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- Flame retardancy (6)
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- Flame retardance (2)
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Eingeladener Vortrag
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Fibre reinforced polymers are used for a large variety of applications such as electronics and electrical engineering, transportation (railway vehicles, shipping, aviation), offshore and construction. In these applications limited fire hazards are a prerequisite. Passing distinct fire tests is demanded according to the different protection goals: mainly reduced ease of ignition and reaction to small flame for electronics, limited flame spread and heat release rate for transportation, and structure integrity under fire for offshore and construction.
Development of a New Intermediate Scale Method for Assessing Cables Reaction to Fire According CPR
(2013)
Nanocomposites of a charring polymer (like polyurethane foam) filled with aluminum phosphinate (AlPi) with or without melamine cyanurate (MelCy) have been prepared by microwave processing and their thermal stability and fire behavior have been studied. Results on the interaction between flame retardants and layered silicates were provided as well as detailed investigation of the char strength, which has been carried out using a suitably developed method based on dynamic-mechanic analysis.
Generally, the thermo-oxidative stability in presence of layered silicates was higher than the counterparts even if an additive rather than synergic effect took place; however, in some cases the interaction between clays and phosphinate led to a significant decrease of weight residue. In nitrogen the residue amounts were about the same but a higher amount of phosphorus was retained in the solid phase in presence of clays. Cone calorimeter results showed that the use of phosphinates led to a decrease of the PHRR; further addition of clays did not reduce the PHRR owing to the worse quality of char layer as demonstrated by the char strength test. However, it has been shown that the partial substitution of aluminum phosphinate with melamine cyanurate gave improved results: the AlPi–MelCy filled foams showed similar pHRR and THE but lower TSR and higher char strength than AlPi filled foams. It was also confirmed that phosphinate acted by flame inhibition but its action was depressed by the use of nanoclays owing to their interaction.
Flame retarded poly(butylene terephthalate) (PBT) is required for electronic applications and is mostly achieved by low molar mass additives so far. Three phosphorus-containing polyesters are suggested as halogen-free and polymeric flame retardants for PBT. Flame retardancy was achieved according to cone calorimeter experiments showing that the peak heat release rate and total heat evolved were reduced because of flame inhibition and condensed-phase activity. The presented polymers containing derivatives of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide form immiscible blend systems with PBT. Shear-rheology shows an increase in storage moduli at low frequencies. This is proposed as quantitative measure for the degree of phase interaction. The phase structure of the blends depends on the chemical structure of the phosphorus polyester and was quite different, depending also on the viscosity ratio between matrix and second phase. A lower viscosity ratio leads to two types of phases with spherical and additionally continuous droplets. Addition of the flame retardants showed no influence on the dielectric properties but on the mechanical behavior. The polymeric flame retardants significantly diminish the impact strength because of several reasons: (1) high brittleness of the phosphorus polyesters themselves, (2) thermodynamic immiscibility, and (3) weak phase adhesion. By adding a copolymer consisting of the two base polymers to the blend, an improvement of impact strength was obtained. The copolymer particularly acts as compatibilizer between the phases and therefore leads to a smaller phase size and to a stronger phase adhesion due to the formation of fibrils.
A test set-up in intermediate scale was conceived to investigate the structural integrity of materials under fire. The task was to develop a realistic test scenario targeting component-like behaviour. Carbon-fibre-reinforced sandwich specimens (500 X 500 X 20 mm) were used to examine failure mechanisms, times to failure and critical failure loads under compression. Fire tests were performed with fully developed fire applied to one side of the specimen by an oil burner. In a first test series, the applied load was varied, but the fully developed fire remained unchanged. In general, times to failure were short. Decreased load levels resulted in prolonged times to failure and led to a different failure mechanism. Results obtained in the test series were compared with a bench-scale study (150 X 150 X 20 mm) investigating identical material. The comparison clearly revealed the influence of size on the time to failure and the load-bearing capacity.
An intermediate-scale fire testing approach on the structural integrity of lightweight materials
(2013)
Carbon or glass über composites and Sandwich structures, the lightweight materials of choice for aviation, naval, offshore and construction show an enormous energy saving potential. Their combination of excellent specific mechanical properties, high corrosive resistance and thermal insulation properties in combination with various adoptable fabrication techniques leading to mass and fuel cost reduction. The most limiting single factor for a wider use of fibre reinforced plastics (FRP) in particular as elements for structural application is believed to be their fire behaviour (Mouritz and Gibson, 2006). FRPs promote burning by themselves consuming the stabilizing polymeric matrix while embedded fibers (glass, carbon) persisting the flame (Mouritz et ah, 2006). Already at elevated temperatures (100 - 200 °C) the matrix softens with a loss in mechanical properties (Perret et al., 2011, Mouritz and Gibson, 2006). For this reason the stability of the structural component is decreased severely. Fire behavior becomes the major hazard to worry about, increasingly demanding targetoriented investigation, suitable testing and tailored development.
Experimental approaches in the bench-scale have been proposed to investigate the structural integrity in the past (La Delfa et al., 2009, Gibson et al., 2010, Seggewiß, 2011, Mouritz and Gardiner, 2002, Schartel et al.). Ascribed to the small-scale neither the mechanical properties nor the effects of fire may be represented satisfactorily. Flence, the task is to perform more realistic investigations under adequate compressive loads in fully developed fires, based on suitable specimen sizes. Also (La Delfa et al., 2009)) have announced that it is evident that larger scale test of composites are needed. The aim of this study is to present a developed intermediate-scale test setup to perform more realistic investigations (Hörold et al.). Mechanical loading is generated by a column furnace in terms of compression due to a more severe response of specimens in fire tests (Seggewiß, 2011, Gibson et al., 2012, Feih et al., 2008, Feih et al., 2007). An oil burner used to determine the burnthrough resistance of thermal/acoustic insulation materials provides fire directly onto one side of the specimen (Federal Aviation Administration, 2003). Generating a fully developed fire the NexGen burner offers a homogenous heat flux of ~ 180 kW/m2. The intermediate-scale is addressed by specimen sizes either 500 x 500 mm or 1000 x 500 mm with a maximum thickness of 50 mm. The specimen attachment is realized by a compression device that was designed to apply the compressive loads, figure 1. The test setup for specimens with component like dimensions allows realistic investigations up to structural failure in absence and presence of fire load. A first test series was carried out with different levels of loading while the fire remained unchanged. Failure mechanisms, temperature distributions, diversity of FRPs regarding fiber, matrix, lay-up and core as well as flame retardant Systems are in the scope of investigation.
Functionalized graphene nanosheets TRGO and MLG 250, prepared from thermally reduced graphite oxide, represent attractive carbon additives for improving the performance of flame retardant polypropylene (PP-FR). The influence of carbon nanofiller type and content on morphology, thermal, mechanical, and electrical properties as well as the fire behavior of melt-extruded PP-FR is investigated. In contrast to conventional nano- and micron-sized carbon fillers such as expanded graphite (EG 40), nano-scaled carbon black (CB), and multiwall carbon nanotubes (CNT), only TRGO and MLG 250 afford uniform dispersion combined with simultaneously improved stiffness (+80%), electrical conductivity (3 × 10-5 S · cm-1) and enhanced flame retardancy of PP-FR, as expressed by lower peak heat release rate (-76%).
The use of coconut fiber (CF) agricultural waste was considered as an environmentally friendly and inexpensive alternative in flame retarded biocomposites. To decrease the high content of aluminum trihydrate (ATH) required, the thermal decomposition (thermogravimetry), flammability [oxygen index (LOI) and UL 94 test] and fire behavior (cone calorimeter) of a combination of CF and ATH were investigated in a commercial blend of thermoplastic starch (TPS) and cellulose derivatives. CF induced some charring activity, slightly decreasing the fire load and burning propensity in cone calorimeter test. ATH decomposes endothermically into water and inorganic residue. Significant fuel dilution as well as a pronounced residual protection layer reduces the fire hazards. Replacing a part of ATH with coconut fibers resulted in improved flame retardancy in terms of ignition, reaction to small flame, and flame-spread characteristics [heat release rate (HRR), fire growth rate (FIGRA), etc.]. The observed ATH and CF synergy opens the door to significant reduction of the ATH contents and thus to interesting flame retarded biocomposites.
Effect of well dispersed amorphous silicon dioxide in flame retarded styrene butadiene rubber
(2013)
Spherically shaped amorphous silicon dioxide with broad size particle distribution was used in combination with aluminium trihydroxide (ATH) in styrene butadiene rubber composites. The pyrolysis, flammability, fire properties, flame spread and gas diffusion were investigated. The kind and amount of ATH, but in particular the fine silicon dioxide chosen as an additive, influenced the thermal decomposition and fire behaviour of styrene butadiene rubber composites. Gravimetric gas sorption measurements showed that the gas diffusion was systematically lower with silicon dioxide. The initial pyrolysis gas release was hindered, increasing the temperature at which decomposition begins as well as the ignition time in fire tests. During combustion, ATH and silicon dioxide accumulate on the surface of the specimen, forming a residual protective layer. A reduced peak heat release rate and fire spread were observed. The addition of a special kind of silicon dioxide is proposed to play a key role in optimising fire retardancy.
The potential of a multi-component laminate composite material in terms of improved flame retardancy and adequate mechanical performance is discussed. A double-layer system based on a biodegradable polyhydroxyalkanoates blend was obtained by compression molding. A thin halogen-free flame-retarded layer was located at the top of a kenaf-fiber-reinforced core. Kenaf fibers acted as a carbonization compound promoting charring and building up a superficial insulating layer that protected the material throughout combustion. The impact of different skin/core thickness on the thermal and fire properties was investigated. Synergistic flame retardancy occurs in the cone calorimeter. Chemical and fire investigations confirmed a changed pyrolysis behavior in multicomponent materials. Promising results are obtained in terms of mechanical performance: higher flexural and impact properties were observed in the single fiber-reinforced layer.
Herein we investigate the influence of carbon additives with different particle sizes and shapes on the flame retardancy and mechanical properties of isotactic polypropylene. Thermally reduced graphite oxide (TRGO) and multi-layer graphene (MLG250), consisting of few graphene layers, are compared with spherical, tubular and platelet-like carbon fillers such as carbon black (CB), multiwall nanotubes (MWNT) and expanded graphite (EG). The different morphologies control the dispersion of the carbon particles in PP and play a key role in structure–property relationships. Uniformly dispersed CB, MLG250 and TRGO shift the onset temperature of PP decomposition to temperatures around 30 °C higher, induce a flow limit in the composites' melt viscosity and change drastically their fire behaviour. The prevented dripping and significantly increased heat absorption result in decreased time to ignition and hardly any change in the reaction to a small flame. Under forced-flaming conditions reductions in the peak heat release rate of up to 74% are achieved due to the formation of a protective layer of residue during combustion. The described effects of carbon nanomaterials on the properties of PP composites are most pronounced for well-exfoliated graphenes, making them preferable to less exfoliated, micron-sized expanded graphite or conventional spherical and tubular carbon nanoparticles.
Herein, we examine the influence of adding functionalized graphene (FG), distinct expanded graphites and carbon nanofillers such as carbon black and multiwall carbon nanotubes on mechanical properties, morphology, pyrolysis, response to small flame and burning behavior of a V-2 classified flame-retarded polypropylene (PP). Among carbon fillers, FG and multilayer graphene (MLG) containing fewer than 10 layers are very effectively dispersed during twin-screw extrusion and account for enhanced matrix reinforcement. In contrast to the other fillers, no large agglomerates are detected for PP-FR/FG and PP-FR/MLG, as verified by electron microscopy. Adding FG to flame-retardant PP prevents dripping due to reduced flow at low shear rates and shifts the onset of thermal decomposition to temperatures 40°C higher. The increase in the onset temperature correlates with the increasing specific surface areas (BET) of the layered carbon fillers. The reduction of the peak heat release rate by 76% is attributed to the formation of effective protection layers during combustion. The addition of layered carbon nanoparticles lowers the time to ignition. The presence of carbon does not change the composition of the evolved pyrolysis gases, as determined by thermogravimetric analysis combined with online Fourier-transformed infrared measurements. FG and well-exfoliated MLG are superior additives with respect to spherical and tubular carbon nanomaterials.