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The manufacturing of Diels-Alder (D-A) crosslinked epoxy nanocomposites is an emerging field with several challenges to overcome: the synthesis is complex due to side reactions, the mechanical properties are hindered by the brittleness of these bonds, and the content of carbon nanotubes (CNT) added to achieve electroactivity is much higher than the percolation thresholds of other conventional resins. In this work, we develop nanocomposites with different D-A crosslinking ratios (0, 0.6, and 1.0) and CNT contents (0.1, 0.3, 0.5, 0.7, and 0.9 wt.%), achieving a simplified route and avoiding the use of solvents and side reactions by selecting a two-step curing method (100 °C-6 h + 60 °C-12 h) that generates the thermo-reversible resins. These reversible nanocomposites show ohmic behavior and effective Joule heating, reaching the dissociation temperatures of the D-A bonds. The fully reversible nanocomposites (ratio 1.0) present more homogeneous CNT dispersion compared to the partially reversible nanocomposites (ratio 0.6), showing higher electrical conductivity, as well as higher brittleness. For this study, the nanocomposite with a partially reversible matrix (ratio 0.6) doped with 0.7 CNT wt.% was selected to allow us to study its new smart functionalities and performance due to its reversible network by analyzing self-healing and thermoforming.

The zinc alkaline battery is one of the most popular sources of portable electrical energy, with more than 300,000 tons being consumed per year. Accordingly, it is critical to recycle its components. In this work, we propose the use of zinc oxide (ZnO) microparticles recovered from worn-out batteries as fillers of epoxy resins. These nanocomposites can be used as protective coatings or pigments and as structural composites with high thermal stability. The addition of ceramic nanofillers, such as ZnO or/and TiO2, could enhance the thermal and mechanical properties, and the hardness and hydrophobicity, of the epoxy resins, depending on several factors. Accordingly, different nanocomposites reinforced with recycled ZnO and commercial ZnO and TiO2 nanoparticles have been manufactured with different nanofiller contents. In addition to the different ceramic oxides, the morphology and size of fillers are different. Recycled ZnO are“desert roses” such as microparticles, commercial ZnO are rectangular parallelepipeds nanoparticles, and commercial TiO2 are smaller spherical nanoparticles. The addition of ceramic fillers produces a small increase of the glass transition temperature (<2%), together with an enhancement of the barrier effect of the epoxy resin, reducing the water diffusion coefficient (<21%), although the maximum water uptake remains constant. The nanocomposite water absorption is fully reversible by subsequent thermal treatment, recovering its initial thermomechanical behavior. The water angle contact (WCA) also increases (~12%) with the presence of ceramic particles, although the highest hydrophobicity (35%) is obtained when the epoxy resin reinforced with recycled flowerlike ZnO microparticles is etched with acid stearic and acetic acid, inducing the corrosion of the ZnO on the surface and therefore the increment of the surface roughness. The presence of desert rose ZnO particles enhances the de lotus effect.

A new manufacturing method of thermosetting resins reinforced with dense particles is developed in the present work. A rotary mold is used, avoiding the natural sedimentation of particles through applying centrifuge forces. A deep study of the sedimentation phenomenon is carried out in order to evaluate the main experimental parameters which influence the manufacturing of composite. The used reinforcement is zinc oxide (ZnO) obtained by a new recycling method from spent alkaline batteries. In order to compare the benefits, commercial ZnO nanoparticles are also analyzed. Recycled ZnO particles enhance the interaction of the epoxy matrix due to their inner moisture, allowing the manufacture of composites with relatively high ceramic content. Moreover, an increment in the glass transition temperature of the epoxy matrix and in the mechanical properties, such as its stiffness and hardness, is achieved.