force microscopy (EFM), focusing on the technical aspects of the experiments. We then describe measurements of the spatial and temporal fluctuations of the electrostatic potential in an InP/InGaAs heterostructure sample by EFM and KPFM using frequency modulation mode atomic force microscopy (AFM). We also describe a new EFM technique capable of detecting charge with single-electron resolution and show that such techniques can be used for quantitative spectroscopic measurements of discrete electronic states such as those in quantum dots. Finally, we compare EFM and KPFM with two non-AFM-based scanning probe techniques with highly sensitive potentiometry and electrometry capability.