TY - JOUR A1 - Ghasem Zadeh Khorasani, Media A1 - Elert, Anna Maria A1 - Hodoroaba, Vasile-Dan A1 - Agudo Jácome, Leonardo A1 - Altmann, Korinna A1 - Silbernagl, Dorothee A1 - Sturm, Heinz T1 - Short- and long-range mechanical and chemical interphases caused by interaction of Boehmite (γ-AlOOH) with anhydride-cured epoxy resins N2 - Understanding the interaction between boehmite and epoxy and the formation of their interphases with different mechanical and chemical structures is crucial to predict and optimize the properties of epoxy-boehmite nanocomposites. Probing the interfacial properties with atomic force microscopy (AFM)-based methods, especially particle-matrix long-range interactions, is challenging. This is due to size limitations of various analytical methods in resolving nanoparticles and their interphases, the overlap of interphases, and the effect of buried particles that prevent the accurate interphase property measurement. Here, we develop a layered model system in which the epoxy is cured in contact with a thin layer of hydrothermally synthesized boehmite. Different microscopy methods are employed to evaluate the interfacial properties. With intermodulation atomic force microscopy (ImAFM) and amplitude dependence force spectroscopy (ADFS), which contain information about stiffness, electrostatic, and van der Waals forces, a soft interphase was detected between the epoxy and boehmite. Surface potential maps obtained by scanning Kelvin probe microscopy (SKPM) revealed another interphase about one order of magnitude larger than the mechanical interphase. The AFM-infrared spectroscopy (AFM-IR) technique reveals that the soft interphase consists of unreacted curing agent. The long-range electrical interphase is attributed to the chemical alteration of the bulk epoxy and the formation of new absorption bands. KW - Nanocomposites KW - Interphase KW - Intermodulation AFM KW - Electron microscopy KW - Infrared nano AFM PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-483672 UR - https://www.mdpi.com/2079-4991/9/6/853/htm DO - https://doi.org/10.3390/nano9060853 SN - 2079-4991 VL - 9 IS - 6 SP - 853, 1 EP - 20 PB - MDPI AN - OPUS4-48367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Topolniak, Ievgeniia A1 - Hodoroaba, Vasile-Dan A1 - Pfeifer, Dietmar A1 - Braun, Ulrike A1 - Sturm, Heinz T1 - Boehmite Nanofillers in Epoxy Oligosiloxane Resins: Influencing the Curing Process by Complex Physical and Chemical Interactions N2 - In this work, a novel boehmite (BA)-embedded organic/inorganic nanocomposite coating based on cycloaliphatic epoxy oligosiloxane (CEOS) resin was fabricated applying UV-induced cationic polymerization. The main changes of the material behavior caused by the nanofiller were investigated with regard to its photocuring kinetics, thermal stability, and glass transition. The role of the particle surface was of particular interest, thus, unmodified nanoparticles (HP14) and particles modified with p-toluenesulfonic acid (OS1) were incorporated into a CEOS matrix in the concentration range of 1–10 wt.%. Resulting nanocomposites exhibited improved thermal properties, with the glass transition temperature (Tg) being shifted from 30 °C for unfilled CEOS to 54 °C (2 wt.% HP14) and 73 °C (2 wt.% OS1) for filled CEOS. Additionally, TGA analysis showed increased thermal stability of samples filled with nanoparticles. An attractive interaction between boehmite and CEOS matrix influenced the curing. Real-time infrared spectroscopy (RT-IR) experiments demonstrated that the epoxide conversion rate of nanocomposites was slightly increased compared to neat resin. The beneficial role of the BA can be explained by the participation of hydroxyl groups at the particle surface in photopolymerization processes and by the complementary contribution of p-toluenesulfonic acid surface modifier and water molecules introduced into the system with nanoparticles. KW - Real-time infrared spectroscopy KW - Boehmite KW - Nanocomposite KW - Cationic photocuring KW - Cycloaliphatic epoxy oligosiloxane KW - Epoxy conversion degree PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-479628 DO - https://doi.org/10.3390/ma12091513 VL - 12 IS - 9 SP - 1513 PB - MDPI AN - OPUS4-47962 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schwibbert, Karin A1 - Menzel, F. A1 - Epperlein, N. A1 - Bonse, Jörn A1 - Krüger, Jörg T1 - Bacterial adhesion on femtosecond laser-modified polyethylene N2 - In this study, femtosecond laser-induced sub-micrometer structures are