Atomic Force Microscopy Signal Research Articles

Machine learning-aided atomic structure identification of interfacial ionic hydrates from AFM images.

Relevant to broad applied fields and natural processes, interfacial ionic hydrates have been widely studied by using ultrahigh-resolution atomic force microscopy (AFM). However, the complex relationship between the AFM signal and the investigated system makes it difficult to determine the atomic structure of such a complex system from AFM images alone. Using machine learning, we achieved precise identification of the atomic structures of interfacial water/ionic hydrates based on AFM images, including the position of each atom and the orientations of water molecules. Furthermore, it was found that structure prediction of ionic hydrates can be achieved cost-effectively by transfer learning using neural network trained with easily available interfacial water data. Thus, this work provides an efficient and economical methodology that not only opens up avenues to determine atomic structures of more complex systems from AFM images, but may also help to interpret other scientific studies involving sophisticated experimental results.

Local electronic transport across probe/ionic conductor interface in scanning probe microscopy

Charge carrier transport through the probe-sample junction can have substantial consequences for outcomes of electrical and electromechanical atomic-force-microscopy (AFM) measurements. For understanding physical processes under the probe, we carried out conductive-AFM (C-AFM) measurements of local current-voltage (I-V) curves as well as their derivatives on samples of a mixed ionic-electronic conductor Li1-xMn2O4 and developed an analytical framework for the data analysis. The implemented approach discriminates between contributions the highly resistive sample surface layer and the bulk with the account of ion redistribution in the field of the probe. It was found that, with increasing probe voltage, the conductance mechanism in the surface layer transforms from Pool-Frenkel to space-charge-limited current. The surface layer significantly alters the ion dynamics in the sample bulk under the probe, which leads, in particular, to a decrease of the effective electromechanical AFM signal associated with the ionic motion in the sample. The framework can be applied for the analysis of electronic transport mechanisms across the probe/sample interface as well as to uncover the role of the charge transport in the electric field distribution, mechanical, and other responses in AFM measurements of a broad spectrum of conducting materials.

Optimization of acoustic coupling for bottom actuated scattering based subsurface scanning probe microscopy.

The characterization of buried nanoscale structures nondestructively is an important challenge in a number of applications, such as defect detection and metrology in the semiconductor industry. A promising technique is Subsurface Scanning Probe Microscopy (SSPM), which combines ultrasound with Atomic Force Microscopy (AFM). Initially, SSPM was used to measure the viscoelastic contrast between a subsurface feature and its surrounding medium. However, by increasing the ultrasonic frequency to >1 GHz, it has been shown that SSPM can also measure acoustic impedance based contrasts. At these frequencies, it becomes difficult to reliably couple the sound into the sample such that the AFM is able to pick up the scattered sound field. The cause is the existence of strong acoustic resonances in the sample, the transducer, and the coupling layer-the liquid layer used to couple the sound energy from the transducer into the sample-in combination with the nonlinearity of the tip-sample interaction. Thus, it is essential to control and measure the thickness of the coupling layer with nanometer accuracy. Here, we present the design of a mechanical clamp to ensure a stable acoustic coupling. Moreover, an acoustic method is presented to measure the coupling layer thickness in real-time. Stable coupling layers with thicknesses of 700 ± 2 nm were achieved over periods of 2-4 h. Measurements of the downmixed AFM signals showed stable signal intensities for >1 h. The clamp and monitoring method introduced here makes scattering based SSPM practical, robust, and reliable and enables measurement periods of hours.

Atomic-scale design of friction and energy dissipation

Study of friction and energy dissipation always relied on direct observations. Actual theories provide limited prediction on the frictional and dissipative properties if only the material chemistry and geometry are known. We here develop a framework to study intrinsic friction and energy dissipation based on the only knowledge of the normal modes of the system at equilibrium. We derive an approximated expression for the first anharmonic term in the potential energy expansion which does not require the computation of the third-order force constants. Moreover, we show how to characterize the frequency content of observed physical quantities and individuate the dissipative processes active during experimental measurements. As a case study, we consider the relative sliding motion of atomic layers in molybdenum disulfide dry lubricant, and we discuss how to extract information on the energetics of sliding from atomic force microscopy signals. The presented framework switches the investigation paradigm on friction and energy dissipation from dynamic to static studies, paving avenues to explore for the design of alternative anisotropic tribological and thermal materials.

A Wavelet Packet Tree Denoising Algorithm for Images of Atomic‐Force Microscopy

AbstractA threshold‐free denoising procedure of acquired discrete Atomic‐force microscopy (AFM) signals using the discrete wavelet transform (DWT) method is presented in this article. The integration of a denoising procedure into a control structure is extremely important for each kind of system to be controlled. The detection of unavoidable measurement noise in the acquired data of the AFM signal is done by using orthogonal wavelets (Daubechies and Symmlet) and with different polynomial approximation order for each family. The proposed denoising algorithm, based on the free wavelet toolboxes from the WaveLab 850 library of the Stanford University (USA), compares the usefulness of Daubechies and Symmlet wavelets with different vanishing moments. With the help of a seminorm the noise of a sequence is defined as a coherent and incoherent part of the AFM signal. In the first step of the procedure the algorithm analyzes the frequency subspaces of the wavelet packets tree and searches for small or opposing components in the wavelet domains. In the second step of the procedure the incoherent components in the low‐ and high frequency domains are localized and the incoherent is then removed from the AFM signal. The proposed algorithm structure is used to improve the quality of the AFM signals and it can be easily integrated into the existing AFM control hard‐ and software structures. The effectiveness of the proposed denoising algorithm is validated with real measurements.

