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Hybrid materials have attracted growing interest during the last decade, particularly due to their extraordinary properties. Cycloalyphatic-epoxy oligosiloxane (CEO) resin was shown to be a good candidate as a barrier material for the encapsulation purposes. Incorporation of inorganic nanoparticles such as Boehmite (BA) into polymers was observed to modify their specific characteristics, in particular, thermal, thermo-oxidative and barrier ones. In this work, novel BA-embedded organic inorganic hybrid nanocomposite material was engineered by combining the advantageous properties of hybrid polymers and nanoparticle enhancement effect. Impacts of particles on the photocuring kinetics, degree of crosslinking and the resultant changes in the thermal properties of the cured films were investigated. CEO synthesis via condensation reaction was confirmed by 1H and 29Si NMR. The particle distribution within the films was verified by SEM including transmission mode coupled with EDX elemental analysis. Photocuring kinetics and thermal properties of the films were studied by in situ FTIR spectroscopy and DSC with TGA, respectively.
Organic-inorganic nanostructured materials have drawn much attention over the past decade, particularly due to their versatile and outstanding properties. Possessing the properties between those of polymers and those of glasses, siloxane-based resins are non-toxic, easy to synthesize and process hybrid materials, that hold a promising potential in the field of advanced coatings.
Photocurable resins are nowadays widely used as coatings due to their unique advantages. In particular, cationic ring-opening curing is not inhibited by oxygen, leads to low degree of shrinkage and superior adhesion. The most important, it enables production of high-quality coatings within short exposure times without applying temperature, thus, minimizing the presence of the thermal stress in the substrate. Photocured Cycloaliphatic-Epoxy Oligosiloxane (CEO) resin was reported to be used as encapsulation material for organic electronics. However, further reinforcement of CEO properties is desired to achieve requested device lifetime. One of the common approaches to improve material characteristics is by embedding inorganic nanoparticles into polymer matrix. It has been shown that the resulted nanocomposites exhibit enhanced functional properties included but not limited by optical, mechanical, thermal and barrier ones.
In this work we focused on the incorporation of Boehmite nanoparticles (BA) into CEO matrix as a tool to strengthen the film properties and to study the main changes occurred in the material behavior with regard to its photocuring kinetics, thermal stability and glass transition. Particular interest was focused on the role of particle surface in nanocomposite properties. Hence, BA particles without (HP14) and with organic surface modifier (OS1) at different loadings
(up to 10 wt%) were applied in this study. Morphology investigation with SEM operated in transmission mode showed good BA dispersion forming
network-like structure. At the same time, distribution of particles differed for HP14 and OS1 as a result of different interaction in CEO-solvent-particles system. CEO structure obtained via non-hydrolytic sol-gel reaction was verified by 13C and 29Si NMR. In situ monitoring of film curing was performed using
RT-IR spectroscopy. A slight increase of final convention degree with particle incorporation was observed in contrast to the considerable decrease of curing efficiency reported previously for similar system. Further, the cured hybrid nanocomposite films were analyzed by TGA and DSC, which revealed impact of surface modifier on thermal stability and glass transition temperature.
UV-curing coatings are nowadays widely used due to their unique advantages. High-quality coatings can be obtained at short curing times and low temperatures so that thermal stress to the substrate is minimised. Photocured Cycloaliphatic-Epoxy Oligosiloxane (CEO) resin was reported to be used as encapsulation material for organic electronics. However, further reinforcement of CEO film properties is desired to achieve requested device lifetime.
In this work we introduced Boehmite nanoparticles (BA) into CEO matrix in order to modify the film properties and study the main changes of the material behaviour with regard to its photocuring kinetics, thermal stability and glass transition. Particular interest was focused on the role of particle surface in nanocomposite properties. Hence, BA particles without (HP14) and with organic surface modifier (OS1) at different loadings (up to 10 wt%) were applied in this study. Morphology investigation with SEM operated in transmission mode showed good BA dispersion forming network-like structure. At the same time, distribution of particles differed for HP14 and OS1 as a result of different interaction in CEO-solvent-particles system. CEO structure obtained via non-hydrolytic sol-gel reaction was verified by 13C and 29Si NMR. In situ monitoring of film curing was performed using RT-IR spectroscopy. No significant modification of final convention degree with particle incorporation was observed in contrast to considerable decrease of curing efficiency reported previously for similar system by Esposito et al.,2008. Further, cured hybrid nanocomposite films were analysed by TGA and DSC, which revealed impact of surface modifier on film thermal properties.
Elastomers are usually mechanically reinforced with high loadings of carbon black (CB) to achieve the properties demanded; high amounts of mineral flame retardants are used to fulfill fire safety requirements. In this study, multilayer graphene (MLG), a nanoparticle made of only 10 graphene sheets, is applied in low loadings, 3 parts per hundred rubber (phr) to reduce the total amount of filler or boost performance in hydrogenated acrylonitrilebutadiene rubber (HNBR). In the HNBR/MLG nanocomposites, 3 phr MLG replaced 15 phr CB, 3 phr aluminum trihydroxide (ATH), or 15 phr CB + 3 phr ATH. The nanocomposites were prepared via master batch by ultrasonically assisted solution mixing and subsequent conventional two-roll milling. A comprehensive study is presented, illustrating the impact of MLG on curing and mechanical properties; e.g. replacing 2.5 phr ATH with 3 phr MLG increased the Young's modulus by over 60% and hardness by 10%, while improving flame retardancy, and reducing the total heat evolved by 10%. MLG is a multifunctional filler, as demonstrated by various enhancements in terms of the mechanical and flame retardancy properties of the rubber composites.
Elastomers, such as hydrogenated acrylonitrile-butadiene rubber (HNBR) are usually mechanically reinforced with high loadings of carbon black (CB) to achieve the properties demanded; high amounts of mineral flame retardants are used to fulfill fire safety requirements. These high filler loadings sometimes cause deterioration of the physical properties of the material. In this study, multilayer graphene (MLG), a nanoparticle made of only 10 graphene sheets, is applied in low loadings (3 phr) to reduce the total amount of filler or boost performance.1,2,3 In former studies nanofiller achieved increased flame retardancy at very low lowdings.4,5,6 The dispersion of the nanofiller is essential for the properties of the nanocomposites.7 The nanocomposites were prepared via master batch by an ultrasonically assisted solution mixing and subsequent conventional two-roll milling.
SEM and TEM micrographs and rheological measurements revealed that the MLG nanoparticles were well dispersed in the HNBR matrix. In the HNBR nanocomposites, 3 phr MLG replaced 15 phr CB, 3 phr ATH or 15 phr CB + 3 phr ATH and achieved large consistent improvement in curing, rheological and mechanical properties of the HNBR. The nanocomposites with partial replaced CB reduced the filler loading up to 60% without any deterioration of the properties. The HNBR/MLG nanocomposites achieved an even higher Young’s modulus, hardness and thermal conductivity. MLG achieved advanced flame retardancy by improving the protection layer. The layer is created during the burning phase and acted as an afterglow suppressor. This study proposed the combination of ATH with MLG as a promising approach to reduce the amount of filler, in addition to improving the mechanical properties and fire performance of HNBR rubbers.