Atomic Force Microscope Head Research Articles

Atomic force microscopy monitoring of subcritical slow crack growth in soda lime silicate glass

Prediction of brittle fracture in silicate glasses requires a fundamental understanding of slow crack growth rates, far below the critical stress intensity (KIC) of the material. Here, atomic force microscopy (AFM) was used to characterize slow crack propagation in soda lime silicate glasses. Using large-sample AFM systems with specialized tips and scanners, fractures less than 20 nm wide were measured as a function of relative humidity (RH). The results were found to be sensitive to the type of AFM tip used and to the dryness of the surface. Continuous scanning and image capture over several days allowed the determination of the crack tip velocity. The dependance of crack tip velocity on RH was measured by enclosing the sample and AFM head in a humidity-controlled chamber. The crack tip velocity was measured as low 4.0×10-12 m/s at 15 % RH and as high as 3.7×10-10 m/s at 40 % RH. Overall crack growth was smooth during the AFM scan. Additionally, recession of the crack tip was noted as the sample dried, indicating crack tip closure may be occurring. Further studies on alternative compositions will provide details on subcritical fracture processes in a range of different environmental conditions.

Thin head atomic force microscope for integration with optical microscope.

We present a novel thin head atomic force microscope (AFM) that can be easily integrated with an upright optical microscope (OM). The optical beam detection unit in the AFM used an obliquely incident laser beam onto the cantilever, reducing the AFM head's effective thickness to 7.3mm. That allows an open space above the cantilever probe to accommodate the objective lens up to 0.6 numerical aperture (N.A.) without obstruction. A multi-function digital controller was developed to control the AFM and reserved interfaces to communicate with the OM. To assess the performance of the developed AFM, we first measured the noise level and bandwidths of the AFM system. Then, the imaging quality of the AFM was evaluated by both calibration grids and two-dimensional materials. Finally, the thin head AFM was integrated into a homemade white light interferometer as a demonstration of combined use with an advanced optical system. The experimental results demonstrated that our developed AFM is suitable for integration under upright OM and brings AFM high-resolution advantages to the existing OM system.

Three-Dimensional Printing of a Model Atomic Force Microscope to Measure Force–Distance Profiles

We report a simple means to build a model atomic force microscope (AFM) using 3D printing of thermoplastic materials that are commercially available. The model has many of the key parts of an actual AFM including a z-axis stage, an AFM head with a cantilever assembly, and a laser source that reflects off of the back of the cantilever. Using a magnet attached to the tip of the cantilever and a metal sample, this model AFM enables acquisition of force–distance profiles with characteristic snap-in, pull-off, separate, and contact regions. The model AFM was designed, printed, and used by first- and second-year undergraduate students. Through completion of this project, students learned scientific instrument design and construction via 3D printing and obtained first-hand practice in the measurement of force–distance profiles and the elastic constants of cantilevers. The open design of the model can easily accommodate additional capabilities in which students are interested, e.g., topographical scanning and using cantilevers made from different materials.

Optimized single-crystal diamond scanning probes for high sensitivity magnetometry

The negatively-charged nitrogen-vacancy center (NV) in diamond forms a versatile system for quantum sensing applications. Combining the advantageous properties of this atomic-sized defect with scanning probe techniques such as atomic force microscopy (AFM) enables nanoscale imaging of e.g. magnetic fields. To form a scanning probe device, we place single NVs shallowly (i.e. < 20 nm) below the top facet of a diamond nanopillar, which is located on a thin diamond platform of typically below 1 μm thickness. This device can be attached to an AFM head, forming an excellent scanning probe tip. Furthermore, it simultaneously influences the collectible photoluminescence (PL) rate of the NV located inside. Especially sensing protocols using continuous optically-detected magnetic resonance benefit from an enhanced collectible PL rate, improving the achievable sensitivity. This work presents a comprehensive set of simulations to quantify the influence of the device geometry on the collectible PL rate for individual NVs. Besides geometric parameters (e.g. pillar length, diameter and platform thickness), we also focus on fabrication uncertainties such as the exact position of the NV or the taper geometry of the pillar introduced by imperfect etching. As a last step, we use these individual results to optimize our current device geometry, yielding a realistic gain in collectible PL rate by a factor of 13 compared to bulk diamond and 1.8 compared to our unoptimized devices.