Electroviscous Dissipation in Aqueous Electrolyte Films with Overlapping Electric Double Layers.

We use dynamic atomic force microscopy (AFM) to investigate the forces involved in squeezing out thin films of aqueous electrolyte between an AFM tip and silica substrates at variable pH and salt concentration. From amplitude and phase of the AFM signal we determine both conservative and dissipative components of the tip sample interaction forces. The measured dissipation is enhanced by up to a factor of 5 at tip–sample separations of ≈ one Debye length compared to the expectations based on classical hydrodynamic Reynolds damping with bulk viscosity. Calculating the surface charge density from the conservative forces using Derjaguin–Landau–Verwey–Overbeek (DLVO) theory in combination with a charge regulation boundary condition we find that the viscosity enhancement correlates with increasing surface charge density. We compare the observed viscosity enhancement with two competing continuum theory models: (i) electroviscous dissipation due to the electrophoretic flow driven by the streaming current that is generated upon squeezing out the counterions in the diffuse part of the electric double layer, and (ii) visco-electric enhancement of the local water viscosity caused by the strong electric fields within the electric double layer. While the visco-electric model correctly captures the qualitative trends observed in the experiments, a quantitative description of the data presumably requires more sophisticated simulations that include microscopic aspects of the distribution and mobility of ions in the Stern layer.

Hall effect in charged conducting ferroelectric domain walls.

Enhanced conductivity at specific domain walls in ferroelectrics is now an established phenomenon. Surprisingly, however, little is known about the most fundamental aspects of conduction. Carrier types, densities and mobilities have not been determined and transport mechanisms are still a matter of guesswork. Here we demonstrate that intermittent-contact atomic force microscopy (AFM) can detect the Hall effect in conducting domain walls. Studying YbMnO3 single crystals, we have confirmed that p-type conduction occurs in tail-to-tail charged domain walls. By calibration of the AFM signal, an upper estimate of ∼1 × 1016 cm−3 is calculated for the mobile carrier density in the wall, around four orders of magnitude below that required for complete screening of the polar discontinuity. A carrier mobility of∼50 cm2V−1s−1 is calculated, about an order of magnitude below equivalent carrier mobilities in p-type silicon, but sufficiently high to preclude carrier-lattice coupling associated with small polarons.

Characterization of a surface reaction by means of atomic force microscopy.

We study a thermally activated on-surface planarization reaction by a detailed analysis of the reactant and reaction products from atomically resolved atomic force microscopy (AFM) images and spectroscopy. The three-dimensional (3D) structure of the reactant, a helical diphenanthrene derivative, requires going beyond constant-height imaging. The characterization in three dimensions is enabled by acquisition and analysis of the AFM signal in a 3D data set. This way, the structure and geometry of nonplanar molecules as well as their reaction products on terraces and at step edges can be determined.

Surface structure. Subatomic resolution force microscopy reveals internal structure and adsorption sites of small iron clusters.

Clusters built from individual iron atoms adsorbed on surfaces (adatoms) were investigated by atomic force microscopy (AFM) with subatomic resolution. Single copper and iron adatoms appeared as toroidal structures and multiatom clusters as connected structures, showing each individual atom as a torus. For single adatoms, the toroidal shape of the AFM image depends on the bonding symmetry of the adatom to the underlying structure [twofold for copper on copper(110) and threefold for iron on copper(111)]. Density functional theory calculations support the experimental data. The findings correct our previous work, in which multiple minima in the AFM signal were interpreted as a reflection of the orientation of a single front atom, and suggest that dual and triple minima in the force signal are caused by dimer and trimer tips, respectively.

Single-cycle-PLL detection for real-time FM-AFM applications.

In this paper we present a novel architecture for phase-locked loop (PLL) based high-speed demodulation of frequency-modulated (FM) atomic force microscopy (AFM) signals. In our approach, we use single-sideband (SSB) frequency upconversion to translate the AFM signal from the position sensitive detector to a fixed intermediate frequency (IF) of 10 MHz. In this way, we fully benefit from the excellent noise performance of PLL-based FM demodulators still avoiding the intrinsic bandwidth limitation of such systems. In addition, the upconversion to a fixed IF renders the PLL demodulator independent of the cantilever's resonance frequency, allowing the system to work with a large range of cantilever frequencies. To investigate if the additional noise introduced by the SSB upconverter degrades the system noise figure we present a model of the AM-to-FM noise conversion in PLLs incorporating a phase-frequency detector. Using this model, we can predict an upper corner frequency for the demodulation bandwidth above which the converted noise from the single-sideband upconverter becomes the dominant noise source and therefore begins to deteriorate the overall system performance. The approach is validated by both electrical and AFM measurements obtained with a PCB-based prototype implementing the proposed demodulator architecture.

