TY - JOUR A1 - Brehme, Sven A1 - Köppl, T. A1 - Schartel, Bernhard A1 - Fischer, O. A1 - Altstädt, V. A1 - Pospiech, D. A1 - Döring, M. T1 - Phosphorus polyester - an alternative to low-molecular-weight flame retardants in poly(butylene terephthalate)? N2 - Pyrolysis, fire behaviour and mechanical properties of a blend of poly(butylene terephthalate) (PBT) with a phosphorus polyester (PET-P-DOPO) are investigated and compared with PBT/aluminium diethylphosphinate (AlPi-Et) composites. The PBT/PET-P-DOPO is immiscible and exhibits gas-phase and condensed-phase activity, whereas AlPi-Et in PBT results mainly in flame inhibition. Only higher loadings of AlPi-Et yield significant condensed-phase activity. Using the same phosphorus content, PBT/PET-P-DOPO and PBT/AlPi-Et exhibit similar reductions in fire load (22%) and flame spread (17% assessed by fire growth rate, FIGRA), compared with PBT. In contrast to AlPi-Et, the addition of PET-P-DOPO does not decrease the tensile strength of PBT. Thus, PET-P-DOPO is an interesting alternative to low-molecular-weight flame retardants. KW - Aluminium phosphinate KW - Blends KW - 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide KW - Flame retardance KW - Polyesters PY - 2012 DO - https://doi.org/10.1002/macp.201200072 SN - 1022-1352 SN - 1521-3935 VL - 213 IS - 22 SP - 2386 EP - 2397 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-26982 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Despinasse, Marie-Claire A1 - Schartel, Bernhard T1 - Influence of the structure of aryl phosphates on the flame retardancy of polycarbonate/acrylonitrile-butadiene-styrene N2 - The impact of the chemical structure of four different aryl bisphosphates on the flame retardancy of bisphenol A polycarbonate/acrylonitrile–butadiene–styrene blends (PC/ABS) was investigated. The impact of the bridging unit was studied, by comparing bisphenol A bis(diphenyl phosphate) BDP with biphenyl bis(diphenyl phosphate) BBDP and hydroquinone bis(diphenyl phosphate) HDP; as well as the influence of an aromatic substitution by comparing BBDP with biphenyl bis (di-2,6-xylyl phosphate) BBXP. The blends were investigated in terms of pyrolysis (thermogravimetry TG, TG coupled with Fourier transformed infrared spectroscopy (FTIR) and mass spectrometry (MS)) and fire performance (cone calorimeter, LOI, UL 94). The decomposition temperature of the flame retardant is a main parameter enabling a condensed phase interaction with PC decomposition products. The phosphate esters reacting with phenolic groups during pyrolysis were shown to increase cross-linking and reduce the hydrolysis/alcoholysis of the carbonate group. Variation of the aromatic substitution with the use of biphenyl bis (di-2,6-xylyl phosphate) led to reduced performance, highlighting the importance of the reactivity of the flame retardant with the decomposing PC. KW - Bisphenol A polycarbonate/acrylonitrile–butadiene–styrene (PC/ABS) KW - Flame retardancy KW - Flammability KW - Phosphate esters KW - Pyrolysis PY - 2012 DO - https://doi.org/10.1016/j.polymdegradstab.2012.07.005 SN - 0141-3910 SN - 1873-2321 VL - 97 IS - 12 SP - 2571 EP - 2580 PB - Applied Science Publ. CY - London AN - OPUS4-26969 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gallo, Emanuela A1 - Schartel, Bernhard A1 - Acierno, Domenico A1 - Cimino, F. A1 - Russo, P. T1 - Tailoring the flame retardant and mechanical performances of natural fiber-reinforced biopolymer by multi-component laminate N2 - 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. KW - A. Fibres KW - A. Layered structures KW - D. Thermal analysis KW - D. Mechanical testing PY - 2013 DO - https://doi.org/10.1016/j.compositesb.2012.07.005 SN - 1359-8368 VL - 44 IS - 1 SP - 112 EP - 119 PB - Elsevier CY - Oxford [u.a.] AN - OPUS4-26741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Köppl, T. A1 - Brehme, Sven A1 - Pospiech, D. A1 - Fischer, O. A1 - Wolff-Fabris, F. A1 - Altstädt, V. A1 - Schartel, Bernhard A1 - Döring, M. T1 - Influence of polymeric flame retardants based on phosphorus-containing polyesters on morphology and material characteristics of poly(butylene terephthalate) N2 - 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. KW - Polyesters KW - Blends KW - Miscibility KW - Rheology KW - Flame retardance PY - 2013 DO - https://doi.org/10.1002/app.38520 SN - 0021-8995 SN - 1097-4628 VL - 128 IS - 5 SP - 3315 EP - 3324 PB - Wiley InterScience CY - Hoboken, NJ AN - OPUS4-27957 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gallo, Emanuela A1 - Sánchez-Olivares, G. A1 - Schartel, Bernhard T1 - Flame retardancy of starch-based biocomposites - aluminium hydroxide-coconut fiber synergy N2 - 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. KW - Biocomposites KW - Flammability KW - Starch KW - Aluminium hydroxide KW - Coconut fiber PY - 2013 SN - 0032-2725 VL - 58 IS - 5 SP - 395 EP - 402 PB - Industrial chemistry research inst CY - Warszawa, Poland AN - OPUS4-28513 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Despinasse, Marie-Claire A1 - Schartel, Bernhard T1 - Aryl phosphate-aryl phosphate synergy in flame-retarded bisphenol A polycarbonate/acrylonitrile-butadiene-styrene N2 - The pyrolysis and fire performance of bisphenol A polycarbonate/acrylonitrile-butadiene-styrene (PC/ABS) flame-retarded by a mixture of two aryl bisphosphates were investigated by thermogravimetry-coupled with FTIR, oxygen index (LOI), UL 94 and cone calorimeter. Both flame retardants, bisphenol A bis (diphenyl phosphate) BDP and hydroquinone bis (diphenyl phosphate) HDP, show gas-phase and condensed-phase actions. When mixed together at different ratios, a synergy is observed in terms of pyrolysis and fire residues as well as in effective heat of combustion (THE/ML). The synergisms were quantified and confirmed mathematically by the evaluation of the synergistic effect index (SE). All LOI values for the flame-retarded blends are between 29% and 32%, as opposed to 23% for PC/ABS, and UL94 testing results in V-0 at 1.6 mm instead of HB. Investigations on the binary system BDP + HDP reveal that BDP and HDP interact with each other, yielding stable intermediate products which are proposed to increase the thermal stability of the PC/ABS + BDP/HDP blends. Oligomeric phosphate esters are presumed to form via transesterification. KW - Flame retardancy KW - PC/ABS KW - Pyrolysis KW - Aryl phosphate KW - Synergy KW - Combustion PY - 2013 DO - https://doi.org/10.1016/j.tca.2013.04.006 SN - 0040-6031 SN - 1872-762X VL - 563 SP - 51 EP - 61 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-28515 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dittrich, Bettina A1 - Wartig, K.-A. A1 - Hofmann, D. A1 - Mülhaupt, R. A1 - Schartel, Bernhard T1 - Flame retardancy through carbon nanomaterials: carbon black, multiwall nanotubes, expanded graphite, multi layer graphene and graphene in polypropylene N2 - 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. KW - Polypropylene KW - Flame retardancy KW - Nanocomposites KW - Graphene KW - Carbon nanomaterials KW - Thermally reduced graphite oxide PY - 2013 DO - https://doi.org/10.1016/j.polymdegradstab.2013.04.009 SN - 0141-3910 SN - 1873-2321 VL - 98 IS - 8 SP - 1495 EP - 1505 PB - Applied Science Publ. CY - London AN - OPUS4-28638 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dittrich, Bettina A1 - Wartig, K.-A. A1 - Hofmann, D. A1 - Mülhaupt, R. A1 - Schartel, Bernhard T1 - Carbon black, multiwall carbon nanotubes, expanded graphite and functionalized graphene flame retarded polypropylene nanocomposites N2 - 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. KW - Graphene KW - Flame retardancy KW - Nanocomposites KW - Polypropylene KW - Carbon nanoparticles PY - 2013 DO - https://doi.org/10.1002/pat.3165 SN - 1042-7147 SN - 1099-1581 VL - 24 IS - 10 SP - 916 EP - 926 PB - John Wiley & Sons, Ltd. CY - Chichester AN - OPUS4-29337 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lorenzetti, A. A1 - Besco, S. A1 - Hrelja, D. A1 - Roso, M. A1 - Gallo, Emanuela A1 - Schartel, Bernhard A1 - Modesti, M. T1 - Phosphinates and layered silicates in charring polymers: The flame retardancy action in polyurethane foams N2 - 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. KW - Phosphinate KW - Nanocomposite KW - Polyurethane KW - Interaction KW - Flame retardant PY - 2013 DO - https://doi.org/10.1016/j.polymdegradstab.2013.08.002 SN - 0141-3910 SN - 1873-2321 VL - 98 IS - 11 SP - 2366 EP - 2374 PB - Applied Science Publ. CY - London AN - OPUS4-29281 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hörold, Andreas A1 - Schartel, Bernhard A1 - Trappe, Volker A1 - Korzen, Manfred A1 - Naumann, Maurice T1 - Structural integrity of sandwich structures in fire: an intermediate-scale approach N2 - 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. KW - Fire testing KW - Structural integrity KW - Carbon-fibre-reinforced plastics KW - Fully developed fire KW - Composites PY - 2013 DO - https://doi.org/10.1080/15685543.2013.816620 SN - 0927-6440 SN - 1568-5543 VL - 20 IS - 9 (Special Issue: ECCM15: Part 3) SP - 741 EP - 759 PB - VSP CY - Zeist AN - OPUS4-29647 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hofmann, D. A1 - Wartig, K.