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 - 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 - Tabaka, Weronika A1 - Timme, Sebastian A1 - Lauterbach, Tobias A1 - Medina, L. A1 - Berglund, L. A. A1 - Carosio, F. A1 - Duquesne, S. A1 - Schartel, Bernhard T1 - Bench-scale fire stability testing - Assessment of protective systems on carbon fibre reinforced polymer composites N2 - Fire resistance testing of components made of carbon fibre reinforced polymers (CFRP) usually demands intermediate-scale or full-scale testing. A bench-scale test is presented as a practicable and efficient method to assess how different fire protective systems improve the structural integrity of CFRPs during fire. The direct flame of a fully developed fire was applied to one side of the CFRP specimen, which was simultaneously loaded with compressive force. Three different approaches (film, non-woven, and coatings) were applied: paper with a thickness in the range of μm consisting of cellulose nanofibre (CNF)/clay nanocomposite, nonwoven mats with thickness in the range of cm and intumescent coatings with a thickness in the range of mm. The uncoated specimen failed after just 17 s. Protection by these systems provides fire stability, as they multiply the time to failure by as much as up to 43 times. The reduced heating rates of the protected specimens demonstrate the reduced heat penetration, indicating the coatings’ excellent heat shielding properties. Bench-scale fire stability testing is shown to be suitable tool to identify, compare and assess different approaches to fire protection. KW - Fire stability KW - Bench-scale fire resistance KW - Carbon fibre reinforced polymer KW - Protective coatings PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-532401 DO - https://doi.org/10.1016/j.polymertesting.2021.107340 SN - 0142-9418 SN - 1873-2348 VL - 102 SP - 7340 PB - Elsevier CY - Amsterdam AN - OPUS4-53240 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jauregui Rozo, Maria A1 - Sunder, S. A1 - Tabaka, Weronika A1 - Klaffke, Benjamin A1 - Ruckdäschel, H. A1 - Schartel, Bernhard T1 - Unveiling aluminum diethyl phosphinate dual identity: Transfer from epoxy resins to glass fiber-reinforced composites N2 - This study examines the transfer of the flame-retardant aluminum diethyl phosphinate (AlPi) from epoxy resins to composites and the impact of AlPi on fire behavior and fire stability. Further, the effects of different particle sizes and the addition of zinc hydroxy stannate (ZHS) and inorganic silicate (InSi) are investigated. The research provides a detailed analysis of the fire behavior, fire stability, pyrolysis, flame-retardant modes of action, and flame retardancy index. Interestingly, the particle sizes did not significantly affect the flammability, fire behavior, or fire stability in the systems investigated. AlPi acts primarily in the gas phase, releasing phosphorus that yields flame inhibition. Adding glass fibers (GFs) to the epoxy resin boosts the flame retardancy in the condensed phase, reducing the heat release rate (HRR), total heat release (THR), and peak heat release rate (PHRR) by about 60%. This improvement is largely due to replacing fuel and forming a protective layer during burning. Despite the differences between thermoset and composite, the study demonstrates an effective transfer of flame-retardant properties from epoxy resins to fiber-reinforced composites, significantly enhancing the flame retardancy performance in both material systems. KW - Aluminum diethyl phosphinate KW - Epoxy resins KW - Fire behavior KW - Fire stability KW - Gas-phase active KW - Glass fiber-reinforced composites KW - Particle sizes PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643013 DO - https://doi.org/10.1002/pc.29911 SN - 1548-0569 SN - 0272-8397 VL - 46 IS - 14 SP - 12981 EP - 12999 PB - Wiley AN - OPUS4-64301 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tabaka, Weronika A1 - Meinel, Dietmar A1 - Schartel, Bernhard T1 - Sacrifice Few to Save Many: Fire Protective Interlayers in Carbon- Fiber-Reinforced Laminates N2 - The fire protection of carbon-fiber-reinforced polymer (CFRP) laminates often relies on flame-retardant coatings, but in some applications, their efficacy may diminish upon direct fire exposure due to rapid pyrolysis. This study introduces an innovative approach by integrating protective interlayers within the laminate structure to enhance the fire resistance. Various materials, including ceramic composite WHIPOX, titanium foil, poly(etherimide) (PEI) foil, basalt fibers, rubber mat, and hemp fibers, were selected as protective interlayers. These interlayers were strategically placed within the laminate layout to form a sacrificial barrier, safeguarding the integrity of the composite. Bench-scale fire resistance tests were conducted, where fire (180 kW/m2) was applied directly to the one side of the specimen by a burner while a compressive load was applied at the same time. Results indicate significant prolongation of time to failure for CFRP laminates with protective interlayers, which is up to 10 times longer. This innovative approach represents a potential advance in fire protection strategies for CFRP laminates, offering improved resilience against fire-induced structural failure. KW - Composites in fire KW - Fire resistance KW - Fire retardant interlayers KW - Laminate design KW - Carbon fibre reinforced PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601943 DO - https://doi.org/10.1021/acsomega.4c01408 SN - 2470-1343 VL - 9 IS - 22 SP - 23703 EP - 23712 PB - ACS AN - OPUS4-60194 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zirnstein, Benjamin A1 - Tabaka, Weronika A1 - Frasca, Daniele A1 - Schulze, Dietmar A1 - Schartel, Bernhard T1 - Graphene / hydrogenated acrylonitrile-butadiene rubber nanocomposites: Dispersion, curing, mechanical reinforcement, multifunctional filler N2 - Elastomers are usually mechanically reinforced with high loadings of carbon black (CB) to achieve the properties demanded; high amounts of mineral flame retardants are used to fulfill fire safety requirements. In this study, multilayer graphene (MLG), a nanoparticle made of only 10 graphene sheets, is applied in low loadings, 3 parts per hundred rubber (phr) to reduce the total amount of filler or boost performance in hydrogenated acrylonitrilebutadiene rubber (HNBR). In the HNBR/MLG nanocomposites, 3 phr MLG replaced 15 phr CB, 3 phr aluminum trihydroxide (ATH), or 15 phr CB + 3 phr ATH. The nanocomposites were prepared via master batch by ultrasonically assisted solution mixing and subsequent conventional two-roll milling. A comprehensive study is presented, illustrating the impact of MLG on curing and mechanical properties; e.g. replacing 2.5 phr ATH with 3 phr MLG increased the Young's modulus by over 60% and hardness by 10%, while improving flame retardancy, and reducing the total heat evolved by 10%. MLG is a multifunctional filler, as demonstrated by various enhancements in terms of the mechanical and flame retardancy properties of the rubber composites. KW - Nanocomposite KW - Rubber KW - Graphene PY - 2018 DO - https://doi.org/10.1016/j.polymertesting.2018.01.035 SN - 0142-9418 SN - 1873-2348 VL - 66 SP - 268 EP - 279 PB - Elsevier Ltd. AN - OPUS4-44457 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fichera, Mario Augusto A1 - Braun, Ulrike A1 - Schartel, Bernhard A1 - Sturm, Heinz A1 - Knoll, Uta A1 - Jäger, Christian T1 - Solid-state NMR investigations of the pyrolysis and thermo-oxidative decomposition products of a polystyrene/red phosphorus/magnesium hydroxide system N2 - Thermal, thermo-oxidative and fire residues of high impact polystyrene/magnesium hydroxide/red phosphorus (HIPS/Mg(OH)2/Pr) are investigated by solid-state NMR and compared with the results for the binary subsystem Mg(OH)2/Pr. The influences of oxygen, nitrogen and temperature are discussed. For a thermal decomposition and pyrolysis during combustion, the main pyrolysis of HIPS takes place while the remaining residue is a rather intact polymer, with a major share of the embedded Pr still present. Subsequently, mainly amorphous phosphates and a slight amount of crystalline Mg3(PO4)2 and Mg2P2O7 are formed at the highest temperatures. Only with increasing mass loss does the remaining polystyrene structure decompose and graphitic structures occur. The influence of oxygen on the decomposition mechanism is most obvious for the binary system Mg(OH)2/Pr. Pr vanishes more rapidly and crystalline, oxygen-rich magnesium phosphates are formed. In HIPS/Mg(OH)2/Pr systems the polymer acts as a barrier to reaction by the embedded particles, so that major characteristics of an anaerobic decomposition are found. Significant amounts of phosphorus are retained in the condensed phase through a reaction of Pr with Mg(OH)2 to mostly amorphous phosphates. This formation of amorphous inorganic magnesium phosphates can act as an additional physical barrier. This study outlines some advanced approaches for controlling the condensed-phase mechanisms of phosphorus and underlines that solid-state NMR is a most powerful tool for investigating the organic and inorganic residues. KW - HIPS KW - Red phosphorus KW - Magnesium hydroxide KW - Solid-state NMR KW - Flame retarded polymers PY - 2007 SN - 0165-2370 SN - 1873-250X VL - 78 IS - 2 SP - 378 EP - 386 PB - Elsevier CY - Amsterdam AN - OPUS4-14517 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tabaka, Weronika A1 - Schartel, Bernhard T1 - Less is More: Optimised Fire Performance in Glass Fibre-reinforced Polybutylene Terephthalate Laminates with Concentrated Flame Retardant Top Layer N2 - To achieve optimum fire performance while maintaining mechanical integrity, flame retardants (FR) were strategically concentrated in the surface layer of a two-layer glass fibre-reinforced polybutylene terephthalate (PBT) laminate structure. Three potentially synergistic FR systems were selected to improve the fire performance of glass fibre-reinforced PBT: boehmite (AlOOH) with melamine polyzinc phosphate (MPZnP), aluminium diethyl phosphinates (AlPi) with melamine cyanurate (MC), and expandable graphite (EG) with melamine polyphosphate (MPP). Limited Oxygen Index (LOI) and UL-94 testing highlighted the influence of laminate architecture on flammability. The cone calorimeter results showed that increasing the FR concentration in the top layer significantly reduced both the peak heat release rate (PHRR) and the maximum average rate of heat emission (MARHE), with improvements depending on the specific FR system used. The laminate L-PBT/GF/AlOOH/MPZnP with a 2:2 thickness ratio showed outstanding performance, achieving a 45 % reduction in MARHE compared to composites with uniform FR distribution. This result showcases the superior thermal barrier properties and synergistic behaviour of AlOOH and MPZnP. The fire performance of laminates containing AlPi and MC was strongly influenced by the distribution and concentration of AlPi/MC. The EG/MPP system was found to be highly effective, forming a protective intumescent layer that significantly reduced both HRR and MARHE, demonstrating the effectiveness of strategically concentrating FR in the top layer. KW - Glass fibres KW - PBT KW - Flame retardants KW - Composites KW - Laminates KW - Fire behaviour KW - Flammability PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626381 DO - https://doi.org/10.1016/j.jcomc.2025.100577 SN - 2666-6820 VL - 16 SP - 1 EP - 15 PB - Elsevier CY - Amsterdam AN - OPUS4-62638 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sturm, Heinz A1 - Schartel, Bernhard A1 - Weiß, André A1 - Braun, Ulrike T1 - SEM/EDX: Advanced investigation of structured fire residues and residue formation N2 - Heterogeneous, gradual or structured morphology of fire residues plays an important role in fire retardancy of polymers. A scanning electron microscope with an attached energy dispersive X-ray spectrometer (SEM/EDX) is highlighted as a powerful tool for the advanced characterization of such complex fire residues, since it offers high resolution in combination with both good depth of field and analysis of chemical composition. Two examples are presented: First, comprehensive SEM/EDX investigation on a complex structured fire residue of glass fibre reinforced polyamide 6,6 (PA 66-GF) flame retarded by diethylaluminium phosphinate, melamine polyphosphate and some zinc borate. A multilayered surface crust (thickness ~ 24 µm) covers a rather hollow area stabilized by GF glued together. The resulting efficient thermal insulation results in self-extinguishing before pyrolysis is completed, even under forced-flaming combustion. Second, sophisticated, quasi online SEM/EDX imaging of the formation of residual protection layer in layered silicate epoxy resin nanocomposites (LSEC). Burning specimens were quenched in liquid nitrogen for subsequent analyses. Different zones were distinguished in the condensed phase characterized by distinct processes such as melting and ablation of organic material, as well as agglomeration, depletion, exfoliation and reorientation of the LS. KW - Fire residue KW - SEM/EDX KW - Fire retardancy KW - PA 66 KW - Layered silicate KW - Diethylaluminium phosphinate PY - 2012 DO - https://doi.org/10.1016/j.polymertesting.2012.03.005 SN - 0142-9418 VL - 31 IS - 5 SP - 606 EP - 619 PB - Elsevier CY - Amsterdam AN - OPUS4-25802 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schneider, I. A1 - Kebelmann, Katharina A1 - Risse, S. A1 - Dieguez-Alonso, A. A1 - Schartel, Bernhard A1 - Strecker, C. A1 - Behrendt, F. T1 - Hydroliquefaction of Two Kraft Lignins in a Semibatch Setup under Process Conditions Applicable for Large-Scale Biofuel Production N2 - Hydroliquefaction is a possible pathway to produce liquid transportation fuels from solid feedstocks like coal or biomass. Though much effort has been put into the investigation of maximizing the oil yield using expensive catalysts and pasting oils in batch setups, little is known about how to commercialize the process. This work aims at the demonstration of lignin hydroliquefaction under conditions interesting for commercial operation. The results from hydroliquefaction experiments of two different lignin types using a cheap iron-based catalyst and anthracene oil as the pasting oil in a semibatch system are presented here. Oil yields of above 50% are reached without observing coke formation. Extensive analyses of the feedstocks and product oils were performed. The process supplies high-quality oil, while differences in the decomposition path of both lignin types are observed. An high heating value of 39 400 J/g and H/C and O/C ratios of up to 1.6 and 0.1, respectively, are detected for the produced bio-oils. KW - Lignin KW - Hydroliquefaction KW - Biofuel PY - 2019 DO - https://doi.org/10.1021/acs.energyfuels.9b02572 SN - 0887-0624 SN - 1520-5029 VL - 33 IS - 11 SP - 11057 EP - 11066 PB - ACS AN - OPUS4-50102 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -