Fast and reliable pre-approach for scanning probe microscopes based on tip-sample capacitance.

Within the last three decades Scanning Probe Microscopy has been developed to a powerful tool for measuring surfaces and their properties on an atomic scale such that users can be found nowadays not only in academia but also in industry. This development is still pushed further by researchers, who continuously exploit new possibilities of this technique, as well as companies that focus mainly on the usability. However, although imaging has become significantly easier, the time required for a safe approach (without unwanted tip-sample contact) can be very time consuming, especially if the microscope is not equipped or suited for the observation of the tip-sample distance with an additional optical microscope. Here we show that the measurement of the absolute tip-sample capacitance provides an ideal solution for a fast and reliable pre-approach. The absolute tip-sample capacitance shows a generic behavior as a function of the distance, even though we measured it on several completely different setups. Insight into this behavior is gained via an analytical and computational analysis, from which two additional advantages arise: the capacitance measurement can be applied for observing, analyzing, and fine-tuning of the approach motor, as well as for the determination of the (effective) tip radius. The latter provides important information about the sharpness of the measured tip and can be used not only to characterize new (freshly etched) tips but also for the determination of the degradation after a tip-sample contact/crash.

Dissipation and resonance frequency shift of a resonator magnetically coupled to a semiclassical spin.

We calculate the change of the properties of a resonator, when coupled to a semiclassical spin by means of the magnetic field. Starting with the Lagrangian of the complete system, we provide an analytical expression for the linear response function for the motion in the case of a mechanical resonator and the current for the case of an electromagnetic resonator, thereby considering the influence of the resonator on the spin and vice versa. This analysis shows that the resonance frequency and effective dissipation factor can change significantly due to the relaxation times of the spin. We first derive this for a system consisting of a spin and mechanical resonator and thereafter apply the same calculations to an electromagnetic resonator. Moreover, the applicability of the method is generalized to a resonator coupled to two-level systems and more, providing a key to understand some of the problems of two-level systems in quantum devices.

Subsurface contrast due to friction in heterodyne force microscopy.

The nondestructive imaging of subsurface structures on the nanometer scale has been a long-standing desire in both science and industry. A few impressive images were published so far that demonstrate the general feasibility by combining ultrasound with an atomic force microscope. From different excitation schemes, heterodyne force microscopy seems to be the most promising candidate delivering the highest contrast and resolution. However, the physical contrast mechanism is unknown, thereby preventing any quantitative analysis of samples. Here we show that friction at material boundaries within the sample is responsible for the contrast formation. This result is obtained by performing a full quantitative analysis, in which we compare our experimentally observed contrasts with simulations and calculations. Surprisingly, we can rule out all other generally believed responsible mechanisms, like Rayleigh scattering, sample (visco)elasticity, damping of the ultrasonic tip motion, and ultrasound attenuation. Our analytical description paves the way for quantitative subsurface-AFM imaging.

Upper Bounds on Spontaneous Wave-Function Collapse Models Using Millikelvin-Cooled Nanocantilevers.

Collapse models predict a tiny violation of energy conservation, as a consequence of the spontaneous collapse of the wave function. This property allows us to set experimental bounds on their parameters. We consider an ultrasoft magnetically tipped nanocantilever cooled to millikelvin temperature. The thermal noise of the cantilever fundamental mode has been accurately estimated in the range 0.03-1 K, and any other excess noise is found to be negligible within the experimental uncertainty. From the measured data and the cantilever geometry, we estimate the upper bound on the continuous spontaneous localization collapse rate in a wide range of the correlation length r_{C}. Our upper bound improves significantly previous constraints for r_{C}>10^{-6} m, and partially excludes the enhanced collapse rate suggested by Adler. We discuss future improvements.

A subsurface add-on for standard atomic force microscopes.

