The growth mode of small Ni clusters evaporated in UHV on HOPG has been investigated by scanning tunnelling microscopy. The size, the size distribution, and the shape of the clusters have been evaluated for different evaporation conditions and annealing temperatures. The total coverage of the surface strongly depends on the evaporation rate and time, whereas the influence of these parameters is low on the cluster size. Subsequent stepwise annealing has been performed. This results in a reduction of the total amount of the Ni clusters accompanied by a decreasing in the overall coverage of the surface. The diameter of the clusters appears to be less influenced by the annealing than is their height. Besides this, the cluster shape is strongly influenced, changing to a quasi-hexagonal geometry after the first annealing step, indicating single-crystal formation. Finally, a reproducible methodology for picking up individual clusters is reported .
clusters; growth mode; Ni; nickel
One of the key goals in atomic force microscopy (AFM) imaging is to enhance material property contrast with high resolution. Bimodal AFM, where two eigenmodes are simultaneously excited, confers significant advantages over conventional single-frequency tapping mode AFM due to its ability to provide contrast between regions with different material properties under gentle imaging conditions. Bimodal AFM traditionally uses the first two eigenmodes of the AFM cantilever. In this work, the authors explore the use of higher eigenmodes in bimodal AFM (e.g., exciting the first and fourth eigenmodes). It is found that such operation leads to interesting contrast reversals compared to traditional bimodal AFM. A series of experiments and numerical simulations shows that the primary cause of the contrast reversals is not the choice of eigenmode itself (e.g., second versus fourth), but rather the relative kinetic energy between the higher eigenmode and the first eigenmode. This leads to the identification of three distinct imaging regimes in bimodal AFM. This result, which is applicable even to traditional bimodal AFM, should allow researchers to choose cantilever and operating parameters in a more rational manner in order to optimize resolution and contrast during nanoscale imaging of materials.
atomic force microscopy; bimodal AFM; cantilever eigenmodes; polymer characterization
We propose a geometry for a piezoelectric SPM sensor that can be used for combined AFM/LFM/STM. The sensor utilises symmetry to provide a lateral mode without the need to excite torsional modes. The symmetry allows normal and lateral motion to be completely isolated, even when introducing large tips to tune the dynamic properties to optimal values.
atomic force microscopy; lateral force microscopy; lateral forces; mechanical vibrations; scanning probe microscopy; scanning tunnelling microscopy
We present polynomial force reconstruction from experimental intermodulation atomic force microscopy (ImAFM) data. We study the tip–surface force during a slow surface approach and compare the results with amplitude-dependence force spectroscopy (ADFS). Based on polynomial force reconstruction we generate high-resolution surface-property maps of polymer blend samples. The polynomial method is described as a special example of a more general approximative force reconstruction, where the aim is to determine model parameters that best approximate the measured force spectrum. This approximative approach is not limited to spectral data, and we demonstrate how it can be adapted to a force quadrature picture.
AFM; atomic force microscopy; force spectroscopy; multifrequency; intermodulation; polynomial
Atomic force microscopes have become indispensable tools for mechanical characterization of nanoscale and submicron structures. However, materials with complex geometries, such as electrospun fiber networks used for tissue scaffolds, still pose challenges due to the influence of tension and bending modulus on the response of the suspended structures. Here we report mechanical measurements on electrospun silk fibers with various treatments that allow discriminating among the different mechanisms that determine the mechanical behavior of these complex structures. In particular we were able to identify the role of tension and boundary conditions (pinned versus clamped) in determining the mechanical response of electrospun silk fibers. Our findings show that high-resolution mechanical imaging with torsional harmonic atomic force microscopy provides a reliable method to investigate the mechanics of materials with complex geometries.
atomic force microscopy; nanomechanical characterization; silk fibers; tissue scaffolds; torsional harmonic cantilevers
We critically discuss the extraction of intrinsic cantilever properties, namely eigenfrequency f
n, quality factor Q
n and specifically the stiffness k
n of the nth cantilever oscillation mode from thermal noise by an analysis of the power spectral density of displacement fluctuations of the cantilever in contact with a thermal bath. The practical applicability of this approach is demonstrated for several cantilevers with eigenfrequencies ranging from 50 kHz to 2 MHz. As such an analysis requires a sophisticated spectral analysis, we introduce a new method to determine k
n from a spectral analysis of the demodulated oscillation signal of the excited cantilever that can be performed in the frequency range of 10 Hz to 1 kHz regardless of the eigenfrequency of the cantilever. We demonstrate that the latter method is in particular useful for noncontact atomic force microscopy (NC-AFM) where the required simple instrumentation for spectral analysis is available in most experimental systems.
AFM; cantilever; noncontact atomic force microscopy (NC-AFM); Q-factor; thermal excitation; resonance; spectral analysis; stiffness
This study investigates the controlled chemical functionalization of silicon oxide nanostructures prepared by AFM-anodization lithography of alkyl-terminated silicon. Different conditions for the growth of covalently bound mono-, multi- or submonolayers of distinctively functional silane molecules on nanostructures have been identified by AFM-height investigations. Routes for the preparation of methyl- or amino-terminated structures or silicon surfaces are presented and discussed. The formation of silane monolayers on nanoscopic silicon oxide nanostructures was found to be much more sensitive towards ambient humidity than, e.g., the silanization of larger OH-terminated silica surfaces. Amino-functionalized nanostructures have been successfully modified by the covalent binding of functional fluorescein dye molecules. Upon excitation, the dye-functionalized structures show only weak fluorescence, which may be an indication of a relatively low surface coverage of the dye molecules on length scale that is not accessible by standard AFM measurements.
AFM lithography; amino-functionalization; local anodic oxidation; octadecyl-trichlorosilane; silicon oxide nanostructures
The recent achievement of atomic resolution with dynamic atomic force microscopy (dAFM) [Fukuma et al., Appl. Phys. Lett.
2005, 87, 034101], where quality factors of the oscillating probe are inherently low, challenges some accepted beliefs concerning sensitivity and resolution in dAFM imaging modes. Through analysis and experiment we study the performance metrics for high-resolution imaging with dAFM in liquid media with amplitude modulation (AM), frequency modulation (FM) and drive-amplitude modulation (DAM) imaging modes. We find that while the quality factors of dAFM probes may deviate by several orders of magnitude between vacuum and liquid media, their sensitivity to tip–sample forces can be remarkable similar. Furthermore, the reduction in noncontact forces and quality factors in liquids diminishes the role of feedback control in achieving high-resolution images. The theoretical findings are supported by atomic-resolution images of mica in water acquired with AM, FM and DAM under similar operating conditions.
atomic force microscopy; dAFM; high-resolution; liquids
We introduce a novel and potentially powerful, yet relatively simple extension of the spectral inversion method, which offers the possibility of carrying out 4-dimensional (4D) atomic force spectroscopy. With the extended spectral inversion method it is theoretically possible to measure the tip–sample forces as a function of the three Cartesian coordinates in the scanning volume (x, y and z) and the vertical velocity of the tip, through a single 2-dimensional (2D) surface scan. Although signal-to-noise ratio limitations can currently prevent the accurate experimental implementation of the 4D method, and the extraction of rate-dependent material properties from the force maps is a formidable challenge, the spectral inversion method is a promising approach due to its dynamic nature, robustness, relative simplicity and previous successes.
atomic force microscopy; spectral inversion; spectroscopy; torsional harmonic cantilever; viscoelasticity
The noise of the frequency-shift signal Δf in noncontact atomic force microscopy (NC-AFM) consists of cantilever thermal noise, tip–surface-interaction noise and instrumental noise from the detection and signal processing systems. We investigate how the displacement-noise spectral density d
z at the input of the frequency demodulator propagates to the frequency-shift-noise spectral density d
f at the demodulator output in dependence of cantilever properties and settings of the signal processing electronics in the limit of a negligible tip–surface interaction and a measurement under ultrahigh-vacuum conditions. For a quantification of the noise figures, we calibrate the cantilever displacement signal and determine the transfer function of the signal-processing electronics. From the transfer function and the measured d
z, we predict d
f for specific filter settings, a given level of detection-system noise spectral density d
ds and the cantilever-thermal-noise spectral density d
th. We find an excellent agreement between the calculated and measured values for d
f. Furthermore, we demonstrate that thermal noise in d
f, defining the ultimate limit in NC-AFM signal detection, can be kept low by a proper choice of the cantilever whereby its Q-factor should be given most attention. A system with a low-noise signal detection and a suitable cantilever, operated with appropriate filter and feedback-loop settings allows room temperature NC-AFM measurements at a low thermal-noise limit with a significant bandwidth.
Cantilever; feedback loop; filter; noncontact atomic force microscopy (NC-AFM); noise
In qPlus atomic force microscopy the tip length can in principle approach the length of the cantilever. We present a detailed mathematical model of the effects this has on the dynamic properties of the qPlus sensor. The resulting, experimentally confirmed motion of the tip apex is shown to have a large lateral component, raising interesting questions for both calibration and force-spectroscopy measurements.
atomic force microscopy; force spectroscopy; lateral forces; mechanical vibrations; qPlus
In this paper we present a comparison of three different methods that can be used for estimating the stiffness of qPlus sensors. The first method is based on continuum theory of elasticity. The second (Cleveland’s method) uses the change in the eigenfrequency that is induced by the loading of small masses. Finally, the stiffness is obtained by analysis of the thermal noise spectrum. We show that all three methods give very similar results. Surprisingly, neither the gold wire nor the gluing give rise to significant changes of the stiffness in the case of our home-built sensors. Furthermore we describe a fast and cost-effective way to perform Cleveland’s method. This method is based on gluing small pieces of a tungsten wire; the mass is obtained from the volume of the wire, which is measured by optical microscopy. To facilitate detection of oscillation eigenfrequencies under ambient conditions, we designed and built a device for testing qPlus sensors.
AFM; Cleveland’s method; cross talk; force; qPlus; stiffness; STM; thermal noise; tuning fork
We recently introduced a method that allows the controlled deposition of nanoscale metallic patterns at defined locations using the tip of an atomic force microscope (AFM) as a “mechano-electrochemical pen”, locally activating a passivated substrate surface for site-selective electrochemical deposition. Here, we demonstrate the reversibility of this process and study the long-term stability of the resulting metallic structures. The remarkable stability for more than 1.5 years under ambient air without any observable changes can be attributed to self-passivation. After AFM-activated electrochemical deposition of copper nanostructures on a polycrystalline gold film and subsequent AFM imaging, the copper nanostructures could be dissolved by reversing the electrochemical potential. Subsequent AFM-tip-activated deposition of different copper nanostructures at the same location where the previous structures were deleted, shows that there is no observable memory effect, i.e., no effect of the previous writing process on the subsequent writing process. Thus, the four processes required for reversible information storage, “write”, “read”, “delete” and “re-write”, were successfully demonstrated on the nanometer scale.
atomic force microscopy; electrochemical deposition; electrochemistry; nanoelectronics; nanofabrication; nanolithography; nanotechnology; MEMS and NEMS; reversible processes; scanning probe microscopy and lithography
A double-lateral-gate p-type junctionless transistor is fabricated on a low-doped (1015) silicon-on-insulator wafer by a lithography technique based on scanning probe microscopy and two steps of wet chemical etching. The experimental transfer characteristics are obtained and compared with the numerical characteristics of the device. The simulation results are used to investigate the pinch-off mechanism, from the flat band to the off state. The study is based on the variation of the carrier density and the electric-field components. The device is a pinch-off transistor, which is normally in the on state and is driven into the off state by the application of a positive gate voltage. We demonstrate that the depletion starts from the bottom corner of the channel facing the gates and expands toward the center and top of the channel. Redistribution of the carriers due to the electric field emanating from the gates creates an electric field perpendicular to the current, toward the bottom of the channel, which provides the electrostatic squeezing of the current.
AFM nanolithography; junctionless transistors; pinch-off; scanning probe microscope; simulation
We present an overview of experimental and numerical methods to determine the spring constant of a quartz tuning fork in qPlus configuration. The simple calculation for a rectangular cantilever is compared to the values obtained by the analysis of the thermal excitation and by the direct mechanical measurement of the force versus displacement. To elucidate the difference, numerical simulations were performed taking account of the real geometry including the glue that is used to mount the tuning fork.
