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In the present paper, friction and mechanical properties of AFM-Scan-Induced ripple structures on films of polystyrene and poly-n-(butyl methacrylate) are investigated. Force volume measurements allow a quantitative analysis of the elastic moduli with nanometer resolution, showing a contrast in mechanical response between bundles and troughs. Additionally, analysis of the lateral cantilever deflection shows a clear correlation between friction and the sample topography. Those results support the theory of crack propagation and the formation of voids as a mechanism responsible for the formation of ripples. This paper also shows the limits of the presented measuring methods for soft, compliant, and small structures.
Contact-resonance AFM (CR-AFM) has been used in recent years for the measurement of mechanical properties. Compared with other techniques, CR-AFM has a much shorter acquisition time, compensating the incomplete theoretical understanding of the underlying physical phenomena. In the present paper, we propose a procedure, which allows to determine the elastic modulus of the sample as a parameter of the fit of the CR frequency as a function of the load. It is concluded that CR measurements are not appropriate for polymer samples. Major drawbacks are the bad resolution for moduli lower than ca. 10 GPa and the lack of a comprehensive physical model.
Force-deformation curves have been acquired using nanoindentation and atomic force microscopy on two amorphous polymer samples. The shape and size of the indenter tip was characterized using a white light interferometer and AFM. The measured nanoindentation curves were fitted with the Hertz equation to calculate the Young's modulus of the polymers. Once the Young's moduli of the polymers were known, AFM was used to acquire force-distance-curves on the same samples. We also used the Hertz theory for the analysis in this case. As a result, the tip radius of the AFM cantilever tip could be measured.
This procedure is proposed as a method to determine the shape and size of AFM tips for the quantitative characterization of surface forces through force-distance curves.
Thin polybutadiene/polystyrene blend films were deposited on glass substrates by spin-coating. The two polymers were chosen, as they are immiscible and differ strongly in their mechanical properties. The blend was characterized with Tapping Mode and force–distance curves. Several advantages of force–distance curves measurements compared to Tapping Mode are shown, most of all the capability of yielding quantitative information about several properties, such as Young's modulus and adhesion. Also the aging behaviour of the blend exposed to air could be observed, in particular the increase of the Young's modulus due to cross-linking and dewetting processes. Additionally, the sample was used to improve the resolution of force–distance curves up to 6 nm, which is to date the best resolution achieved with force–distance curves. Such an improvement resolves the major disadvantage of force–distance curves, compared to other scanning mode, i.e. its inferior resolution.
Force–distance curves have been acquired with an Atomic Force Microscope on polymethyl methacrylate with embedded glass spheres. The glass spheres provide a stiff substrate with an irregular and complex topography hidden underneath a compliant and even polymer film. This situation is a special case of a mechanical double-layer, which we examined in detail in previous experiments. Up to now uniform and non-uniform polymer films on an even substrate were examined. The film thickness on each point of the sample surface was known and force–distance curves could be averaged in groups according to the film thickness. In this way we were able to develop a semi empirical approach which allows describing the shape of averaged force–distance curves depending on the Youngs moduli of the involved materials and on the film thickness. In this experiment we reconstruct a hidden topography, i.e., we determine the polymer thickness on each point of the sample by analyzing single force–distance curves with our semi empirical equation. The accuracy reached by this approach permits to obtain a reconstruction of the shape and position of the embedded particles limited by a maximum detection depth. Single curves are also analyzed qualitatively in order to locate areas where the adhesion at the polymer/glass interface is weak or the two phases are detached.