The application of ultrasound in an Atomic Force Microscope (AFM) gives access to subsurface information. However, no commercially AFM exists that is equipped with this technique. The main problems are the electronic crosstalk in the AFM setup and the insufficiently strong excitation of the cantilever at ultrasonic (MHz) frequencies. In this paper, we describe the development of an add-on that provides a solution to these problems by using a special piezo element with a lowest resonance frequency of 2.5 MHz and by separating the electronic connection for this high frequency piezo element from all other connections. In this sense, we support researches with the possibility to perform subsurface measurements with their existing AFMs and hopefully pave also the way for the development of a commercial AFM that is capable of imaging subsurface features with nanometer resolution.

Atomic resolution scanning tunneling microscopy in a cryogen free dilution refrigerator at 15 mK.

Pulse tube refrigerators are becoming more common, because they are cost efficient and demand less handling than conventional (wet) refrigerators. However, a downside of a pulse tube system is the vibration level at the cold-head, which is in most designs several micrometers. We implemented vibration isolation techniques which significantly reduced vibration levels at the experiment. These optimizations were necessary for the vibration sensitive magnetic resonance force microscopy experiments at milli-kelvin temperatures for which the cryostat is intended. With these modifications we show atomic resolution scanning tunneling microscopy on graphite. This is promising for scanning probe microscopy applications at very low temperatures.

Single molecule binding dynamics measured with atomic force microscopy.

We present a new method to analyse simultaneous Topography and RECognition Atomic Force Microscopy data such that it becomes possible to measure single molecule binding rates of surface bound proteins. We have validated this method on a model system comprising a S-layer surface modified with Strep-tagII for binding sites and strep-tactin bound to an Atomic Force Microscope tip through a flexible Poly-Ethylene-Glycol linker. At larger distances, the binding rate is limited by the linker, which limits the diffusion of the strep-tactin molecule, but at lateral distances below 3 nm, the binding rate is solely determined by the intrinsic molecular characteristics and the surface geometry and chemistry of the system. In this regime, Kon as determined from single molecule TREC data is in agreement with Kon determined using traditional biochemical methods.

Cantilever dynamics in Heterodyne Force Microscopy.

Experiments in Heterodyne Force Microscopy (HFM) show the possibility to image deeply buried nanoparticles below a surface. However, the contrast mechanism and the motion of the cantilever, which detects the subsurface signal, are not yet understood. We present a numerical study of the cantilever motion in different HFM modes using realistic tip-sample interactions. The results provide information on the sensitivity to the heterodyne signal. The parameters in our calculations are chosen as closely as possible to the situation in real experiments to enable (future) comparisons based on our predictions. In HFM both the tip and the sample are excited at slightly different ultrasonic frequencies such that a difference frequency is generated that can contain subsurface information. We calculate the amplitude and phase of the difference frequency generated by the motion of the cantilever. The amplitude shows a local maximum in the attractive Van-der-Waals regime and an even higher plateau in the repulsive regime. The phase shifts 180° or 90°, depending on the mode of operation. Finally, we observe oscillations in both the amplitude and the phase of the difference frequency, which are caused by a shift of the resonance frequency of the cantilever and an involved transient behavior.

Subsurface-AFM: sensitivity to the heterodyne signal.

Applying heterodyne force microscopy (HFM), it has been impressively demonstrated that it is possible to obtain subsurface information: 20 nm large gold nanoparticles that were buried 500 nm deep have been imaged. It is the heterodyne signal that contains the subsurface information. We elucidate, both theoretically and experimentally, the sensitivity to the heterodyne signal as a function of the tip-sample distance. This is crucial information for experiments as the distance, and therefore the sensitivity, is tunable. We show that the amplitude of the heterodyne signal has a local maximum in the attractive part of the tip-sample interaction, before it surprisingly reaches an even higher plateau, when the tip-sample interaction is repulsive. This can only be explained by a non-decreasing amplitude of the ultrasonic motion of the tip, although it is in full contact with the surface. We confirm this counterintuitive tip behavior experimentally even on a hard surface like silicon.

Subsurface atomic force microscopy: towards a quantitative understanding.

