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Organisationseinheit der BAM
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- 1 Analytische Chemie; Referenzmaterialien (1)
Paper des Monats
- ja (2)
After a delamination process in a C-fiber reinforced polymer composite, the identification of the polymer residue of poly-(phenylene sulphide) on carbon fiber surfaces gives important information on the composite failure mechanism. Using scanning force microscopy (SFM) in its lateral force imaging mode or with the stiffness imaging mode, it is almost impossible to distinguish the two composite components owing to a very low material-based contrast of the local friction and compliance. The new technique using contrast based on a local AC current measurement allows a clear identification of the conducting carbon fiber and the non-conducting polymer coverage.
Scanning force microscopy (SFM) has been used to assess the local mechanical properties of fibre-reinforced polymers. Using a sinusoidal displacement modulation (DM) and lock-in technique the method allows to characterize local viscoelastic properties with a high lateral resolution. The simultaneous measurement of the local electrical conductivity is proposed which facilitates the interpretation of the mechanical data. The investigation of cross-sections perpendicular to the axis of carbon fibres embedded in PPS delivers some information about the change in local stiffness within the interfacial region. As a first approach, assuming a single-exponential decrease in local stiffness along a radial line from fibre to polymer we find characteristic decay lengths which are distributed in a range between 20 and 80nm. Further, a modified DM-mode is proposed which is expected to provide a contrast enhancement of the signal which is related to local stiffness. This can be achieved by installing an additional feedback loop which keeps constant the amplitude of dynamic indentation (CDI-mode).
Ti:sapphire laser pulses of 130 fs and 800 nm were focused on 3.2-7m-thick TiN films by a 60-mm focal length lens in air. The morphology of the ablated areas generated by laser pulses at a fluence slightly above the ablation threshold was characterized in dependence on the pulse number by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The cavity profiles, depths, diameters, and volumes were quantitatively evaluated by AFM. The polarization state of the laser light is discussed as a further parameter, in addition to fluence and pulse number, that influences and controls the ablation precision of these materials. It was observed that circularly polarized radiation enhances the average ablation rates and reduces the roughness in the cavities by a factor of 2-3 as compared to linearly polarized radiation of the same incident laser fluence. Special attention was paid to the interfacial region between the coating and substrate. Ultrashort-pulse laser drilling into the Si substrate revealed the generation of columnar features which even may surmount the original coating under laser conditions.
Applying a high-frequency lateral vibration between the sample surface and the tip of a scanning force microscope (SFM), a harmonically modulated lateral (friction) force image can be obtained using lock-in techniques. The principles of operation are explained, in particular the dramatic decrease of image artefacts generally caused by topography cross-talk and laser beam interference. Flat interfaces between the two immiscible polymers, poly(methyl methacrylate) (PMMA) and polystyrene (PS), are prepared on a sodium chloride single crystal from the melt. These samples are used to evaluate the appropriate model for the tip-sample interaction geometry. The relationship between frictional and normal force does not follow Amonton's law. This shows that a single-asperity interaction between the tip and sample surface can be considered. Using the new technique, local measurements of shear strength and Young's modulus can be performed.
Applying a high-frequency lateral vibration between tip and sample in a scanning force microscope (SFM), a harmonically modulated lateral (friction) force image can be obtained using lock-in techniques. Harmonically modulated lateral force microscopy (HM-LFM) offers several advantages compared with standard lateral force microscopy (LFM). After a brief investigation of the scan velocity dependence of LFM and HM-LFM, two samples were investigated. First, the surface of a poly(acrylonitrile-co-styrene)/polybutadiene blend (ABS) was used to demonstrate the ability of the new technique to decrease the stick effects of the SFM tip. Second, an interface between two chemically very similar polymers was prepared by melting polypropylene (PP) and poly(propene-block-ethene) (PP-block-PE) films on each other. After cutting, the surface roughness of this sample was very high. It is shown that only HM-LFM clearly resolves the local micromechanical properties without artefacts.
The use of a fibre-based light sensor for the calibration of Scanning Probe Microscopy piezos
(1999)
The physical properties as well as the thickness of the interphase between polymer and reinforcing phase are generally expected to show a strong influence on the macroscopic mechanical properties of composite materials. In this study the scanning force microscope (SFM) has been applied for detecting stiffness gradients near the interface between copper and epoxide. In displacement modulation mode the load exerted by the tip is modulated sinusoidally by vibrating the normal position of the cantilever or the sample. The corresponding amplitude of dynamic cantilever bending is related to local surface stiffness. Thus, using the SFM, the local mechanical properties of the surface under investigation can be probed. When scanning the tip across the reinforcement/polymer interface, the polymeric interphasial zone can be identified with the observed stiffness gradient. For a commercial epoxide based on diglycidyl ether of bisphenol A (DGEBA) cured with an amine-containing hardener, a stiffness gradient was detected that could be fitted by a Gaussian profile typical for diffusional processes. The width of the stiffness gradient was 280 nm. The observation is discussed in terms of interface-induced segregation processes between resin and hardener, as well as heat conduction mechanisms that can occur during the exothermic curing reaction. Both mechanisms are diffusional in nature and, via the local network structure, are expected to show some influence on the local stiffness of the cured epoxy. Copyright © 2000 John Wiley & Sons, Ltd.