Modelling and experimental study of nanoscratching process on PMMA thin-film using AFM tip-based nanomachining approach

This paper proposes a nanogroove machined depth prediction model for the atomic force microscopy (AFM) tip-based scratching method on the polymer thin-film. This model is used to predict the normal load required to just cut through the polymer thin-film without contacting the silicon substrate excessively to reduce the tip wear. In this proposed theoretical model, the AFM tip is assumed as a rectangular pyramid with a spherical apex. The elastic recovery, material pile-up, adhesive friction coefficient and mounted angle of the tip on the AFM head are considered in the developed model. Nanogrooves are scratched on a poly(methyl methacrylate) (PMMA) thin film by a silicon AFM tip. Results show that the bulk volume of the material pile–up can be enlarged after scratching with a relatively sharp tip. The equivalent height value of the material pile-up is thus introduced into the theoretical model, and the relationship between the equivalent height values of the material pile-up and the radius of the tip is analyzed in detail. Based on the proposed model and the experimental results, the effect of the radius of the AFM tip on the flow stress and adhesive friction coefficient is studied. Finally, several nanogrooves when the tip just cutting through the polymer thin-film are achieved on the polymer thin-films with different thicknesses using the tips with various radii.

Atomic force microscope scanning head with 3-dimensional orthogonal scanning to eliminate the curved coupling

An atomic force microscopy (AFM) scanning head is designed with the probe orthogonal scanning mode for metrological AFM to eliminate the curvature distortion. The AFM probe is driven by piezostage and the scanning trajectory of the probe in 3 directions are orthogonal to reduce the cross coupling. A new optical lever amplification optical path is developed to eliminate the coupling error. The tracing lens and probe tip are moved as an integrated part. The AFM is operated at contacting mode. The step approach process of the probe tip is tested to the sample surface and the noise of the AFM head is analyzed. The response of the probe demonstrates a 0.5 nm resolution of the probe head in the z direction. Finally, the planar scanning performance of the scanning head is demonstrated compared with tube scanning AFM.

A low-noise measurement system for scanning thermal microscopy resistive nanoprobes based on a transformer ratio-arm bridge

Atomic force microscopy (AFM) is a widely used technology for the investigation and characterization of nanomaterials. Its functionality can be easily expanded by applying dedicated extension modules, which can measure the electrical conductivity or temperature of a sample. In this paper, we introduce a transformer ratio-arm bridge setup dedicated to AFM-based thermal imaging. One of the key features of the thermal module is the use of a low-power driving signal that prevents undesirable tip heating during resistance measurement, while the other is the sensor location in a ratio-arm transformer bridge working in the audio frequency range and ensuring galvanic isolation of the tip, enabling contact-mode scanning of electronic circuits. The proposed expansion module is compact and it can be integrated onto the AFM head close to the cantilever. The calibration process and the resolution of 11 mK of the proposed setup are shown.

A novel AFM-based 5-axis nanoscale machine tool for fabrication of nanostructures on a micro ball.

This paper presents a novel atomic force microscopy (AFM)-based 5-axis nanoscale machine tool developed to fabricate nanostructures on different annuli of the micro ball. Different nanostructures can be obtained by combining the scratching trajectory of the AFM tip with the movement of the high precision air-bearing spindle. The center of the micro ball is aligned to be coincided with the gyration center of the high precision to guarantee the machining process during the rotating of the air-bearing spindle. Processing on different annuli of the micro ball is achieved by controlling the distance between the center of the micro ball and the rotation center of the AFM head. Nanostructures including square cavities, circular cavities, triangular cavities, and an annular nanochannel are machined successfully on the three different circumferences of a micro ball with a diameter of 1500 μm. Moreover, the influences of the error motions of the high precision air-bearing spindle and the eccentric between the micro ball and the gyration center of the high precision air-bearing spindle on the processing position error on the micro ball are also investigated. This proposed machining method has the potential to prepare the inertial confinement fusion target with the expected dimension defects, which would advance the application of the AFM tip-based nanomachining approach.