QPlus: atomic force microscopy on single-crystal insulators with small oscillationamplitudes at 5 K

Based on a proven low temperature scanning tunneling microscope (STM) platform, wehave integrated a QPlus sensor, which employs a quartz tuning fork for force detection innon-contact atomic force microscopy (AFM). For combined STM operation, this sensor haskey advantages over conventional sensors. For quantitative force spectroscopy oninsulating thin films or semiconductors, decoupling of the tunneling current and thepiezo-electrically induced AFM signal is important. In addition, extremely low signalsrequire the first amplification stage to be very close to the sensor, i.e. to be compatiblewith low temperatures. We present atomic resolution imaging on single-crystalNaCl(100) with oscillation amplitudes below 100 pm (peak-to-peak) and operation athigher flexural modes in constant frequency shift (df) imaging feedback. We alsopresent atomic resolution measurements on MgO(100) and Au(111), and firstevaluation measurements of the QPlus sensor in Kelvin probe microscopy on Si(111)7 × 7.

Mode shape imaging of out-of-plane and in-plane vibrating RF micromechanical resonators by atomic force microscopy

The application of atomic force microscopy (AFM) for mode shape imaging of both out-of-plane and in-plane vibrating RF micromechanical resonators is described in this work. The modulation of the amplitude of the resonator together with the lock-in detection of the AFM signal at the modulation frequency allows to achieve picometer-scale sensitivity for detecting the resonator vibration at arbitrarily large frequencies. We compare the application of this method for the characterization of the main out-of-plane thickness mode of an AlN film bulk acoustic resonator (FBAR) at 1.595 GHz and the in-plane vibrating first radial and wine-glass modes of a poly-SiGe disk resonator at 34.5 and 47.6 MHz, respectively. Our results demonstrate the capability of this method to image in-plane vibrating modes by measuring their small Poisson-coupled out-of-plane component.

Dynamic Adsorption Behavior of Poly(3-hydroxybutyrate) Depolymerase onto Polyester Surface Investigated by QCM and AFM

Time-dependent adsorption behavior of poly(3-hydroxybutyrate) (PHB) depolymerase from Ralstonia pickettiiT1 on a polyester surface was studied by complementary techniques of quarts crystal microbalance (QCM) and atomic force microscopy (AFM). Amorphous poly(l-lactide) (PLLA) thin films were used as adsorption substrates. Effects of enzyme concentration on adsorption onto the PLLA surface were determined time-dependently by QCM. Adsorption of PHB depolymerase took place immediately after replacement of the buffer solutions with the enzyme solutions in the cell, followed by a gradual increase in the amount over 30 min. The amount of PHB depolymerase molecules adsorbed on the surface of amorphous PLLA thin films increased with an increase in the enzyme concentration. Time-dependent AFM observation of enzyme molecules was performed during the adsorption of PHB depolymerase. The phase response of the AFM signal revealed that the nature of the PLLA surface around the PHB depolymerase molecule was changed due to the adsorption function of the enzyme and that PHB depolymerase adsorbed onto the PLLA surface as a monolayer at a lower enzyme concentration. The number of PHB depolymerase molecules on the PLLA surface depended on the enzyme concentration and adsorption time. In addition, the height of the adsorbed enzyme was found to increase with time when the PLLA surface was crowded with the enzymes. In the case of higher enzyme concentrations, multilayered PHB depolymerases were observed on the PLLA thin film. These QCM and AFM results indicate that two-step adsorption of PHB depolymerase occurs on the amorphous PLLA thin film. First, adsorption of PHB depolymerase molecules takes place through the characteristic interaction between the binding domain of PHB depolymerase and the free surface of an amorphous PLLA thin film. As the adsorption proceeded, the surface region of the thin film was almost covered with the enzyme, which was accompanied by morphological changes. Second, the hydrophobic interactions among the enzymes in the adlayer and the solution become more dominant to stack as a second layer.

Inverting dynamic force microscopy: from signals to time-resolved interaction forces.

Transient forces between nanoscale objects on surfaces govern friction, viscous flow, and plastic deformation, occur during manipulation of matter, or mediate the local wetting behavior of thin films. To resolve transient forces on the (sub) microsecond time and nanometer length scale, dynamic atomic force microscopy (AFM) offers largely unexploited potential. Full spectral analysis of the AFM signal completes dynamic AFM. Inverting the signal formation process, we measure the time course of the force effective at the sensing tip. This approach yields rich insight into processes at the tip and dispenses with a priori assumptions about the interaction, as it relies solely on measured data. Force measurements on silicon under ambient conditions demonstrate the distinct signature of the interaction and reveal that peak forces exceeding 200 nN are applied to the sample in a typical imaging situation. These forces are 2 orders of magnitude higher than those in covalent bonds.