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Characterisation of the fibre/matrix interface in reinforced polymers by the push-in technique
(1997)
The push-in test is the only micromechanical test method that is not restricted to artificial fibre/matrix arrangements, but allows the in situ characterisation of interfaces in composites fabricated and stressed under realistic conditions. However, with the application of this method to reinforced polymers some problems arise both in the mathematical model for evaluating test data and in the practical performance of the test. Because in some cases the deformation of the relatively compliant polymeric matrices cannot be neglected, an extension of the existing model is required. For this purpose, the elastic energy of the material around the debonded part of the fibre is estimated and included in the energy-balance analysis. Because of the small diameter of the fibres usually used for reinforcing polymers, a test apparatus was designed which ensures a high positioning accuracy in the xy plane as well as in the z direction. In order to minimise thermal and mechanical influences, the microscope for fibre selection and the force sensor/indenter are directly connected together and the apparatus is designed to be stiff in all components. A solid-state bending joint guarantees very precise control of the axial movement. Three examples of the application of this easy-to-handle and low-cost test apparatus are presented briefly in the paper: assess fibre/matrix combinations, measures to improve the interfacial adhesion and the influence of water on the interface.
Binary hydrogels,. in which a niobium or tantalum oxide gel and a pyrolysable organic compound are combined, were prepared as preceramic materials. Carbonaceous gel or saccharose is used as the organic gel constituent, and alkoxides or peroxo acids are the starting materials for the transition metal component. Under pyrolysis at 600-700°C, the gels are transformed into carbide precursors in which a reactive carbon and finely dispersed oxide particles are mixed intimately. The subsequent carbothermal reduction proceeds at lower temperatures compared to physical mixtures of oxides and carbon black. The high-temperature treatment was monitored by TG/DTA, X-ray diffraction and nitrogen adsorption. Microporosity is generated in the temperature range 700-800°C, and mesoporosity is additionally formed at higher temperatures. The changes in porosity are controlled by the processes of crystallization, carbothermal reduction and sintering. The final products at 1400-1500°C are assemblages of fine particles of the face-centred cubic carbides with grain sizes of 1 µm and less.
Binary organic-inorganic gels have been prepared by mixing a carbonaceous hydrosol and a Nb2O5 or Ta2O5 sol derived by hydrolysis of the alkoxides. The gels are pyrolyzed under an inert atmosphere into precursors in which carbon and the metal oxides are mixed very intimately. High temperature treatment converts the precursors into the cubic face centered carbides. The precursors as well as the carbides have been shown to be micro- and mesoporous materials. Measurements of nitrogen adsorption reveal a characteristic change of the shapes of the isotherms (Type I → Type IV) and of the hysteresis loops (H4 → H2 → H1) during the thermal processes. Pore widening has been observed with rising temperature. The phenomena of crystallization, carbothermal reduction and sintering were found to control the pore shape and size. The results of the adsorption measurement correlate well with those of the thermoanalytical and X-ray diffraction studies.
Curved substrates can be micro-structured by laser ablation, which is not possible with standard lithographic methods. The novel femtosecond-pulse laser technique allows the production of defined and reproducible micro-perforations of originally analyte-impermeable membranes. The trans-membrane analyte flux can be controlled both by the variation of the laser focus diameter resulting in different areas of single perforations, and the number of perforations in arrays on small membrane areas. This leads to a higher degree of variability as well as reproducibility of the diffusion qualities of sensor membranes, and marks the main innovation with this technique compared to the hand-made mechanical perforation by specially grinded needles used up to now. Touchless micro-perforation of small membrane areas with negligible heat damage of the structures adjacent to the perforation allows the application of analyte door membranes directly onto curved surfaces of miniaturized needle-sensors assigned for in vivo glucose monitoring, for the first time.