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Flame retarded polymeric materials are used in various applications in which a certain fire behavior is demanded. Protection goals are defined, such as limited flammability in terms of hindered sustained ignition or limited contribution to a fire, and these protection levels are tested with defined specimens or components in defined fire scenarios, that is to say, different fire tests. Passing a specific fire test by meeting whatever its demands is often the most important development goal, so the parameters of the different fire tests vary widely to emphasize different fire properties. Some fire tests are used to screen or provide a general assessment of flame retardant polymers during development, while other fire tests and tailored experiments are performed to address special phenomena or understand the flame retardancy modes of action. For all fire testing, the devil is in the details – demanding know-how and crucial efforts to manage the quality of investigations and advanced interpretation. This chapter aims to offer a structured overview of all these aspects.
Phosphonium-modified layered silicate epoxy resin nanocomposites were evaluated by testing the thermal/thermo-mechanical properties [differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), torsional pendulum, Sharpy toughness], flammability (limiting oxygen index LOI) and fire behavior (cone calorimeter with different irradiations). The morphology of the composites was determined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The drying conditions of phosphonium-modified layered silicate were varied in order to improve the nanocomposite formation and properties. The results were compared with using a commercial ammonium-modified montmorillonite. Enhanced nanocomposite formation was found for the commercial systems due to the amount of excess surfactant, but this effect was overcompensated through the advanced morphology of the phosphonium-modified systems. Several fire retardancy mechanisms and their specific influence on the different fire properties, such as ignitability, flammability, flame spread, total heat release (fire load), and the production of CO and smoke were discussed comprehensively. The main mechanism of layered silicate is a barrier formation influencing the flame spread in developing fires. Several minor mechanisms are significant, but important fire properties such as flammability or fire load are hardly influenced. Hence combinations with aluminum hydroxide and organo-phosphorus flame retardants were evaluated. The combination with aluminum hydroxide was a promising approach since it shows superposition in properties such as the fire load and only in some properties very little antagonism. The combination with an organo-phosphorus flame retardant disillusions, since it was characterized mainly by antagonism.
The thermal degradation and the combustion behavior of glass fiber-reinforced PA 66 materials containing red phosphorus were investigated. Thermogravimetry (TG), TG coupled with FTIR, and TG coupled with mass spectroscopy were used to investigate the thermal decomposition. The flame retardant red phosphorus was investigated with respect to the decomposition kinetics and the release of volatile products. The combustion behavior was characterized using a cone calorimeter. Fire risks and fire hazards were monitored versus external heat fluxes between 30 and 75 kW/m2. Red phosphorus acts in the solid phase and its efficiency depends on the external heat flux. The use of red phosphorus results in an increased amount of residue and in a corresponding decrease in total heat release. The decrease of the mass loss rate peak results in a corresponding decrease of the peak heat release. With increasing external heat flux applied the first effect on the total heat release decreases linearly, whereas the second effect on the peak heat release expands linearly. The investigation provides insight into the mechanisms of how the fire retardant PA 66 is achieved by red phosphorus controlling the degradation kinetics. Taking into account that a decrease of the volatile products also leads to a decrease of heat production in the flame zone and that the char acts as heat transfer barrier, a reduced pyrolysis temperature is suggested as a further feedback effect.
The flame retardant effect of zinc sulphide (ZnS) in plasticised poly(vinyl chloride) (PVC-P) materials was investigated. PVC-P containing different combinations of additives such as 5% ZnS, 5% of antimony oxide (Sb2O3) and 5% of mixtures based on Sb2O3 and ZnS were compared. The thermal degradation and the combustion behaviour were studied using thermogravimetry (TG), coupled with FTIR (TG-FTIR) or with mass spectroscopy (TG-MS), and a cone calorimeter, respectively. A detailed and unambiguous understanding of the decomposition and release of the pyrolysis products was obtained using both TG-MS and TG-FTIR. The influence of ZnS, Sb2O3 and the corresponding mixtures on the thermal decomposition of PVC-P was demonstrated. Synergism was observed for the combination of the two additives. The combustion behaviour (time to ignition, heat release, smoke production, mass loss, CO production) was monitored versus external heat fluxes between 30 and 75 kW m-2 with the cone calorimeter. Adding 5% of ZnS has no significant influence on the fire behaviour of PVC-P materials beyond a dilution effect, whereas Sb2O3 works as an effective fire retardant. Synergism of ZnS and Sb2O3 allows the possibility of replacing half of Sb2O3 by ZnS to reach equivalent fire retardancy.
