TY - JOUR A1 - Tomiak, F. A1 - Schartel, Bernhard A1 - Wolf, M. A1 - Drummer, D. T1 - Particle Size Related Effects of Multi-Component Flame-Retardant Systems in poly(butadiene terephthalate) N2 - Aluminum tris (diethylphosphinate) (AlPi) is known to have an efficient flame-retardant effect when used in poly(butadiene terephthalates) (PBT). Additionally, better flame-retardant effects can be achieved through the partial substitution of AlPi by boehmite in multi-component systems, which have been shown to be an effective synergist due to cooling effects and residue formation. Although the potential of beneficial effects is generally well known, the influence of particle sizes and behavior in synergistic compositions are still unknown. Within this paper, it is shown that the synergistic effects in flammability measured by limiting oxygen index (LOI) can vary depending on the particle size distribution used in PBT. In conducting thermogravimetric analysis (TGA) measurements, it was observed that smaller boehmite particles result in slightly increased char yields, most probably due to increased reactivity of the metal oxides formed, and they react slightly earlier than larger boehmite particles. This leads to an earlier release of water into the system enhancing the hydrolysis of PBT. Supported by Fourier transformation infrared spectroscopy (FTIR), we propose that the later reactions of the larger boehmite particles decrease the portion of highly flammable tetrahydrofuran in the gas phase within early burning stages. Therefore, the LOI index increased by 4 vol.% when lager boehmite particles were used for the synergistic mixture. KW - Flame retardants KW - Aluminum diethylphosphinate KW - Boehmite KW - Poly(butadiene terephthalates) (PBT) KW - Mechanical properties PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509286 DO - https://doi.org/10.3390/polym12061315 SN - 2073-4360 VL - 12 IS - 6 SP - 1315 PB - MDPI AN - OPUS4-50928 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Santandrea, A. A1 - Vignes, A. A1 - Krietsch, Arne A1 - Brunello, D. A1 - Perrin, L. A1 - Laurent, A. A1 - Dufaud, O. T1 - Evaluating the explosion severity of nanopowders: International standards versus reality N2 - The maximum explosion overpressure and the maximum rate of pressure rise, which characterize thedust explosion severity, are commonly measured in apparatuses and under specific conditions defined byinternational standards. However, those standards conditions, designed for micropowders, may not befully adapted to nanoparticles. Investigations were conducted on different nanopowders (nanocellulose,carbon black, aluminum) to illustrate their specific behaviors and highlight the potential inadequacyof the standards. The influence of the sample preparation was explored. Various testing procedureswere compared, focusing on the dust cloud turbulence and homogeneity. Dust dispersion experimentsevidenced the importance of the characterization of the dust cloud after dispersion, due to the frag-mentation of agglomerates, using metrics relevant with nanoparticles reactivity (e.g. surface diameterinstead of volume diameter). Moreover, the overdriving phenomenon (when the experimental resultsbecome dependent of the ignition energy), already identified for micropowders, can be exacerbated fornanoparticles due to their low minimum ignition energy and to the high energy used under standardconditions. It was evidenced that for highly sensitive nanopowders, pre-ignition phenomenon can occur.Finally, during severe explosions and due to a too long opening delay of the ‘fast acting valve’, the flamecan go back to the dust container. KW - Dust explosions KW - Gas explosions KW - Minimum ignition temperature KW - Hybrid mixtures PY - 2020 DO - https://doi.org/10.1016/j.psep.2020.04.011 VL - 138 SP - 279 EP - 291 PB - Elsevier B.V. AN - OPUS4-50944 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Palis, Stephan A1 - Sträubig, Felix A1 - Voigt, Sascha A1 - Knaust, Christian T1 - Experimental investigation of the impact of water mist on high-speed non-premixed horizontal methane jet fires N2 - In this paper, the influence of a fixed water mist firefighting system on a high-speed non-premixed horizontal methane jet fire is investigated with focus on its effect on temperatures and heat load of the jet fire and on ist surroundings. Six tests are performed in which gas is released out of an orifice with a diameter of 1 mm and a release pressure of up to 186 bar. In addition to temperature and radiation measurements, the release pressure, gas mass flow rate and exhaust gas concentrations are detected to determine the heat release. Video and IRanalysis are used to evaluate the interactions between jet fire and water mist. The experiments show, that water mist reduces the temperatures inside the jet fire flow field and its radiative heat flux. It can lower the Risk of ignition of adjacent surfaces and materials, as temperatures fall below autoignition temperatures of common materials like plastics. Although water mist does not extinguish the fire, it has an impact on the energy release by reducing combustion efficiency due to heat exchange with the water mist and oxygen displacement. KW - Fixed firefighting system KW - Jet fire KW - Water mist KW - Fire test KW - Methane KW - Supersonic flow PY - 2020 DO - https://doi.org/10.1016/j.firesaf.2020.103005 VL - 114 SP - 103005 PB - Elsevier Ltd. AN - OPUS4-50963 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Voigt, Sascha A1 - Sträubig, Felix A1 - Palis, Stephan A1 - Kwade, A. A1 - Knaust, Christian T1 - CFD-analysis of Sensible Enthalpy Rise Approach to determine the heat release rate of electric-vehicle-scale lithium-ion batteries N2 - This paper analyses the suitability of the Sensible Enthalpy Rise Approach for measuring the heat release rate of electric-vehicle-scale lithium-ion batteries. An apparatus is designed that meets the conditions of an electric-vehicle-scale lithium-ion battery fire by using cement board as wall material. Modifications of the Sensible Enthalpy Rise Methodology are presented due to the high emissivity and inhomogeneous temperature distribution of the apparatus wall material: a power 4 approach for the heat flow from the walls to the ambient air and an alternative determination methodology for the wall temperature. A one factor at a time parameter study is performed with Computational Fluid Dynamics simulations, investigating a new calibration method based on a fit approach compared to common methods, the wall temperature determination, the approach for the ambient heat flow, the calibration power and the volume flow at the outlet. The simulations show, that suitable estimations of the heat release rate are obtained by using the modifications for wall temperature determination and the power 4 approach for the ambient heat flow. The three calibration methods provide suitable constants, if the calibration power in the same order of magnitude as the mean of the heat release rate profile of the test object. KW - Lithium-ion batteries KW - Heat Release Rate KW - Calorimetry KW - Sensible Enthalpy Rise Approach KW - Computational Fluid Dynamics PY - 2020 DO - https://doi.org/10.1016/j.firesaf.2020.102989 VL - 114 SP - 1 EP - 14 PB - Elsevier Ltd. AN - OPUS4-50964 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Morys, Michael A1 - Häßler, Dustin A1 - Krüger, Simone A1 - Schartel, Bernhard A1 - Hothan, Sascha T1 - Beyond the standard time-temperature curve: Assessment of intumescent coatings under standard and deviant temperature curves N2 - Nowadays there are intumescent coatings available for diverse applications. There is no established assessment of their protection performance besides the standard time-temperature curve, but natural fire scenarios often play an important role. A reliable straightforward performance-based assessment is presented. The effective thermal conductivity per thickness is calculated based on intermediate-scale fire tests. The optimum thermal insulation, the time to reach it, and the time until contingent failure of the coating are used for an assessment independent of the heating curve. The procedure was conducted on four different commercially intumescent coatings for steel construction, one solvent-based, one waterborne, one epoxy-based, and a bandage impregnated with a waterborne coating. The performance was studied under four different but similar shaped heating curves with different maximum temperatures (standard time-temperature curve, hydrocarbon curve and two self-designed curves with reduced temperature). The thermal protection performance is crucially affected by the residue morphology. Therefore, a comprehensive morphology analysis, including micro-computed tomography and scanning electron microscopy, was conducted on small-scale residues (7.5 x 7.5 cm2). Two different types of inner structures and the residue surface after different heat exposures were discussed in terms of their influence on thermal protection performance. KW - Intumescence KW - Coating KW - Computed tomography KW - Small scale KW - Heating curves KW - Residue morphology PY - 2020 DO - https://doi.org/10.1016/j.firesaf.2020.102951 SN - 0379-7112 VL - 112 SP - 102951 PB - Elsevier Ltd. AN - OPUS4-50334 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, Martin A1 - Wu, Dejian A1 - Zhao, P. A1 - Tan, X. A1 - Huang, W. A1 - Qianc, X. T1 - Minimum explosion concentrations of coal dusts with CH4/H2/CO below the gas lower explosion limit N2 - A 20-L spherical explosion chamber was used to investigate the explosion characteristics of dust clouds in air with the presence of flammable gas which is lower than its lower explosion limit (LEL). including minimum explosion concentration (MEC) of dust. Explosion pressure (Pex) and explosion pressure rise (dp/dt)ex). Two dust samples (anthracite coal, bituminous coal) and were three flammable gases (CH4, H2 and CO) were tested. Experimental results showed that the explosion of hybrid mixtures occurs when both dust and gas concentrations are lower than the LEL/MEC of the single substances. Meanwhile. all flammable gases with different volume fractions have distinct effects on the MEC. Pex and (dp/dt)ex of the dust samples. With the increase of the flammable gas concentration. either the Pex and (dp/dt)ex increase or the MEC decreases for all the hybrid mixtures of both two dust samples. At the same concentration of coal dusts. the addition of CH4 promotes higher explosion risks than the other two flammable gases. The distribution of (dp/dt)ex is quite different with the restricted area defined by empirical formulas. These results improve our understanding of the explosion behaviour and the explosion risk of hybrid dust-gas mixtures in air. KW - Dust explosions KW - Gas explosions KW - Minimum explosible concentration KW - Lower explosion limit KW - Hybrid mixtures PY - 2020 DO - https://doi.org/10.1016/j.fuel.2019.116401 SN - 0032-5910 VL - 260 SP - UNSP 116401 PB - Elsevier Sci. Ltd. AN - OPUS4-49956 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wu, Dejian A1 - Schmidt, Martin A1 - Tan, X. A1 - Zhao, P. A1 - Huang, W. A1 - Qian, X. T1 - Minimum ignition temperature of carbonaceous dust clouds in air with CH4/H-2/CO below the gas lower explosion limit N2 - Godbert-Greenwald furnace was used to investigate the minimum ignition temperature of dust clouds (MITC) in air with the presence of flammable gas which is lower than its lower explosion limit (LEL). Three flammable gases (CH4, H2 and CO) and three carbonaceous dusts (anthracite coal, bituminous coal and sweet potato starch) were tested. Results showed that all flammable gases have distinct effects on the MITC of the dust samples and volatile matter content of dust plays an important role during the ignition process. Specifically, the MITC of anthracite coal dust decreased from 610 °C to 560 °C, 580 °C and 570 °C with 3% CH4, 3% CO and 2.5% H2, respectively. Moreover, a heterogeneous ignition mechanism model was proposed to verify the equally global ignition characteristic between hybrid anthracite coal-CxHy mixture and bituminous coal. All three gases had an ignorable effect on the MITC of starch dust considering the experimental error. The presence of CO and H2 slightly promoted the ignition of bituminous coal dust, but the addition of CH4 showed a distinct concentration effect on the MITC of bituminous coal: the MITC decreased with 1% CH4 while increased with 2% and 3% CH4. This negative-effect of flammable gases at such low concentrations on ignition temperature of bituminous coal dusts was found for the first time. Furthermore, the presence of the 2nd flammable gas had a smaller effect on the MITC of dust samples with a higher volatile content, resulted from the competition of heterogeneous and homogeneous ignition mechanisms. KW - Dust explosions KW - Gas explosions KW - Minimum ignition temperature KW - Hybrid mixtures PY - 2020 DO - https://doi.org/10.1016/j.fuel.2019.116811 SN - 0016-2361 VL - 264 SP - 116811 PB - Elsevier Ltd. AN - OPUS4-50856 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schartel, Bernhard T1 - Flammschutz für technische Kunststoffte für elektronische Anwendungen N2 - Das Brandverhalten stellt wie das ausgezeichnete elektrische Isolationsverhalten, die geringen elektrischen Verluste, die Verarbeitbarkeit und Formbarkeit eine der wesentlichen Schlüsseleigenschaften im Eigenschaftsprofil von Polymerwerkstoffen in der Elektronik und der Elektrotechnik dar. Dabei bedarf es einer Ausrüstung der Polymerwerkstoffe mit Flammschutzmittel. Die Entwicklung von immer effizienteren, synergistischen und multifunktionalen Multikomponentensystemen ist dabei eine herausragende Quelle für Innovation. Die Entwicklung und Verbesserung der werkstoff- und anwendungsspezifischen Flammschutzlösungen bestimmen die aktuellen und zukünftigen Polymermaterialien in der Elektronik und Elektrotechnik mit. Der Vortrag stellt anhand von Beispielen einige der erfolgreichen Konzepte dar. Es wird versucht, über das wissenschaftlich-systematische Verständnis Grundprinzipien und vielversprechende Lösungsstrategien zu verdeutlichen. T2 - Kunststoff trifft Elektronik, KUZ Kunststoffzentrum in Leipzig CY - Leipzig, Germany DA - 29.01.2020 KW - Flame retardant KW - Ssynergy KW - Flame retardant mode of action KW - UL 94 KW - Cone calorimeter PY - 2020 AN - OPUS4-50495 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Schartel, Bernhard A1 - Kebelmann, Katharina ED - Hu, Y. ED - Wang, X. T1 - Fire testing for the development of flame retardant polymeric materials N2 - 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. KW - Fire testing KW - Flame retardant KW - Fire retardant KW - Flammability KW - Ignition KW - Oxygen index KW - Cone calorimeter KW - UL 94 KW - Developing fire KW - Uncertainty KW - Fire resistance PY - 2020 SN - 978-1-138-29578-7 SP - 35 EP - 55 PB - CRC Press AN - OPUS4-50236 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Battig, Alexander A1 - Markwart, J. C. A1 - Wurm, F. R. A1 - Schartel, Bernhard T1 - Sulfur's role in the flame retardancy of thio-ether–linked hyperbranched polyphosphoesters in epoxy resins N2 - Hyperbranched polyphosphoesters are promising multifunctional flame retardants for epoxy resins. These polymers were prepared via thiol-ene polyaddition reactions. While key chemical transformations and modes of actions were elucidated, the role of sulfur in the chemical composition remains an open question. In this study, the FR-performance of a series of phosphorus-based flame retardant additives with and without sulfur (thioethers or sulfones) in their structure are compared. The successful synthesis of thio-ether or sulfone-containing variants is described and verified by 1H and 31P NMR, also FTIR and MALDI-TOF. A decomposition process is proposed from pyrolytic evolved gas analysis (TG-FTIR, Py-GC/MS), and flame retardancy effect on epoxy resins is investigated under pyrolytic conditions and via fire testing in the cone calorimeter. The presence of sulfur increased thermal stability of the flame retardants and introduced added condensed phase action. Likely, Sulfur radical generation plays a key role in the flame-retardant mode of action, and sulfones released incombustible SO2. The results highlight the multifunctionality of the hyperbranched polymer, which displays better fire performance than its low molar mass thio-ether analogue due to the presence of vinyl groups and higher stability than its monomer due to the presence of thio-ether groups. KW - Phosphoester KW - Hyperbranched KW - Sulfur KW - Thio-ether KW - Flame retardant KW - Epoxy resin PY - 2020 DO - https://doi.org/10.1016/j.eurpolymj.2019.109390 SN - 0014-3057 VL - 122 SP - 109390 PB - Elsevier Ltd. AN - OPUS4-50238 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -