Silicon Nitride Cantilever Research Articles

Fabrication of near‐field optical apertures in aluminium by a highly selective corrosion process in the evanescent field

A simple, one-step process to fabricate high-quality apertures for scanning near-field optical microscope probes based on aluminium-coated silicon nitride cantilevers is presented. A thin evanescent optical field at a glass-water interface was used to heat the aluminium at the tip apex due to light absorption. The heat induced a breakdown of the passivating oxide layer and local corrosion of the metal, which selectively exposed the front-most part of the probe tip from the aluminium. Apertures with a protruding silicon nitride tip up to 72 nm in height were fabricated. The height of the protrusion was controlled by the extent of the evanescent field, whereas the diameter depended on the geometry of the probe substrate. The corrosion process proved to be self-terminating, yielding highly reproducible tip heights. Near-field optical resolution in a transmission mode of 85 nm was demonstrated.

Self-sensing and self-actuating probe based on quartz tuning fork combined with microfabricated cantilever for dynamic mode atomic force microscopy

A novel probe based on a commercial quartz tuning fork and a microfabricated cantilever is presented. The U-shaped cantilever with a monolithic tip is combined with the tuning fork in a symmetrical arrangement, such that each of the two legs of the cantilever is fixed to one of the prongs of the tuning fork. The tuning fork is used as an oscillatory force sensor. Its frequency and amplitude governs that of the vibrating tip, while the cantilever determines the spring constant of the whole probe. Several probes with different cantilevers in terms of material and spring constant are studied. A typical silicon nitride cantilever has a spring constant of 0.1 N/m and those made of silicon have 1.2–319 N/m. Monoatomic terraces of highly oriented pyrolytic graphite (HOPG) was successfully imaged in the intermittent contact mode with the silicon probes. Both types of probes are suited for batch fabrication and assembling and, therefore enlarges the applications of the tuning fork based AFM.

Symmetrically arranged quartz tuning fork with soft cantilever for intermittent contact mode atomic force microscopy

A self-sensing and -actuating probe for dynamic mode atomic force microscopy (AFM) based on a commercial quartz tuning fork and a microfabricated cantilever is presented. The U-shaped cantilever, exhibiting a sharp tip, is combined with the tuning fork in a symmetrical arrangement, such that each of the two legs of the cantilever is fixed to one of the prongs of the tuning fork. The tuning fork is used as an oscillatory force sensor. Its frequency and amplitude govern that of the tip vibration, while the cantilever determines the spring constant of the whole probe. The frequency of the tip vibration for AFM operations can be much higher than the resonance frequency of the cantilever. A probe comprising a silicon nitride cantilever (0.1 N/m) is used to image monoatomic terraces of graphite in the intermittent contact mode. A much softer cantilever (0.01 N/m) is used to analyze the topography of a microelectronic chip in the same mode. Moreover, a bacterial surface layer hexagonally packed intermediate layer of Deinococcus radiodurans is imaged in a buffer solution. The tip vibration was again generated by the tuning fork while the sample interaction was measured using the standard optical detection scheme in this experiment. These probes are suited for batch fabrication and assembly and, therefore, enlarge the applications for the tuning fork based AFM.

Chemical Force Microscopy Investigation of Phosphate Adsorption on the Surfaces of Iron(III) Oxyhydroxide Particles

Phosphate-modified AFM tips were prepared by the deposition of self-assembled monolayers (SAMs) of bis(11-thioundecyl) phosphate on Au-coated silicon nitride cantilevers. The properties of the PO 2H-terminated SAMs were investigated by studying the pH-dependent force interactions of the tips with phosphate- and carboxylic acid-terminated SAM control surfaces. The PO 2H functional groups had a p K a of ≈5.0. A chemical force microscopy (CFM) study was conducted on the interactions between the probes and the surfaces of hydrous ferric oxide particles prepared in our laboratory by hydrolytic precipitation from FeCl 3. The forces between PO 2H probes and the hydrous ferric oxide surfaces were seen to exhibit a strong pH dependence, with maximum attractive forces occurring for pH values between 5 and 8. The effects of postprecipitation of the hydrous ferric oxide colloids with orthophosphate, H 2PO 4 −, dimethylphosphate, (CH 3O) 2PO 2H (DMP), and tannic acid (TA) on the adhesive interactions between the PO 2H tips and the solids were also investigated. Attenuated total reflectance infrared spectroscopy (ATR-IR) was used to verify the presence of surface-adsorbed species and zeta potentiometric measurements to determine surface charge on the colloids. We show that the method of chemical force titration using phosphate-terminated tips can differentiate between these various colloids and that it shows promise as a general method for studying this environmentally important class of compounds.

The Influence of Fatty Acids and Humidity on Friction and Adhesion of Hydrophilic Polymer Surfaces

Monolayers of saturated fatty acids of different chain lengths and of 9-cis-octadecenoic acid were physisorbed onto regenerated cellulose surfaces to study their effect on friction and adhesion. Lateral and normal force measurements on these surfaces were carried out at different humidities using an atomic force microscope with chemically functionalized silicon nitride cantilevers. Friction and adhesion of clean cellulose increased significantly with humidity. Adhesion forces at high humidity were predicted well by theory that accounted for the effect of the Laplace pressure due to capillary condensation. The magnitude of friction and adhesion and their dependence on humidity decreased with increasing hydrophobicity of the contacting surfaces. Friction of cellulose surfaces impregnated with different saturated fatty acids decreased sharply from a high level to a low level at a carbon chain length above 14 carbon atoms. Contact angle data indicated that only saturated fatty acids with 16 carbon atoms or more in the carbon chain formed vertically oriented monolayers on cellulose. Our results suggest that friction of hydrophilic polymer surfaces under ambient conditions is greatly influenced by capillary condensation. Furthermore, lubrication by fatty acids is achieved through the formation of vertically oriented, hydrophobic monolayers that can withstand the normal and shear stresses during sliding and increase the hydrophobicity of the polymer surface, thereby decreasing the degree of capillary condensation.

Subwavelength-sized aperture fabrication in aluminum by a self-terminated corrosion process in the evanescent field

We present a simple, one-step process to fabricate apertures of high quality for scanning near-field optical microscope probes based on aluminum-coated silicon-nitride cantilevers. An evanescent optical field at the glass–water interface is used to heat up the aluminum at the tip apex due to light absorption. The heat induces breakdown of the passivating oxide layer and corrosion of the metal. Apertures with a protruding silicon-nitride tip of up to 30 nm height and minimal diameter of 38 nm are fabricated. The diameter is predefined by the lateral dimension of the silicon-nitride tip while the tip height is controlled by the penetration depth of the evanescent field. The corrosion process proves to be self-terminating, yielding highly reproducible tip heights. Near-field optical resolution in the transmission mode of 85 nm is demonstrated.

Mapping of lateral vibration of the tip in atomic force microscopy at the torsional resonance of the cantilever

Lateral vibration of the tip in atomic force microscopy was mapped at the torsional resonance of the cantilever by attaching a shear piezo element at the base of the cantilever or under the sample. Fixed frequency excitation and self-excitation of torsional motion were implemented. The lateral vibration utilized as measured by an optical lever was in the order of 10 pm to 3 nm, and its frequency approximately 450 kHz for a contact-mode silicon nitride cantilever. The amplitude and phase of the torsional motion of the cantilever was measured by a lock-in-amplifier or a rectifier and plotted in x and y as the sample was raster scanned. The imaging technique gave contrast between graphite terraces, self-assembled monolayer domains, silicon and silicon dioxide, graphite and mica. Changing contrast was observed as silicon islands oxidized in atmosphere, showing that the imaging technique can detect change in lateral tip mobility due to changes occurring near the surface. Torsional self-excitation showed nanometric features of self-assembled monolayer islands due to different lateral dissipation. Dependence of torsional resonance frequency on excitation amplitude, and contrast change due to driving frequency around resonance were observed.

Pull-off forces measured between hexadecanethiol self-assembled monolayers in air using an atomic force microscope: analysis of surface free energy

The pull-off forces were measured between hexadecanethiol monolayers, self-assembled on gold-coated silicon nitride cantilever tip and silicon wafer, using atomic force microscopy (AFM). The blind tip reconstruction technique was used for determination of the curvature of the AFM tip. The measured pull-off force value remained practically unaffected by a variation of the maximum applied load in a range of 5–80 nN. This result suggests that the use of continuum elastic contact mechanics in the analysis of AFM pull-off force measurements is not as straightforward as usually assumed in the literature reports on similar systems. The surface free energy of hexadecanethiol monolayer on a gold film of γ = 24–27 mJ/m2 was calculated based on the pull-off forces (F), measured using R = 60–80 nm radius tips, and next applying the Derjaguin approximation: F = 4πRγ. These γ-values were found to match the surface free energy value calculated from contact angle data and using Lewis acid–base interfacial free energy theory.

A study of friction by carbon nanotube tip

The carbon nanotube (CNT) probe, where a multi-walled (MW) CNT is attached onto the tip apex of a commercial silicon nitride cantilever, is applied to study friction on the nanometer scale using contact atomic force microscope (AFM). The friction versus load curve using CNT tip shows a completely different behavior from that of conventional tip, which is ascribed to the unique shape of CNT. In addition, strong scanning length dependency of the friction force is found due to the deformation of CNT.

Single cell detection with micromechanical oscillators

The ability to detect small amounts of materials, especially pathogenic bacteria, is important for medical diagnostics and for monitoring the food supply. Engineered micro- and nanomechanical systems can serve as multifunctional, highly sensitive, immunospecific biological detectors. We present a resonant frequency-based mass sensor, comprised of low-stress silicon nitride cantilever beams for the detection of Escherichia coli (E. coli)-cell-antibody binding events with detection sensitivity down to a single cell. The binding events involved the interaction between anti-E. coli O157:H7 antibodies immobilized on a cantilever beam and the O157 antigen present on the surface of pathogenic E. coli O157:H7. Additional mass loading from the specific binding of the E. coli cells was detected by measuring a resonant frequency shift of the micromechanical oscillator. In air, where considerable damping occurs, our device mass sensitivities for a 15 μm and 25 μm long beam were 1.1 Hz/fg and 7.1 Hz/fg, respectively. In both cases, utilizing thermal and ambient noise as a driving mechanism, the sensor was highly effective in detecting immobilized anti-E. coli antibody monolayer assemblies, as well as single E. coli cells. Our results suggest that tailoring of oscillator dimensions is a feasible approach for sensitivity enhancement of resonant mass sensors.

Quantitative surface stress measurements using a microcantilever

A method for calculating the surface stress associated with the deflection of a micromechanical cantilever is presented. This method overcomes some of the limitations associated with Stoney’s formula by circumventing the need to know the cantilever’s Young’s modulus, which can have a high level of uncertainty, especially for silicon nitride cantilevers. The surface stress is calculated using readily measurable cantilever properties, such as its geometry, spring constant, and deflection. The method is applicable to both rectangular and triangular cantilevers. A calibration of the deflection measurement is also presented. The surface stress measurement is accurate to within 4%–7%.

Characterisation of adhesional properties of lactose carriers using atomic force microscopy.

The atomic force microscopy (AFM) colloid probe technique was investigated as a method for the characterisation of adhesional properties of pharmaceutical powder surfaces. Lactose carriers used in dry powder inhaler (DPI) formulations were chosen for investigation since adhesion between the carrier surface and drug particles has been proposed to affect the dispersion of drug particles. Individual adhesion forces were determined by measuring the detachment forces in air between the colloid probe and the lactose particle surface. The colloid probe consisted of a silica sphere (10 microm diameter) attached to a V-shaped silicon nitride cantilever (spring constant, k=0.42 N/m). Adhesion forces were calculated from individual force-distance curves using Hooke's Law. Individual forces measured at various adhesion sites were observed to be reproducible and stable over 10 min (coefficient of variation, CV below 5%). The adhesion force distribution determined from measurements at multiple sites (n>50) on each sample followed a log-normal relationship (regression coefficient, r(2) ranged between 0.95 and 0.99). This enabled characterisation in terms of the geometric mean adhesion force and a geometric standard deviation (GSD). Significant differences (P<0.001) in adhesion force were observed between samples, ranging from 37.47+/-1.95 to 117.48+/-2.20 nN. This study demonstrates the suitability of AFM as sensitive technique for the characterisation of adhesional properties of pharmaceutical particles.

A nondestructive technique for determining the spring constant of atomic force microscope cantilevers

We present a simple, accurate, and nondestructive method to determine cantilever spring constants by measuring the resonant frequency before and after the addition of a thin gold layer. The method for resonating the cantilevers uses electrostatic force modulation, which has been described for conductive cantilevers, but we demonstrate it can also be applied to silicon nitride cantilevers. The variations in spring constant for cantilevers of the same type across the same wafer are also explored.

Analysis of Atomic Force Curve Data for Mapping of Surface Properties in Water

This paper presents an analysis of atomic force versus distance curves for a silicon nitride probe and a silicon sample immersed in water. A custom-built atomic force microscope (AFM) was adapted for working in water by building a water cell from a liquid drop caught between a glass lamella fixed on the top of the cantilever base and the sample surface. An algorithm for processing of force curve data for long- and short-range forces is described. The force curve data taken for a sample consisting of a silicon wafer Si(111) patterned with V-shaped grooves and a silicon nitride cantilever in water were digitally acquired and automatically processed for mapping of surface properties. A weak repulsive double layer force with no relevant dependence on sample topography was observed on the force curves taken during approach movement of the cantilever. On the other hand, the attractive hydration force showed a strong dependence on the sample topography. Large hydration force values were noticed on the inclined faces of the V-shaped grooves while small hydration force values were noticed outside the grooves. The result was explained by the dependence of the tip curvature radius at the contact region on the tilt of the sample surface.

Adsorption-Induced Failure Modes of Thin-Film Resonators

ABSTRACTThe mechanical and resonant properties of thin film resonators are influenced by the surrounding environment. Adsorption- and surface oxidation-induced stiffening effect was observed on silicon nitride and silicon carbide cantilever beams. The resonance frequency increased logarithmically in time upon exposure to ambient air. The variations of surface stress and spring constant of the SiNx cantilever beam were calculated. Further oxynitride formation on the surface increased the stability of the resonators. The shock response of the structures was studied in various environments. The resonance frequency abruptly dropped due to cracking of the absorbed surface layer, than recovered logarithmically. The initial drop and the recovery rate is environment dependant. Humidity increased, while argon and nitrogen rich environments mitigated the degrading effects. The SiCx is more inert to the environmental effects and proved to be a promising candidate as structural material in resonant MEMS devices.

Chemical sensing in Fourier space

Chemical sensing using optical diffraction from an array of microcantilevers is demonstrated. Properly fashioned arrays of micromachined silicon-nitride cantilevers containing embedded deformable diffraction gratings are functionalized with chemically selective coatings. Adsorption of specific molecules on the cantilever leads to bending, which changes the diffraction pattern of a laser beam reflecting off the array. Quantitative chemical information can be obtained by monitoring the displacement of diffraction peaks as a function of analyte exposure.

Changes in surface stress at the liquid/solid interface measured with a microcantilever

The bending of microfabricated silicon nitride cantilevers was used to determine surface stress changes at solid–liquid interfaces. The radius of curvature of the bent cantilever is directly proportional to changes in the differential surface stress between its opposite sides. To demonstrate the possibilities and limitations of the technique, cantilevers coated on both sides with gold and densely packed monolayers of different thiols were put in a constant flow of aqueous electrolyte solution and the deflection was measured using a optical lever technique. Changes in the surface stress for the different thiol monolayers due to specific proton adsorption are presented. Possible applications and improvements of this technique are discussed.

Effect of Sample Topography on Adhesive Force in Atomic Force Spectroscopy Measurements in Air

The effect of local curvature of a sample surface on capillary and interface tension adhesion forces of the water meniscus formed between the AFM tip and sample in air is demonstrated both theoretically and experimentally. We propose an analytical solution for capillary and tension adhesive force derived from approximation of the thermodynamic equilibrium of a symmetric water meniscus formed at the tip−sample contact region. It is shown that the sample local curvature strongly affects the water meniscus geometry and the adhesion force. Compared to the force computed for a flat sample surface, the theoretical model predicts a larger/smaller adhesive force for a concave/convex local curvature. Our theoretical predictions were confirmed by experiment. Atomic force spectroscopy measurements were performed for a silicon nitride cantilever and a standard sample of platinum-covered quartz patterned with 1.5 × 1.5 μm square, 20 nm deep pits. Maps of sample surface topography and adhesive force showed a much larger force at the bottom of the pit edge, where the local curvature was concave. This was contrasted with a much smaller force observed at the top of the pit edge, where the local curvature was convex.

Quality factors in micron- and submicron-thick cantilevers

Micromechanical cantilevers are commonly used for detection of small forces in microelectromechanical sensors (e.g., accelerometers) and in scientific instruments (e.g., atomic force microscopes). A fundamental limit to the detection of small forces is imposed by thermomechanical noise, the mechanical analog of Johnson noise, which is governed by dissipation of mechanical energy. This paper reports on measurements of the mechanical quality factor Q for arrays of silicon-nitride, polysilicon, and single-crystal silicon cantilevers. By studying the dependence of Q on cantilever material, geometry, and surface treatments, significant insight into dissipation mechanisms has been obtained. For submicron-thick cantilevers, Q is found to decrease with decreasing cantilever thickness, indicating surface loss mechanisms. For single-crystal silicon cantilevers, significant increase in room temperature Q is obtained after 700/spl deg/C heat treatment in either N/sub 2/ Or forming gas. At low temperatures, silicon cantilevers exhibit a minimum in Q at approximately 135 K, possibly due to a surface-related relaxation process. Thermoelastic dissipation is not a factor for submicron-thick cantilevers, but is shown to be significant for silicon-nitride cantilevers as thin as 2.3 /spl mu/m.

Scanning gate spectroscopy on nanoclusters

A gated probe for scanning tunneling microscopy (STM) has been developed. The probe extends normal STM operations by means of an additional electrode fabricated next to the tunneling tip. The extra electrode does not make contact with the sample and can be used as a gate. We report on the recipe used for fabricating the tunneling tip and the gate electrode on a silicon nitride cantilever. We demonstrate the functioning of the scanning gate probes by performing single-electron tunneling spectroscopy on 20-nm-gold clusters for different gate voltages.