-A. A1 - Thomann, R. A1 - Dittrich, Bettina A1 - Schartel, Bernhard A1 - Mülhaupt, R. T1 - Functionalized graphene and carbon materials as additives for melt-extruded flame retardant polypropylene N2 - 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%). KW - Extrusion KW - Flame retardance KW - Graphene KW - Nanocomposite KW - Polypropylene PY - 2013 DO - https://doi.org/10.1002/mame.201200433 SN - 1438-7492 SN - 1439-2054 VL - 298 IS - 12 SP - 1322 EP - 1334 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-29817 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Damerau, Thomas A1 - Hennecke, Manfred T1 - Photo- and thermo-oxidative stability of aromatic spiro-linked bichromophoric cross-shaped molecules N2 - An extensive investigation of the photostability and the thermo-oxidative stability is presented for 2,2,7,7-tetrakis(biphenyl-4-yl)-9,9-spirobifluorene and 2,2,4,4,7,7-hexakis(biphenyl-4-yl)-9,9-spirobifluorene. Both compounds are conjugated fully aromatic systems that are being discussed as active functional materials for a variety of advanced applications. The effect of atmosphere, sample thickness and preparation procedure on photo-oxidative degradation are investigated in detail by absorption and fluorescence spectroscopy. Distinct mechanisms are described in terms of relevant parameters such as the quantum yields of the photo-oxidation and the fluorescence. No oxidative degradation could be detected under nitrogen. In ambient air a strong decrease of the fluorescence performance is found due to effective quenching by defective chromophores. Chemiluminescence investigations were performed to characterise the thermo-oxidative behaviour in the temperature region between 300 and 450 K. It becomes clear that even a stable chemical structure such as the investigated aromatic system does not guarantee sufficient photostability with regard to light emitting properties. About this Journal PY - 2000 DO - https://doi.org/10.1039/b004931j SN - 1463-9076 SN - 1463-9084 VL - 2 IS - 20 SP - 4690 EP - 4696 PB - The Royal Soc. of Chemistry CY - Cambridge AN - OPUS4-1002 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Krüger, Simone A1 - Wachtendorf, Volker A1 - Hennecke, Manfred T1 - Excitation energy transfer of a bichromophoric cross-shaped molecule investigated by polarized fluorescence spectroscopy N2 - The excitation energy transfer (EET) of a bichromophoric cross-shaped molecule was investigated by stationary polarized fluorescence spectroscopy in the solid state. For this purpose 2,2[prime],7,7[prime]-tetrakis(biphenyl-4-yl)-9,9[prime]-spirobifluorene was embedded in a polymeric bisphenol-A-polycarbonate (PC) matrix. The dependence of the fluorescence on concentration and wavelength was determined. The role of the intermolecular and intramolecular EET is dealt with separately and discussed by means of the degree of polarization. The intermolecular excitation energy transfer is described in terms of a Förster transfer mechanism. The intramolecular transfer is prevented for the zero-point vibrational levels by the molecular cross-shaped structure, but is found for a wide range of wavelength, presumably based on vibrationally excited states. PY - 2000 DO - https://doi.org/10.1063/1.481620 SN - 0021-9606 SN - 1089-7690 VL - 112 IS - 22 SP - 9822 EP - 9827 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-1038 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Kunze, Ralf A1 - Neubert, Dietmar A1 - Tidjani, Adams T1 - ZnS as fire retardant in plasticised PVC N2 - 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. KW - PVC KW - ZnS KW - Fire retardancy KW - TG-FTIR KW - Cone calorimeter PY - 2002 DO - https://doi.org/10.1002/pi.845 SN - 0959-8103 SN - 1097-0126 SN - 0007-1641 VL - 51 IS - 3 SP - 213 EP - 222 PB - Wiley InterScience CY - Chichester, West Sussex AN - OPUS4-1291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Kunze, Ralf A1 - Neubert, Dietmar T1 - Red Phosphorus-Controlled Decomposition for Fire Retardant PA 66 N2 - 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. T2 - 8th European Conference on fire retardant polymers CY - Alessandria, Italy DA - 2001-06-24 KW - PA 66 KW - Red phosphorus KW - Fire retardancy KW - TG-FTIR KW - Cone calorimeter PY - 2002 DO - https://doi.org/10.1002/app.10144 SN - 0021-8995 SN - 1097-4628 VL - 83 IS - 10 SP - 2060 EP - 2071 PB - Wiley InterScience CY - Hoboken, NJ AN - OPUS4-1234 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Kühn, Gerhard A1 - Mix, Renate A1 - Friedrich, Jörg Florian T1 - Surface Controlled Fire Retardancy of Polymers Using Plasma Polymerisation N2 - 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. KW - Cone calorimeter KW - Flame retardance KW - Heat release KW - Plasma polymerization KW - Polyamides PY - 2002 DO - https://doi.org/10.1002/1439-2054(20020901)287:9<579::AID-MAME579>3.0.CO;2-6 SN - 1438-7492 SN - 1439-2054 VL - 287 IS - 9 SP - 579 EP - 582 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-1537 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lehmann, M. A1 - Schartel, Bernhard A1 - Hennecke, Manfred A1 - Meier, H. T1 - Dendrimers consisting of stilbene or distyrylbenzene building blocks synthesis and stability N2 - On the basis of Wittig-Horner reactions and protection group techniques compound 7 for the core and the components 9a-c and 11a-c for the dendrons were prepared and linked in the final step. The convergent synthesis yielded constitutionally and configurationally pure dendrimers (2a-c, 2a'-c') which consist of distyrylbenzene units. Their thermo-oxidative stability in the presence of air was studied by chemiluminescence and compared to the dendrimers 1 consisting of stilbene units. KW - Chemiluminescence KW - Dendrimers KW - Diphenylethylenderivate KW - Oxidation KW - Wittig reactions PY - 1999 DO - https://doi.org/10.1016/S0040-4020(99)00823-6 SN - 0040-4020 SN - 1464-5416 VL - 55 IS - 47 SP - 13377 EP - 13394 PB - Elsevier Science CY - Kidlington AN - OPUS4-1539 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Xu, C. A1 - Battig, Alexander A1 - Schartel, Bernhard A1 - Siegel, R. A1 - Senker, J. A1 - von der Forst, I. A1 - Unverzagt, C. A1 - Agarwal, S. A1 - Möglich, A. A1 - Greiner, A. T1 - Investigation of the Thermal Stability of Proteinase K for the Melt Processing of Poly(L‑lactide) N2 - The enzymatic degradation of aliphatic polyesters offers unique opportunities for various use cases in materials science. Although evidently desirable, the implementation of enzymes in technical applications of polyesters is generally challenging due to the thermal lability of enzymes. To prospectively overcome this intrinsic limitation, we here explored the thermal stability of proteinase K at conditions applicable for polymer melt processing, given that this hydrolytic enzyme is well established for its ability to degrade poly(L-lactide) (PLLA). Using assorted spectroscopic methods and enzymatic assays, we investigated the effects of high temperatures on the structure and specific activity of proteinase K. Whereas in solution, irreversible unfolding occurred at temperatures above 75−80 °C, in the dry, bulk state, proteinase K withstood prolonged incubation at elevated temperatures. Unexpectedly little activity loss occurred during incubation at up to 130 °C, and intermediate levels of catalytic activity were preserved at up to 150 °C. The resistance of bulk proteinase K to thermal treatment was slightly enhanced by absorption into polyacrylamide (PAM) particles. Under these conditions, after 5 min at a temperature of 200 °C, which is required for the melt processing of PLLA, proteinase K was not completely denatured but retained around 2% enzymatic activity. Our findings reveal that the thermal processing of proteinase K in the dry state is principally feasible, but equally, they also identify needs and prospects for improvement. The experimental pipeline we establish for proteinase K analysis stands to benefit efforts directed to this end. More broadly, our work sheds light on enzymatically degradable polymers and the thermal processing of enzymes, which are of increasing economical and societal relevance. KW - Enzymatic degradation KW - Poly(L‑lactide) KW - Polyesters