Direct deformation study of AFM probe tips modified by hydrophobic alkylsilane self-assembled monolayers

The in-use wear of atomic force microscopy (AFM) probe tips is crucial for the reliability of AFM measurements. Increase of tip size for several nanometers is difficult to monitor but it can already taint subsequent AFM data. We have developed a method to study the shape evolution of AFM probe tips in nanometer scale. This approach provides direct comparison of probe shape profiles, and thus can help in evaluation of the level of tip damage and quality of acquired AFM data. Consequently, the shape degradation of probes modified by hydrophobic alkylsilane self-assembled monolayers (SAMs) was studied. The tip wear length and wear volume were adopted to quantitatively verify the effectiveness of hydrophobic coatings. When compared with their silicon counterparts, probes modified by SAM materials exhibit superior wear-resistant behavior in tapping mode scans.     

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Complex dynamics of carbon nanotube probe tips

Carbon nanotube (CNT) tips in tapping mode atomic force microscopy (AFM) enable very high-resolution imaging, measurements, and manipulation at the nanoscale. We present recent results based on experimental analysis that yield new insights into the dynamics of CNT probe tips in tapping mode AFM. Experimental measurements are presented of the frequency response and dynamic amplitude-distance data of a high-aspect-ratio multi-walled (MW) CNT tip. Higher harmonics of the microcantilever are measured in frequency ranges corresponding to attractive regime and the repulsive regime where the CNT buckles dynamically. Surface scanning is performed using a MWCNT tip on a SiO(2) grating to verify the imaging instabilities associated with MWCNT buckling when used with normal control schemes in the tapping mode. Lastly, the choice of optimal setpoints for tapping mode control using CNT tip are discussed using the experimental results.     

Attachment of carbon nanotubes to atomic force microscope probes

In atomic force microscopy (AFM) the accuracy of data is often limited by the tip geometry and the effect on this geometry of wear. One way to improve the tip geometry is to attach carbon nanotubes (CNT) to AFM tips. CNTs are ideal because they have a small diameter (typically between 1 and 20nm), high aspect ratio, high strength, good conductivity, and almost no wear. A number of methods for CNT attachment have been proposed and explored including chemical vapour deposition (CVD), dielectrophoresis, arc discharge and mechanical attachment. In this work we will use CVD to deposit nanotubes onto a silicon surface and then investigate improved methods to pick-up and attach CNTs to tapping mode probes. Conventional pick-up methods involve using standard tapping mode or non-contact mode so as to attach only those CNTs that are aligned vertically on the surface. We have developed improved methods to attach CNTs using contact mode and reduced set-point tapping mode imaging. Using these techniques the AFM tip is in contact with a greater number of CNTs and the rate and stability of CNT pick-up is improved. The presence of CNTs on the modified AFM tips was confirmed by high-resolution AFM imaging, analysis of the tips dynamic force curves and scanning electron microscopy (SEM).     

Controlling tip–sample interaction forces during a single tap for improved topography and mechanical property imaging of soft materials by AFM

We introduce a method that exploits the “active” nature of the force-sensing integrated readout and active tip (FIRAT), a recently introduced atomic force microscopy (AFM) probe, to control the interaction forces during individual tapping events in tapping mode (TM) AFM. In this method the probe tip is actively retracted if the tip–sample interaction force exceeds a user-specified force threshold during a single tap while the tip is still in contact with the surface. The active tip control (ATC) circuitry designed for this method makes it possible to control the repulsive forces and indentation into soft samples, limiting the repulsive forces during the scan while avoiding instability due to attractive forces. We demonstrate the accurate topographical imaging capability of this method on suitable samples that possess both soft and stiff features.     

Phase imaging quality improvement by modification of AFM probes’ cantilever

Imaging of the surface of materials by atomic force microscopy under tapping and phase imaging mode, with use of modified probes is addressed. In this study, the circularly shaped holes located in varying distance from the probe base, were cut out by focused ion beam. Such modification was a consequence of the results of the previous experiments (probe tip sharpening and cantilever thinning) where significant improvement of image quality in tapping and phase imaging mode has been revealed. The solution proposed herein gives similar results, but is much simpler from the technological point of view. Shorter exposition time of the tip onto gallium ions during FIB processing allows to reduce material degradation. The aim of this modification was to change harmonic oscillators’ properties in the simplest and fastest way, to obtain stronger signal for higher resonant frequencies, which can be advantageous for improving the quality of imaging in PI mode. Probes shaped in that way were used for AFM investigations with Bruker AFM nanoscope 8. As a testing material, titanium roughness standard sample, supplied by Bruker, was used. The results have shown that the modifications performed within these studies influence the oscillation of the probes, which in some cases may result in deterioration of the imaging quality under tapping mode for one or both self‐resonant frequencies. However, phase imaging results obtained using modified probes are of higher quality. The numerical simulations performed by application of finite element method were used to explain the results obtained experimentally. Phenomenon described within this study allows to apply developed modelling methodology for prediction of effects of various modifications on the probes' tip, and as a result, to predict how proposed modifications will affect AFM imaging quality.     

Quality assessment of atomic force microscopy probes by scanning electron microscopy: correlation of tip structure with rendered images

While image quality from instruments such as electron microscopes, light microscopes, and confocal laser scanning microscopes is mostly influenced by the alignment of optical train components, the atomic force microscope differs in that image quality is highly dependent upon a consumable component, the scanning probe. Although many types of scanning probes are commercially available, specific configurations and styles are generally recommended for specific applications. For instance, in our area of interest, tapping mode imaging of biological constituents in fluid, double ended, oxide-sharpened pyramidal silicon nitride probes are most often employed. These cantilevers contain four differently sized probes; thick- and thin-legged 100 microm long and thick- and thin-legged 200 microm long, with only one probe used per cantilever. In a recent investigation [Taatjes et al. (1997) Cell Biol. Int. 21:715-726], we used the scanning electron microscope to modify the oxide-sharpened pyramidal probe by creating an electron beam deposited tip with a higher aspect ratio than unmodified tips. Placing the probes in the scanning electron microscope for modification prompted us to begin to examine the probes for defects both before and after use with the atomic force microscope. The most frequently encountered defect was a mis-centered probe, or a probe hanging off the end of the cantilever. If we had difficulty imaging with a probe, we would examine the probe in the scanning electron microscope to determine if any defects were present, or if the tip had become contaminated during scanning. Moreover, we observed that electron beam deposited tips were blunted by the act of scanning a hard specimen, such as colloidal gold with the atomic force microscope. We also present a mathematical geometric model for deducing the interaction between an electron beam deposited tip and either a spherical or elliptical specimen. Examination of probes in the scanning electron microscope may assist in interpreting images generated by the atomic force microscope.     

A torsional resonance mode AFM for in-plane tip surface interactions

Changing the method of tip/sample interaction leads to contact, tapping and other dynamic imaging modes in atomic force microscopy (AFM) feedback controls. A common characteristic of these feedback controls is that the primary control signals are based on flexural deflection of the cantilever probes, statically or dynamically. We introduce a new AFM mode using the torsional resonance amplitude (or phase) to control the feedback loop and maintain the tip/surface relative position through lateral interaction. The torsional resonance mode (TRmode™) provides complementary information to tapping mode for surface imaging and studies. The nature of tip/surface interaction of the TRmode facilitates phase measurements to resolve the in-plane anisotropy of materials as well as measurements of dynamic friction at nanometer scale. TRmode can image surfaces interleaved with TappingMode™ with the same probe and in the same area. In this way we are able to probe samples dynamically in both vertical and lateral dimensions with high sensitivity to local mechanical and tribological properties. The benefit of TRmode has been proven in studies of water adsorption on HOPG surface steps. TR phase data yields approximately 20 times stronger contrast than tapping phase at step edges, revealing detailed structures that cannot be resolved in tapping mode imaging. The effect of sample rotation relative to the torsional oscillation axis of the cantilever on TR phase contrast has been observed. Tip wear studies of TRmode demonstrated that the interaction forces between tip and sample could be controlled for minimum tip damage by the feedback loop.     

Developments of scanning probe microscopy with stress/strain fields

An innovative stress/strain fields scanning probe microscopy in ultra high vacuum (UHV) environments is developed for the first time. This system includes scanning tunneling microscope (STM) and noncontact atomic force microscope (NC-AFM). Two piezo-resistive AFM cantilever probes and STM probes used in this system can move freely in XYZ directions. The nonoptical frequency shift detection of the AFM probe makes the system compact enough to be set in the UHV chambers. The samples can be bent by an anvil driven by a step motor to induce stress and strain on their surface. With a direct current (dc) power source, the sample can be observed at room and high temperatures. A long focus microscope and a monitor are used to observe the samples and the operation of STM and AFM. Silicon(111) surface in room temperature and silicon(001) surface in high temperature with stress were investigated to check the performance of the scanning probe microscope.     

Variable-force tapping atomic force microscopy as a tool in the characterization of organic devices

A common method for characterizing the phase separation of materials in mixtures is tapping mode atomic force microscopy (AFM). However, AFM results are influenced by surface-energy effects and the employed tapping force, and it might therefore be difficult to attain correct information regarding the bulk with such a surface-imaging technique. In this work, we present a way of imaging material phase separation in an improved manner by recording a series of AFM images at different tapping force. More specifically, we have employed the variable-force AFM method on organic mixtures, comprising a conjugated polymer (MEH-PPV) and an ion-conducting polymer electrolyte (PEO-XCF(3)SO(3), X=Li, K, Rb), and we demonstrate that it is capable of reversibly sampling such materials not only on the surface, but also (indirectly) in the topmost part of the bulk. The analysis of the evolution of AFM phase images allows us to (indirectly) gain information about the bulk-phase separation of materials. We find that the variable-force AFM results correlate well with the device performance of light-emitting electrochemical cells employing such organic mixtures as the active material.     

Cleaning AFM colloidal probes by mechanically scrubbing with supersharp “brushes”

Contamination control of atomic force microscope (AFM) tips (including standard but supersharp imaging tips and particle/colloidal probes) is very important for reliable AFM imaging and surface/interface force measurements. Traditional cleaning methods such as plasma, UV–ozone and solvent treatments have their shortcomings. Here, we demonstrate that calibration gratings with supersharp spikes can be employed to scrub away contaminants accumulated on a colloidal sphere probe by scanning the probe against the spikes at high load at constant-force mode. The present method is superior to traditional cleaning methods in several aspects. First, accumulated lump-like organic/inorganic material can be removed; second, removal is non-destructive and highly efficient based on a “targeted removal” strategy; third, removal and probe shape/morphology study can be completed in a single step (we report, to our best knowledge, the first evidence of the wear of the colloidal sphere during force measurements); and fourth, both colloidal/particle probes and standard but supersharp AFM imaging tips can be treated.     

Analysis of simulated scanning of atomic-scale silicon surface by atomic force microscopy

This study constructs a contact-mode atomic force microscopy (AFM) simulation measurement model with constant force mode to simulate and analyze the outline scanning measurement by AFM. The simulation method is that when the probe passes the surface of sample, the action force of the atom of sample received by the atom of the probe can be calculated by using Morse potential. Through calculation, the equivalent force on the cantilever of probe can be acquired. By using the deflection angle equation for the cantilever of probe developed and inferred by this study, the deflection angle of receiving action force can be calculated. On the measurement point, as the deflection angle reaches a fixed deflection angle, the scan height of this simulation model can be acquired. By scanning in the right order, the scan curve of the simulation model can be obtained. By using this simulation measurement model, this study simulates and analyzes the scanning of atomic-scale surface outline. Meanwhile, focusing on the tip radii of different probes, the concept of sensitivity analysis is employed to investigate the effects of the tip radius of probe on the atomic-scale surface outline. As a result, it is found from the simulation on the atomic-scale surface that within the simulation scope of this study, when the tip radius of probe is greater than 12 nm, the effects of single atom on the scan curve of AFM can be better decreased or eliminated.     

Adhesive-free colloidal probes for nanoscale force measurements: production and characterization

We describe novel approaches for the production and characterization of epoxy- and adhesive-free colloidal probes for atomic force microscopy (AFM). Borosilicate glass microspheres are strongly attached to commercial AFM cantilevers exploiting the capillary adhesion force due to the formation of a water meniscus, and then a thermal annealing of the sphere-cantilever system at a temperature slightly below the softening point of borosilicate glass. Controlling the wettability of the surfaces involved turned out to be a crucial element for the control of surface adhesion and for the implementation of a completely adhesive-free production method of colloidal probes. Moreover, we present a statistical characterization protocol of the probe dimensions and roughness based on the AFM inverse imaging of colloidal probes on spiked gratings. We have assessed the influence of defects of the grating on the characterization of the probe, and discussed the accuracy of our characterization technique in comparison to the methods based on scanning electron or optical microscopy, or on the manual analysis of AFM inverse images.     

Print your atomic force microscope

Progress in scanning probe microscopy profited from a flourishing multitude of new instrument designs, which lead to novel imaging modes and as a consequence to innovative microscopes. Often these designs were hampered by the restrictions, which conventional milling techniques impose. Modern rapid prototyping techniques, where layer by layer is added to the growing piece either by light driven polymerization or by three-dimensional printing techniques, overcome this constraint, allowing highly concave or even embedded and entangled structures. We have employed such a technique to manufacture an atomic force microscopy (AFM) head, and we compared its performance with a copy milled from aluminum. We tested both AFM heads for single molecule force spectroscopy applications and found little to no difference in the signal-to-noise ratio as well as in the thermal drift. The lower E modulus seems to be compensated by higher damping making this material well suited for low noise and low drift applications. Printing an AFM thus offers unparalleled freedom in the design and the rapid production of application-tailored custom instruments.     

Mapping of enzyme activity by detection of enzymatic products during AFM imaging with integrated SECM-AFM probes

With the integration of submicro- and nanoelectrodes into atomic force microscopy (AFM) probes using microfabrication techniques, an elegant approach combining scanning electrochemical microscopy (SECM) with AFM has recently been introduced. Simultaneous contact mode imaging of a micropatterned sample with immobilized enzyme spots and imaging of enzyme activity is shown. In contrast to force spectroscopy the conversion of an enzymatic byproduct is directly detected during AFM imaging and correlated to the activity of the enzyme.     

High-resolution constant-height imaging with apertured silicon cantilever probes

We present high-resolution aperture probes based on non-contact silicon atomic force microscopy (AFM) cantilevers for simultaneous AFM and near-infrared scanning near-field optical microscopy (SNOM). For use in near-field optical microscopy, conventional AFM cantilevers are modified by covering their tip side with an opaque aluminium layer. To fabricate an aperture, this metal layer is opened at the end of the polyhedral probe using focused ion beams (FIB). Here we show that apertures of less than 50 nm can be obtained using this technique, which actually yield a resolution of about 50 nm, corresponding to λ/20 at the wavelength used. To exclude artefacts induced by distance control, we work in constant-height mode. Our attention is particularly focused on the distance dependence of resolution and to the influence of slight cantilever bending on the optical images when scanning at such low scan heights, where first small attractive forces exerted on the cantilever become detectable.     

A relocated technique of atomic force microscopy (AFM) samples and its application in molecular biology

A kind of simple atomic force microscopy (AFM) relocated technique, which takes advantage of homemade sample locator system, is used for investigating repeatedly imaging of some specific species on the whole substrate (over 1 x 1 cm2) with resolution about 400 nm. As applications of this sample locator system, single extended DNA molecules and plasmid DNA network are shown in different AFM operational modes: tapping mode and contact mode with different tips after the substrates have been moved.     

Microfabricated torsion levers optimized for low force and high-frequency operation in fluids

We developed a mass production fabrication process for making symmetrically supported torsion cantilevers/oscillators with highly compliant springs. These torsion probes offer advantages in atomic force microscopy (AFM) because they are small, have high optical gain, do not warp and can be made with two independent axes. Compared to traditional AFM cantilevers, these probes have higher frequency response, higher Q, lower noise, better optics (since the mirror does not bend) and two data channels. Soft small levers with sub-pN force resolution can resonate cleanly above 10 kHz in water. When fabricated with a ferromagnetic coating on the rigid reflecting pad, they can be driven magnetically or serve as high-resolution magnetometers. Asymmetric levers can be tapping mode probes or high-resolution accelerometers. The dual axis gimbaled probes with two orthogonal axes can operate on a standard AFM with single beam illumination. These probes can be used as self-referencing, drift free, cantilevers where one axis senses the substrate position and the other the sample position. These levers can be optimized for differential contrast or high-resolution friction imaging.     

Analysis of dynamic cantilever behavior in tapping mode atomic force microscopy

Tapping mode atomic force microscopy (AFM) provides phase images in addition to height and amplitude images. Although the behavior of tapping mode AFM has been investigated using mathematical modeling, comprehensive understanding of the behavior of tapping mode AFM still poses a significant challenge to the AFM community, involving issues such as the correct interpretation of the phase images. In this paper, the cantilever's dynamic behavior in tapping mode AFM is studied through a three dimensional finite element method. The cantilever's dynamic displacement responses are firstly obtained via simulation under different tip‐sample separations, and for different tip‐sample interaction forces, such as elastic force, adhesion force, viscosity force, and the van der Waals force, which correspond to the cantilever's action upon various different representative computer‐generated test samples. Simulated results show that the dynamic cantilever displacement response can be divided into three zones: a free vibration zone, a transition zone, and a contact vibration zone. Phase trajectory, phase shift, transition time, pseudo stable amplitude, and frequency changes are then analyzed from the dynamic displacement responses that are obtained. Finally, experiments are carried out on a real AFM system to support the findings of the simulations. Microsc. Res. Tech. 78:935–946, 2015. © 2015 Wiley Periodicals, Inc.     

Adaptive Q control for tapping-mode nanoscanning using a piezoactuated bimorph probe

A new approach, called adaptive Q control, for tapping-mode atomic force microscopy (AFM) is introduced and implemented on a homemade AFM setup utilizing a laser Doppler vibrometer and a piezoactuated bimorph probe. In standard Q control, the effective Q factor of the scanning probe is adjusted prior to the scanning depending on the application. However, there is a trade-off in setting the effective Q factor of an AFM probe. The Q factor is either increased to reduce the tapping forces or decreased to increase the maximum achievable scan speed. Realizing these two benefits simultaneously using standard Q control is not possible. In adaptive Q control, the Q factor of the probe is set to an initial value as in standard Q control, but then modified on the fly during scanning when necessary to achieve this goal. In this article, we present the basic theory behind adaptive Q control, the electronics enabling the online modification of the probe's effective Q factor, and the results of the experiments comparing three different methods: scanning (a) without Q control, (b) with standard Q control, and (c) with adaptive Q control. The results show that the performance of adaptive Q control is superior to the other two methods.