Vibration isolator carrying atomic force microscope’s head

For high-resolution imaging in harsh environments this paper proposes a vibration isolation system that actively positions the head of an atomic force microscope (AFM) to maintain the vertical distance to the sample. On the moving platform carrying the AFM head, a displacement sensor is installed to detect the vibrations between the probe and the sample that impair the imaging quality. The detected vibrations are rejected by vertically moving the platform with feedback control. For the motion, flexure-guided Lorentz actuators are designed, such that the resulting suspension mode occurs around the major spectrum of the floor vibrations. By feedback control design, the high gain of the suspension mode is used to increase the open-loop gain for better vibration rejection. The experimental results demonstrate that the vibration isolation system can reject 99.3% of the vibrations. As a result, AFM imaging of nanoscale features is successfully performed in a vibrational environment.

A Novel White Light Interference Based AFM Head

A novel atomic force microscope (AFM) head based on white light interference (WLI) is developed for nanoscale surface measurement. In this head, instead of an optical beam deflection (OBD) technique for AFM probe position, WLI fringes on the surface of the probe cantilever are analyzed for probe position. The probe adjustment mechanism is designed, an algorithm based on wavelet transform and Hilbert transform is presented for accurate zero-order fringe positioning, and a calibration method is developed for the relationship between the position of the interference fringes on the surface of the probe cantilever and the vertical displacement of the probe. By these approaches, advantage of high vertical resolution of WLI is combined with that of high horizontal resolution of atomic force probe for nanometer resolution surface measurement. Experiments have been carried out to verify the feasibility and accuracy of the head for AFM measurement. And compared with a commercial AFM, 3-D measurement results of a standard grating prove that the measurement speed of proposed AFM head is 22% faster.

An Atomic Force Microscope with Dual Actuation Capability for Biomolecular Experiments.

We report a modular atomic force microscope (AFM) design for biomolecular experiments. The AFM head uses readily available components and incorporates deflection-based optics and a piezotube-based cantilever actuator. Jetted-polymers have been used in the mechanical assembly, which allows rapid manufacturing. In addition, a FeCo-tipped electromagnet provides high-force cantilever actuation with vertical magnetic fields up to 0.55 T. Magnetic field calibration has been performed with a micro-hall sensor, which corresponds well with results from finite element magnetostatics simulations. An integrated force resolution of 1.82 and 2.98 pN, in air and in DI water, respectively was achieved in 1 kHz bandwidth with commercially available cantilevers made of Silicon Nitride. The controller and user interface are implemented on modular hardware to ensure scalability. The AFM can be operated in different modes, such as molecular pulling or force-clamp, by actuating the cantilever with the available actuators. The electromagnetic and piezoelectric actuation capabilities have been demonstrated in unbinding experiments of the biotin-streptavidin complex.

A miniaturized, high frequency mechanical scanner for high speed atomic force microscope using suspension on dynamically determined points.

One of the major limitations in the speed of the atomic force microscope (AFM) is the bandwidth of the mechanical scanning stage, especially in the vertical (z) direction. According to the design principles of "light and stiff" and "static determinacy," the bandwidth of the mechanical scanner is limited by the first eigenfrequency of the AFM head in case of tip scanning and by the sample stage in terms of sample scanning. Due to stringent requirements of the system, simply pushing the first eigenfrequency to an ever higher value has reached its limitation. We have developed a miniaturized, high speed AFM scanner in which the dynamics of the z-scanning stage are made insensitive to its surrounding dynamics via suspension of it on specific dynamically determined points. This resulted in a mechanical bandwidth as high as that of the z-actuator (50 kHz) while remaining insensitive to the dynamics of its base and surroundings. The scanner allows a practical z scan range of 2.1 μm. We have demonstrated the applicability of the scanner to the high speed scanning of nanostructures.

