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Force measurements with the atomic force microscope - Technique, interpretation and applications
(2005)
The atomic force microscope (AFM) is not only a tool to image the topography of solid surfaces at high resolution. It can also be used to measure force-versus-distance curves. Such curves, briefly called force curves, provide valuable information on local material properties such as elasticity, hardness, Hamaker constant, adhesion and surface charge densities. For this reason the measurement of force curves has become essential in different fields of research such as surface science, materials engineering, and biology.
Another application is the analysis of surface forces per se. Some of the most fundamental questions in colloid and surface science can be addressed directly with the AFM: What are the interactions between particles in a liquid? How can a dispersion be stabilized? How do surfaces in general and particles in particular adhere to each other? Particles and surfaces interactions have major implications for friction and lubrication. Force measurements on single molecules involving the rupture of single chemical bonds and the stretching of polymer chains have almost become routine. The structure and properties of confined liquids can be addressed since force measurements provide information on the energy of a confined liquid film.
After the review of Cappella [B. Cappella, G. Dietler, Surf. Sci. Rep. 34 (1999) 1104] 6 years of intense development have occurred. In 1999, the AFM was used only by experts to do force measurements. Now, force curves are used by many AFM researchers to characterize materials and single molecules. The technique and our understanding of surface forces has reached a new level of maturity. In this review we describe the technique of AFM force measurements. Important experimental issues such as the determination of the spring constant and of the tip radius are discussed. Current state of the art in analyzing force curves obtained under different conditions is presented. Possibilities, perspectives but also open questions and limitations are discussed.
Force-distance curves have been acquired with an atomic force microscope on perfluorpolyether films. It is shown that curves acquired on films of different thickness, at different rates and with different dwell times can be overlapped by rescaling the time or distance axis.When the time or distance axis is rescaled,the force depends only on the surface tension of perfluorpolyether and on geometrical properties of thetip (aperture and perimeter of the tip at a given distance from the apex). Hence, curves acquired with thesame tip overlap.
By comparing curves acquired at different rates the dynamics of tip-wetting can be investigated. Fur-thermore, rescaled force-distance curves have been matched with the perimeter of cross sections ofthe tip, i.e. with the perimeter of the three-phase contact line. Such measurements pave the way for anon-destructive investigation of the tip shape.
We present dynamic plowing nanolithography on polymethylmethacrylate films, performed with a scan-linearized atomic force microscope able to scan up to 250 μm with high resolution. Modifications of the surface are obtained by plastically indenting the film surface with a vibrating tip. By changing the oscillation amplitude of the cantilever, i.e., the indentation depth, surfaces can be either imaged or modified. A program devoted to the control of the scanning process is also presented. The software basically converts the gray scale of pixel images into voltages used to control the dither piezo driving cantilever oscillations. The advantages of our experimental setup and the dependence of lithography efficiency on scanning parameters are discussed. Some insights into the process of surface modifications are presented.
The topography of wear scars on the surface of a steel disc coated with a diamond-like carbon (DLC) layer has been investigated with an Atomic Force Microscope (AFM). AFM topography images have been combined together taking advantage of the stitching technique for the study of wear scars in their initial stage. Moreover, the topography of the sample has been acquired before and after the sliding tests. In this way even very small changes of the sample surface (<10 nm) can be detected. Three main phenomena taking place at the very initial stage of wear could be identified: the abrasion of small asperities bulging out of the sample surface, the carving of swallow grooves with depth under 20 nm, and the partial or total closure of cavities present on the surface. This last phenomenon shows that, before the carving of a wear scar, the plastic deformation of particular regions of the sample, i.e. the volume around the cavities, takes place already after few cycles (in this case between 400 and 800) in the initial phase of the sliding test.
Force-displacement curves have been obtained with a commercial atomic force microscope (AFM) at different temperatures and probe rates on a thick film of poly(n-butyl methacrylate) (PnBMA). The analysis of the force-displacement curves has been focused on the contact portion of the curves, giving information about the stiffness of the sample and its Young's modulus. A novel model of sample deformations that extends the basic equations of the elastic continuum contact theories to the plastic deformations is presented. This model gives several insights into the processes of deformation of soft samples and permits to calculate not only the parameters of the Williams-Landel-Ferry equation but also the Young's modulus and the yielding force of the polymer as a function of temperature and/or probe rate. These quantities have been measured in a wide range of temperatures (70 K) and probe rates (6 decades) for the first time with the AFM, and the results are in very good agreement with measurements performed with customary techniques, such as broadband spectroscopy and dynamic mechanical analysis.
Wear test results exhibit often large scattering. Hence, the study of spreading of experimental results requires big datasets.
In various studies, wear coefficients were found to have lognormal distributions. Therefore, it was supposed that the wear coefficient is affected by two normally distributed variables, which combine through a product.
In the present study, we demonstrate that a lognormal distribution may arise from a nonconstant wear coefficient, too, i.e., when a system does not follow Archard’s law.
Force-displacement curves have been acquired with a commercial atomic force microscope on a thin film of poly(n-butyl methacrylate) on glass substrates. The film thickness is nonuniform, ranging in the measured area from 0 to 30 nm, and gives the possibility to survey the so-called "mechanical double-layer" topic, i.e., the influence of the substrate on the mechanical properties of the film in dependence of the film thickness. The stiffness and the deformation for each force-distance curve were determined and related to the film thickness. We were able to estimate the resolution of the film thickness that can be achieved by means of force-distance curves. By exploiting the data acquired in the present and in a previous experiment, a novel semiempirical approach to describe the mechanical properties of a mechanical double-layer is introduced. The mathematical model, with which deformation-force curves can be described, permits to calculate the Young's moduli of film and substrate in agreement with literature values and to determine the film thickness in agreement with the topography.
Forcedisplacement curves have been acquired with a commercial atomic force microscope on thin films of poly(n-butyl methacrylate) on glass substrates. Different film thicknesses, from 10 up to 430 nm, were chosen to examine in detail the so called mechanical double-layer topic, i.e., the influence of the substrate on the determination of the mechanical properties of thin films. Taking advantage of the Hertz theory we calculated for all films the contact radius between tip and sample as a function of the applied load. Further Young's modulus of the samples was derived from the experimental data as a function of the applied load and, alternatively, of the deformation. The results of this analysis for 10 different film thicknesses were fitted with several half empirical equations proposed by several researchers. The focus of this work is to evaluate such existing half empirical theories for mechanical double-layers and to show the need for an alternative consistent approach.
The concept behind this Research Topic (RT) was to collect works, in which Atomic Force Microscopy (AFM) techniques are employed to study tribological phenomena and to push the resolution of measurements towards single asperity contact. Thanks to the direct determination of sample height with sub-nanometer resolution and the possibility of measuring local friction, AFM can be employed after a tribotest to detect topography and friction changes at the nanometer scale. Recently, efforts are being expended to use AFM cantilevers as tribometers, i.e., as probes altering the volume of suitable samples, thereby measuring tip and/or sample wear and friction at the nano/microscale. Thus, single asperity contact, friction, and wear can be investigated. Since friction and wear at the macroscale are the result of asperities interactions, such experiments are of great importance for better understanding of tribological processes.
Adhesion of amorphous polymers as a function of temperature probed with AFM force-distance curves
(2005)
Forcedisplacement curves have been obtained with a commercial atomic force microscope at different temperatures and probe rates on a thick film of poly(n-butyl methacrylate) and on two films of polystyrene with different molecular weight. In a previous publication [B. Cappella, S.K. Kaliappan, H. Sturm, Macromolecules 38 (2005)1874] the analysis of forcedisplacement curves has been focused on the stiffness and on the Young's modulus of the samples. In the present publication we consider the temperature dependence of the work of adhesion. We have obtained master curves of the work of adhesion at fixed maximum loads and, by comparing the results of the two analysis, we show that the work of adhesion follows the WilliamsLandelFerry equation with the same coefficients previously found for the Young's modulus. Furthermore, we show that the temperature dependence of the work of adhesion of the polymers is a consequence of the temperature dependence of the tipsample contact area and in the end of the temperature dependence of the stiffness and of the elasticplastic properties of the samples.