KW - biodegradation PY - 2022 DO - https://doi.org/10.1021/acs.biomac.2c01008 SN - 1525-7797 SN - 1526-4602 VL - 23 IS - 11 SP - 4841 EP - 4850 PB - ACS Publications AN - OPUS4-56292 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Battig, Alexander A1 - Garfias González, Karla I. A1 - Schartel, Bernhard T1 - Valorizing “non-vegan” bio-fillers: Synergists for phosphorus flame retardants in epoxy resins N2 - Sustainable, biogenic flame retardant adjuvants for epoxy resins are receiving increased focus. Zoological products like insects, bone meal, and eggshells are available in large quantities, but remain uninvestigated as functional fillers to epoxy resins, although they are potential synergists to flame retardants. The efficacy and flame retardancy of “non-vegan” additives in combination with flame retardants is investigated and the fire behavior and thermal decomposition of bio-sourced epoxy resin composites is characterized. By comparing the fire performance of composites containing flame retardants or fillers at varying loadings (5, 10, and 20%), their role as synergists that enhance the function of organophosphorus flame retardants in bio-epoxy composites is identified and quantified. Peak heat release rates were 44% lower in composites containing both filler and flame retardant versus those containing only flame retardants, and fire loads were reduced by 44% versus the pure resin, highlighting the ability of “non-vegan” fillers to function as synergists. KW - Flame retardancy KW - Synergy KW - Bio-composite KW - Epoxy resin KW - Biogenic KW - Renewable PY - 2022 DO - https://doi.org/10.1016/j.polymdegradstab.2022.109875 SN - 0141-3910 VL - 198 SP - 109875 PB - Elsevier Ltd. AN - OPUS4-54438 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strommer, Bettina A1 - Battig, Alexander A1 - Frasca, Daniele A1 - Schulze, Dietmar A1 - Huth, Christian A1 - Böhning, Martin A1 - Schartel, Bernhard T1 - Multifunctional Property Improvements by Combining Graphene and Conventional Fillers in Chlorosulfonated Polyethylene Rubber Composites N2 - The incorporation of nanoparticles like multilayer graphene (MLG) into elastomeric composites boosts their technical performance, such as their mechanical behavior and electrical conductivity. Common filler types (carbon black (CB) and aluminum trihydroxide (ATH)) generally fulfill single, specific purposes and are often used in high loadings. CB typically reinforces rubber mechanically, while ATH increases flame retardancy. Small amounts of MLG reduce these high filler contents and maintain the multifunctional characteristics of rubber composites. In chlorosulfonated polyethylene (CSM) + ATH, an intrinsically flame-retardant rubber was designed to achieve the highest standards such as maximum average of heat emission (MARHE) <90 kW m−2, 3 phrMLG was substituted for 15 phr CB and/or 3 phr ATH via an industrially applicable processing approach. Replacing either CB or ATH resulted in a property profile that was multifunctionally improved in terms of features such as mechanical performance, reduced sorption, and flame retardance. MLG nanocomposites are reported to show promise as an industrially utilizable route to obtain multifunctional high-performance rubbers. KW - Nanocomposites KW - Rubber KW - Multilayer graphene KW - Flame retardancy KW - Synergy KW - Nanoparticles KW - Elastomers PY - 2022 DO - https://doi.org/10.1021/acsapm.1c01469 SN - 2637-6105 VL - 4 IS - 2 SP - 1021 EP - 1034 PB - ACS Publ. CY - Washington, DC AN - OPUS4-54330 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tan, Yi A1 - Wachtendorf, Volker A1 - Klack, Patrick A1 - Kukofka, Tobias A1 - Ruder, J. A1 - Schartel, Bernhard T1 - Durability of the flame retardance of ethylene-vinyl acetate copolymer cables: Comparing different flame retardants exposed to different weathering conditions N2 - 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. KW - Durability KW - Flame retardant KW - Cable KW - Weathering KW - Cone calorimeter PY - 2020 DO - https://doi.org/10.1002/APP.47548 SN - 0021-8995 VL - 137 IS - 1 SP - 47548 PB - Wiley AN - OPUS4-50237 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Bahr, Horst A1 - Braun, Ulrike A1 - Recknagel, Christoph T1 - Short communication: Fire risks of burning asphalt N2 - Eyewitnesses describe burning pavement surfaces in extreme fire scenarios. However, it was believed that the pavement plays a negligible role in comparison to other items feeding such an extreme fire at the same time. The asphalt mixtures used differ widely, thus raising the question as to whether this conclusion holds for all kinds of such materials. Three different kinds of asphalt mixtures were investigated with the aim of benchmarking the fire risks. Cone calorimeter tests are performed at an irradiance of 70kWm-2. All three investigated asphalts burn in extreme fire scenarios. The fire response (fire load, time to ignition, maximum heat release rate and smoke production) is quite different and varies by factors of up to 10 when compared to each other. The fire load per mass is always very low due to the high content of inert minerals, whereas the effective heat of combustion of the volatiles is quite typical of non-flame retarded organics. The heat release rate and fire growth indices are strongly dependent on the fire residue and thus the kind of mineral filler used. Comparing with polymeric materials, the investigated Mastic Asphalt and Stone Mastic Asphalt may be called intrinsically flame resistant, whereas the investigated Special Asphalt showed a pronouncedly greater fire risk with respect to causing fire growth and smoke. Thus the question is raised as to whether the use of certain kinds of asphalts in tunnels must be reconsidered. Apart from the binder used, the study also indicates varying the kind of aggregate as a possible route to eliminate the problem. KW - Asphalt KW - Cone calorimeter KW - Fire behaviour PY - 2010 DO - https://doi.org/10.1002/fam.1027 SN - 0308-0501 SN - 1099-1018 VL - 34 IS - 7 SP - 333 EP - 340 PB - Heyden CY - London AN - OPUS4-22172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wawrzyn, Eliza A1 - Schartel, Bernhard A1 - Seefeldt, Henrik A1 - Karrasch, A1 - Jäger, Christian T1 - What reacts with what in bisphenol A polycarbonate/silicon rubber/bisphenol A bis(diphenyl phosphate) during pyrolysis and fire behavior? N2 - The pyrolysis and flame retardancy of a bisphenol A polycarbonate/silicon rubber/bisphenol A bis(diphenyl phosphate) (PC/SiR/BDP) blend were investigated and compared to those of PC/BDP and PC/SiR. The impact modifier SiR consists mainly of poly(dimethylsiloxane) (PDMS > 80 wt %). The pyrolysis of PC/SiR/BDP was studied by thermogravimetry (TG), TG–FTIR to analyze the evolved gases, and a Linkam hot stage cell within FTIR as well as 29Si NMR and 31P NMR to analyze the solid residue. The fire performance was determined by PCFC, LOI, UL 94, and a cone calorimeter under different external irradiations. The fire residues were studied by using ATR-FTIR as well as the additional binary systems PC + PDMS, PC + BDP, and BDP + PDMS, focusing on the specific chemical interactions. The decomposition pathways are revealed, focusing on the competing interaction between the components. Fire retardancy in PC/SiR/BDP is caused by both flame inhibition in the gas phase and inorganic-carbonaceous residue formation in the condensed phase. The PC/SiR/BDP does not work as well superimposing the PC/SiR and PC/BDP performances. PDMS reacts with PC and BDP, decreasing BDP's mode of action. Nevertheless, the flammability (LOI > 37%, UL 94 V-0) of PC/SiR/BDP equals the high level of PC/BDP. Indeed, SiR in PC/SiR/BDP is underlined as a promising impact modifier in flame-retarded PC/impact modifier blends as an alternative to highly flammable impact modifiers such as acrylonitrile–butadiene–styrene (ABS), taking into account that the chosen SiR leads to PC blends with a similar mechanical performance. KW - PC KW - BDP KW - PDMS KW - Flame retardancy KW - Flammability KW - Decomposition KW - Pyrolysis PY - 2012 DO - https://doi.org/10.1021/ie201908s SN - 0888-5885 SN - 1520-5045 VL - 51 IS - 3 SP - 1244 EP - 1255 PB - American Chemical Society CY - Washington, DC AN - OPUS4-25460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wawrzyn, Eliza A1 - Schartel, Bernhard A1 - Ciesielski, M. A1 - Kretzschmar, B. A1 - Braun, Ulrike A1 - Döring, M. T1 - Are novel aryl phosphates competitors for bisphenol A bis(diphenyl phosphate) in halogen-free flame-retarded polycarbonate/acrylonitrile-butadiene-styrene blends? N2 - The reactivity of the flame retardant and its decomposition temperature control the condensed-phase action in bisphenol A polycarbonate/acrylonitrile–butadiene–styrene/polytetrafluoroethylene (PC/ABSPTFE) blends. Thus, to increase charring in the condensed phase of PC/ABSPTFE + aryl phosphate, two halogen-free flame retardants were synthesized: 3,3,5-trimethylcyclohexylbisphenol bis(diphenyl phosphate) (TMC-BDP) and bisphenol A bis(diethyl phosphate) (BEP). Their performance is compared to bisphenol A bis(diphenyl phosphate) (BDP) in PC/ABSPTFE blend. The comprehensive study was carried out using thermogravimetry (TG); TG coupled with Fourier transform infrared spectrometer (TG-FTIR); the Underwriters Laboratory burning chamber (UL 94); limiting oxygen index (LOI); cone calorimeter at different irradiations; tensile, bending and heat distortion temperature tests; as well as rheological studies and differential scanning calorimeter (DSC). With respect to pyrolysis, TMC-BDP works as well as BDP in the PC/ABSPTFE blend by enhancing the cross-linking of PC, whereas BEP shows worse performance because it prefers cross-linking with itself rather than with PC. As to its fire behavior, PC/ABSPTFE + TMC-BDP presents results very similar to PC/ABSPTFE + BDP; the blend PC/ABSPTFE + BEP shows lower flame inhibition and higher total heat evolved (THE). The UL 94 for the materials with TMC-BDP and BDP improved from HB to V0 for specimens of 3.2 mm thickness compared to PC/ABSPTFE and PC/ABSPTFE + BEP; the LOI increased from around 24% up to around 28%, respectively. BEP works as the strongest plasticizer in PC/ABSPTFE, whereas the blends with TMC-BDP and BDP present the same rheological properties. PC/ABSPTFE + TMC-BDP exhibits the best mechanical properties among all flame-retarded blends. KW - Polycarbonate (PC) KW - Aryl phosphate KW - Flame retardancy KW - Pyrolysis KW - PC/ABS PY - 2012 DO - https://doi.org/10.1016/j.eurpolymj.2012.06.015 SN - 0014-3057 SN - 1873-1945 VL - 48 IS - 9 SP - 1561 EP - 1574 PB - Elsevier CY - Oxford AN - OPUS4-26292 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Krüger, Simone A1 - Wachtendorf, Volker A1 - Hennecke, Manfred T1 - Chemiluminescence: A promising new testing method for plastic optical fibers N2 - The thermo-oxidative degradation of a polymeric optical cable is investigated by chemiluminescence, The results are reliable and reproducible. Two distinct processes are reported marked by a peak and a plateau behavior versus the time, respectively. Both processes are ruled by thermally activated processes. Beside the dependencies of temperature and time, the influence of absorbed water is discussed. Chemiluminescence is proposed as a promising candidate for a suitable testing method assessing the thermo-oxidative stability of plastic optical fibers and cables. it requires not more than a simple one-day testing procedure and has the advantage that it can be carried out even within the lo cv temperature ranges of the cables' intended use. KW - Chemiluminescence KW - Chemilumineszenz PY - 1999 DO - https://doi.org/10.1109/50.803022 SN - 0733-8724 SN - 1558-2213 VL - 17 IS - 11 SP - 2291 EP - 2296 PB - Institute of Electrical and Electronics Engineers CY - New York, NY AN - OPUS4-718 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Wendorff, J. H. T1 - Molecular composites for molecular reinforcement: A promising concept between success and failure N2 - The basic principles of molecular reinforcement and especially the specific approaches to obtain homogeneous composites with molecularly dispersed rigid rods are focused on and discussed. Brief overviews and successful examples of the available data covering the main characteristics are summarized. KW - Verbundwerkstoffe KW - Molecular Reinforcement KW - Homogene Mischbarkeit PY - 1999 SN - 0032-3888 SN - 1548-2634 VL - 39 IS - 1 SP - 128 EP - 151 PB - Wiley CY - Hoboken, NY AN - OPUS4-731 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gallo, Emanuela A1 - Schartel, Bernhard A1 - Schmaucks, G. A1 - von der Ehe, Kerstin A1 - Böhning, Martin T1 - Effect of well dispersed amorphous silicon dioxide in flame retarded styrene butadiene rubber N2 - 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. KW - Flame retardancy KW - Styrene butadiene rubber KW - SBR KW - Silicon dioxide KW - Aluminium trihydroxide KW - ATH PY - 2013 DO - https://doi.org/10.1179/1743289812Y.0000000012 SN - 1465-8011 SN - 1743-2898 VL - 42 IS - 1 SP - 34 EP - 42 PB - IOM Communications CY - London, UK AN - OPUS4-27626 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Frasca, Daniele A1 - Schulze, Dietmar A1 - Böhning, Martin A1 - Krafft, Bernd A1 - Schartel, Bernhard T1 - Chlorbutylkautschuk/Multilayergraphen-Nanocomposites N2 - In den letzten Jahren werden zunehmend Nanopartikel als Füllstoff für Polymere vorgeschlagen und auch erfolgreich in Elastomer-Nanocomposites eingesetzt. In dieser Arbeit wird Multilayergraphen (MLG) als Nanofüllstoff näher untersucht, der sich bereits bei geringen Konzentrationen als effizient erweist. MLG besteht aus nur etwa zehn Graphenlagen. Chlorbutylkautschuk (CIIR)/MLG-Nanocomposites mit verschiedenen MLG-Gehalten wurden mit Hilfe eines ultraschallunterstützen Mischverfahrens in Lösung hergestellt und auf einem Walzwerk weiterverarbeitet. Das Einmischen von MLG führt zu einer deutlichen Verbesserung der rheologischen und mechanischen Eigenschaften, des Vernetzungsverhaltens sowie der Barrierewirkung gegenüber Gasen. Bereits der Zusatz von 3 phr MLG zu CIIR führt zu einem mehr als zweifach höheren E-Modul und zu einer Reduktion der Permeabilität von O2 und CO2 um 30 %. Höhere Konzentrationen an Nanofüllstoff resultieren in einer weiteren Verbesserung der Eigenschaften der Nanocomposites. Weiterhin zeigten die CIIR/MLG-Nanocomposites auch eine geringere Entflammbarkeit. KW - Elastomere KW - Nanokomposite KW - Graphen KW - Chlorbutylkautschuk PY - 2017 SN - 0176-1625 VL - 70 IS - 5 SP - 311 EP - 322 PB - Dr. Gupta Verlag CY - Ratingen AN - OPUS4-40327 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sut, Aleksandra A1 - Greiser, Sebastian A1 - Jäger, Christian A1 - Schartel, Bernhard T1 - Interactions in multicomponent flame-retardant polymers: Solid-state NMR identifying the chemistry behind it N2 - 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 1H–31P 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. KW - Synergy KW - Solid-state NMR KW - Flame retardancy KW - SEBS KW - Aluminium diethylphosphinate KW - Magnesium hydroxide KW - Zinc borate KW - Poly(phenylene) oxide PY - 2015 DO - https://doi.org/10.1016/j.polymdegradstab.2015.08.018 SN - 0141-3910 SN - 1873-2321 VL - 121 SP - 116 EP - 125 PB - Applied Science Publ. CY - London AN - OPUS4-34306 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rockel, Daniel A1 - Sanchez Olivares, G. A1 - Calderas, F. A1 - Schartel, Bernhard T1 - It’s not waste, it’s a resource: Utilizing industrial waste fibers/mineral fillers to attain flame retardant biocomposites N2 - Integrating natural fibers derived from local industrial waste streams into thermoplastic starch (TPS) proves to be a promising approach towards sustainable flame retardant biocomposites. Initially, three types of waste fibers from the agave, coconut, and leather industries were evaluated for their flame retardant properties in combination with aluminum trihydroxide (ATH), an environmental friendly flame retardant. Leather fiber (BLF) exhibited the best flame retardant performance and were further investigated along with ATH and varying amounts of bentonite nanoclay to enhance the residual protective layer. The combination of multiple components shows improvement in performance while reducing the total load of filler. The images of the fire residues revealed that a more enclosed surface correlates with a reduction in the peak of heat release rate. Whereas higher amounts of bentonite does not deliver further inprovements, only 1 phr nanoclay in the novel multicomponent system of TPS, ATH, BLF, and bentonite synergistically improved the UL-94 rating from HB to V1. The proposed system brings together the different approaches using a renewable biopolymer, natural waste fibres, and envirnmentally friendly flame retardancy and thus, is striking for its combination of outstanding sustainablity, instant feasability, and sufficient fire performance. KW - Biocomposites KW - Flame retardancy KW - Residue analysis KW - Sustainability KW - Waste streams PY - 2025 DO - https://doi.org/10.1177/08927057241297083 SN - 0892-7057 SN - 1530-7980 VL - 38 IS - 6 SP - 2225 EP - 2252 PB - Sage AN - OPUS4-63431 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sunder, S. A1 - Jauregui Rozo, Maria A1 - Inasu, S. A1 - Meinel, Dietmar A1 - Schartel, Bernhard A1 - Ruckdäschel, H. T1 - Effect of Ammonium Polyphosphate/Silicate Content on the