An ultra-low noise optical head for liquid environment atomic force microscopy.

The design considerations and eventual performance of a new, ultra-low noise optical head for dynamic atomic force microscopy (AFM) are presented. The head, designed specifically for the study of hydration layers and ion organization next to solid surfaces and biomolecules, displays an integrated tip-sample distance noise below 3 pm. The sensitivity of the optical beam deflection sensor, operating at frequencies up to 8.6 MHz (3 dB roll-off), is typically below 10 fm/√Hz, enabling utilization of high frequency cantilevers of low thermal noise for fundamental and higher mode imaging. Exceptional signal stability and low optical noise are achieved by replacing the commonly used laser diode with a helium-neon laser. An integral photothermal excitation of the cantilever produces pure harmonic oscillations, minimizing the generation of higher cantilever modes and deleterious sound waves characterizing the commonly used excitation by a piezoelectric crystal. The optical head is designed to fit on top of the widespread Multimode(®) (Bruker) piezo-tube and accommodate its commercial liquid cell. The performance of the new AFM head is demonstrated by atomic resolution imaging of a muscovite mica surface in aqueous solution.

Implementation of a four quadrant optic fibre bundle as a deflection sensor to get rid of heat sources in an AFM head

In the frame of developing a thermally passive atomic force microscope head, a new kind of 2D displacement sensor based on a four quadrant optic fibre bundle has been implemented. The aim is to replace the quad cell photodiode used in the optical beam deflection method to detect cantilever deflection. The use of the bundle as a position sensor has already been modelled and experimentally evaluated in a previous work. This article reports on the implementation of the bundle as a deflection sensor for atomic force microscopy. The main motivation for such a development was to reduce the heat sources in the instrument. To reach this goal the photodiode and its conditioning circuit used for the measurement of cantilever deflection has been externalized from the AFM head. For the same reason, the laser diode and its electronic driver have been deported using optic fibre. To test the AFM head prototype in real conditions, approach curves and AFM images have been performed. The results show that the bundle is very well suited for AFM applications that require very low heat sources such as metrological AFM where each error source has to be managed.

Accurate calibration and uncertainty estimation of the normal spring constant of various AFM cantilevers.

Measurement of force on a micro- or nano-Newton scale is important when exploring the mechanical properties of materials in the biophysics and nanomechanical fields. The atomic force microscope (AFM) is widely used in microforce measurement. The cantilever probe works as an AFM force sensor, and the spring constant of the cantilever is of great significance to the accuracy of the measurement results. This paper presents a normal spring constant calibration method with the combined use of an electromagnetic balance and a homemade AFM head. When the cantilever presses the balance, its deflection is detected through an optical lever integrated in the AFM head. Meanwhile, the corresponding bending force is recorded by the balance. Then the spring constant can be simply calculated using Hooke’s law. During the calibration, a feedback loop is applied to control the deflection of the cantilever. Errors that may affect the stability of the cantilever could be compensated rapidly. Five types of commercial cantilevers with different shapes, stiffness, and operating modes were chosen to evaluate the performance of our system. Based on the uncertainty analysis, the expanded relative standard uncertainties of the normal spring constant of most measured cantilevers are believed to be better than 2%.

High-speed imaging upgrade for a standard sample scanning atomic force microscope using small cantilevers.

We present an atomic force microscope (AFM) head for optical beam deflection on small cantilevers. Our AFM head is designed to be small in size, easily integrated into a commercial AFM system, and has a modular architecture facilitating exchange of the optical and electronic assemblies. We present two different designs for both the optical beam deflection and the electronic readout systems, and evaluate their performance. Using small cantilevers with our AFM head on an otherwise unmodified commercial AFM system, we are able to take tapping mode images approximately 5-10 times faster compared to the same AFM system using large cantilevers. By using additional scanner turnaround resonance compensation and a controller designed for high-speed AFM imaging, we show tapping mode imaging of lipid bilayers at line scan rates of 100-500 Hz for scan areas of several micrometers in size.

Piezoelectric bimorph-based scanner in the tip-scan mode for high speed atomic force microscope

A piezoelectric bimorph-based scanner operating in tip-scan mode for high speed atomic force microscope (AFM) is first presented. The free end of the bimorph is used for fixing an AFM cantilever probe and the other one is mounted on the AFM head. The sample is placed on the top of a piezoelectric tube scanner. High speed scan is performed with the bimorph that vibrates at the resonant frequency, while slow scanning is carried out by the tube scanner. The design and performance of the scanner is discussed and given in detailed. Combined with a commercially available data acquisition system, a high speed AFM has been built successfully. By real-time observing the deformation of the pores on the surface of a commercial piezoelectric lead zirconate titanate (PZT-5) ceramics under electric field, the dynamic imaging capability of the AFM is demonstrated. The results show that the notable advantage of the AFM is that dynamic process of the sample with large dimensions can be easily investigated. In addition, this design could provide a way to study a sample in real time under the given experimental condition, such as under an external electric field, on a heating stage, or in a liquid cell.

Development of a large-range atomic force microscope measuring system for optical free form surface characterization

In this paper, a large-range atomic force microscope (AFM) measuring system is developed for optical free form surface characterization. Based on the self-sensing tuning fork probe, a compact AFM head is developed, which is easy to combine with a scanning stage. Depending on the probe's unique structure and the usage of dynamic working mode, the tip–sample interaction force is reduced, improving the system's dynamic response performance. A two-platform structure is applied in the system, which combines a PZT stage with a motor driving platform. A dual feedback strategy is applied to ensure a measuring range up to 25 mm × 25 mm × 5 mm. The system includes three laser interferometers to make the measuring data traced to the ‘meter’ definition. A standard one-dimensional grating is tested to show the performance of the system. A millimeter scale optical free form surface with a sinusoidal structure array is measured relying on the two-platform structure implemented. The high frequency information and low frequency information of the sample are separated automatically, which represent the profile and roughness, respectively.

A general approach for the microrheology of cancer cells by atomic force microscopy

The determination of the viscoelastic properties of cells by atomic force microscopy (AFM) is mainly realized by looking at the relaxation of the force when a constant position of the AFM head is maintained or at the evolution of the indentation when a constant force is maintained. In both cases the analysis rests on the hypothesis that the motion of the probe before the relaxation step is realized in a time which is much smaller than the characteristic relaxation time of the material. In this paper we carry out a more general analysis of the probe motion which contains both the indentation and relaxation steps, allowing a better determination of the rheological parameters. This analysis contains a correction of the Hertz model for large indentation and also the correction due to the finite thickness of the biological material; it can be applied to determine the parameters representing any kind of linear viscoelastic model. This approach is then used to model the rheological behavior of one kind of cancer cell called Hep-G2. For this kind of cell, a power law model does not well describe the low and high frequency modulus contrary to a generalized Maxwell model.

Microcantilever-based mass sensors: working at higher modes against reducing the dimensions

Enhanced sensitivity and quality factor of microcantilever (MC)-based mass sensors when working at higher modes and reducing the dimensions are compared. By analysing the out-of-plane vibration signals recorded using an atomic force microscopy head, seven unique modes of a low spring constant MC are identified and mode shapes are assigned with the help of finite element method simulations. Polymer coating on the MC is applied by a precise dip coating setup and shift in frequency because of added mass is used to estimate the mass sensitivity. Similar measurements were also carried out for different dimensions of MC. The authors found that mass sensitivity increases with increase of eigenvalue (λ2n) and decreasing dimensions (T/L2) where T is thickness and L is length of MC. Although mass sensitivity was found to enhance by either method, quality factor was found to decrease at higher modes after the addition of polymer mass.