TY - JOUR A1 - Schartel, Bernhard A1 - Weiß, André A1 - Mohr, F. A1 - Kleemeier, M. A1 - Hartwig, A. A1 - Braun, Ulrike T1 - Flame retarded epoxy resins by adding layered silicate in combination with the conventional protection-layer-building flame retardants melamine borate and ammonium polyphosphate N2 - The pyrolysis and flammability of phosphonium-modified layered silicate epoxy resin nanocomposites (EP/LS) were evaluated when LS was combined with two flame retardants, melamine borate (MB) and ammonium polyphosphate (APP), that also act via a surface protection layer. Thermogravimetry (TG), TG coupled with Fourier Transform Spectroscopy (TG-FTIR), oxygen index (LOI), UL 94 burning chamber (UL 94) and cone calorimeter were used. The glassy coating because of 10 wt % MB during combustion showed effects in the cone calorimeter test similar to nanodispersed LS, and somewhat better flame retardancy in flammability tests, such as LOI and UL 94. Adding APP to EP resulted in intumescent systems. The fire retardancy was particularly convincing when 15 wt % APP was used, especially for low external heat flux, and thus, also in flammability tests like LOI and UL 94. V0 classification is achieved when 15 wt % APP is used in EP. The flame retardancy efficiency of the protection layers formed does not increase linearly with the MB and APP concentrations used. The combination of LS with MB or APP shows antagonism; thus the performance of the combination of LS with MB or APP, respectively, was disappointing. No optimization of the carbonaceous-inorganic surface layer occurred for LS-MB. Combining LS with APP inhibited the intumescence, most probably through an increase in viscosity clearly above the value needed for intumescent behavior. KW - Nanocomposites KW - Fire retardance KW - Thermosets KW - Organoclay KW - Ammonium polyphosphate KW - Melamine borate PY - 2010 DO - https://doi.org/10.1002/app.32512 SN - 0021-8995 SN - 1097-4628 VL - 118 IS - 2 SP - 1134 EP - 1143 PB - Wiley InterScience CY - Hoboken, NJ AN - OPUS4-21725 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hübert, Thomas A1 - Unger, Brita A1 - Bücker, Michael T1 - Sol-gel derived TiO2 wood composites N2 - The sol–gel process was applied to enhance properties of pine sapwood. For this purpose wood prisms were soaked in nanoscaled precursor solutions prepared from titanium(IV) n-butoxide and titanium(IV) iso-propoxide, respectively, using vacuum impregnation technique. The wet composites were cured by special program with final heat treatment at 103 °C. Weight percent gains (WPG) of the wood specimen in the range of 19-25% were obtained due to these procedures. SEM investigations show that precursor solutions penetrate into the whole wood body and the titania formed after heat treatment in the composites is deposited in the pores (lumen) and partly in the cell walls of the wooden matrix. The moisture sorption was investigated in long term tests for a period of some months by storage at 20-23 °C in humid air (relative humidity of 99%) and ambient atmosphere (relative humidity 40-60%), respectively. For untreated reference samples the moisture sorption results in increasing of mass and volume according to saturation values of 24 and 13%, respectively, after about 15 days. The incorporation of titania reduces the saturation values of the moisture sorption by up to 12% in mass and by up to 5% in volume at a relative humidity of 99%. Thus, an enhancement of the dimensional stability of about 60% is obtained at best. The results demonstrate that modification of wood with sol-gel derived precursors can enhance its dimensional stability, which prevents the formation of cracks. Because of that reduced moisture sorption biological attacks should be delimited. Additionally, thermal analyses show a retarded combustion of the wood matrix due to titania infiltration. KW - Titania KW - Sol-gel KW - Nanocomposites KW - Wood protection KW - Water sorption PY - 2010 DO - https://doi.org/10.1007/s10971-009-2107-y SN - 0928-0707 SN - 1573-4846 VL - 53 IS - 2 SP - 384 EP - 389 PB - Kluwer Academic Publ. CY - Dordrecht AN - OPUS4-20892 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hübert, Thomas A1 - Hattermann, Hilke A1 - Griepentrog, Michael T1 - Sol-gel-derived nanocomposite coatings filled with inorganic fullerene-like WS2 N2 - Silica coatings filled with nanoscaled inorganic fullerene-like tungsten disulphide (IF-WS2) have been prepared through a sol–gel process on stainless steel substrates, and the structure and mechanical properties have been investigated. The precursor was prepared from a mixture of colloidal silica, 3-glycidoxypropyltrimethoxysilane (GLYMO), water and ethanol, adjusted to pH 4 with HNO3. In this solution WS2 is dispersed and in some cases immediately before coating ethylenediamine (ED) is added. The stainless steel substrates are dip-coated, dried in air and heat-treated in the temperature range of either 150–360 °C in air or up to 900 °C in vacuum. The solidification process is followed by differential thermal analysis (DTA). The resulting brown coloured coatings have a thickness of 1.5–4 µm. Scanning electron microscopy investigations (SEM) show that the WS2 nanoparticles are embedded as small aggregates in a hybrid silica matrix. X-ray diffraction (XRD) measurements prove that most of the tungsten disulphide embedded in the matrix can be protected against oxidation even after curing the samples at temperatures up to 900 °C. Hardness and modulus of the hybrid silica films were measured through an instrumented indentation test. Increasing the temperature of the heat treatment yields an increase of hardness from 0.3 to 1 GPa and of modulus from 3 to 17 GPa. The amount of up to 10 wt.