Recent experiments in the field of subsurface atomic force microscopy have demonstrated that it is possible to nondestructively image micro- and even nanoparticles that are embedded significantly deep within the bulk of a sample. In order to get insights into the contrast formation mechanism, we performed a finite element analysis and an analytical study, in which we calculated the amplitude and phase variation on the surface of an ultrasound wave that has traveled through the sample. Our calculations were performed as closely as possible to the situation in the experiments to enable a (future) comparison based on our predictions. We show that Rayleigh scattering of acoustic waves accounts for the measured contrast and we verify the characteristic Rayleigh dependences. The numerical results show that the contrast is independent of the depth at which a particle is buried, whereas the analytical study reveals a 1/depth dependence. In addition, we find a large deviation in the width of the particle in the contrast at the surface when applying the numerical or the analytical calculation respectively. These results indicate the importance of both the reflections of sound waves at the sample interfaces and bulk damping, as both are treated differently in our two models.

Determination of the size distribution of blood microparticles directly in plasma using atomic force microscopy and microfluidics.

Microparticles, also known as microvesicles, found in blood plasma, urine, and most other body fluids, may serve as valuable biomarkers of diseases such as cardiovascular diseases, systemic inflammatory disease, thrombosis, and cancer. Unfortunately, the detection and quantification of microparticles are hampered by the microscopic size of these particles and their relatively low abundance in blood plasma. The use of a combination of microfluidics and atomic force microscopy to detect microparticles in blood plasma circumvents both problems. In this study, capture of a specific subset of microparticles directly from blood plasma on antibody-coated mica surface is demonstrated. The described method excludes isolation and washing steps to prepare microparticles, improves the detection sensitivity, and yields the size distribution of the captured particles. The majority of the captured particles have a size ranging from 30 to 90 nm, which is in good agreement with prior results obtained with microparticles immediately isolated from fresh plasma. Furthermore, the qualitative shape of the size distribution of microparticles is shown not to be affected by high-speed centrifugation or the use of the microfluidic circuit, demonstrating the relative stable nature of microparticles ex vivo.

Magnetic resonance force microscopy of paramagnetic electron spins at millikelvin temperatures.

Magnetic resonance force microscopy (MRFM) is a powerful technique to detect a small number of spins that relies on force detection by an ultrasoft magnetically tipped cantilever and selective magnetic resonance manipulation of the spins. MRFM would greatly benefit from ultralow temperature operation, because of lower thermomechanical noise and increased thermal spin polarization. Here we demonstrate MRFM operation at temperatures as low as 30 mK, thanks to a recently developed superconducting quantum interference device (SQUID)-based cantilever detection technique, which avoids cantilever overheating. In our experiment, we detect dangling bond paramagnetic centres on a silicon surface down to millikelvin temperatures. Fluctuations of such defects are supposedly linked to 1/f magnetic noise and decoherence in SQUIDs, as well as in several superconducting and single spin qubits. We find evidence that spin diffusion has a key role in the low-temperature spin dynamics.

MEMS-based high speed scanning probe microscopy.

The high speed performance of a scanning probe microscope (SPM) is improved if a microelectromechanical systems (MEMS) device is employed for the out-of-plane scanning motion. We have carried out experiments with MEMS high-speed z-scanners (189 kHz fundamental resonance frequency) in both atomic force microscope and scanning tunneling microscope modes. The experiments show that with the current MEMS z-scanner, lateral tip speeds of 5 mm/s can be achieved with full feedback on surfaces with significant roughness. The improvement in scan speed, obtained with MEMS scanners, increases the possibilities for SPM observations of dynamic processes. Even higher speed MEMS scanners with fundamental resonance frequencies in excess of a megahertz are currently under development.

A compact multipurpose nanomanipulator for use inside a scanning electron microscope.

A compact, two-stage nanomanipulator was designed and built for use inside a scanning electron microscope. It consists of a fine stage employing piezostacks that provide a 15 microm range in three dimensions and a coarse stage based on commercially available stick-slip motors. Besides the fabrication of enhanced probes for scanning probe microscopy and the enhancement of electron field emitters, other novel manipulation processes were developed, such as locating, picking up, and positioning small nanostructures with an accuracy of approximately 10 nm. In combination with in situ I-V experiments, welding, and etching, this results in a multipurpose nanofactory, enabling a new range of experiments.

MEMS-based fast scanning probe microscopes.

Scanning probe microscopy is a frequently used nanometer-scale surface investigation technique. Unfortunately, its applicability is limited by the relatively low image acquisition speed, typically seconds to minutes per image. Higher imaging speeds are desirable for rapid inspection of samples and for the study of a range of dynamic surface processes, such as catalysis and crystal growth. We have designed a new high-speed scanning probe microscope (SPM) based on micro-electro mechanical systems (MEMS). MEMS are small, typically micrometer size devices that can be designed to perform the scanning motion required in an SPM system. These devices can be optimized to have high resonance frequencies (up to the MHz range) and have very low mass (10(-11)kg). Therefore, MEMS can perform fast scanning motion without exciting resonances in the mechanical loop of the SPM, and hence scan the surface without causing the image distortion from which conventional piezo scanners suffer. We have designed a MEMS z-scanner which we have integrated in commercial AFM (atomic force microscope) and STM (scanning tunneling microscope) setups. We show the first successful AFM experiments.

Atomic force microscopy: a novel approach to the detection of nanosized blood microparticles.

BACKGROUND: Microparticles (MPs) are small vesicles released from cells of different origin, bearing surface antigens from parental cells. Elevated numbers of blood MPs have been reported in (cardio)vascular disorders and cancer. Most of these MPs are derived from platelets. OBJECTIVES: To investigate whether atomic force microscopy (AFM) can be used to detect platelet-derived MPs and to define their size distribution. METHODS: Blood MPs isolated from seven blood donors and three cancer patients were immobilized on a modified mica surface coated with an antibody against CD41 prior to AFM imaging. AFM was performed in liquid-tapping mode to detect CD41-positive MPs. In parallel, numbers of CD41-positive MPs were measured using flow cytometry. Mouse IgG1 isotype control was used as a negative control. RESULTS: AFM topography measurements of the number of CD41-positive MPs were reproducible (coefficient of variation=16%). Assuming a spherical shape of unbound MPs, the calculated diameter of CD41-positive MPs (dsph) ranged from 10 to 475 nm (mean: 67.5+/-26.5 nm) and from 5 to 204 nm (mean: 51.4+/-14.9 nm) in blood donors and cancer patients, respectively. Numbers of CD41-positive MPs were 1000-fold higher than those measured by flow cytometry (3-702x10(9) L(-1) plasma vs. 11-626x10(6) L(-1) plasma). After filtration of isolated MPs through a 0.22-microm filter, CD41-positive MPs were still detectable in the filtrate by AFM (mean dsph: 37.2+/-11.6 nm), but not by flow cytometry. CONCLUSIONS: AFM provides a novel method for the sensitive detection of defined subsets of MPs in the nanosize range, far below the lower limit of what can be measured by conventional flow cytometry.

Isotope-selective detection and imaging of organic nanolayers.

Magnetic resonance force microscopy (MRFM) makes use of the spectroscopic nature of magnetic resonance to add unambiguous elemental selectivity to scanning probe microscopy. We show isotopic selectivity of MRFM for three nuclei, (1)H, (31)P, and (13)C, in organic materials. We also detect a roughly 1 nm thick layer of naturally occurring adsorbates on a gold surface by measuring the magnetic resonance signal of the hydrogen contained in the layer. Finally, we detect the signal from hydrogen present on a carbon nanotube and use it to perform a three-dimensional magnetic resonance image of the 10 nm diameter object.

The electron conduction of photosynthetic protein complexes embedded in a membrane.

The conductivity of two photosynthetic protein-pigment complexes, a light harvesting 2 complex and a reaction center, was measured with an atomic force microscope capable of performing electrical measurements. Current-voltage measurements were performed on complexes embedded in their natural environment. Embedding the complexes in lipid bilayers made it possible to discuss the different conduction behaviors of the two complexes in light of their atomic structure.