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Eingeladener Vortrag
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A report is presented on the development of a test for determining the long-term oxidation resistance of polyolefin materials, which is accelerated not only by elevated temperatures but also by increased oxygen pressure and a stirred aqueous medium. The method permits durability tests to be carried out at markedly lower temperatures with reasonable testing durations and significantly reduced diffusion limited oxidation effects and allows for physical and chemical impacts of aqueous media. Oxidative durability can be assessed by autoclave immersion exposures at three different temperatures (60, 70 and 80 degrees C) and 50 bar oxygen pressure and at 80 degrees C and two different oxygen pressures (usually 10 and 20 bar). Accelerated test data are evaluated by modified Arrhenius equations with the application of a three-dimensional regression analysis. The application of the test method to various materials, including PP non-woven materials and geosynthetics is demonstrated. 10 refs.
In der vorliegenden Arbeit wurden mittels eines Rasterkraftmikroskopes (Scanning Force Microscope, SFM) nanomechanische Experimente zur Charakterisierung des Grenzbereiches (Interphase) zwischen einer polymeren Matrix und anorganischen Verstärkungskomponenten durchgeführt. Ziel der Untersuchungen war es, mit Hilfe einer sinusförmigen Modulation der Auflagekraft zwischen SFM-Spitze und Probe innerhalb der polymerseitigen Interphase vorhandene Steifigkeitsgradienten zu detektieren sowie ihren Verlauf zu charakterisieren. Es konnte gezeigt werden, dass die Steifigkeitsmessung im SFM die Möglichkeit bietet, Grenzphasen über die lokalen Änderungen im Elastizitätsmodul quantitativ zu charakterisieren.
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).
Laser ablation of single-crystalline indium phosphide (InP) was performed in air by means of linearly polarized Ti:sapphire femtosecond-pulses (800 nm, 130 fs, 10 Hz). As a result of the first laser pulses, several morphological changes (crater formation, rim formation, ripple structures and cones) were observed. These effects were explored using force modulation microscopy (FMM), a technique based on scanning force microscopy (SFM), allowing the simultaneous imaging of both topography and local stiffness at a high lateral resolution. The first laser pulse induces the formation of a protruding rim (height <20 nm, width ~300 nm) bordering the ablated crater. A Fourier-analysis of the multi-pulse generated topographies reveals the formation of wavelength-sized periodic ripples (modulation depth <100 nm) with an orientation perpendicular to that of the electric field vector of the laser radiation. Besides these morphological alterations, also material modifications were observed in the irradiated regions by means of the FFM technique. Within the ablated craters, local stiffness variations were found revealing an inhomogeneous material composition/structure as a consequence of the femtosecond pulse laser treatment.
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.