Nanoscale mapping of contact stiffness and damping by contact resonance atomic force microscopy

In this work, a new procedure is demonstrated to retrieve the conservative and dissipative contributions to contact resonance atomic force microscopy (CR-AFM) measurements from the contact resonance frequency and resonance amplitude. By simultaneously tracking the CR-AFM frequency and amplitude during contact AFM scanning, the contact stiffness and damping were mapped with nanoscale resolution on copper (Cu) interconnects and low-k dielectric materials. A detailed surface mechanical characterization of the two materials and their interfaces was performed in terms of elastic moduli and contact damping coefficients by considering the system dynamics and included contact mechanics. Using Cu as a reference material, the CR-AFM measurements on the patterned structures showed a significant increase in the elastic modulus of the low-k dielectric material compared with that of a blanket pristine film. Such an increase in the elastic modulus suggests an enhancement in the densification of low-k dielectric films during patterning. In addition, the subsurface response of the materials was investigated in load-dependent CR-AFM point measurements and in this way a depth dimension was added to the common CR-AFM surface characterization. With the new proposed measurement procedure and analysis, the present investigation provides new insights into characterization of surface and subsurface mechanical responses of nanoscale structures and the integrity of their interfaces.     

Higher-order electromechanical response of thin films by contact resonance piezoresponse force microscopy

Piezoresponse scanning force microscopy (PFM) has turned into an established technique for imaging ferroelectric domains in ferroelectric thin films. At least for soft cantilevers, the piezoresponse signal is not only dependent on the elastic properties of the material under investigation but also on the elastic properties of the cantilever. Due to this dependency, the cantilever response and, therefore, the measured properties depend on the frequency of the small alternating current (AC) testing voltage. At the contact resonance, the cantilever response is maximum, and this increased sensitivity can be used to detect very small signals or to decrease the voltage applied to the sample. We have shown that by using the hysteretic ferroelectric switching, it is possible to separate the signal into its components (viz. electromechanical and electrostatic contributions). Additionally, the measurement frequency can be tuned such that the second and third harmonics of the electromechanical response can be detected at the cantilever resonance, providing information about the higher-order electromechanical coefficients. We assume that this nonlinear behavior seen in local and macroscopic measurements is rooted in the nonlinearity of the dielectric permittivity. Our results are of crucial importance for the study of ferroelectric and electromechanical properties of nanostructures.     

Mapping nanomechanical properties of live cells using multi-harmonic atomic force microscopy

The nanomechanical properties of living cells, such as their surface elastic response and adhesion, have important roles in cellular processes such as morphogenesis, mechano-transduction, focal adhesion, motility, metastasis and drug delivery. Techniques based on quasi-static atomic force microscopy techniques can map these properties, but they lack the spatial and temporal resolution that is needed to observe many of the relevant details. Here, we present a dynamic atomic force microscopy method to map quantitatively the nanomechanical properties of live cells with a throughput (measured in pixels/minute) that is ～10-1,000 times higher than that achieved with quasi-static atomic force microscopy techniques. The local properties of a cell are derived from the 0th, 1st and 2nd harmonic components of the Fourier spectrum of the AFM cantilevers interacting with the cell surface. Local stiffness, stiffness gradient and the viscoelastic dissipation of live Escherichia coli bacteria, rat fibroblasts and human red blood cells were all mapped in buffer solutions. Our method is compatible with commercial atomic force microscopes and could be used to analyse mechanical changes in tumours, cells and biofilm formation with sub-10?nm detail.     

Measurement of elastic properties of calcium silicate hydrate with atomic force microscopy

Atomic force microscopy (AFM) based indentation is compared to conventional nanoindentation for measuring mechanical properties of cement pastes. In evaluating AFM as a mechanical characterization tool, various analytical and numerical modeling approaches are compared. The disparities between the numerical self-consistent approach and analytical solutions are determined and reported. The measured elastic Young’s modulus determined from AFM indentation tests are compared to elastic Young’s modulus determined from nanoindentation tests of cement paste. These results indicate that the calcium silicate hydrate (C-S-H) phase of hydrated Portland cement has different properties on the different length scales probed by AFM versus nanoindenters. Packing density of C-S-H particles is proposed as an explanation for the disparity in the measured results.     

Electrical transport properties of oligothiophene-based molecular films studied by current sensing atomic force microscopy

Using conducting probe atomic force microscopy (CAFM) we have investigated the electrical conduction properties of monolayer films of a pentathiophene derivative on a SiO(2)/Si-p+ substrate. By a combination of current-voltage spectroscopy and current imaging we show that lateral charge transport takes place in the plane of the monolayer via hole injection into the highest occupied molecular orbitals of the pentathiophene unit. Our CAFM data suggest that the conductivity is anisotropic relative to the crystalline directions of the molecular lattice.     

Towards a better understanding of wood cell wall characterisation with contact resonance atomic force microscopy

Nowadays, the multi-scale modelling of wood has a great need for measurements of structural, chemical and mechanical properties at the lowest level. In this paper, the viscoelastic properties in the layers of a wood cell wall are investigated using the contact resonance mode of an atomic force microscope (CR-AFM). A detailed experimental protocol suitable for obtaining reproducible and quantifiable data is proposed. It is based on three main steps: sample preparation to obtain a good surface state, calibration of the contact modulus using reference samples, and image processing to produce the viscoelastic images. This protocol is applied on chestnut tension wood. The obtained topography and semi-quantitative viscoelastic maps are discussed with respect to the cell wall structure, sample preparation effects, and AFM measurement specificity compared with nanoindentation.     

Contact force identification using the subharmonic resonance of a contact-mode atomic force microscopy

We propose a step-by-step experimental procedure for characterization of the nonlinear contact stiffness on surfaces using contact-mode atomic force microscopy. Our approach directly estimates the first-, second-, and third-order coefficients of the contact stiffness. It neither uses nor requires the underlying assumptions of the Hertzian contact theory. We use a primary resonance excitation of the probe to estimate the linear coefficient of the contact stiffness. We use the method of multiple scales to obtain closed-form expressions approximating the response of the probe to a subharmonic resonance excitation of order one-half. We utilize these expressions and higher-order spectral measurements to independently estimate the quadratic and cubic coefficients of the contact stiffness.     

Relating elastic modulus to indentation response using atomic force microscopy

Abstracts are not published in this journal     

Nanoplough-constrictions on thin YBCO films made with atomic force microscopy

Utilizing atomic force microscope (AFM) with a diamond tip, we were able to successfully plough nano-constrictions on epitaxially grown YBa2Cu3O(7-x) thin films deposited on MgO substrates. The thickness, width, and length of the obtained constrictions were in the range of a few 100 nm. Furthermore, we managed to produce a new S-type constriction, of which the dimensions are easier to control than for conventional constrictions.     

Quantitative subsurface contact resonance force microscopy of model polymer nanocomposites

We present experimental results on the use of quantitative contact resonance force microscopy (CR-FM) for mapping the planar location and depth of 50?nm diameter silica nanoparticles buried beneath polystyrene films 30-165?nm thick. The presence of shallowly buried nanoparticles, with stiffness greater than that of the surrounding matrix, is shown to locally affect the surface contact stiffness of a material for all depths investigated. To achieve the necessary stiffness sensitivity, the CR-FM measurements are obtained utilizing the fifth contact eigenmode. Stiffness contrast is found to increase rapidly with initial increases in force, but plateaus at higher loads. Over the explored depth range, stiffness contrast spans roughly one order of magnitude, suggesting good depth differentiation. Scatter in the stiffness contrast for single images reveals nonuniformities in the model samples that can be explained by particle size dispersity. Finite element analysis is used to simulate the significant effect particle size can have on contact stiffness contrast. Finally, we show how measurements at a range of forces may be used to deconvolve particle size effects from depth effects.     

The determination of the elastic modulus of microcantilever beams using atomic force microscopy

An investigation into the determination of the micromechanical properties of thin film materials has been performed. Thin metal and ceramic films are used extensively in the computer microprocessor industry and in the field of micro-electromechanical systems (MEMS). The demand for miniaturization and increased performance has resulted in the use of materials without a clear understanding of their mechanical properties on this scale. Micromechanical properties are difficult to obtain due to the lack of adequate testing equipment. The atomic force microscope (AFM), most commonly used as an imaging tool, lends itself to mechanical interaction with the sample surface utilizing a cantilever probe. An array of aluminum microcantilever beams were fabricated using standard IC processing techniques. The microbeams were deflected by the AFM cantilever probe and from this, the micromechanical properties of stiffness and elastic modulus were determined. Initial results indicate that this technique reliably determines the micromechanical properties of thin films.     

Atomic force microscopy and atomic force acoustic microscopy characterization of photo-induced changes in some Ge-As-S amorphous films

Amorphous Ge₂₇As₁₃S₆₀, Ge₁₄As₂₇S₅₉ and Ge₁₆As₂₆S₅₈ thin films were prepared by thermal evaporation. Well annealed films were photodarkened by the photons with energy little exceeding the band gap energy. Using Atomic Force Microscopy we observed significant photoexpansion of studied films. Atomic Force Acoustic Microscopy revealed domains like structure of the surface and near surface parts of the samples which one was found to be more disintegrated after illumination.     

Morphology and current-voltage characteristics of nanostructured pentacene thin films probed by atomic force microscopy

Atomic force microscopy was used to study the growth modes (on SiO2, MoS2, and Au substrates) and the current-voltage (I-V) characteristics of organic semiconductor pentacene. Pentacene films grow on SiO2 substrate in a layer-by-layer manner with full coverage at an average thickness of 20 A and have the highest degree of molecular ordering with large dendritic grains among the pentacene films deposited on the three different substrates. Films grown on MoS2 substrate reveal two different growth modes, snowflake-like growth and granular growth, both of which seem to compete with each other. On the other hand, films deposited on Au substrate show granular structure for thinner coverages (no crystal structure) and dendritic growth for higher coverages (crystal structure). I-V measurements were performed with a platinum tip on a pentacene film deposited on a Au substrate. The I-V curves on pentacene film reveal symmetric tunneling type character. The field dependence of the current indicates that the main transport mechanism at high field intensities is hopping (Poole-Frenkel effect). From these measurements, we have estimated a field lowering coefficient of 9.77 x 10(-6) V-1/2 m1/2 and an ideality factor of 18 for pentacene.     

Study of the surfaces of CVD-WO3 films, by atomic force microscopy and spectroscopic ellipsometry

Atomic force microscopy imaging of chemical vapor deposition WO₃ films reveals the presence of domed crystallites that resemble the florets of cauliflowers with a rough surface texture. Annealing at 400 °C and above leads to further surface roughening, with estimated root mean square roughness values of 40–50 nm. Spectroscopic ellipsometry analysis shows that the surface layer becomes thicker with increasing oxygen flow rate during film deposition. This layer is predominantly amorphous for as-deposited films, and predominantly crystalline after annealing.     

原子力显微镜探针悬臂弹性常数校正技术进展

利用原子力显微镜对材料表面的力学性能进行定量表征时,需要准确知道原子力显微镜探针悬臂的弹性常数,所以对弹性常数进行校正十分重要。该文综述近年来对探针悬臂弹性常数的校正方法,主要包括维度法、静态挠度法、动态挠度法。维度法对不同悬臂形状(主要针对矩形、V型)进行阐述,分析不同方法使用的数学模型与优缺点;静态挠度法不仅对方法的数学模型进行阐述,还着重介绍近年来对该方法精确度的改进研究;动态挠度法以附加质量法、Sader法与热调谐法分别阐述,比较3种方法的模型特点与先进性;最后分析常用探针适合使用的校正方法,对今后校正方法的发展提供参考。     

Studying the high-field electron conduction of tetrahedral amorphous carbon thin films by conducting atomic force microscopy

The high-field electron conduction of tetrahedral amorphous carbon (ta-C) thin films substrate has been studied using a conducting atomic force microscope (C-AFM). The ta-C thin films with a high concentration of sp³ bonding (80–90%) were deposited on Si by field arc deposition (FAD). The high-field “conductance” and surface morphology were mapped simultaneously. At low bias, the “conductance” exhibits inhomogeneities on a large scale, presumably due to thickness variations or interface defects. However, at high bias, the small difference in “conductance” due to thickness variations or interface defects was buried by the high intrinsic “conductivity.” It has also been shown that high field causes electric breakdown in these films by converting sp³ bonding to sp² at high electric field.     

Precise control of nanofabrication by atomic force microscopy

With an aim of the precise control of the anodic oxidation process by atomic force microscopy, the technical improvement has been carried out based on the mechanism studies. The accuracy and reliability of the nanofabrication have been improved by the combination of ambient humidity control, improvement of instrumental performance and meniscus lifetime control. In parallel, the mechanism study has been proceeded through the detection of Faradaic current. The in situ Faradaic current detection of the nano-oxidation process can actually work as a sensitive monitor for the nano-oxidation process with a high reliability. From an engineering viewpoint with an eye to practical applications, controllable physical parameters which affect on the product size are enumerated to consider what we should do to raise the precision of nano-oxidation. Then the fast fabrication in a large area by a patchwork method, Faradaic current detection during oxidation-reduction reaction, and nanofabrication by current-control are shown as examples.