Sharp Atomic Force Microscopy Tips Research Articles

Enhancing the precision of 3D sidewall measurements of photoresist using atomic force microscopy with a tip-tilting technique

A key issue associated with advanced lithography techniques for semiconductor-device manufacturing is the reduction in the sidewall roughness of photoresist line patterns, known as line-edge roughness (LER). We have developed a technique for measuring the sidewall of the resist pattern using atomic force microscopy (AFM) that enables three-dimensional (3D), high-resolution, low-noise, and nondestructive measurements. Conventional LER measurement technology using scanning electron microscopy (SEM) causes shrinkage of the resist pattern due to electron-beam (EB) exposure, whereas our new AFM technique can in principle avoid EB-induced shrinkage. This AFM technology is capable of 3D measurements because it employs a tip-tilting mechanism that enables the sharp AFM tip to scan the vertical sidewalls, which is difficult for a conventional AFM technique. In addition, laser interferometers are equipped for the measurement of the AFM tip displacement, which yields high-resolution, high-accuracy, and low-noise results. This technology overcomes issues such as low resolution, noise, and destructive measurements that afflict conventional SEM measurements. In addition, it enables observations and quantitative analyses of the 3D sidewall roughness. For example, in the present experiment, we observed that grain shapes (several tens of nm in size) were formed randomly on the resist sidewall and that there were almost no footing shapes. By analyzing the sidewall profiles with a height resolution of 1 nm, we obtain the roughness (self-affine fractal) parameters at each height. This AFM-based resist sidewall measurement technique can, thus, provide important insights into resist patterning and related process technologies for next-generation semiconductor-device manufacturing.

Variation of the frictional anisotropy on ventral scales of snakes caused by nanoscale steps

The ventral scales of most snakes feature micron-sized fibril structures with nanoscale steps oriented towards the snake’s tail. We examined these structures by microtribometry as well as atomic force microscopy (AFM) and observed that the nanoscale steps of the micro-fibrils cause a frictional anisotropy, which varies along the snake’s body in dependence of the height of the nanoscale steps. A significant frictional behavior is detected when a sharp AFM tip scans the nanoscale steps up or down. Larger friction peaks appear during upward scans (tail to head direction), while considerably lower peaks are observed for downward scans (head to tail direction). This effect causes a frictional anisotropy on the nanoscale, i.e. friction along the head to tail direction is lower than in the opposite direction. The overall effect increases linearly with the step height of the micro-fibrils. Although the step heights are different for each snake, the general step height distribution along the body of the examined snakes follows a common pattern. The frictional anisotropy, induced by the step height distribution, is largest close to the tail, intermediate in the middle, and lower close to the head. This common distribution of frictional anisotropy suggests that snakes even optimized nanoscale features like the height of micro-fibrils through evolution in order to achieve optimal friction performance for locomotion. Finally, ventral snake scales are replicated by imprinting their micro-fibril structures into a polymer. As the natural prototype, the artificial surface exhibits frictional anisotropy in dependence of the respective step height. This feature is of high interest for the design of tribological surfaces with artificial frictional anisotropy.

Nanoscale friction and wearing of octadecyltrichlorosilane covered silicon surface

Silicon wafers were silanized by plasma hydroxylation and chemical vapour deposition of octadecyltrichlorosilane [OTS, CH3(CH2)17SiCl3]. Then, the OTS covered silicon samples were used in atomic force microscopy (AFM) measurements of wearing and friction at nanoscale. Wearing experiment performed by 1000 cycles of forwards and backwards movements of sharp AFM tip revealed formation of a wearing track with a depth that was much smaller than the thickness of OTS coating, which confirmed a very good wearing property of OTS coating. Friction versus normal loading force experiments performed with the same AFM tip revealed a nonlinear dependence of friction force on the normal loading force in agreement with prediction of Bowden and Tabor’s theory of friction and an increase of friction with the moving speed. Dependence of friction force on the sliding speed is attributed to a transfer of kinetic energy from the moving AFM tip to individual molecules of OTS coating.

Mechanical properties of Ropaque hollow nanoparticles

The elastic properties and strength upon compression of commercial Ropaque polystyrene hollow particles were investigated by atomic force microscopy (AFM). These particles are commonly used in paints as opacifying agents, as their internal air void effectively scatters light. A sharp AFM tip was used to apply a point load to the particle surface, and increased to probe both the elastic and plastic deformation of the shell, and then further until the shell broke. For small deformations, the deformation increased linearly with applied force. The Young's modulus was calculated by accounting for the effect of the rigid substrate, and compared to the modulus obtained from the Reissner and Hertz models. The minimum stress needed to destroy the integrity of the shell was extracted and found to be smaller than or close to that of silica hollow particles with different shell thickness tested in the literature.

Measured pulmonary arterial tissue stiffness is highly sensitive to AFM indenter dimensions

The mechanical properties of pulmonary tissues are important in normal function and the development of diseases such as pulmonary arterial hypertension. Hence it is critical to measure lung tissue micromechanical properties as accurately as possible in order to gain insight into the normal and pathological range of tissue stiffness associated with development, aging and disease processes. In this study, we used atomic force microscopy (AFM) micro-indentation to characterize the Young's modulus of small human pulmonary arteries (vessel diameter less than 100µm), and examined the influence of AFM tip geometry and diameter, lung tissue section thickness and the range of working force applied to the sample on the measured modulus. We observed a significant increase of the measured Young's modulus of pulmonary vessels (one order of magnitude) associated with the use of a pyramidal sharp AFM tips (20nm radius), compared to two larger spherical tips (1 and 2.5µm radius) which generated statistically indistinguishable results. The effect of tissue section thickness (ranging from 10 to 50 μm) on the measured elastic modulus was relatively smaller (<1-fold), but resulted in a significant increase in measured elastic modulus for the thinnest sections (10 μm) relative to the thicker (20 and 50 μm) sections. We also found that the measured elastic modulus depends modestly (again <1-fold), but significantly, on the magnitude of force applied, but only on thick (50 μm) and not thin (10 μm) tissue sections. Taken together these results demonstrate a dominant effect of indenter shape/radius on the measured elastic modulus of pulmonary arterial tissues, with lesser effects of tissue thickness and applied force. The results of this study highlight the importance of AFM parameter selection for accurate characterization of pulmonary arterial tissue mechanical properties, and allow for comparison of literature values for lung vessel tissue mechanical properties measured by AFM across a range of indenter and indentation parameters.

Understanding the plasmonics of nanostructured atomic force microscopy tips

Structured metallic tips are increasingly important for optical spectroscopies such as tip-enhanced Raman spectroscopy, with plasmonic resonances frequently cited as a mechanism for electric field enhancement. We probe the local optical response of sharp and spherical-tipped atomic force microscopy (AFM) tips using a scanning hyperspectral imaging technique to identify the plasmonic behaviour. Localised surface plasmon resonances which radiatively couple with far-field light are found only for spherical AFM tips, with little response for sharp AFM tips, in agreement with numerical simulations of the near-field response. The precise tip geometry is thus crucial for plasmon-enhanced spectroscopies, and the typical sharp cones are not preferred.

Nanomechanical and topographical imaging of living cells by atomic force microscopy with colloidal probes.

Atomic Force Microscopy (AFM) has a great potential as a tool to characterize mechanical and morphological properties of living cells; these properties have been shown to correlate with cells' fate and patho-physiological state in view of the development of novel early-diagnostic strategies. Although several reports have described experimental and technical approaches for the characterization of cellular elasticity by means of AFM, a robust and commonly accepted methodology is still lacking. Here, we show that micrometric spherical probes (also known as colloidal probes) are well suited for performing a combined topographic and mechanical analysis of living cells, with spatial resolution suitable for a complete and accurate mapping of cell morphological and elastic properties, and superior reliability and accuracy in the mechanical measurements with respect to conventional and widely used sharp AFM tips. We address a number of issues concerning the nanomechanical analysis, including the applicability of contact mechanical models and the impact of a constrained contact geometry on the measured Young's modulus (the finite-thickness effect). We have tested our protocol by imaging living PC12 and MDA-MB-231 cells, in order to demonstrate the importance of the correction of the finite-thickness effect and the change in Young's modulus induced by the action of a cytoskeleton-targeting drug.

Nanoscale stiffness topography reveals structure and mechanics of the transport barrier in intact nuclear pore complexes.

The nuclear pore complex (NPC) is the gate for transport between the cell nucleus and the cytoplasm. Small molecules cross the NPC by passive diffusion, but molecules larger than ~5 nm must bind to nuclear transport receptors to overcome a selective barrier within the NPC1. Whilst the structure and shape of the cytoplasmic ring of the NPC are relatively well characterized2-5, the selective barrier is situated deep within the central channel of the NPC and depends critically on unstructured nuclear pore proteins5,6, and is therefore not well understood. Here, we show that stiffness topography7 with sharp atomic force microscopy tips can generate nanoscale cross sections of the NPC. The cross sections reveal two distinct structures, a cytoplasmic ring and a central plug structure, which are consistent with the three-dimensional NPC structure derived from electron microscopy2-5. The central plug persists after reactivation of the transport cycle and resultant cargo release, indicating that the plug is an intrinsic part of the NPC barrier. Added nuclear transport receptors accumulate on the intact transport barrier and lead to a homogenization of the barrier stiffness. The observed nanomechanical properties in the NPC indicate the presence of a cohesive barrier to transport, and are quantitatively consistent with the presence of a central condensate of nuclear pore proteins in the NPC channel.

The Influence of Physical and Physiological Cues on Atomic Force Microscopy-Based Cell Stiffness Assessment

Atomic force microscopy provides a novel technique for differentiating the mechanical properties of various cell types. Cell elasticity is abundantly used to represent the structural strength of cells in different conditions. In this study, we are interested in whether physical or physiological cues affect cell elasticity in Atomic force microscopy (AFM)-based assessments. The physical cues include the geometry of the AFM tips, the indenting force and the operating temperature of the AFM. All of these cues show a significant influence on the cell elasticity assessment. Sharp AFM tips create a two-fold increase in the value of the effective Young’s modulus (Eeff) relative to that of the blunt tips. Higher indenting force at the same loading rate generates higher estimated cell elasticity. Increasing the operation temperature of the AFM leads to decreases in the cell stiffness because the structure of actin filaments becomes disorganized. The physiological cues include the presence of fetal bovine serum or extracellular matrix-coated surfaces, the culture passage number, and the culture density. Both fetal bovine serum and the extracellular matrix are critical for cells to maintain the integrity of actin filaments and consequently exhibit higher elasticity. Unlike primary cells, mouse kidney progenitor cells can be passaged and maintain their morphology and elasticity for a very long period without a senescence phenotype. Finally, cell elasticity increases with increasing culture density only in MDCK epithelial cells. In summary, for researchers who use AFM to assess cell elasticity, our results provide basic and significant information about the suitable selection of physical and physiological cues.

The Effect of the Endothelial Cell Cortex on Atomic Force Microscopy Measurements

We examined whether the presence of the cell cortex might explain, in part, why previous studies using atomic force microscopy (AFM) to measure cell modulus (E) gave higher values with sharp tips than for larger spherical tips. We confirmed these AFM findings in human umbilical vein endothelial cells (HUVEC) and Schlemm’s canal (SC) endothelial cells with AFM indentation ≤ 400 nm, two cell types with prominent cortices (312 ± 65 nm in HUVEC and 371 ± 91 nm in SC cells). With spherical tips, E (kPa) was 0.71 ± 0.16 in HUVEC and 0.94 ± 0.06 in SC cells. Much higher values of E were measured using sharp tips: 3.23 ± 0.54 in HUVEC and 6.67 ± 1.07 in SC cells. Previous explanations for this difference such as strain hardening or a substrate effect were shown to be inconsistent with our measurements. Finite element modeling studies showed that a stiff cell cortex could explain the results. In both cell types, Latrunculin-A greatly reduced E for sharp and rounded tips, and also reduced the ratio of the values measured with a sharp tip as compared to a rounded tip. Our results suggest that the cell cortex increases the apparent endothelial cell modulus considerably when measured using a sharp AFM tip.

The profile of a capillary liquid bridge between solid surfaces

Scanning force microscopy, such as atomic force microscopy (AFM) is complicated by the capillary force of a water meniscus formed in air between the probe tip and the sample. This small liquid bridge between the hydrophilic sample and the sharp AFM tip can be formed by capillary condensation from the vapor phase. We present an analytical model that describes the shape of the meniscus in which the pressure difference across the curved liquid air interface is taken into account. The analysis is based on a minimization of the liquid surface energy, together with the boundary condition of a given pressure drop across the surface as determined by the relative humidity of the vapor. The capillary forces that the wetting liquid exerts on the AFM tip are derived from the model. The resulting expressions can be used to describe arbitrary axial symmetric liquid air interfaces with nonzero total curvature, such as fluid bridges between two surfaces and droplets under a uniform force. The model illustrates some of the basic concepts of capillarity, such as surface tension forces and interfacial pressure drops.

Sharp High-Aspect-Ratio AFM Tips Fabricated by a Combination of Deep Reactive Ion Etching and Focused Ion Beam Techniques

The shape and dimensions of an atomic force microscope tip are crucial factors to obtain high resolution images at the nanoscale. When measuring samples with narrow trenches, inclined sidewalls near 90 degrees or nanoscaled structures, standard silicon atomic force microscopy (AFM) tips do not provide satisfactory results. We have combined deep reactive ion etching (DRIE) and focused ion beam (FIB) lithography techniques in order to produce probes with sharp rocket-shaped silicon AFM tips for high resolution imaging. The cantilevers were shaped and the bulk micromachining was performed using the same DRIE equipment. To improve the tip aspect ratio we used FIB nanolithography technique. The tips were tested on narrow silicon trenches and over biological samples showing a better resolution when compared with standard AFM tips, which enables nanocharacterization and nanometrology of high-aspect-ratio structures and nanoscaled biological elements to be completed, and provides an alternative to commercial high aspect ratio AFM tips.

Antibacterial action of dispersed single-walled carbon nanotubes on Escherichia coli and Bacillus subtilis investigated by atomic force microscopy

Single-walled carbon nanotubes (SWCNTs) exhibit strong antibacterial activities. Direct contact between bacterial cells and SWCNTs may likely induce cell damages. Therefore, the understanding of SWCNT-bacteria interactions is essential in order to develop novel SWCNT-based materials for their potential environmental, imaging, therapeutic, and military applications. In this preliminary study, we utilized atomic force microscopy (AFM) to monitor dynamic changes in cell morphology and mechanical properties of two typical bacterial models (gram-negative Escherichia coli and gram-positive Bacillus subtilis) upon incubation with SWCNTs. The results demonstrated that individually dispersed SWCNTs in solution develop nanotube networks on the cell surface, and then destroy the bacterial envelopes with leakage of the intracellular contents. The cell morphology changes observed on air dried samples are accompanied by an increase in cell surface roughness and a decrease in surface spring constant. To mimic the collision between SWCNTs and cells, a sharp AFM tip of 2 nm was chosen to introduce piercings on the cell surface. No clear physical damages were observed if the applied force was below 10 nN. Further analysis also indicates that a single collision between one nanotube and a bacterial cell is unlikely to introduce direct physical damage. Hence, the antibacterial activity of SWCNTs is the accumulation effect of large amount of nanotubes through interactions between SWCNT networks and bacterial cells.

Improving Accuracy of Sample Surface Topography by Atomic Force Microscopy

We describe method for improving the accuracy of sample surface topography by atomic force microscopy (AFM). It takes into account the effect of the AFM tip shape and image reconstruction on the acquired AFM images. The dilation effect due to the use of a finite-sized tip shape can be minimized by using a sharp AFM tip and scanning at the most symmetric direction of tip geometry. Reconstruction of AFM image could produce more accurate sample surface features. The method is useful to AFM measurement and is significant because AFM has become a fundamental tool in nanoscience and nanotechnology with multiple applications in a wide range of disciplines ranging from biology to physics and material science.

Electrostatic force spectroscopy on insulating surfaces: the effect of capacitiveinteraction

Scanning surface probes delivered from atomic force microscopy (AFM) are expected toinvestigate local electrostatic properties on insulating surfaces by forces. Electrostatic forcespectroscopy is especially suitable to clarify the capacitive interaction. In order to performit at a well-defined tip–surface separation, we developed a dynamic mode, in which thetip–surface separation is regulated by maintaining the cantilever oscillation amplitude withan active feedback, while the electrostatic force gradient is simultaneously detected with avariable resonant frequency shift. Using the method, it turns out that the quadraticdependence of the electrostatic force gradient on an applied bias observed on an insulatingAl2O3(0001) is comparable to those on a metallic Au(111). It results from the potential differencebetween the tip and the insulator surface being only one order smaller than that betweenthe tip and the metal surface despite the spacing between electrodes for the insulator being106 times larger than for the metal, because the capacitive interaction is modified primarilybetween the sharp AFM tip and the surface.

Hollow Silica Spheres: Synthesis and Mechanical Properties

Core-shell polystyrene-silica spheres with diameters of 800 nm and 1.9 microm were synthesized by soap-free emulsion and dispersion polymerization of the polystyrene core, respectively. The polystyrene spheres were used as templates for the synthesis of silica shells of tunable thickness employing the Stöber method [Graf et al. Langmuir 2003, 19, 6693]. The polystyrene template was removed by thermal decomposition at 500 degrees C, resulting in smooth silica shells of well-defined thickness (15-70 nm). The elastic response of these hollow spheres was probed by atomic force microscopy (AFM). A point load was applied to the particle surface through a sharp AFM tip, and successively increased until the shell broke. In agreement with the predictions of shell theory, for small deformations the deformation increased linearly with applied force. The Young's modulus (18 +/- 6 GPa) was about 4 times smaller than that of fused silica [Adachi and Sakka J. Mater. Sci. 1990, 25, 4732] but identical to that of bulk silica spheres (800 nm) synthesized by the Stöber method, indicating that it yields silica of lower density. The minimum force needed to irreversibly deform (buckle) the shell increased quadratically with shell thickness.

Volume of a Nanoscale Water Bridge

Water bridges formed through capillary condensation at nanoscale contacts first stretch and then break during contact rupture. Atomic force microscopy (AFM) pull-off experiments performed in air with hydrophilic tips and samples show that stretched nanoscopic water bridges are in mechanical equilibrium with the external pull-off force acting at the contact but not in thermodynamic equilibrium with the water vapor in air. The experimental findings are explained by a theoretical model that considers constant water volume and decrease of water meniscus curvature during meniscus stretching. The model predicts that the water bridge breakup distance will be roughly equal to the cubic root of the water bridge volume. A thermodynamic instability was noticed for large water bridges formed at the contact of a blunt AFM tip (curvature radius of 400 nm) with a flat sample. In this case, experiments showed rise and stabilization of the volume of the water at the contact in about 1 s. For sharp AFM tips (curvature radius below 50 nm), the experiments indicated that formation of stable water bridges occurs in a much shorter time (below 5 ms).

Novel Approach to Identifying Supersaturated Metastable Ambient Aerosol Particles

Atomic force microscopy (AFM) was used to determine the shape of fine and ultrafine ambient aerosol particles with sizes between 25 and 700 nm after soft landing on a solid substrate. The particles were collected in summer during daytime at a relative humidity around 50%. To avoid kinetically induced deformation, as previously observed using high-velocity sampling in impactors, the particles were collected on pore filters at very low face velocities (on the order of 10 cm/s). The shape of the collected particles was quantified in terms of their height and apparent diameter. The amount of broadening introduced by the pyramidal shape of the nonideally sharp AFM tips was calibrated using Latex reference spheres with a range of diameters. The height-to-diameter ratios, H/D, of the collected aerosol particles could be extracted from the measured data. Specified in terms of volume-equivalent (dry) diameters, Dv, the size selected frequency distributions of the H/Dv-ratios were found to be bimodal. A small mode centered at H/Dv = 1.0 +/- 0.1 is attributed to nonhygroscopic particles that retained their shape after deposition on the substrate. The large mode, with a peak at H/Dv = 0.65 +/- 0.05, reflects soft particles which were strongly deformed due to vertical collapse after deposition. The pronounced deformation suggests that these particles had previously experienced deliquescence and, when collected at a comparatively low humidity, were in a metastable, supersaturated aqueous state. After landing and indoor sample storage the water evaporated, resulting in minimum H/Dv-ratios as low as 0.45. The dried metastable fraction amounted to 81 +/- 12% in the size range 150 < Dv < 700 nm, and 79 +/- 10% for 50 < or = Dv < or = 150 nm, but only 26 +/- 10% for Dv < 50 nm. Comparison with recently reported data suggests that the observed metastable fraction is the same as the hygroscopic fraction identified by other means. The interpretation is further substantiated by a comparison of the size distributions of collected and airborne particles.

Atomic force microscopy-induced electric field in ferroelectric thin films

The use of atomic force microscopy (AFM) to tailor and image ferroelectric domains in the submicron and nanometer ranges is gaining increasing attention. Many applications have been developed that make use of the superhigh electric field generated by the sharp AFM tip in a local area. In this article, we derive an explicit expression for the AFM-induced electric field in a ferroelectric thin film. Based on a similar approach, we also obtain the depolarization field created by polarization charges using the Green function technique. Based on the expressions derived, the effects of the substrate are discussed.

Friction of ice measured using lateral force microscopy

The friction of nanometer thin ice films grown on mica substrates is investigated using atomic force microscopy (AFM). Friction was found to be of similar magnitude as the static friction of ice reported in macroscopic experiments. The possible existence of a lubricating film of water due to pressure melting, frictional heating, and surface premelting is discussed based on the experimental results using noncontact, contact, and lateral force microscopy. We conclude that AFM measures the dry friction of ice due to the low scan speed and the squeezing out of the water layer between the sharp AFM tip and the ice surface.