atomic force microscopy; finite element method; spring constant; thermal fluctuation; tuning fork
Scanning- and colloidal-probe atomic force microscopy were used to study the mechanical properties of poly(L-lysine)/hyaluronan (PLL/HA)n films as a function of indentation velocity and the number of polymer deposition steps n. The film thickness was determined by two independent AFM-based methods: scratch-and-scan and newly developed full-indentation. The advantages and disadvantages of both methods are highlighted, and error minimization techniques in elasticity measurements are addressed. It was found that the film thickness increases linearly with the bilayer number n, ranging between 400 and 7500 nm for n = 12 and 96, respectively. The apparent Young’s modulus E ranges between 15 and 40 kPa and does not depend on the indenter size or the film bilayer number n. Stress relaxation measurements show that PLL/HA films have a viscoelastic behaviour, regardless of their thickness. If indentation is performed several times at the same lateral position on the film, a viscous/plastic deformation takes place.
atomic force microscopy; polyelectrolyte multilayers; stress relaxation; viscoelasticity; Young’s modulus
Modern high-speed atomic force microscopes generate significant quantities of data in a short amount of time. Each image in the sequence has to be processed quickly and accurately in order to obtain a true representation of the sample and its changes over time. This paper presents an automated, adaptive algorithm for the required processing of AFM images. The algorithm adaptively corrects for both common one-dimensional distortions as well as the most common two-dimensional distortions. This method uses an iterative thresholded processing algorithm for rapid and accurate separation of background and surface topography. This separation prevents artificial bias from topographic features and ensures the best possible coherence between the different images in a sequence. This method is equally applicable to all channels of AFM data, and can process images in seconds.
adaptive algorithm; artifact correction; atomic force microscopy; high-speed atomic force microscope; image processing
We report on the use of scanning force microscopy as a versatile tool for the electrical characterization of nanoscale memristors fabricated on ultrathin La0.7Sr0.3MnO3 (LSMO) films. Combining conventional conductive imaging and nanoscale lithography, reversible switching between low-resistive (ON) and high-resistive (OFF) states was locally achieved by applying voltages within the range of a few volts. Retention times of several months were tested for both ON and OFF states. Spectroscopy modes were used to investigate the I–V characteristics of the different resistive states. This permitted the correlation of device rectification (reset) with the voltage employed to induce each particular state. Analytical simulations by using a nonlinear dopant drift within a memristor device explain the experimental I–V bipolar cycles.
conductive scanning probe micoscopy; memristor; 3-D modes; resistive switching; scanning probe microscopy
Background: Characterization at the atomic scale is becoming an achievable task for FM-AFM users equipped, for example, with a qPlus sensor. Nevertheless, calculations are necessary to fully interpret experimental images in some specific cases. In this context, we developed a numerical AFM (n-AFM) able to be used in different modes and under different usage conditions.
Results: Here, we tackled FM-AFM image calculations of three types of graphitic structures, namely a graphite surface, a graphene sheet on a silicon carbide substrate with a Si-terminated surface, and finally, a graphene nanoribbon. We compared static structures, meaning that all the tip and sample atoms are kept frozen in their equilibrium position, with dynamic systems, obtained with a molecular dynamics module allowing all the atoms to move freely during the probe oscillations.
Conclusion: We found a very good agreement with experimental graphite and graphene images. The imaging process for the deposited nanoribbon demonstrates the stability of our n-AFM to image a non-perfectly planar substrate exhibiting a geometrical step as well as a material step.
calculations; FM-AFM; graphene; graphite; image; nanoribbon
This work introduces the concept of time–frequency map of the phase difference between the cantilever response signal and the driving signal, calculated with a wavelet cross-correlation technique. The wavelet cross-correlation quantifies the common power and the relative phase between the response of the cantilever and the exciting driver, yielding “instantaneous” information on the driver-response phase delay as a function of frequency. These concepts are introduced through the calculation of the response of a free cantilever subjected to continuous and impulsive excitation over a frequency band.
AFM; band excitation; force; wavelet transforms
We investigated the adsorption of 4-methoxy-4′-(3-sulfonatopropyl)stilbazolium (MSPS) on different ionic (001) crystal surfaces by means of noncontact atomic force microscopy. MSPS is a zwitterionic molecule with a strong electric dipole moment. When deposited onto the substrates at room temperature, MSPS diffuses to step edges and defect sites and forms disordered assemblies of molecules. Subsequent annealing induces two different processes: First, at high coverage, the molecules assemble into a well-organized quadratic lattice, which is perfectly aligned with the <110> directions of the substrate surface (i.e., rows of equal charges) and which produces a Moiré pattern due to coincidences with the substrate lattice constant. Second, at low coverage, we observe step edges decorated with MSPS molecules that run along the <110> direction. These polar steps most probably minimize the surface energy as they counterbalance the molecular dipole by presenting oppositely charged ions on the rearranged step edge.
alkali halide surface; noncontact atomic force microscopy; organic molecule; self-organization; zwitterion
We present the results of simultaneous scanning-tunneling and frequency-modulated dynamic atomic force microscopy measurements with a qPlus setup. The qPlus sensor is a purely electrical sensor based on a quartz tuning fork. If both the tunneling current and the force signal are to be measured at the tip, a cross-talk of the tunneling current with the force signal can easily occur. The origin and general features of the capacitive cross-talk will be discussed in detail in this contribution. Furthermore, we describe an experimental setup that improves the level of decoupling between the tunneling-current and the deflection signal. The efficiency of this experimental setup is demonstrated through topography and site-specific force/tunneling-spectroscopy measurements on the Si(111) 7×7 surface. The results show an excellent agreement with previously reported data measured by optical interferometric deflection.
AFM; cross-talk; current; dissipation; force; qPlus; STM; tuning fork
In frequency-modulation atomic force microscopy the direct observable is the frequency shift of an oscillating cantilever in a force field. This frequency shift is not a direct measure of the actual force, and thus, to obtain the force, deconvolution methods are necessary. Two prominent methods proposed by Sader and Jarvis (Sader–Jarvis method) and Giessibl (matrix method) are investigated with respect to the deconvolution quality. Both methods show a nontrivial dependence of the deconvolution quality on the oscillation amplitude. The matrix method exhibits spikelike features originating from a numerical artifact. By interpolation of the data, the spikelike features can be circumvented. The Sader–Jarvis method has a continuous amplitude dependence showing two minima and one maximum, which is an inherent property of the deconvolution algorithm. The optimal deconvolution depends on the ratio of the amplitude and the characteristic decay length of the force for the Sader–Jarvis method. However, the matrix method generally provides the higher deconvolution quality.
frequency-modulation atomic force microscopy; force deconvolution; numerical implementation
Measurements of the frequency shift versus distance in noncontact atomic force microscopy (NC-AFM) allow measurements of the force gradient between the oscillating tip and a surface (force-spectroscopy measurements). When nonconservative forces act between the tip apex and the surface the oscillation amplitude is damped. The dissipation is caused by bistabilities in the potential energy surface of the tip–sample system, and the process can be understood as a hysteresis of forces between approach and retraction of the tip. In this paper, we present the direct measurement of the whole hysteresis loop in force-spectroscopy curves at 77 K on the PTCDA/Ag/Si(111) √3 × √3 surface by means of a tuning-fork-based NC-AFM with an oscillation amplitude smaller than the distance range of the hysteresis loop. The hysteresis effect is caused by the making and breaking of a bond between PTCDA molecules on the surface and a PTCDA molecule at the tip. The corresponding energy loss was determined to be 0.57 eV by evaluation of the force–distance curves upon approach and retraction. Furthermore, a second dissipation process was identified through the damping of the oscillation while the molecule on the tip is in contact with the surface. This dissipation process occurs mainly during the retraction of the tip. It reaches a maximum value of about 0.22 eV/cycle.
atomic force microscopy; energy dissipation; force spectroscopy; hysteresis loop; PTCDA/Ag/Si(111) √3 × √3
Bimodal atomic force microscopy is a force-microscopy method that requires the simultaneous excitation of two eigenmodes of the cantilever. This method enables the simultaneous recording of several material properties and, at the same time, it also increases the sensitivity of the microscope. Here we apply fractional calculus to express the frequency shift of the second eigenmode in terms of the fractional derivative of the interaction force. We show that this approximation is valid for situations in which the amplitude of the first mode is larger than the length of scale of the force, corresponding to the most common experimental case. We also show that this approximation is valid for very different types of tip–surface forces such as the Lennard-Jones and Derjaguin–Muller–Toporov forces.
AFM; atomic force microscopy; bimodal AFM; frequency shift; integral calculus applications