Postfire Mechanics of Epoxy Glass-Fiber Composites Using Facile Chocolate Bar-Inspired Structures N2 - This study investigates the postfire mechanical properties of epoxy glass-fiber reinforced composites (EP GFRCs) using increasing concentrations of ammonium polyphosphate (APP) and inorganic silicate (InSi) to modify the char and fire residue. A facile chocolate bar-inspired structure was introduced for fire exposure and subsequent flexural testing of the GFRCs. The resin matrix used here was a diglycidyl ether of bisphenol-A (DGEBA) resin, cured with dicyandiamide (DICY), and accelerated by Urone. The microstructures of the degraded composites after three-point bending tests, were evaluated using scanning electron microscopy (SEM) and x-ray computed tomography (XCT) imaging. A previous study showed that increasing the APP and InSi content significantly enhanced flame retardancy, via improved char formation under fire conditions. However, flexural properties and fire resistance were adversely affected after fire exposure, highlighting a trade-off effect. Fiber breakage and delamination of the composites increased upon failure with increasing APP + InSi content in the composite due to unconsolidated char. The experimental values for the postfire flexural mechanics were in good agreement with the two-layer model proposed in literature. This paper presents a preliminary basis for postfire mechanical testing of epoxy composites for use in fire-safe structures, using a combination of standardized testing norms. KW - Flame retardants KW - Post-fire KW - Epoxy KW - Gass fiber composites KW - Prepregs PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-627176 DO - https://doi.org/10.1002/fam.3280 SN - 0308-0501 SN - 1099-1018 VL - 49 IS - 3 SP - 329 EP - 346 PB - Wiley AN - OPUS4-62717 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bibinger, J. A1 - Eibl, S. A1 - Gudladt, H.-J. A1 - Schartel, Bernhard A1 - Höfer, P. T1 - Pushing the limits of thermal resistance in nanocomposites: A comparative study of carbon black and nanotube modifications N2 - Enhancing the thermal resistance of carbon fiber-reinforced polymers (CFRPs) with flame retardants or coatings often leads to increased weight and reduced mechanical integrity. To address these challenges, this study introduces an innovative approach for developing nanocomposites using carbon-based nanoparticles, while preserving the structural lightweight properties. For this, carbon black particles (CBPs) up to 10% and carbon nanotubes (CNTs) up to 1.5% were incorporated into the RTM6/G939 composite material. The obtained samples were then analyzed for their properties and heat resistance under one-sided thermal loading at a heat flux of 50 kW/m2. Results demonstrate that integrating these particles improves heat conduction without compromising the material’s inherent advantages. As a result, thermo-induced damage and the resulting loss of mechanical strength are delayed by 17% with CBPs and 7% with CNTs compared to the unmodified material. Thereby, the thermal behavior can be accurately modeled by a straightforward approach, using calibrated, effective measurements of the nanoparticles in the polymer matrix rather than relying on theoretical assumptions. This approach thus provides a promising methode to characterize and improve thermal resistance without significant trade-offs. KW - Nanomaterial KW - Cabon fiber-reinforced polymer (CFRP) KW - Carbon black (CB) KW - Carbon nanotube (CNT) KW - Improving heat conduction KW - Prediction thermal properties PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-628632 DO - https://doi.org/10.3390/nano15070546 SN - 2079-4991 VL - 15 IS - 7 SP - 1 EP - 23 PB - MDPI CY - Basel AN - OPUS4-62863 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wagner, Jan A1 - Dudziak, Mateusz A1 - Falkenhagen, Jana A1 - Rockel, Daniel A1 - Reimann, H.-A A1 - Schartel, Bernhard T1 - This is the way: An evidence based route to phytic-acid–based flame retardant poly(lactide acid) N2 - A systematic sequence of materials was investigated to develop phytic-acid (Phyt)–based flame retarded poly (lactide acid) (PLA), while factoring in molecular weight (MW), crystallinity and mechanical properties. Synergistic approaches were developed based on combinations with lignin and expandable graphite (EG), as well as by applying different Phyt salts of melamine (Mel), piperazine (Pip), and arginine (Arg). Compounds were twin screw extruded, injection molded, hot pressed and investigated with thermal analysis, size exclusion chromatography, infrared spectroscopy, tensile testing, limited oxygen index (LOI), UL 94, cone calorimeter, and scanning electron microscope. 16.7 wt.% flame retardant (FR) slightly enhances crystallization while MW remains unchanged in PLA Phyt Arg and PLA Phyt Mel. LOI was improved to 43.7 vol.% for PLA Phyt Arg, UL 94 V0 achieved for PLA Phyt Pip. Cone calorimeter results show total heat evolved reduced by 14 %, maximum average rate of heat emission 43 % lower, and peak heat release rate reduced by 50 % for PLA Phyt Mel. Phyt Mel combined with EG increased the char yield of PLA to 20 wt.% and 15.5 wt.% at 600 and 900 ◦C, respectively. Phyt is exploited to enhance char yield, stabilize the intumescent char, and lower the apparent effective heat of combustion. The combination of Phyt Mel and EG was proposed as an efficient FR for PLA via an evidence based developing route. KW - Polylactide acid KW - Intumescent flame retardant KW - Phosphorous flame retardant KW - Phytic acid KW - Expandable graphite KW - Melamine PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626395 DO - https://doi.org/10.1016/j.polymdegradstab.2025.111242 SN - 1873-2321 SN - 0141-3910 VL - 234 SP - 1 EP - 14 PB - Elsevier Ltd. AN - OPUS4-62639 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hupp, Vitus A1 - Schartel, Bernhard A1 - Flothmeier, K. A1 - Hartwig, A. T1 - Flame Retarded Adhesive Tapes and Their Influence on the Fire Behavior of Bonded Parts N2 - Pressure-sensitive adhesive tapes are used in automotives, railway vehicles and construction, where flame retardancy is of major importance. This is why industrial applicants often buy, and industrial tape manufacturers often produce, flame-retardant adhesive tapes, advertised for their good flammability characteristics. Yet, how flame-retardant tapes influence the fire behavior of bonded materials is a rather open question. To investigate this issue, three different substrates were bonded, using eight double-sided adhesive tapes containing two different carriers and two different flame retardants. The bonded substrates were compared to their monolithic counterparts in terms of flammability, fire behavior and fire stability. The fire behavior of adhesive tape bonded materials differed significantly from the monolithic substrates. The usage of different adhesive tapes let to different burning behavior of the bonded materials mainly due to different carrier systems. In contrast, the implementation of flame retardant into the adhesive had rather minor or no effect on the burning behavior of the bonded substrates despite their positive effect on the flammability of the free-standing tape. The carrier changed the HRR curve in the cone calorimeter and was able to both, reduce and increase fire hazards. Using the carrier with the better fire performance can lower the fire growth rate by 20%, the peak of heat release rate by 27%, and the maximum average rate of heat emission by 30% in cone calorimeter tests. Overall, the fire behavior of bonded materials is a complex interaction between substrate, adhesive, and carrier, and depends on the fire scenario the materials are exposed to. KW - Pressure-sensitive adhesive tapes KW - Bonded materials KW - Fire behaviour KW - Fire resistance KW - Flame retardant KW - Cone calorimeter PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626006 DO - https://doi.org/10.1007/s10694-024-01637-2 SN - 1572-8099 SN - 0015-2684 VL - 61 IS - 2 SP - 729 EP - 749 PB - Springer Nature AN - OPUS4-62600 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jauregui Rozo, Maria A1 - Sunder, S. A1 - Inasu, S. A1 - Meinel, Dietmar A1 - Ruckdäschel, H. A1 - Schartel, Bernhard T1 - Weaving Through Fire and Force: Fire Behavior and Fire Stability of Unidirectional, Bidirectional, and Woven Roving Glass-Fiber Composites N2 - This study systematically investigates the transfer of flame retardants (FRs) from epoxy resins to composites. The flame-retardant composites are formulated using bisphenol A diglycidyl ether as the resin and dicyandiamide as the hardener, reinforced with glass fibers (GFs) using various textile architectures: unidirectional (UD), bidirectional (BD), and woven rovings (WR). These composites are evaluated using bench-scale fire stability tests and cone calorimeter experiments to assess critical parameters, including the temperature at failure, time to failure, and fire behavior. Among the tested configurations, UD-GFs demonstrate superior flame retardancy, fire stability, flammability, and mechanical performance, attributed to their higher residue yield, forming a more efficient protective char layer. However, the addition of FRs is limited by their impact on the material's mechanical properties. When the FR content increases to 30 and 50 wt.% of the resin, the composites exhibit a decrease in mechanical performance, adversely affecting both time to failure and temperature at failure. While adding FRs reduces the risk of fire propagation, it does not substantially enhance fire stability or mechanical performance. KW - Fire Resistance KW - Fiber-Reinforced Polymer Composites KW - Fire Stability KW - Glass Fibers KW - Fire Behavior PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-631220 SN - 1438-7492 SN - 1439-2054 VL - 310 IS - 5 SP - 2400432 PB - Wiley VHC-Verlag AN - OPUS4-63122 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dey, R. A1 - Dudziak, Mateusz A1 - Prescher, A. A1 - Kreitsmann, T. A1 - Zhang, K. A1 - Posten, C. A1 - Thomson, C. A1 - Schartel, Bernhard A1 - Ullrich, M. S. A1 - Thomson, L. T1 - Sustainable Flame-Retardant Poly Lactic AcidBiocomposites Reinforced with Polyphosphate-EnrichedMicroalgae: Unlocking the Potential of Hyper-Compensation N2 - This study examines the dual benefits of microalgae cultivation for wastewatertreatment and the enhancement of polylactic acid-based biocomposites. UsingDesmodesmus sp. in a photobioreactor, both batch and continuous operationsachieve total nitrogen (TN) and total phosphorus (TP) removal rates of up to99.9%, maintaining TN and TP levels below 0.02 mg L−1 in the effluent, aligningwith European discharge standards. Continuous cultivation increases biomassproductivity from 0.102 to 0.43 g L−1 day−1 , a 322% improvement over batchoperations. Nutrient starvation followed by reintroduction to nutrient-richwastewater induces hyper-compensation luxury uptake, with P-enrichedcells accumulating 1.33% intracellular P within six hours — 21% higherthan natural accumulation. The results reveal that luxury phosphorus uptakein microalgae follows a triphasic system of uptake and storage, challengingthe previously suggested biphasic model. When incorporated into Poly lacticacid (PLA), the biomass enhances versatility, offering potential replacementof inorganic P in industrial applications, particularly flame retardants.Pyrolysis and cone calorimetry confirm the thermal and fire-retardantbenefits, with a 20% reduction in peak heat release rate and increased charyield. This work highlights microalgae’s role in sustainable biocomposites,supporting wastewater treatment, nutrient recovery, and CO2 sequestration. KW - biocomposites KW - biopolymers KW - Flame-retardant KW - Hyper compensation KW - Phycoremediation KW - Wastewater treatment PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-640408 DO - https://doi.org/10.1002/adsu.202500251 SN - 2366-7486 VL - 9 IS - 8 SP - 1 EP - 11 PB - Wiley VHC-Verlag AN - OPUS4-64040 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dudziak, Mateusz A1 - Bhatia, Riya A1 - Dey, R. A1 - Falkenhagen, Jana A1 - Ullrich, M. S. A1 - Thomsen, C. A1 - Schartel, Bernhard T1 - Wastewater phosphorus enriched algae as a sustainable flame retardant in polylactide N2 - Revolutionizing our polymer industry for adaption to a sustainable carbon circular economy has become one of today’s most demanding challenges. Exploiting renewable resources to replace fossil-fuel—based plastics with biopolymers such as poly(lactic acid) (PLA) is inevitable while using waste streams as a raw material resource at least is promising. When it comes to using PLA as technical polymer, its high flammability must be addressed by flame retardants compatible with the thermoplastic processing of PLA and its compostability. This study proposes microalgae enriched with phosphorus from wastewater (P-Algae) as an elegant way towards a kind of sustainable organophosphorus flame retardant. The concept is demonstrated by investigating the processing, pyrolysis, flammability, and fire behavior of PLA/P-Algae, while varying the P-Algae content and comparing P-Algae with four alternative bio-fillers (phosphorylated lignin, biochar, thermally treated sewage sludge, and metal phytate) with different P-contents as meaningful benchmarks. KW - PLA KW - Flame Retardancy KW - Phosphorylated Algae KW - Wastewater flame retardants KW - Zink phytate KW - Phosphorylated lignin KW - Thermally treated sludge PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-604150 DO - https://doi.org/10.1016/j.polymdegradstab.2024.110885 SN - 1873-2321 SN - 0141-3910 VL - 227 SP - 1 EP - 11 PB - Elsevier Ltd. AN - OPUS4-60415 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strommer, Bettina A1 - Schulze, Dietmar A1 - Schartel, Bernhard A1 - Böhning, Martin T1 - Networking Skills: The Effect of Graphene on the Crosslinking of Natural Rubber Nanocomposites with Sulfur and Peroxide Systems N2 - Tailored crosslinking in elastomers is crucial for their technical applications. The incorporation of nanoparticles with high surface-to-volume ratios not only leads to the formation of physical networks and influences the ultimate performance of nanocomposites, but it also affects the chemical crosslinking reactions. The influence of few-layer graphene (FLG) on the crosslinking behavior of natural rubber is investigated. Four different curing systems, two sulfur-based with different accelerator-to-sulfur ratios, and two peroxide-based with different peroxide concentrations, are combined with different FLG contents. Using differential scanning calorimetry (DSC), vulcametry (MDR) and swelling measurements, the results show an accelerating effect of FLG on the kinetics of the sulfur-based curing systems, with an exothermic reaction peak in DSC shifted to lower temperatures and lower scorch and curing times in the MDR. While a higher accelerator-to-sulfur ratio in combination with FLG leads to reduced crosslinking densities, the peroxide crosslinkers are hardly affected by the presence of FLG. The good agreement of crosslink densities obtained from the swelling behavior confirms the suitability of vulcameter measurements for monitoring the complex vulcanization process of such nanocomposite systems in a simple and efficient way. The reinforcing effect of FLG shows the highest relative improvements in weakly crosslinked nanocomposites. KW - Nanocomposite KW - Elastomers KW - Graphene KW - Crosslinking KW - Network KW - Rubber KW - Vulcanization PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560409 DO - https://doi.org/10.3390/polym14204363 VL - 14 IS - 20 PB - MDPI AN - OPUS4-56040 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strommer, Bettina A1 - Schulze, Dietmar A1 - Schartel, Bernhard A1 - Böhning, Martin T1 - The quantification of anisotropy in graphene/natural rubber nanocomposites: Evaluation of the aspect ratio, concentration, and crosslinking N2 - In the processing of nanocomposites, high shear stresses at elevated tempera-tures orient two-dimensional nanoparticles like graphene. This orientationleads to anisotropic mechanical, thermal or barrier properties of the nanocom-posite. This anisotropy is addressed in this study by comparing graphene (few-layer graphene, FLG) with a nanoscaled carbon black (nCB) at a filler contentof 3 phr, by varying the vulcanization, and by comparing different FLG con-tents. Transmission electron microscopy gives insight into the qualitative ori-entation in the nanocomposite with FLG or nCB. The storage moduli paralleland normal to the orientation reveal the direction dependency of reinforce-ment through dynamic mechanical analysis (DMA). Dimensional swellingmeasurements show a restriction of the expansion parallel to the FLG orienta-tion, and an increased expansion normal to the orientation. The vulcanizationsystem and crosslinking determine the respective level of property values, andhigher crosslinking densities increase the anisotropy in DMA resulting invalues of up to 2.9 for the quantified anisotropy factor. With increasing FLGcontent, the anisotropy increases. A comparison of the results reveals swellingmeasurements as the most suitable method for the determination of anisot-ropy. Compared to recent literature, the presented processing induces higheranisotropy, leading to higher reinforcing effects in the direction of orientation KW - Natural rubber KW - Graphene KW - Nanocomposite KW - Mechanical properties KW - Swelling PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571522 DO - https://doi.org/10.1002/app.53753 SN - 1097-4628 VL - 140 IS - 16 SP - 1 EP - 15 PB - Wiley online library CY - Hoboken, New Jersey (USA) AN - OPUS4-57152 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Kunze, Ralf A1 - Hennecke, Manfred A1 - Kettner, A. A1 - Wendorff, J. H. T1 - On the thermal behaviour and thermo-oxidative stability of liquid crystalline triphenylene compounds N2 - Columnar discotic materials are considered for applications in the area of photoconductivity and light-emitting diodes. A major requirement is their stability at elevated temperatures and in the presence of oxygen. The thermal and thermo-oxidative behaviour of discotic triphenylene derivatives was investigated by us using various methods, in particular by chemiluminescence (CL), UV-vis absorption spectroscopy and in situ thermogravimetry-mass spectroscopy (TG-MS). Various degradation processes are described for increasing temperature, and their influences on functional properties are discussed. KW - Liquid crystal KW - Oxidation KW - Thermogravimetry PY - 1999 DO - https://doi.org/10.1002/(SICI)1099-0712(199903/04)9:2<55::AID-AMO366>3.3.CO;2-R SN - 1057-9257 SN - 1099-0712 VL - 9 IS - 2 SP - 55 EP - 64 PB - Wiley CY - Chichester AN - OPUS4-732 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Wachtendorf, Volker A1 - Hennecke, Manfred A1 - Grell, M. A1 - Bradley, D.D.C. T1 - Polarized fluorescence and orientational order parameters of a liquid-crystalline conjugated polymer N2 - We report a study of the orientational order of aligned thin films of the liquid crystalline conjugated polymer poly(9,9-dioctylfluorene). Steady state polarized fluorescence measurements were used to determine the orientational order parameter and . The influence of intermolecular and intramolecular excitation energy transfer on the degree of polarization is discussed. The role of film morphology is also examined by comparison of the results for glassy and crystalline films. KW - Liquid-cristalline conjugated Polymer KW - Polarized fluorescence measurements PY - 1999 SN - 1098-0121 SN - 0163-1829 SN - 0556-2805 SN - 1095-3795 SN - 1550-235X VL - 60 IS - 1 SP - 277 EP - 283 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-735 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Hennecke, Manfred T1 - Thermo-oxidative stability of a conjugated polymer by chemiluminescence N2 - Conjugated polymers based on 1,4-phenylenevinylene units are very promising materials for applications as light-emitting diodes. A major requirement is their stability at elevated temperatures of operation. The thermo-oxidative behaviour of a soluble poly(1,4-phenylenevinylene) derivative, poly[2,5-bis(2-ethylhexyloxy)-1,4-phenylene vinylene], was investigated by using chemiluminescence and UV–Vis absorption spectroscopy. Extremely sensitive chemiluminescence is successfully applied since even minor chemical changes could lead to a considerable loss of photo- and electro-optical properties. Various degradation processes are described as a function of time and temperature and their influences on functional properties are discussed. The investigated material does not show sufficient thermo-oxidative stability within the temperature range of intended use in contact with air. For industrial application, direct contact with oxygen during processing and operation has to be avoided. KW - Chemiluminescence KW - Conjugated polymer KW - Thermal-oxidation KW - Stability PY - 2000 DO - https://doi.org/10.1016/S0141-3910(99)00120-2 SN - 0141-3910 SN - 1873-2321 VL - 67 IS - 2 SP - 249 EP - 253 PB - Applied Science Publ. CY - London AN - OPUS4-853 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böhning, Martin A1 - Goering, Harald A1 - Fritz, Andreas A1 - Brzezinka, Klaus-Werner A1 - Turky, Gamal A1 - Schönhals, Andreas A1 - Schartel, Bernhard T1 - Dielectric Study of Molecular Mobility in Poly(propylene-graft-maleic anhydride)/Clay Nanocomposites N2 - Polymer/clay nanocomposite materials based on poly(propylene-graft-maleic anhydride) (PPgMAH) and two different organophilic modified clays were investigated by dielectric relaxation spectroscopy (DRS). In contrast to ungrafted polypropylene (PP), PPgMAH shows a dielectrically active relaxation process which can be assigned to localized fluctuations of the polar maleic anhydride groups. Its relaxation rate exhibits an unusual temperature dependence, which could be attributed to a redistribution of water molecules in the polymeric matrix. This is confirmed by a combination of Raman spectroscopy and thermogravimetric experiments (TGA) with real-time dielectric measurements under controlled atmospheres. In the nanocomposites this relaxation process is shifted to higher frequencies up to 3 orders of magnitude compared to the unfilled polymer. This indicates a significantly enhanced molecular mobility in the interfacial regions. In the nanocomposite materials a separate high-temperature process due to Maxwell-Wagner-Sillars (MWS) polarization was observed. The time constant of this MWS process can be correlated with characteristic length scales in nanocomposites and therefore provides additional information on dispersion and delamination/exfoliation of clay platelets in these materials. These properties also influence the diffusivity of the water molecules as revealed by real-time dielectric investigations. KW - Polymer clay nanocomposites KW - Molecular mobility KW - Dielectric relaxation spectroscopy PY - 2005 DO - https://doi.org/10.1021/ma048315c SN - 0024-9297 SN - 1520-5835 VL - 38 IS - 7 SP - 2764 EP - 2774 PB - American Chemical Society CY - Washington, DC AN - OPUS4-7281 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böhning, Martin A1 - Tidjani, Adams A1 - Wald, Oliver A1 - Brzezinka, Klaus-Werner A1 - Turky, Gamal A1 - Goering, Harald A1 - Schartel, Bernhard A1 - Schönhals, Andreas T1 - Dielectric and gas transport properties of polypropylene-clay nanocomposites T2 - Frühjahrstagung des Arbeitskreises Festkörperphysik bei der DPG CY - Regensburg, Germany DA - 2002-03-11 PY - 2002 SN - 0420-0195 SN - 0372-5448 SN - 0343-9216 IS - CPP 5.4 SP - 425 CY - Bad Honnef AN - OPUS4-2036 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Frasca, Daniele A1 - Schulze, Dietmar A1 - Wachtendorf, Volker A1 - Krafft, Bernd A1 - Morys, Michael A1 - Böhning, Martin A1 - Rybak, Thomas T1 - Multilayer graphene rubber nanocomposites N2 - Multilayer Graphene (MLG), a nanoparticle with a specific surface of BET = 250 m²/g and thus made of only approximately 10 graphene sheets, is proposed as a nanofiller for rubbers. When homogenously dispersed, it works at low loadings enabling the replacement of carbon black (CB), increase in efficiency, or reduction in filler concentration. Actually the appropriate preparation yielded nanocomposites in which just 3 phr are sufficient to significantly improve the rheological, curing and mechanical properties of different rubbers, as shown for Chlorine-Isobutylene-Isoprene Rubber (CIIR), Nitrile-Butadiene Rubber (NBR), Natural Rubber (NR), and Styrene-Butadiene Rubber (SBR). A mere 3 phr of MLG tripled the Young’s modulus of CIIR, an effect equivalent to 20 phr of carbon black. Similar equivalents are observed for MLG/CB mixtures. MLG reduces gas permeability, increases thermal and electrical conductivities, and retards fire behavior. The later shown by the reduction in heat release rate in the cone calorimeter. The higher the nanofiller concentration is (3 phr, 5 phr, and 10 phr was investigated), the greater the improvement in the properties of the nanocomposites. Moreover, the MLG nanocomposites improve stability of mechanical properties against weathering. An increase in UV-absorption as well as a pronounced radical scavenging are proposed and were proved experimentally. To sum up, MLG is interesting as a multifunctional nanofiller and seems to be quite ready for rubber development. T2 - TOP 2016, VIII International Conference on “Times of Polymers and Composites” CY - Naples, Italy DA - 19.06.2016 KW - Graphene KW - Nanocomposite KW - Rubber PY - 2016 SN - 978-0-7354-1390-0 DO - https://doi.org/10.1063/1.4949621 SN - 0094-243X SN - 1551-7616 VL - 1736 SP - 020046, 1 EP - 4 PB - AIP AN - OPUS4-36864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sut, Aleksandra A1 - Greiser, Sebastian A1 - Jäger, Christian A1 - Schartel, Bernhard T1 - Synergy in flame-retarded epoxy resin - Identification of chemical interactions by solid-state NMR N2 - The potential synergists aluminium diethylphosphinate (AlPi), boehmite (AlO(OH)) and melamine polyphosphate (MPP) were compared in flame-retardant epoxy resin (EP)/melamine poly(magnesium phosphate) (S600). The pyrolysis, the fire behaviour as well as the chemical interactions in the gas and condensed phases were investigated by various methods. Flammability was investigated by cone calorimeter and oxygen index (OI). The thermal and thermo-oxidative decomposition were studied by thermogravimetric analysis coupled with FTIR spectrometer. The special focus was on the Investigation of structural changes in the condensed phase via solid-state NMR of 27Al and 31P nuclei. By the comparison of epoxy resin with only one additive or with S600 in combination with AlPi, AlO(OH) or MPP, it was possible to calculate the synergy index. The best performance in terms of fire behaviour was observed for EP/S600/MPP with a PHRR (Peak heat release rate) of 208 kW m-2 due to slight synergy. In the case of THE (total heat evolved), clear synergy occurred for EP/S600/AlPi and EP/S600/AlO(OH). By solid-state NMR, different phosphates and aluminates were identified, indicating the chemical interactions between S600 and AlPi, AlO(OH) or MPP. The systematic multi-methodical approach yielded insight into the synergistic effects in the flame-retarded epoxy resin. KW - Synergy KW - Epoxy resin KW - Flame retardancy KW - Melamine poly(magnesium phosphate) KW - Solid-state NMR PY - 2017 DO - https://doi.org/10.1007/s10973-016-5934-4 SN - 1388-6150 SN - 1588-2926 VL - 128 IS - 1 SP - 141 EP - 153 PB - Springer AN - OPUS4-39298 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sut, Aleksandra A1 - Greiser, Sebastian A1 - Jäger, Christian A1 - Schartel, Bernhard T1 - Aluminium diethylphosphinate versus ammonium polyphosphate: A comprehensive comparison of the chemical interactions during pyrolysis in flame-retarded polyolefine/poly(phenylene oxide) N2 - A systematic comparison of chemical interactions and fire behaviour is presented for the thermoplas-tic elastomer (block copolymer styrene-ethylene-butadiene-styrene) (TPE-S)/diethyl- and methylvinylsiloxane (Si)/poly(phenylene oxide) (PPO), flame-retarded with aluminium diethylphosphinate (AlPi)and with ammonium polyphosphate (APP), respectively. TPE-S/APP/Si/PPO performed better in the conecalorimeter test (reduction in peak heat release rate from 2042 to 475 kW m−2), but TPE-S/AlPi/Si/PPO inthe flammability tests (oxygen index (OI) and UL 94). This difference was caused by the different modes ofaction of APP (more in the condensed phase) and AlPi (mainly in the gas phase). Thermogravimetry cou-pled with Fourier transform infrared spectroscopy (TG-FTIR) was used to analyse the mass loss and theevolved gas products, while a Linkam hot-stage cell to investigate the decomposition in the condensedphase. Moreover, a detailed analysis of the fire residues was done using solid-state NMR.13C MAS NMRshowed that both flame-retarded compositions form graphite-like amorphous carbonaceous char, orig-inating from PPO.31P MAS NMR and29Si MAS NMR delivered important information about interactionbetween phosphorus and the siloxane. For TPE-S/AlPi/Si/PPO aluminium phosphate and silicon dioxideoccurred, while also silicophosphate was produced in TPE-S/APP/Si/PPO. The direct comparison of two ofthe most prominent halogen-free flame retardants containing phosphorus delivered meaningful insightsinto the modes of action and molecular mechanisms controlling flame retardancy. KW - Aluminium diethylphosphinate KW - Ammonium polyphosphate KW - Flame retardancy KW - Solid-state NMR KW - SEBS PY - 2016 SN - 0040-6031 SN - 1872-762X VL - 640 SP - 74 EP - 84 PB - Elsevier AN - OPUS4-37802 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Langfeld, Kirsten A1 - Wilke, Antje A1 - Sut, Aleksandra A1 - Greiser, Sebastian A1 - Ulmer, B. A1 - Andrievici, V. A1 - Limbach, P. A1 - Bastian, Martin A1 - Schartel, Bernhard T1 - Halogen-free fire retardant styrene-ethylene-butylene-styrene-based thermoplastic elastomers using synergistic aluminium diethylphosphinate-based combinations N2 - 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. KW - Flame retardancy KW - Aluminium phosphinate KW - Thermoplastic elastomers KW - Cone calorimetry KW - Flammability PY - 2015 DO - https://doi.org/10.1177/0734904114565581 SN - 0734-9041 SN - 1530-8049 VL - 33 IS - 2 SP - 157 EP - 177 PB - Sage CY - London AN - OPUS4-32692 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strommer, Bettina A1 - Battig, Alexander A1 - Schulze, Dietmar A1 - Agudo Jácome, Leonardo A1 - Schartel, Bernhard A1 - Böhning, Martin T1 - Shape, orientation, interaction, or dispersion: valorization of the influence factors in natural rubber nanocomposites N2 - The addition of nanoparticles as reinforcing fillers in elastomers yields nanocomposites with unique property profiles, which opens the door for various new application fields. Major factors influencing the performance of nanocomposites are studied by varying the type and shape of nanoparticles and their dispersion in the natural rubber matrix. The industrial applicability of these nanocomposites is put into focus using two types of graphene and a nanoscale carbon black, all commercially available, and scalable processing techniques in the form of a highly filled masterbatch production via latex premixing by simple stirring or ultrasonically assisted dispersing with surfactant followed by conventional two-roll milling and hot pressing. Different processing and measurement methods reveal the potential for possible improvements: rheology, curing behavior, static and dynamic mechanical properties, swelling, and fire behavior. The aspect ratio of the nanoparticles and their interaction with the surrounding matrix prove to be crucial for the development of superior nanocomposites. An enhanced dispersing method enables the utilization of the improvement potential at low filler loadings (3 parts per hundred of rubber [phr]) and yields multifunctional rubber nanocomposites: two-dimensional layered particles (graphene) result in anisotropic material behavior with strong reinforcement in the in-plane direction (157% increase in the Young's modulus). The peak heat release rate in the cone calorimeter is reduced by 55% by incorporating 3 phr of few-layer graphene via an optimized dispersing process. KW - Graphene KW - Natural rubber KW - Nanocomposites KW - Anisotropy KW - Fire behavior PY - 2023 DO - https://doi.org/10.5254/rct.23.77961 SN - 0035-9475 SN - 1943-4804 VL - 96 IS - 1 SP - 40 EP - 58 PB - Allen Press CY - Lawrence (KA), USA AN - OPUS4-57568 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sunder, S. A1 - Jauregui Rozo, Maria A1 - Deshpande, H. A1 - Neyer, A. A1 - Papaiya, V. A1 - Meinel, Dietmar A1 - Schartel, Bernhard A1 - Ruckdäschel, H. T1 - Char to the Rescue: Processing and Transfer of Flame-Retardant Epoxy Resins, Adjusting the Fire Behavior and Post-Fire Structural Integrity of Glass Fiber Composites N2 - Epoxy (EP) glass fiber reinforced composites (GFRCs) are extensively used in structural applications due to their excellent thermal and mechanical properties, but their inherent flammability limits fire-safe deployment. While numerous studies examine the flame retardancy of resins or individual composite systems, comprehensive studies evaluating simultaneous improvements in flame retardancy and post-fire mechanical integrity, specifically through prepreg processing, remain challenging. This study investigates the effectiveness and transferability of phosphorus-based flame retardant (FR) systems to diglycidyl ether of bisphenol A (DGEBA) and EP novolac resin matrices and their corresponding bidirectional glass fiber composites via prepregs. The FRs are chosen based on varying modes of action: ammonium polyphosphate with inorganic silicate (APP/InSi) primarily acts in the condensed phase (CP), and aluminum diethyl phosphinate with zinc hydroxystannate (AldietPO2/ZHS) is known to demonstrate both gas-phase (GP) and CP activity. Fire residues are tailored to compensate for structural defects from fire exposure. EP novolac, with higher aromaticity and cross-linking, possesses better inherent flame resistance compared to DGEBA. The novolac composites containing AldietPO2/ZHS simultaneously showed the highest retention of flexural properties after fire exposure and the best fire safety index. The experimental values of the post-fire flexural properties in the composites calibrated damage parameters in two theoretical models. KW - Composites KW - DGEBA KW - Epoxy novolac KW - Post-fire KW - Prepregs PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643752 DO - https://doi.org/10.1002/pol.20250692 SN - 2642-4169 SN - 2642-4150 VL - 63 IS - 20 SP - 4295 EP - 4309 PB - Wiley AN - OPUS4-64375 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -