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The fire behaviour of light-weight material used in structural applications is regarded as the main challenge to be solved for mass transportation. The task is to perform realistic experiments, including a mechanical test scenario under fully developed fires, to improve the material's reliability in structural applications. Our approach utilises an intermediate-scale test set-up (specimen size 500 × 500 mm) to apply realistic compressive loads and fully developed fires directly to one side of a carbon-fibre-reinforced sandwich composite. Three different intumescent coatings were applied to sandwich structures and compared to a bench-scale study. The results emphasise intumescent coatings as a promising method to sustain fire resistance, multiplying the time to failure. Nevertheless, the realistic intermediate-scale test using severe direct flame application underlines the extremely short failure times when the actual composite components are tested without any additional insulation.
Distinct approaches are used to reduce the fire risks of polymers, a key issue for many industrial applications. Among the variety of approaches, the use of synergy in halogen-free multicomponent systems is one of the most auspicious. To optimize the composition of such flame-retardant systems it is essential to understand the mechanisms and the corresponding chemistry in the condensed phase. In this work different methods are used, including cone calorimeter, thermogravimetry (TG), and TG-FTIR, with the main focus on the solid-state NMR analysis of the solid residues. The structural changes in the condensed phase of two thermoplastic elastomer systems based on copolymer styrene-ethylene-butadiene-styrene (TPE-S) were investigated: TPE-S/aluminium diethylphosphinate (AlPi)/magnesium hydroxide (MH) and TPE-S/AlPi/zinc borate (ZB)/poly(phenylene oxide) (PPO). Strong flame inhibition is synergistically combined with protective layer formation. 13C-, 27Al-, 11B- and 31P MAS NMR (magic angle spinning nuclear magnetic resonance) experiments using direct excitation with a single pulse and 1H31P cross-polarization (CP) were carried out as well as double resonance techniques. Magnesium phosphates were formed during the pyrolysis of TPE-S/AlPi/MH, while for the system TPE-S/AlPi/ZB/PPO zinc phosphates and borophosphates were observed. Thus, the chemistry behind the chemical interaction was characterized unambiguously for the investigated systems.
An experimental and numerical investigation of the effect of bisphenol A bis(diphenyl phosphate) (BDP) and polytetrafluoroethylene (PTFE) on the fire behaviour of bisphenol A polycarbonate/acrylonitrile butadiene styrene (PC/ABS) in the vertical UL 94 scenario is presented. Four PC/ABS blends were discussed, which satisfy different UL 94 classifications due to the competing effects of gasification, charring, flame inhibition and melt flow/dripping. For numerical investigation, the particle finite element method (PFEM) is used. Its capability to model the complex fire behaviour of polymers in the UL 94 is analysed. The materials' properties are characterised, in particular the additives impact on the dripping behaviour during thermal exposure. BDP is an efficient plasticiser; adding PTFE prevents dripping by causing a flow limit. PFEM simulations reproduce the dripping and burning behaviour, in particular the competition between gasification and dripping. The thermal impact of both the burner and the flame is approximated taking into account flame inhibition, charring and effective heat of combustion. PFEM is a promising numerical tool for the investigation of the fire behaviour of polymers, particularly when large deformations are involved. Not only the principal phenomena but also the different UL 94 classifications and the extinction times are well predicted.
Elastomers are usually reinforced and employed in different applications. Various different nanoparticles, including layered silicates, carbon nanotubes, and expanded graphite, are currently being used as nanofiller. Multilayer Graphene (MLG) is proposed as promising nanofiller to improve the functional properties of Chlorine-Isobutylene-Isoprene Rubber (CIIR), Nitrile-Butadiene Rubber (NBR), Natural Rubber (NR) and Styrene–Butadiene Rubber (SBR) at low concentrations. MLG is constituted by only approximately 10 graphene sheets. Nanocomposites with extremely low MLG content (3 phr) showed evident improvement in rheological, mechanical and curing properties. The Young's modulus of the nanocomposites increased more than twice in comparison with the unfilled rubbers. MLG also improved the weathering resistance of the different rubbers. The nanocomposites conserved their initial mechanical properties against weathering exposure.
The influence of distinct carbon based nanofillers: expanded graphite (EG), conducting carbon black (CB), thermally reduced graphene oxide (TRGO) and multi-walled carbon nanotubes (CNT) on the thermal, dielectric, electrical and rheological properties of polybutylene terephthalate (PBT) was examined. The glass transition temperature (Tg) of PBT nanocomposites is independent of the filler type and content. The carbon particles act as nucleation agents and significantly affect the melting temperature (Tm), the crystallization temperature (Tc) and the degree of crystallinity of PBT composites. PBT composites with EG show insulating behaviour over the tested concentration range of 0.5 to 2 wt.-% and hardly changed rheological behaviour. CB, CNT and TRGO induce electrical conductivity to their particular PBT composites by forming a conducting particle network within the polymer matrix. CNT reached the percolation threshold at the lowest concentration (<0.5 wt.-%), followed by TRGO (<1 wt.-%) and CB (<2 wt.-%). With the formation of a particle network, the flow behaviour of composites with CB, CNT and TRGO is affected, i.e., a flow limit occurs and the melt viscosity increases. The degree of influence of the carbon nanofillers on the rheological properties of PBT composites follows the same order as for electrical conductivity. Electrical and rheological results suggest an influence attributed to the particle dispersion, which is proposed to follow the order of EG<< CB<TRGO<CNT.
The characteristic influences of increasing concentrations of graphene, expanded graphite (EG), carbon black (CB), and multiwall carbon nanotubes (MWNT) are investigated on pyrolysis, reaction to small flame, burning behavior, and on electrical, thermal, and rheological properties of flame retarded polypropylene (PP-FR). The property-concentration dependency is different for the various material properties, as threshold, linear, and leveling off functions were observed. Increasing concentrations of carbon nanoparticles resulted in a decrease in the electrical resistivity of the polymer by crossing the percolation threshold. The developing nanoparticle network changes melt flow behavior for small shear rates, increases thermal conductivity and therefore, affects the UL 94 classification and oxygen index. The onset temperature of PP decomposition is shifted to temperatures up to 37°C higher; the peak heat release rate is reduced by up to 74% compared to PP-FR. Both effects leveled off with increasing particle concentration. Among the four carbon nanomaterials tested, graphene presents superior influence on composite properties over the tested concentration range and outperforms commercial CB, MWNT, and EG. POLYM. COMPOS., 36:12301241, 2015.
Multicomponent flame retardant systems containing aluminum diethylphosphinate in thermoplastic styrene–ethylene–butylene–styrene elastomers are investigated (oxygen index, UL 94, cone calorimeter, and mechanical testing). Solid-state nuclear magnetic resonance, scanning electron microscopy, and elemental analysis illuminate the interactions in the condensed phase. Thermoplastic styrene–ethylene–butylene–styrene elastomers are a challenge for flame retardancy (peak heat release rate at 50 kW m-2 > 2000 kW m-2, oxygen index = 17.2 vol%, no UL-94 horizontal burn rating) since it burns without residue and with a very high effective heat of combustion. Adding aluminum diethylphosphinate results in efficient flame inhibition and improves the reaction to small flame, but it is less effective in the cone calorimeter. Its efficacy levels off for amounts >~25 wt%. As the most promising synergistic system, aluminum diethylphosphinate/melamine polyphosphate was identified, combining the main gas action of aluminum diethylphosphinate with condensed phase mechanisms. The protection layer was further improved with several adjuvants. Keeping the overall flame retardant content at 30 wt%, aluminum diethylphosphinate/melamine polyphosphate/titanium dioxide and aluminum diethylphosphinate/melamine polyphosphate/boehmite were the best approaches. An oxygen index of up to 27 vol% was achieved and a horizontal burn rating in UL 94 with immediate self-extinction; peak heat release rate decreased by up to 85% compared to thermoplastic styrene–ethylene–butylene–styrene elastomers, to <300 kW m-2.