generated to modify polyethylene (PE) surface topographies. These surfaces were subjected to bacterial colonization studies with Escherichia coli and Staphylococcus aureus as test strains. The results reveal that the nanostructures do not influence S. aureus coverage, while the adhesion of E. coli is reduced. KW - Bacterial adhesion KW - Laser-modified surface KW - Polyethylene KW - Laser-induced nanostructures KW - Biofilm PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-492280 DO - https://doi.org/10.3390/ma12193107 VL - 12 IS - 19 SP - 3107 PB - MDPI CY - Basel, Schweiz AN - OPUS4-49228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mezera, M. A1 - Bonse, Jörn A1 - Römer, G.R.B.E. T1 - Influence of Bulk Temperature on Laser-Induced Periodic Surface Structures on Polycarbonate N2 - In this paper, the influence of the bulk temperature (BT) of Polycarbonate (PC) on the occurrence and growth of Laser-induced Periodic Surface Structures (LIPSS) is studied. Ultrashort UV laser pulses with various laser peak fluence levels F_0 and various numbers of overscans (N_OS) were applied on the surface of pre-heated Polycarbonate at different bulk temperatures. Increased BT leads to a stronger absorption of laser energy by the Polycarbonate. For N_OS < 1000 High Spatial Frequency LIPSS (HSFL), Low Spatial Frequency LIPSS perpendicular (LSFL-I) and parallel (LSFL-II) to the laser polarization were only observed on the rim of the ablated tracks on the surface but not in the center of the tracks. For N_OS ≥ 1000 , it was found that when pre-heating the polymer to a BT close its glass transition temperature (T_g), the laser fluence to achieve similar LIPSS as when processed at room temperature decreases by a factor of two. LSFL types I and II were obtained on PC at a BT close to T_g and their periods and amplitudes were similar to typical values found in the literature. To the best of the author’s knowledge, it is the first time both LSFL types developed simultaneously and consistently on the same sample under equal laser processing parameters. The evolution of LIPSS from HSFL, over LSFL-II to LSFL I, is described, depending on laser peak fluence levels, number of pulses processing the spot and bulk temperature. KW - Laser-induced periodic surface structures (LIPSS) KW - Polycarbonate KW - Bulk temperature KW - Ultrashort laser pulses PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-498242 UR - https://www.mdpi.com/2073-4360/11/12/1947 DO - https://doi.org/https://doi.org/10.3390/polym11121947 SN - 2073-4360 VL - 11 IS - 12 SP - 1947 PB - MDPI CY - Basel, Switzerland AN - OPUS4-49824 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Legall, Herbert A1 - Schwanke, Christoph A1 - Bonse, Jörn A1 - Krüger, Jörg T1 - The influence of processing parameters on X‑ray emission during ultra‑short pulse laser machining N2 - During ultra-short laser material processing at high laser pulse repetition rates unwanted X-ray radiation can be generated in a quantity that may constitute a potential risk for health. An adequate X-ray radiation protection requires a thoroughly understanding of the influence of the laser processing parameters on the generation of X-ray radiation. In the present work, the generated X-ray dose during laser machining was investigated in air for varying beam scanning conditions at a pulse duration of 925 fs, a center wavelength of 1030 nm and a laser peak intensity of 2.6 × 10^14 W/cm^2. The X-ray radiation dose and the corresponding spectral X-ray emission were investigated in dependence on the laser’s pulse repetition rate and on the beam scanning speed. The results show a strong dependence of the X-ray emission on these laser processing parameters. KW - Laser-induced X-ray emission KW - Ultrashort laser material interaction KW - Femtosecond laser KW - Radiation protection PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-486441 DO - https://doi.org/10.1007/s00339-019-2827-y SN - 0947-8396 SN - 1432-0630 VL - 125 IS - 8 SP - 570, 1 EP - 8 PB - Springer AN - OPUS4-48644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ghasem Zadeh Khorasani, Media A1 - Silbernagl, Dorothee A1 - Platz, D. A1 - Sturm, Heinz T1 - Insights into Nano-Scale Physical and Mechanical Properties of Epoxy/Boehmite Nanocomposite Using Different AFM Modes N2 - Understanding the interaction between nanoparticles and the matrix and the properties of interphase is crucial to predict the macroscopic properties of a nanocomposite system. Here, we investigate the interaction between boehmite nanoparticles (BNPs) and epoxy using different atomic force microscopy (AFM) approaches. We demonstrate benefits of using multifrequency intermodulation AFM (ImAFM) to obtain information about conservative, dissipative and van der Waals tip-surface forces and probing local properties of nanoparticles, matrix and the interphase. We utilize scanning kelvin probe microscopy (SKPM) to probe surface potential as a tool to visualize material contrast with a physical parameter, which is independent from the mechanics of the surface. Combining the information from ImAFM stiffness and SKPM surface potential results in a precise characterization of interfacial region, demonstrating that the interphase is softer than epoxy and boehmite nanoparticles. Further, we investigated the effect of boehmite nanoparticles on the bulk properties of epoxy matrix. ImAFM stiffness maps revealed the significant stiffening effect of boehmite nanoparticles on anhydride-cured epoxy matrix. The energy Dissipation of epoxy Matrix locally measured by ImAFM shows a considerable increase compared to that of neat epoxy. These measurements suggest a substantial alteration of epoxy structure induced by the presence of boehmite. KW - Nanomechanics KW - Intermodulation-AFM KW - Interphase KW - Boehmite KW - Epoxy PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-476040 DO - https://doi.org/10.3390/polym11020235 SN - 2073-4360 VL - 11 IS - 2 SP - 235, 1 EP - 19 PB - MDPI AN - OPUS4-47604 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ghasem Zadeh Khorasani, Media A1 - Silbernagl, Dorothee A1 - Szymoniak, Paulina A1 - Hodoroaba, Vasile-Dan A1 - Sturm, Heinz T1 - The effect of boehmite nanoparticles (gamma‐AlOOH) on nanomechanical and thermomechanical properties correlated to crosslinking density of epoxy N2 - We show that complex physical and chemical interactions between boehmite nanoparticles and epoxy drastically affect matrix properties, which in the future will provide tuning of material properties for further optimization in applications from automotive to aerospace. We utilize intermodulation atomic force microscopy (ImAFM) for probing local stiffness of both particles and polymer matrix. Stiff particles are expected to increase total stiffness of nanocomposites and the stiffness of polymer should remain unchanged. However, ImAFM revealed that stiffness of matrix in epoxy/boehmite nanocomposite is significantly higher than unfilled epoxy. The stiffening effect of the boehmite on epoxy also depends on the particle concentration. To understand the mechanism behind property alteration induced by boehmite nanoparticles, network architecture is investigated using dynamic mechanical thermal analysis (DMTA). It was revealed that although with 15 wt% boehmite nanoparticles the modulus at glassy state increases, crosslinking density of epoxy for this composition is drastically low. KW - Crosslinking density KW - Epoxy KW - Intermodulation KW - Atomic force microscopy KW - Nanomechanical properties KW - Boehmite nanoparticles PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-476050 DO - https://doi.org/10.1016/j.polymer.2018.12.054 SN - 0032-3861 SN - 1873-2291 VL - 164 SP - 174 EP - 182 PB - Elsevier AN - OPUS4-47605 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Greco, A. A1 - Starostin, V. A1 - Karapanagiotis, C. A1 - Hinderhofer, A. A1 - Gerlach, A. A1 - Pithan, L. A1 - Liehr, Sascha A1 - Schreiber, Frank A1 - Kowarik, Stefan T1 - Fast fitting of reflectivity data of growing thin films using neural networks N2 - X-ray reflectivity (XRR) is a powerful and popular scattering technique that can give valuable insight into the growth behavior of thin films. This study Shows how a simple artificial neural network model can be used to determine the thickness, roughness and density of thin films of different organic semiconductors [diindenoperylene, copper(II) phthalocyanine and alpha-sexithiophene] on silica from their XRR data with millisecond computation time and with minimal user input or a priori knowledge. For a large experimental data set of 372 XRR curves, it is shown that a simple fully connected model can provide good results with a mean absolute percentage error of 8–18% when compared with the results obtained by a genetic least mean squares fit using the classical Parratt formalism. Furthermore, current drawbacks and prospects for improvement are discussed. KW - Artificial neural networks KW - X-ray reflectivity PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-498997 DO - https://doi.org/10.1107/S1600576719013311 SN - 1600-5767 VL - 52 SP - 1342 EP - 1347 PB - Wiley AN - OPUS4-49899 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zirnstein, Benjamin A1 - Schulze, Dietmar A1 - Schartel, Bernhard T1 - Mechanical and fire properties of multicomponent flame retardant EPDM rubbers using aluminum trihydroxide, ammonium polyphosphate, and polyaniline N2 - In this study, multicomponent flame retardant systems, consisting of Ammonium polyphosphate (APP), aluminum trihydroxide (ATH), and polyaniline (PANI), were used in ethylene propylene diene monomer (EPDM) rubber. The multicomponent system was designed to improve flame retardancy and the mechanical properties of the rubber compounds, while simultaneously reducing the amount of filler. PANI was applied at low loadings (7 phr) and combined with the phosphorous APP (21 phr) and the mineral flame retardant ATH (50 phr). A comprehensive study of six EPDM rubbers was carried out by systematically varying the fillers to explain the impact of multicomponent flame retardant systems on mechanical properties. The six EPDM materials were investigated via the UL 94, limiting oxygen index (LOI), FMVSS 302, glow wire tests, and the cone calorimeter, showing that multicomponent flame retardant systems led to improved fire performance. In cone calorimeter tests the EPDM/APP/ATH/PANI composite reduced the maximum average rate of heat emission (MARHE) to 142 kW·m-2, a value 50% lower than that for the unfilled EPDM rubber. Furthermore, the amount of phosphorus in the residues was quantified and the mode of action of the phosphorous flame retardant APP was explained. The data from the cone calorimeter were used to determine the protective layer effect of the multicomponent flame retardant systems in the EPDM compounds. KW - EPDM KW - Rubber KW - Flame retardant KW - Polyaniline KW - Aluminum trihydroxide (ATH) PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-482769 DO - https://doi.org/10.3390/ma12121932 SN - 1996-1944 VL - 12 IS - 12 SP - 1932, 1 EP - 22 PB - MDPI AN - OPUS4-48276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Battig, Alexander A1 - Markwart, J. C. A1 - Wurm, F. R. A1 - Schartel, Bernhard T1 - Hyperbranched phosphorus flame retardants: multifunctional additives for epoxy resins N2 - We successfully synthesized multifunctional P-based hyperbranched polymeric flame retardants (hb-FRs) with varying oxygen-to-nitrogen (O : N) content and characterized them via 1H and 31P NMR and GPC. Their miscibility in epoxy resins (EP) and impact on glass-transition temperatures (Tg) were determined via differential scanning calorimetry (DSC). Using thermogravimetric and evolved gas Analysis (TGA, TG-FTIR), pyrolysis gas chromatography/mass spectrometry (Py-GC-MS), hot stage FTIR, flammability tests UL-94 and LOI, fire testing via cone calorimetry, residue analysis via scanning electron microscopy (SEM) and elemental analysis, detailed decomposition mechanisms and modes of action are proposed. hb-polymeric FRs have improved miscibility and thermal stability, leading to high FR performance even at low loadings. Polymeric, complex FRs increase flame retardancy, mitigate negative effects of low molecular weight variants, and can compete with commercial aromatic FRs. The results illustrate the role played by the chemical structure in flame retardancy and highlight the potential of hb-FRs as multifunctional additives. KW - Flame retardant KW - Hyperbranched PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-486589 DO - https://doi.org/10.1039/c9py00737g SN - 1759-9962 SN - 1759-9954 VL - 10 IS - 31 SP - 4346 EP - 4358 PB - RSC AN - OPUS4-48658 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Markwart, J. C. A1 - Battig, Alexander A1 - Velencoso, M. M. A1 - Pollok, D. A1 - Schartel, Bernhard A1 - Wurm, F. R. T1 - Aromatic vs. Aliphatic Hyperbranched Polyphosphoesters as Flame Retardants in Epoxy Resins N2 - The current trend for future flame retardants (FRs) goes to novel efficient halogen-free materials, due to the ban of several halogenated FRs. Among the most promising alternatives are phosphorus-based FRs, and of those, polymeric materials with complex shape have been recently reported. Herein, we present novel halogen-free aromatic and aliphatic hyperbranched polyphosphoesters (hbPPEs), which were synthesized by olefin Metathesis polymerization and investigated them as a FR in epoxy resins. We compare their efficiency (aliphatic vs. aromatic) and further assess the differences between the monomeric compounds and the hbPPEs. The decomposition and vaporizing behavior of a compound is an important factor in its flame-retardant behavior, but also the interaction with the pyrolyzing matrix has a significant influence on the performance. Therefore, the challenge in designing a FR is to optimize the chemical structure and its decomposition pathway to the matrix, with regards to time and temperature. This behavior becomes obvious in this study, and explains the superior gas phase activity of the aliphatic FRs. KW - Phosphorus KW - Metathesis KW - Dendritic KW - Cone calorimeter KW - Fire test PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-494535 DO - https://doi.org/10.3390/molecules24213901 SN - 1420-3049 VL - 24 IS - 21 SP - 3901 PB - MDPI AN - OPUS4-49453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lenz, J. A1 - Pospiech, D. A1 - Paven, M. A1 - Albach, R. W. A1 - Günther, Martin A1 - Schartel, Bernhard A1 - Voit, B. T1 - Improving the Flame Retardance of Polyisocyanurate Foams by Dibenzo[d,f][1,3,2]dioxaphosphepine 6-Oxide-Containing Additives N2 - A series of new flame retardants (FR) based on dibenzo[d,f][1,3,2]dioxaphosphepine 6-oxide (BPPO) incorporating acrylates and benzoquinone were developed previously. In this study, we examine the fire behavior of the new flame retardants in polyisocyanurate (PIR) foams. The foam characteristics, thermal decomposition, and fire behavior are investigated. The fire properties of the foams containing BPPO-based derivatives were found to depend on the chemical structure of the substituents. We also compare our results to state-of-the-art non-halogenated FR such as triphenylphosphate and chemically similar phosphinate, i.e. 9,10-dihydro-9-oxa-10- phosphaphenanthrene-10-oxide (DOPO), based derivatives to discuss the role of the phosphorus oxidation state. KW - Polyisocyanurate KW - Dibenzo[d,f][1,3,2]dioxaphosphepine 6-oxide KW - Phospha-Michael addition KW - Flame retardant KW - Foams PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-485590 DO - https://doi.org/10.3390/polym11081242 SN - 2073-4360 VL - 11 IS - 8 SP - Article 1242 PB - MDPI AN - OPUS4-48559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Markwart, J. C. A1 - Battig, Alexander A1 - Kuckhoff, T. A1 - Schartel, Bernhard A1 - Wurm, F. R. T1 - First phosphorus AB2 monomer for flame-retardant hyperbranched polyphosphoesters: AB2vs. A2 + B3 N2 - Branched polymers are an important class of polymers with a high number of terminal groups, lower viscosity compared to their linear analogs and higher miscibility, which makes them especially interesting for flame retardant applications, where the flame retardants (FR) are blended with another polymer matrix. Hyperbranched polyphosphoesters (hbPPEs) are gaining more and more interest in the field of flame retardancy, as low molar mass FRs often have the disadvantage of blooming out or leaching, which is not desired in consumer products. Here, we present the first phosphorus-based AB2 monomer for the synthesis of hbPPEs and assess its flame-retardant performance in an epoxy resin compared to a hbPPE synthesized by an A2 + B3 approach. The hbPPE synthesized from an AB2 monomer exhibited a slightly higher performance compared to a similar hbPPE, which was prepared by A2 + B3 polyaddition, probably due to its higher phosphorus content. KW - Polyphosphoester KW - Hyperbranched KW - Flame retardant KW - Synthesis PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-497570 DO - https://doi.org/10.1039/c9py01156k SN - 1759-9962 VL - 10 IS - 43 SP - 5920 EP - 5930 PB - RSC AN - OPUS4-49757 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mieller, Björn T1 - Influence of test procedure on dielectric breakdown strength of alumina N2 - Dielectric strength testing of ceramics can be performed with various setups and parameters. Comparisons of results from different sources are often not meaningful, because the results are strongly dependent on the actual testing procedure. The aim of this study is to quantify the influence of voltage ramp rate, electrode size, electrode conditioning, and sample thickness on the measured AC dielectric strength of a commercial alumina. Mean values, Weibull moduli, and failure probabilities determined in standardized short time tests are evaluated and related to withstand voltage tests. Dielectric strength values in the range from 21.6 to 33.2 kV/mm were obtained for the same material using different testing procedures. Short time tests resulted in small standard deviations (< 2 kV/mm) and high Weibull moduli around 30, while withstand tests at voltage levels with low and virtual zero failure probability in short time tests resulted in large scatter of withstand time and Weibull moduli < 1. The strong decrease in Weibull moduli is attributed to progressive damage from partial discharge and depolarization during AC testing. These findings emphasize the necessity of a thorough documentation of testing procedure and highlight the importance of withstand voltage tests for a comprehensive material characterization. KW - Ceramic KW - High-voltage testing KW - Dielectric breakdown KW - Alumina PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-483852 DO - https://doi.org/10.1007/s40145-018-0310-4 SN - 2226-4108 SN - 2227-8508 VL - 8 IS - 2 SP - 247 EP - 255 PB - Springer AN - OPUS4-48385 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rabe, Sebastian A1 - Sánchez-Olivares, G. A1 - Pérez-Chávez, R. A1 - Schartel, Bernhard T1 - Natural keratin and coconut fibres from industrial wastes in flame retarded thermoplastic starch biocomposites N2 - Natural keratin fibres derived from Mexican tannery waste and coconut fibres from coconut processing waste were used as fillers in commercially available, biodegradable thermoplastic starch-polyester blend to obtain sustainable biocomposites. The morphology, rheological and mechanical properties as well as pyrolysis, flammability and forced flaming combustion behaviour of those biocomposites were investigated. In order to open up new application areas for these kinds of biocomposites, ammonium polyphosphate (APP) was added as a flame retardant. Extensive flammability and cone calorimeter studies revealed a good flame retardance effect with natural fibres alone and improved effectiveness with the addition of APP. In fact, it was shown that replacing 20 of 30 wt. % of APP with keratin fibres achieved the same effectiveness. In the case of coconut fibres, a synergistic effect led to an even lower heat release rate and total heat evolved due to reinforced char residue. This was confirmed via scanning electron microscopy of the char structure. All in all, these results constitute a good approach towards sustainable and biodegradable fibre reinforced biocomposites with improved flame retardant properties. KW - Biomaterials KW - Biodegradable KW - Calorimetry KW - Composites KW - Flame retardance PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-472518 DO - https://doi.org/10.3390/ma12030344 SN - 1996-1944 VL - 12 IS - 3 SP - 344, 1 EP - 24 PB - MDPI AN - OPUS4-47251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sut, Aleksandra A1 - Metzsch-Zilligen, E. A1 - Großhauser, M. A1 - Pfaendner, R. A1 - Schartel, Bernhard T1 - Synergy between melamine cyanurate, melamine polyphosphate and aluminum diethylphosphinate in flame retarded thermoplastic polyurethane N2 - The multicomponent flame retardant system of melamine polyphosphate (MPP), melamine cyanurate (MC) and aluminum diethylphosphinate (AlPi) is proposed and investigated for thermoplastic polyurethane (TPU). The synergy between those additives and the resulting superior fire performance are discussed. Systematically varied sets of flame retarded TPU with various MPP/MC/AlPi ratios were investigated in terms of fire behavior, pyrolysis products and mechanical properties. The total amount of the additives was always 30 wt.-%. Further, the influence of various AlPi concentrations was investigated. The optimal MPP:MC ratio was determined while keeping the amount of AlPi constant. The combination of 8 wt.-% MPP, 12 wt.-% MC and 10 wt.-% is proposed as the most promising halogen free flame retardant formulation for TPU, because it yielded a reduction in PHRR from 2660 kW/m2 (TPU) to 452 kW/m2 and enabled V-0 classification in the UL 94 test. Combinations of MPP and MC as well a high concentration of AlPi are beneficial for the mechanical properties e.g. tensile strength and elongation at break of the formulations and could be a strong competitor to commercial flame retarded TPUs. KW - Thermoplastic polyurethane KW - Synergy KW - Melamine cyanurate KW - Melamine polyphosphate KW - Aluminum diethylphosphinate KW - Rapid mass calorimeter PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-472523 DO - https://doi.org/10.1016/j.polymertesting.2019.01.001 SN - 0142-9418 VL - 74 SP - 196 EP - 204 PB - Elsevier Ltd. AN - OPUS4-47252 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -