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Epoxy/Carbon nanotube (CNT) composites are interesting materials that could be used in a wide variety of applications. In this study, CNT contents of 0.25, 0.5, 1 and 2 wt% were used for reinforcing epoxy. A nanoindentation device and a temperature regulating system were developed in order to investigate the effect of CNTs on the time-dependent properties of epoxy using relaxations and creep tests on the nano scale. The relaxation tests showed a significant shift for the relaxation spectrum towards shorter times with introducing a low CNT content of 0.25 wt%. Additionally, creep tests showed that both the holding time at a constant load and the unloading velocity have a major effect on the contact stiffness. However, there was no effect for the CNTs on the creep behavior with contents lower than 1 wt%, which was related to the presence of a percolation threshold around this value.
Characterization of the mechanical properties of interphases is essential when designing multicomponent materials such as fiber-reinforced matrices, protective coatings or multi-layered structures for integrated circuits. It can provide vital information about the durability of the finished product as a composite because failure is often initiated in the interfacial region induced by internal or external stress during fabrication or service. Nanoindentation is a powerful tool for investigating mechanical properties on the micro/nano scale. However, there are some challenges associated with conducting nanoindentation near interface regions. One main challenge is that the small thickness of the interphase region (typically 1-2µm) makes it difficult to apply several adjacent indents without overlap. Another issue is that the indentations are usually restricted by local reinforcement, and it becomes difficult to isolate the change in mechanical properties due solely to interphase formation. In this study we try to gauge the feasibility of nanoindentation for characterizing epoxy/Cu interphases. We develop a sample preparation method and optimize nanoindentation parameters in an attempt to avoid the restrictions mentioned above. Atomic force microscopy (AFM) and finite element analysis are employed as reference techniques to evaluate the effectiveness of our technique. We show the influence of preparation method and nanoindentaion parameters on measurements of interphase properties and how they relate the mentioned challenges.
Thermosetting materials are gaining increasing attention in many structural composite applications. However, the incorporation of inorganic nanoparticles (NPs) into polymer matrix is a promising approach to enhance their functional characteristics, and thus, to enable the development of thermosets advanced application. It has been shown that Boehmite Alumina (BA) used as nanofillers can improve different parameters of polymers. This NPs can be easily tailored enabling desirable interactions with a big range of polymers. However, the overall effect of nanofiller depends on many factors, therefore, making it hard to predict the resulted performance of nanocomposites. In the current contribution we would like to discuss the impact of Boehmite NPs on two different epoxy resin nanocomposite systems with the focus on the possible influence mechanisms of this nanofiller.
As the first system, UV curable Cycloaliphatic-Epoxy Oligosiloxane (CEOS) resin/Boehmite nanocomposites were investigated by FTIR, TGA, DSC and T-SEM. It was observed that incorporation of BA leads to the reinforcement of glass transition (Tg) and overall thermal stability indicating the attractive interactions between BA and CEOS network. In addition, an increase in epoxy conversion of CEOS was concluded for nanocomposites assuming that particles are involved in UV polymerisation processes.
The second epoxy/Boehmite nanocomposite is based on the bisphenol-A-diglycidyl ether (DGEBA) cured with methyl tetrahydrophtalic acid anhydride (MTHPA). Thermomechanical as well as nanomechanical properties of this material were investigated by DMTA and IR spectroscopy and the advanced Intermodulation AFM, respectively. In contrast to the first system, it was found that BA leads to a decrease of Tg and crosslink density of the polymer while the young’s modulus of the composite and local stiffness of polymer matrix increase significantly.
As a result, the versatile role of Boehmite was detected depending on the investigated systems. Based on the obtained results, the parameters indicating property-efficient epoxy/Boehmite system are suggested.
Although in the last decades epoxy-based nanocomposites have been successfully adopted by the marine, automotive and aerospace industries they are still rarely studied on a fundamental level. This work deals with an in-depth comparative investigation of the structure, molecular mobility and vitrification kinetics of three bisphenol A diglycidyl ether (DGEBA)-based materials with different nanofillers: I) taurine-modified layered double hydroxide (T-LDH), II) boehmite (BNPs) and III) halloysite nanotubes (HNTs). Moreover, the effect of different hardeners (diethylene triamine and methyl tetrahydrophtalic acid anhydride) on the unfilled epoxy matrix is addressed as well. The chosen methodology comprises I) small – and wide – angle X-ray scattering (SAXS/WAXS) II) calorimetry in the forms of a) conventional DSC and b) static fast scanning calorimetry (FSC), III) broadband dielectric spectroscopy (BDS), as well as IV) specific heat spectroscopy in the forms of a) temperature modulated DSC, and b) temperature modulated FSC. The combination of these techniques proved an intrinsic spatial heterogeneity of epoxy-based materials, evidenced by two separate segmental relaxation processes. Although, depending on the hardener the response of the systems to calorimetric and dielectric investigations was different, in a broader sense similar conclusions can be extracted on the structural heterogeneity. As expected from the two distinct α-processes, it was shown that, in parallel to the main glass transition, epoxy-based materials can exhibit an additional low temperature vitrification mechanism, which was not discussed in prior studies for an unfilled network former. Furthermore, the interfacial region (so-called rigid amorphous fraction) was qualitatively and quantitatively addressed, in dependence of the employed nanofiller structure.
Products and by-products of the invertebrate and vertebrate farming, respectively, are shown to be promising bio-based flame retardant adjuvants in epoxy thermosets. While the addition of bone meal results in the formation of an inorganic shield, protein-based powders from insects provide an intumescent behavior under forced flaming conditions. Combining the latter with a common flame retardant such as ethylene diamine phosphate, the charring efficiency and self-extinguishing properties can be further enhanced.