Communication: Fire retardant coatings are deposited on polyamide-66 using plasma polymerisation. Chemical composition and thickness of deposits are adjusted varying the plasma treatment based on hexamethydisiloxane mixed with oxygen. The fire retardancy performances are evaluated using a cone calorimeter. The correlation between fire retardancy and thickness as well as chemical composition is discussed.
On the basis of two examples, temperature measurements are proposed within burning polymer specimen during the cone calorimeter test; especially to gain deeper insight into the actual pyrolysis conditions and flame retardancy mechanism. The heating and pyrolysis within a poly(methyl methacrylate) specimen were characterized, discussing the characteristic maximum heating rates (165-90°Cmin-1 decreasing with depth within the specimen and >275°Cmin-1 at the initial surface), pyrolysis temperature (454-432°C decreasing in accordance with decreasing heating rates), thickness of the pyrolysis zone (0.5-1.3 mm) and its velocity (1.2-2.1 mm min-1) as a function of sample depth and burning time. Thermally thick behaviour corresponds to a pyrolysis zone thickness of 0.74 mm and a velocity of 1.51 mm min-1 and occurs until the remaining specimen thickness is less than 8 mm. The shielding effect against radiation occurring in a layered silicate epoxy resin nanocomposite was investigated. It is the main flame retardancy effect of the silicate-carbon surface layer formed under fire. The reradiation from the hot surface is increased by a factor of around 4-5 when an irradiance of 70kWm-2 is applied. The energy impact into the pyrolysis zone is crucially reduced, resulting in a reduction of fuel production and thus heat release rate.
Fire retardancy effects in single and double layered sol-gel derived TiO2 and SiO2-wood composites
(2012)
Sol–gel derived TiO2 and SiO2-wood inorganic composites are prepared by direct vacuum infiltration of silicon and titanium alkoxide based precursors in pine sapwood in one or two cycles followed by a controlled thermal curing process. The resulting flame retardancy effect is investigated under two different fire scenarios using cone calorimetry and oxygen index (LOI). Heat release rates (HRR) especially the values for the second peak, are reduced moderately for all single layered composites. This effect is more pronounced for double layered composites where HRR was reduced up to 40 % showing flame retardancy potential in developing fires. Beside this, smoke release was lowered up to 72 % indicating that these systems had less fire hazards compared to untreated wood, whereas no meaningful improvement is realized in terms of fire load (total heat evolved) and initial HRR increase. However impressively, the LOI of the composites were increased up to 41 vol% in comparison to 23 vol% for untreated wood displaying a remarkable flame retardancy against reaction to a small flame. An approximate linear interdependence among the fire properties and the material loading as well as fire residue was observed. A residual protection layer mechanism is proposed improving the residue properties for the investigated composites.
Scientific publications addressing the durability of the flame retardance of cables during their long-term application are rare and our understanding lacks. Three commercial flame retardants, aluminum hydroxide, aluminum diethyl phosphinate (AlPi-Et), and intumescent flame retardant based on ammonium polyphosphate, applied in ethylene-vinyl acetate copolymer (EVA) model cables, are investigated. Different artificial aging scenarios were applied: accelerated weathering (UV-irradiation/temperature/rain phases), humidity exposure (elevated temperature/humidity), and salt spray exposure. The deterioration of cables’ surface and flame retardancy were monitored through imaging, color measurements, attenuated total reflectance Fourier transform infrared spectroscopy, and cone calorimeter investigations. Significant degradation of the materials’ surface occurred. The flame retardant EVA cables are most sensitive to humidity exposure; the cable with AlPi-Et is the most sensitive to the artificial aging scenarios. Nevertheless, substantial flame retardance persisted after being subjected for 2000 h, which indicates that the equivalent influence of natural exposure is limited for several years, but less so for long-term use.