Graphene oxide incorporating carbon fibre-reinforced composites submitted to simultaneous impact and fire: Physicochemical characterisation and toxicology of the by-products.

The toxicological profile of particulates released from carbon fibre-reinforced composites (CFC) incorporating nanoadditives, under impact and fire conditions (e.g. aircraft crash), is unknown to date. Our aim was to investigate the effects of simultaneous impact and fire on the physicochemical features of the particles released from CFCs produced from a graphene oxide (GO)-reinforced epoxy resin and the consequences on its toxicological profile. CFC samples with (CFC + GO) or without GO (CFC) were subjected to simultaneous impact and fire through a specific setup. Soot and residues were characterised and their toxicity was compared to that of virgin GO. Virgin GO was not cytotoxic but induced pro-inflammatory and oxidative stress responses. The toxicity profile of CFC was similar for soot and residue: globally not cytotoxic, inducing a pro-inflammatory response and no oxidative stress. However, an increased cytotoxicity at the highest concentration was potentially caused by fibres of reduced diameters or fibril bundles, which were observed only in this condition. While the presence of GO in CFC did not alter the cytotoxicity profile, it seemed to drive the pro-inflammatory and oxidative stress response in soot. On the contrary, in CFC + GO residue the biological activity was decreased due to the physicochemical alterations of the materials.

Functionalisable Epoxy-rich Electrospun Fibres Based on Renewable Terpene for Multi-Purpose Applications.

New bio-based polymers capable of either outperforming fossil-based alternatives or possessing new properties and functionalities are of relevant interest in the framework of the circular economy. In this work, a novel bio-based polycarvone acrylate di-epoxide (PCADE) was used as an additive in a one-step straightforward electrospinning process to endow the fibres with functionalisable epoxy groups at their surface. To demonstrate the feasibility of the approach, poly(vinylidene fluoride) (PVDF) fibres loaded with different amounts of PCADE were prepared. A thorough characterisation by TGA, DSC, DMTA and XPS showed that the two polymers are immiscible and that PCADE preferentially segregates at the fibre surface, thus developing a very simple one-step approach to the preparation of ready-to-use surface functionalisable fibres. We demonstrated this by exploiting the epoxy groups at the PVDF fibre surface in two very different applications, namely in epoxy-based carbon fibre reinforced composites and membranes for ω-transaminase enzyme immobilisation for heterogeneous catalysis.

Effect of Thermal Ageing on the Impact and Flexural Damage Behaviour of Carbon Fibre-Reinforced Epoxy Laminates.

Most of the composite materials that are used in aerospace structures have been manufactured using a thermostable matrix, as epoxy resin. The region of stability of these polymers is defined by the glass transition temperature (Tg). However, operating temperatures close and above the Tg can cause a variation in the properties of the polymer and consequently, modify the mechanical properties of the composite material. Therefore, it is necessary to understand the failure mechanisms that occur in the material in order to ensure stability and durability. The effect of temperature and time of exposure on the impact and flexural mechanical responses of carbon/epoxy composites are studied in this work. For that purpose, ageing treatments at temperatures below and above the Tg have been considered and then, impact and flexural tests have been performed. It was observed that thermal ageing cause two different effects: at temperatures below the Tg, there is an increase of the maximum strength because of a post-curing effect; however, the mechanical properties decrease at higher temperatures of thermal ageing due to the thermo-oxidation of the epoxy resin and the loss of adhesion in the matrix/fibre interface.

Effect of Thermal Ageing on the Impact Damage Resistance and Tolerance of Carbon-Fibre-Reinforced Epoxy Laminates.

Composite structures are particularly vulnerable to impact, which drastically reduces their residual strength, in particular, at high temperatures. The glass-transition temperature (Tg) of a polymer is a critical factor that can modify the mechanical properties of the material, affecting its density, hardness and rigidity. In this work, the influence of thermal ageing on the low-velocity impact resistance and tolerance of composites is investigated by means of compression after impact (CAI) tests. Carbon-fibre-reinforced polymer (CFRP) laminates with a Tg of 195 °C were manufactured and subjected to thermal ageing treatments at 190 and 210 °C for 10 and 20 days. Drop-weight impact tests were carried out to determine the impact response of the different composite laminates. Compression after impact tests were performed in a non-standard CAI device in order to obtain the compression residual strength. Ultrasonic C-scanning of impacted samples were examined to assess the failure mechanisms of the different configurations as a function of temperature. It was observed that damage tolerance decreases as temperature increases. Nevertheless, a post-curing process was found at temperatures below the Tg that enhances the adhesion between matrix and fibres and improves the impact resistance. Finally, the results obtained demonstrate that temperature can cause significant changes to the impact behaviour of composites and must be taken to account when designing for structural applications.

Flame Retardancy of Low-Viscosity Epoxy Resins and Their Carbon Fibre Reinforced Composites via a Combined Solid and Gas Phase Mechanism.

Low viscosity, potentially renewable aliphatic epoxy resins, appropriate for processing with injection techniques were flame retarded with the use of resorcinol bis(diphenyl phosphate) (RDP), acting predominantly in the gas phase, ammonium polyphosphate (APP), acting in the solid phase, and their combination. Samples of gradually increasing phosphorus (P) content (1%, 2%, 3%, 4%, and 5%) and mixed formulations with 2% P from APP and 2% P from RDP were prepared. The fire retardancy of matrix and carbon fibre reinforced samples was examined by limiting oxygen index (LOI), UL-94 tests, and mass loss calorimetry. The thermal stability of the matrices was investigated by thermogravimetric analysis, whereas the effect of flame retardants (FRs) on the crosslinking process and glass transition temperature was evaluated by differential scanning calorimetry in matrices and by dynamic mechanical analysis in composites. According to the results, although the trifunctional glycerol -based (GER) and the tetrafunctional pentaerythritol-based (PER) epoxy resins have a similar initial LOI and horizontal burning rate, GER has an approximately 1.5 times higher peak of heat release rate (pHRR) than PER. At least 4% P content is necessary to reach a reasonable improvement in fire performance in these resin transfer molding (RTM)-compatible systems and with the same FR-content PER reaches better fire performance. RDP has an early gas phase effect at the beginning of degradation, while later on the solid phase action of APP prevails, although in composites hindered by the reinforcing carbon fibres. In PER composites, the combination of APP and RDP had a synergistic effect, leading to a pHRR of 218 kW/m² and total heat release of 18.2 MJ/m².