% WS2 in the coatings has no remarkable influence on hardness and modulus of the samples. KW - Nanocomposites KW - Tungsten disulphide KW - Sol-gel KW - Mechanical properties PY - 2009 DO - https://doi.org/10.1007/s10971-009-1896-3 SN - 0928-0707 SN - 1573-4846 VL - 51 IS - 3 SP - 295 EP - 300 PB - Kluwer Academic Publ. CY - Dordrecht AN - OPUS4-19713 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hao, Ning A1 - Böhning, Martin A1 - Wohlrab, Sebastian A1 - Schönhals, Andreas T1 - Polymer Based Nanocomposites with PhenethylPOSS as Nanofilter Investigated by Dielectric Spectroscopy and Gas Transport Measurements N2 - Polyhedral oligomeric silsesquioxane with phenethyl substituents (PhenethylPOSS) as nanofiller was incorporated within Poly(bisphenol A carbonate) (PBAC) as matrix. Dielectric spectroscopy proved an almost complete miscibility of PhenethylPOSS up to 7 wt. %. At higher concentrations phase separation yields composites with a PBAC-rich matrix and POSS-rich domains which posses well shaped interfaces. The nanocomposites were also investigated with respect to their gas transport behaviour. An increase of the gas permeability was found at higher PhenethylPOSS concentrations, which is due to the phase separated structure. KW - Dielectric measurements KW - Nanocomposites KW - Permeation KW - Polycarbonates KW - Polyhedral oligomeric silsesquioxanes PY - 2008 DO - https://doi.org/10.1002/masy.200850712 SN - 1022-1360 SN - 0258-0322 SN - 1521-3900 VL - 267 IS - 1 SP - 69 EP - 73 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-17751 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pawlowski, Kristin A1 - Schartel, Bernhard T1 - Flame retardancy mechanisms of aryl phosphates in combination with boehmite in bisphenol A polycarbonate/acrylonitrile-butadiene-styrene blends N2 - The influence of nano-dispersed 5 wt.% boehmite (AlOOH) and 5 wt.% AlOOH combined with bisphenol A bis(diphenyl phosphate) (BDP) in bisphenol A polycarbonate/acrylonitrile–butadiene–styrene (PC/ABS) + poly(tetrafluoroethylene) (PTFE), and 1 wt.% AlOOH with and without BDP, resorcinol bis(diphenyl phosphate) (RDP), and triphenyl phosphate (TPP), on PC/ABS + PTFE has been investigated. Possible flame retardancy mechanisms are revealed. Thermogravimetry (TG) and evolved gas analysis (TG-FTIR) are used to study pyrolysis, a cone calorimeter applying different external heat fluxes is used to investigate fire behaviour, and LOI and UL 94 are used to investigate flammability. Fire residues were investigated using ATR-FTIR. Adding 5 wt.% AlOOH decreases the peak heat release rate, as also has been reported for polymer nanocomposites with other layered structures. AlOOH releases water, and adding 5 wt.% AlOOH crucially influences thermal decomposition by enhancing the hydrolysis of PC and of BDP. For PC/ABS + PTFE + BDP + 5 wt.% AlOOH, the formation of AlPO4, for instance, results in antagonistic effects on the charring of PC + BDP, whereas synergy is observed in LOI. When only 1 wt.% AlOOH is added to the PC/ABS + PTFE with and without BDP, RDP and TPP, respectively, no significant influence is observed on thermal decomposition, UL 94, LOI or performance in the cone calorimeter. KW - Aryl phosphates KW - Boehmite KW - PC/ABS KW - Flammability KW - Nanocomposites KW - Flame retardant PY - 2008 DO - https://doi.org/10.1016/j.polymdegradstab.2008.01.002 SN - 0141-3910 SN - 1873-2321 VL - 93 IS - 3 SP - 657 EP - 667 PB - Applied Science Publ. CY - London AN - OPUS4-17121 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Schartel, Bernhard ED - Morgan, A. ED - Wilkie, C. T1 - Considerations regarding specific impacts of the principal fire retardancy mechanisms in nanocomposites KW - Nanocomposites KW - Fire retardancy KW - Layered silicate KW - Cone calorimeter KW - Multiwall carbon nanotubes KW - LOI KW - UL 94 PY - 2007 SN - 978-0-471-73426-0 IS - Kap. 5 SP - 107 EP - 129 PB - John Wiley & Sons, Ltd. CY - New York AN - OPUS4-14844 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Bartholmai, Matthias A1 - Knoll, Uta T1 - Some comments on the main fire retardancy mechanisms in polymer nanocomposites N2 - Barrier formation and increasing the melt viscosity are addressed as the two main general fire retardancy mechanisms of polymer nanocomposites. They result in specific impacts on fire properties that consequentially cause varying flame retardancy efficiency in different fire tests. The barrier formation retards mainly flame spread (peak of heat release rate) in developing fires, but does not reduce fire load (total heat evolved), ignitability or flammability (limiting oxygen index, UL 94). Furthermore, this flame retardancy effect increases with increasing irradiation and vanishes with decreasing irradiation. The increased melt viscosity prevents dripping, which is beneficial or disadvantageous depending on the fire test used. In some test, it become the dominant influence, transforming self-extinguishing samples into flammable materials or causing wicking. Advantages and the limits are sketched comprehensively for exploiting the main general fire retardancy mechanisms of polymer nanocomposites. It is concluded that barrier formation and changing the melt viscosity in nanocomposites are not sufficient for most applications, but must be accompanied by additional mechanisms in special systems or in combination with other flame retardants. KW - Flame retardance KW - Nanocomposites KW - Organoclay KW - Cone calorimeter KW - Flammability PY - 2006 DO - https://doi.org/10.1002/pat.792 SN - 1042-7147 SN - 1099-1581 VL - 17 IS - 9-10 SP - 772 EP - 777 PB - John Wiley & Sons, Ltd. CY - Chichester AN - OPUS4-13868 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Knoll, Uta A1 - Hartwig, A. A1 - Pütz, D. T1 - Phosphonium-modified layered silicate epoxy resins nanocomposites and their combinations with ATH and organo-phosphorus fire retardants N2 - Phosphonium-modified layered silicate epoxy resin nanocomposites were evaluated by testing the thermal/thermo-mechanical properties [differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), torsional pendulum, Sharpy toughness], flammability (limiting oxygen index LOI) and fire behavior (cone calorimeter with different irradiations). The morphology of the composites was determined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The drying conditions of phosphonium-modified layered silicate were varied in order to improve the nanocomposite formation and properties. The results were compared with using a commercial ammonium-modified montmorillonite. Enhanced nanocomposite formation was found for the commercial systems due to the amount of excess surfactant, but this effect was overcompensated through the advanced morphology of the phosphonium-modified systems. Several fire retardancy mechanisms and their specific influence on the different fire properties, such as ignitability, flammability, flame spread, total heat release (fire load), and the production of CO and smoke were discussed comprehensively. The main mechanism of layered silicate is a barrier formation influencing the flame spread in developing fires. Several minor mechanisms are significant, but important fire properties such as flammability or fire load are hardly influenced. Hence combinations with aluminum hydroxide and organo-phosphorus flame retardants were evaluated. The combination with aluminum hydroxide was a promising approach since it shows superposition in properties such as the fire load and only in some properties very little antagonism. The combination with an organo-phosphorus flame retardant disillusions, since it was characterized mainly by antagonism. KW - Flame retardance KW - Nanocomposites KW - Organoclay KW - Epoxy resin KW - Cone calorimeter PY - 2006 DO - https://doi.org/10.1002/pat.686 SN - 1042-7147 SN - 1099-1581 VL - 17 IS - 4 SP - 281 EP - 293 PB - John Wiley & Sons, Ltd. CY - Chichester AN - OPUS4-12519 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schartel, Bernhard A1 - Bartholmai, Matthias A1 - Braun, Ulrike ED - Le Bras, M. T1 - Barrier effects for the fire retardancy of polymers T2 - 9th European Meeting on Fire Retardancy and Protection of Materials CY - Lille, France DA - 2003-09-15 KW - Fire retardancy KW - Nanocomposites KW - Red Phosphorus KW - Mg(OH)2 KW - Cone Calorimeter KW - LOI PY - 2005 SN - 0-85404-582-1 VL - 9 SP - 264 EP - 275 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-7377 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Bartholmai, Matthias A1 - Knoll, Uta T1 - Some comments on the use of cone calorimeter data N2 - The cone calorimeter has become one of the most important and widely used instruments for the research and development of fire retarded polymeric materials. The paper addresses three important ways in which the principal setup influences the results — factors which sometimes do not receive due consideration when drawing conclusions. The paper discusses in detail the impact on cone calorimeter results of the choice of external heat flux, the influence on the peak of heat release rate of sample thickness and thermal feedback from the back of the sample, and the influence on irradiance of the horizontal and vertical distances from the cone heater. KW - Cone Calorimeter KW - Fire retardancy KW - Fire testing KW - Nanocomposites KW - Intumescence PY - 2005 DO - https://doi.org/10.1016/j.polymdegradstab.2004.12.016 SN - 0141-3910 SN - 1873-2321 VL - 88 IS - 3 SP - 540 EP - 547 PB - Applied Science Publ. CY - London AN - OPUS4-7211 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -