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Stiffness variation in the interphase of amine-cured epoxy adjacent to copper microstructures
(2007)
In an effort to expand the understanding of the mechanical properties of the polymeric interphase on a metal surface, a composite consisting of epoxy and copper was prepared and analyzed. Scanning force microscopy-based force modulation microscopy (SFM-FMM) was employed along with dynamic mechanical analysis (DMA) and energy dispersive X-ray analysis (EDX). Diglycidyl ether of bisphenol A (DGEBA)-based epoxy resins were applied with amine curing agents. The samples were made taking advantage of electron beam lithography (EBL) in order to produce sharp edges of copper structures and a flat surface suitable for the SFM-FMM analysis, which was able to depict the stiffness within the interphase. It is considered significant information because the mechanical characteristic within the narrow interphase was revealed. Comparing with DMA and EDX, the stiffness information of SFM-FMM demonstrated a matching correlation and agreement in terms of preferential adsorption of the curing agent in the vicinity of the interface. The stiffness profiles of the two epoxy systems turned out to be different, and it shows the material dependence of the interphase characteristics.
Laminates of carbon fiber reinforced plastic (CFRP), which are manufactured by injection technology, are reinforced with boehmite particles. This doping strengthens the laminates, whose original properties are weaker than those of prepregs. Besides the shear strength, compression strength and the damage tolerance, the mode of action of the nanoparticles in resin and in CFRP is also analyzed. It thereby reveals that the hydroxyl groups and even more a taurine modification of the boehmites' surface alter the elementary polymer morphology. Consequently a new flow and reaction comportment, lower glass transition temperatures and shrinkage, as well as a changed mechanical behavior occur. Due to a structural upgrading of the matrix (higher shear stiffness, reduced residual stress), a better fiber-matrix adhesion, and differing crack paths, the boehmite nanoparticles move the degradation barrier of the material to higher loadings, thus resulting in considerably upgraded new CFRP.
Boehmite nanoparticles show great potential in improving mechanical properties of fiber reinforced polymers. In order to predict the properties of nanocomposites, knowledge about the material parameters of the constituent phases, including the boehmite particles, is crucial. In this study, the mechanical behavior of boehmite is investigated using Atomic Force Microscopy (AFM) experiments and Molecular Dynamic Finite Element Method (MDFEM) simulations. Young’s modulus of the perfect crystalline boehmite nanoparticles is derived from numerical AFM simulations. Results of AFM experiments on boehmite nanoparticles deviate significantly. Possible causes are identified by experiments on complementary types of boehmite, that is, geological and hydrothermally synthesized samples, and further simulations of imperfect crystals and combined boehmite/epoxy models. Under certain circumstances, the mechanical behavior of boehmite was found to be dominated by inelastic effects that are discussed in detail in the present work.The studies are substantiated with accompanying X-ray diffraction and Raman experiments.
The image designed by Natalia Cano Murillo and colleagues shows the cross section of a ternary composite (boehmite/polycarbonate/epoxy, 80μm x 80μm). The surface was measured by AFM kelvin probe microscopy, yielding the surface potential which is shown as 3D‐surface and contour lines. The sample was further subjected to AFM force spectroscopy with a lateral resolution of 1μm², yielding the local Young's modulus, projected in false colors on the 3D surface. The ternary system, containing boehmite nanoparticles, shows a broad distribution of modulus, desirable for optimized macroscopic mechanical properties, such as high stiffness as well as toughness.
Understanding the interaction between nanoparticles and the matrix and the properties of interphase is crucial to predict the macroscopic properties of a nanocomposite system. Here, we investigate the interaction between boehmite nanoparticles (BNPs) and epoxy using different atomic force microscopy (AFM) approaches. We demonstrate benefits of using multifrequency intermodulation AFM (ImAFM) to obtain information about conservative, dissipative and van der Waals tip-surface forces and probing local properties of nanoparticles, matrix and the interphase.
We utilize scanning kelvin probe microscopy (SKPM) to probe surface potential as a tool to visualize material contrast with a physical parameter, which is independent from the mechanics of the surface. Combining the information from ImAFM stiffness and SKPM surface potential results in a precise characterization of interfacial region, demonstrating that the interphase is softer than epoxy and boehmite nanoparticles. Further, we investigated the effect of boehmite nanoparticles on the bulk properties of epoxy matrix. ImAFM stiffness maps revealed the significant stiffening effect of boehmite nanoparticles on anhydride-cured epoxy matrix. The energy Dissipation of epoxy Matrix locally measured by ImAFM shows a considerable increase compared to that of neat epoxy. These measurements suggest a substantial alteration of epoxy structure induced by the presence of boehmite.
We show that complex physical and chemical interactions between boehmite nanoparticles and epoxy drastically affect matrix properties, which in the future will provide tuning of material properties for further optimization in applications from automotive to aerospace. We utilize intermodulation atomic force microscopy (ImAFM) for probing local stiffness of both particles and polymer matrix. Stiff particles are expected to increase total stiffness of nanocomposites and the stiffness of polymer should remain unchanged. However, ImAFM revealed that stiffness of matrix in epoxy/boehmite nanocomposite is significantly higher than unfilled epoxy. The stiffening effect of the boehmite on epoxy also depends on the particle concentration. To understand the mechanism behind property alteration induced by boehmite nanoparticles, network architecture is investigated using dynamic mechanical thermal analysis (DMTA). It was revealed that although with 15 wt% boehmite nanoparticles the modulus at glassy state increases, crosslinking density of epoxy for this composition is drastically low.