7.5 Technische Eigenschaften von Polymerwerkstoffen
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Organisationseinheit der BAM
- 7 Bauwerkssicherheit (195)
- 7.5 Technische Eigenschaften von Polymerwerkstoffen (195)
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Das langsame Risswachstum (slow crack growth, SCG) sowie der umgebungsbedingte Spannungsriss (environmental stress cracking, ESC) sind relevante Schädigungsmechanismen für teilkristalline Werkstoffe auf Basis von Polyethylen hoher Dichte (PE-HD).
Der Vortrag gibt einerseits einen Überblick über die grundlegenden Struktur-Eigenschafts-Beziehungen in diesem Kontext, andererseits werden auch verschiedene praxisorientierte Prüfverfahren vorgestellt. Letztere wurden in gemeinsamen Forschungsprojekten von BAM und LBF mit dem Schwerpunkt Gefahrgutbehälter bzw. Pflanzenschutzmittel vergleichend untersucht und durch weitergehende Analytik ergänzt.
Thermal runaway investigations were performed by subjecting single and double NMC pouch cells to thermal abuse condition inside an air-tight reactor vessel with an internal volume of 100 dm³. The study was divided into two series. The findings revealed the thermal runaway-induced explosion in the cells results in a rate of temperature increase greater than 10 K/s. The highest gaseous production was achieved at a range of 90 – 100% SOC and higher battery capacities 0.79 L/Wh (Series 1, 10 Ah cell) and 0.87 L/Wh (Series 2, 32 Ah cell). The investigation showed between 25 m³ and 84 m³ of explosible gas mixture could be released from electric vehicles of nominal useable electrical energy from 32 kWh up to 108 kWh at thermal runaway. It was also found that, the release of these explosible gases could undergo a secondary explosion.
The need to develop effective flame retardants that retain polymer properties and are safe for consumers and the environment is a continuous challenge for material scientists. While halogenated flame retardants were once commonplace, the shift to non-halogenated materials has steadily progressed due to concerns over impact on health and the environment. One prominent group of flame retardants has become a viable alternative for halogenated materials, namely phosphorus-based flame retardants. The chemical versatility of phosphorus-based flame retardants and the ability to work as reactive or additive compounds makes them ideally suited for modern materials. There exists a trend toward complex, polymeric, and multifunction flame retardants, as these materials show greater flame retardancy performance than low molecular weight counterparts and affect material properties to a much lesser extent.
One group of organophosphorus flame retardants that shows great potential for high-performance polymers like epoxy resins are hyperbranched phosphorus-based polymers. These additives exhibit great miscibility with the polymer matrix and a significantly decreased diffusion through the material, which greatly reduce leaching or blooming out of the matrix. Moreover, the material’s thermal stability remains intact at elevated temperatures due to its low impact on the glass transition temperature. Finally, following market trends and legislation such as the guidelines for the Restriction of Hazardous Substances Directive implemented by REACH (Registration, Evaluation, Authorization and Restriction of Chemicals) in the EU, these macromolecules are non-accumulating, non-toxic and have a lower risk of leeching or blooming from the matrix, further reducing environmental impact.
The work presented herein focusses on two distinct parts studying hyperbranched polymeric flame retardants and their corresponding monomeric compounds.
The first part, involving the low molecular weight components, investigated the role of the chemical surrounding of phosphorus in terms of flame retardant efficacy. Here, a systematic variance of the surrounding of phosphorus was investigated: by changing the ratio of oxygen to nitrogen (4:0 until 1:3), four materials, namely phosphoester (4:0), phosphoramidate (3:1), phosphorodiamidate (2:2), and phosphoramide (1:3), were synthesized, characterized, and finally added to Bisphenol A based epoxy resins (10 wt.-% loading). Pyrolysis investigations showed that low molecular weight components volatize at lower temperatures than the polymer matrix. Additionally, cone calorimeter measurements and TGA-FTIR investigations show trends in respect to FR efficacy in pyrolysis and full flaming conditions.
The second part involves the hyperbranched variants of the monomeric counterparts and investigates the role of complex shape on flame retardant efficacy. By comparing the low to the high molecular weight compounds, the influence of the complex shape becomes apparent and can be quantified. Cone calorimeter measurements show an increase in flame retardancy for some materials, while for others, the mode of action is altered.
By implementing a multi-methodical approach, various flame retardancy aspects, from pyrolysis behavior in the gas and condensed phase, to ignitability / reaction-to-small-flame performance, to action in forced flammability experiments, are identified and quantified, allowing for a clearer understanding of the behavior in fire of these novel flame retardants. By comprehending the roles of chemical composition and complex shape, it opens the path for new and effective multifunctional, polymeric flame retardants with decreased PBT, higher miscibility, and low impact on Tg.
This work is funded by the Deutsche Forschungsgemeinschaft (DFG: SCHA 730/15-1; WU 750/8-1).
Multifunctional Graphene in Flame Retarded Polybutadiene/ Chloroprene/ Carbon Black Composites
(2021)
Multilayer graphene is investigated as a multifunctional nanofiller to polybutadiene/ chloroprene rubbers (BR/CR) that partially substitutes carbon black (CB) and aluminum trihydroxide (ATH). Loadings of only 3 parts per hundred rubber (phr) MLG replaced 15 phr of CB and/or 3 phr of ATH in BR/CR nanocomposites. Mechanical and fire behavior were investigated, and results point to improved rheological, curing and mechanical properties of MLG-containing rubber composites.
The demands for modern flame retardants are higher than ever: a flame retardant must function effectively in a certain polymer matrix and avoid critical alterations to the material’s properties. Ideally, a flame retardant additive should be easily miscible and show no sign of leaching or blooming from the matrix. Additionally, the flame retardant should be non-toxic, non-accumulating and biocompatible. Hyperbranched polymers are a promising group of multifunctional flame retardants which fulfill these demands: their complex shape enables high miscibility and avoids leaching or blooming, while their high molecular weight potentially increases biocompatibility and lowers accumulation and toxicity. Moreover, they exhibit a low impact on polymer properties and a good flame retardant performance.
This work examines the efficacy and mode of action of phosphorus-based hyperbranched polymeric flame retardants in bisphenol A-based epoxy matrices. To investigate the effect of the complex shape, the hyperbranched polymers are compared to their corresponding monomeric variants. Furthermore, the materials are synthesized to contain systematically varying oxygen-to-nitrogen ratios, allowing for new insight into what role the chemical surrounding of phosphorous plays in flame retardant efficacy.
Using a multi-methodical approach, including thermogravimetric analysis coupled with Fourier transform infrared spectroscopy (FTIR), hot stage FTIR, micro combustion calorimetry, differential scanning calorimetry, oxygen index (LOI), UL-94 tests and cone calorimetry experiments, the decomposition mechanisms and the flame retardant modes of action of these flame retardants in epoxy resins are investigated, shedding new light on the chemistry of flame retardancy.
Benefits of hyperbranched structure:
Molecular weight, miscibility, number of FR groups, end-group functionalization, glass transition temperature, decreased PBT.
Examples of hyperbranched FRs:
Charring agent, silicone, triazine, etc.
Systematic study of effect of chemical surrounding and impact of Complex shape of phosphorus-based hyperbranched polymers on flame retardant efficacy in epoxy resins.
Most synthetic polymers have a high fire load, and as a result, they require flame retardants (FRs) to ensure their safe use. Phosphorus plays an important role in flame retardancy and has the potential to replace halogenated variants, which are assumed to be harmful to the environment and health. Among phosphorus-based FRs, there exists a trend towards polymeric, high molar mass molecules with complex molecular architectures. In this project, we synthesized a novel series of so-called phosphorus-based hyperbranched polymeric FRs and investigated their use as multifunctional additives to high-performance polymers, i.e. epoxy resins. By cleverly designing the chemical structure to contain varying amounts of P-O and P-N bonds, new insight into the chemical mechanism of flame retardancy was gained, and by comparing the hyperbranched polymers to their monomeric counterparts, a greater understanding of the role of complex architecture was won. This talk aims at presenting some of these results and proposes chemical mechanisms that illustrate what role these novel hyperbranched flame retardants play in molecular firefighting.
In recent years superglassy polymers exhibiting intrinsic microporosity established a new perspective for a number of applications, especially for gas separation membranes as These polymers Combine extremely high permeabilities with attractive selectivities. The essential factor governing the structure Formation in the solid film or layer is either a contorted rigid Backbone (polymers of intrinsic microporosity - PIMs) or extremely bulky side groups (polynorbornenes and polytricyclonenenes).
For a deeper understanding of both types of such high-Performance polymers for gas separation membranes and their further development broadband dielectric spectroscopy (BDS) can provide a substantial contribution.
BDS addresses molecular relaxations characterizing the dynamics of the solid polymer as a major factor determining the gas transport properties but also the physical aging behavior which is an essential issue for such polymers.
BDS is applied on PIMs where fluctuations of molecular dipoles connected to the backbone can be directly monitored. Furthermore, also polynorbornenes were investigated which carry no dipole moment in their repeat unit - the high resolution of modern equipment allows for the detailed analysis also for very small dielectric losses originating from partially oxidized moieties or marginal catalyst residues.
Additionally, from interfacial polarization phenomena, such as Maxwell-Wagner-Sillars (MWS) polarization due to blocking of charge carriers at internal interfacial boundaries on a mesoscopic length scale, valuable information on the intrinsic microporosity and its changes induced by physical aging can be obtained.
Finally, also conductivity can be characterized in detail in such polymeric systems revealing contributions of interactions of aromatic moieties (π-π-stacking) or the drift motion of charge carriers. These features also determine the structure formation in the solid state.
Polymers of intrinsic microporosity (PIMs) have recently emerged as novel materials for a broad range of high-performance applications from gas separation to electronic devices. The very rigid, contorted polymer chains show only limited molecular mobility and therefore pack inefficiently giving rise to intrinsic microporosity with pore sizes generally smaller than 1 nm resulting in BET surface areas larger than 700 m2/g. Using conventional thermal analysis techniques, no glass transition temperature (Tg) of PIMs could be unambiguously detected up to now. Employing fast scanning calorimetry (FSC) based on a one chip sensor, decoupling the time scales responsible for the glass transition and the thermal decomposition is a reliable strategy to overcome this limitation. The FSC device is capable to heat and cool a small sample (ng-range) with ultrafast rates of several ten thousand K/s. Evidence of a glass transition is obtained for a series of PIMs with different chain rigidities. Local small-scale fluctuations are held responsible for the glass transition of highly rigid PIMs rather than segmental motions as in conventional polymers.
Slow crack growth (SCG) under the influence of external fluid media, usually termed environmental stress cracking (ESC), is still one of the most frequent origins of severe damage and failure of polymeric materials. For polyethylene (PE) this is relevant for mass products, like bottles for consumer products, but also for high-performance materials for pipes or industrial packaging, including containers for chemicals and other dangerous goods. Especially for high-density polyethylene (PE-HD) the susceptibility to SGC and ESC is depending on the complex interplay between molecular weight and architecture and the resulting semicrystalline morphology, especially the formation of tie-molecules.
A reliable assessment of the resistance against this damage phenomenon is essential for demanding as well as safety-critical applications and has to take into account suitable testing methodologies and conditions in combination with environmental media reflecting the properties representative for typical fillings and relevant components causing ESC. In this context a better understanding of different influencing factors, such as sorption, swelling or surface activity is necessary together with a detailed characterization of different stages of crack propagation and underlying mechanisms. Therefor well-established testing methods, such as the Full Notch Creep Test (FNCT), were complemented by detailed fracture surface analysis using e.g. LSM and SEM in combination with a time-dependent optical monitoring of the progressing crack growth.
For the crack growth also the ratio of fibrillated craze zone to crack opening is important for the deeper understanding of crack propagation and related material parameters which can be additionally addressed by X-ray computed tomography.
Elastomers are usually reinforced by large amount of fillers like carbon black (CB) or silica in order to improve various mechanical properties, such as Young’s modulus, hardness, tear resistance, abrasion resistance, and gas barrier properties. In recent years, such improvements were also obtained by using nanoparticles at significantly lower filler loadings. Graphene is a twodimensional (2D) sheet of a thickness in the atomic scale, composed of a honeycomb structure of sp2 carbon atoms. Besides significant mechanical reinforcement, graphene harbors the potential to be used as a multifunctional filler, as it can also increase the conductivity and weathering stability of elastomer matrices. Ultraviolet (UV) irradiation and oxidative agents can lead to the degradation of elastomers due to a multistep photooxidative process, including the formation of radicals. Carbon-based fillers have an influence on these reactions, as they can absorb UV radiation and act as radical scavengers.
This chapter summarizes the results of our larger project on multilayer graphene (MLG)/elastomer nanocomposites, previously published, which present a comprehensive case study of MLG as a multifunctional nanofiller in elastomer/graphene nanocomposites. Different elastomeric matrices are compared in order to demonstrate the outstanding impact of MLG as a general benefit. The dependency of this effect on concentration is discussed in detail. Taking into account the key role of dispersion, different mixing procedures are compared, evaluating a facile implementation of graphene nanocomposites into conventional rubber processing. Finally, the most probable commercial uses of MLG nanofillers in combination with conventional CB are studied. The nanocomposites were prepared in the kg scale in order to obtain enough specimens to investigate various properties of the uncured and vulcanized rubbers at the highest quality level, including rheology, curing, morphology, several mechanical properties, abrasion, conductivity, gas permeation, burning behavior, and weathering stability. The structure property relationships are asserted and questioned, for example, by investigating the radical scavenging ability or aspect ratio of the MLG. This chapter illustrates the state of the art of graphene/rubber nanocomposites targeted for commercial mass applications.
This study aims at investigating the use of coal fly ash-based alkali activated mortars as passive fire protection system for steel structures. These systems are used to slow down the temperature rise of the steel substrate in case of fire. In addition, the protective system should guarantee the ability to prevent and/or mitigate steel corrosion phenomena. The behavior of a light-weight mortar was compared to that of a normal-weight mortar. Density and porosity were measured to better characterize the physical properties of the mortars. The degree of protection in case of fire was assessed by performing medium-scale fire tests. Acoustic emission measurements were conducted to analyze cracking phenomena during the high temperature exposure. The corrosion process was evaluated using an electrochemical approach in order to monitor the durability of the developed material. Preliminary results show that a 20 mm-thick layer of light-weight mortar is able to protect the steel substrate from reaching the critical temperature of 500 °C for 38 minutes in case of cellulosic fire. In addition, alkali activated mortars provide protection for carbon steel in presence of aggressive environment (i.e. presence of chlorides). The corrosion resistance is strictly related to the physical properties of the developed mortars.
The present study aims to investigate the use of geopolymer mortars as passive fire protection system for steel structures. Coal fly ashes were used as aluminosilicate source and perlite was employed as aggregate to obtain a lightweight system. In addition, a geopolymer mortar containing quartz aggregate was produced for comparison. The geopolymer mortars were applied on stainless steel plates and exposed to both, cellulosic and hydrocarbon standard fire curves, according to ISO 834-1 and EN 1363-2, respectively. Acoustic emission measurements were conducted to analyze cracking phenomena during the high temperature exposure. The resulting temperature-time curves showed that the investigated system is effective in retarding the temperature rise of the steel plates. When the cellulosic fire curve was applied, a 20 mm [0.79 in.] thick layer of lightweight geopolymer mortar protected the steel substrate from reaching the critical temperature of 500 °C [932 °F] for at least 30 minutes, avoiding the rapid decrease of its mechanical properties and thus representing an important safety measure against accidental fires. No spalling phenomena on heating were detected; however, significant cracking was observed on cooling.
Bare steel constructions are often integrated in modern buildings. Intumescent coatings are widely used to protect the steel from heating up too quickly in a case of fire. As the functionality of intumescent coatings decreases with the impact of weathering processes, it is important to understand the mechanisms of material degradation to maintain long durability. The weathering-induced degradation behavior of a water-borne intumescent coating was examined, and the weakest points of the formulation were identified by a systematic approach. Resulting from this investigation, adjustments to the formula were made, leading to improved weathering resistance.
High-throughput fire tests and weathering-induced degradation behaviour of intumescent coatings
(2018)
In this work, the weathering-induced degradation of intumescent coatings was investigated by a systematic and comprehensive approach. A mechanism is revealed that is proposed to be responsible for the loss of function of intumescent coatings induced by weathering.
First, the thermal decomposition of artificially weathered intumescent coatings was examined. To get a better understanding of the weathering and ageing phenomena, the degradation behaviour of the single ingredients during the weathering process was investigated, as well as their chemical and physical interactions. For the systematic approach, the materials that are essential for intumescence (ammonium polyphosphate, pentaerythritol, titanium dioxide, melamine and the binder) are treated with moisture, elevated temperature and UV radiation.
Thermogravimetry (TG) and IR spectroscopy were used to compare the initial samples with their different grades of weathering. We demonstrate that ammonium polyphosphate, melamine and the binder are mainly responsible for the ageing process. Further, it was demonstrated that TG and IR spectroscopy are suitable measuring methods to detect the effects of weathering on intumescent coatings.
Finally, a small-scale fire test procedure is introduced. Based on the reduction of the sample size, up to 50 samples can be tested in a single fire test. The results of this fire test have the same quality as the results from standard intermediate fire tests corresponding to DIN 4102-8.
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.
Polymeric membranes represent a cost- and energy-efficient solution for gas separation. Recently Polymers of Intrinsic Microporosity (PIMs) have been in a great interest because of their outstanding BET surface area larger than 700m2/g and pore size smaller than 1 nm. PIMs are a promising candidate in gas separation with high permeability and appealing selectivity due to their inefficient packing derived from a combination of ladder-like rigid segments with sites of contortion. However, it is recognized this class of polymers suffer from decrease in performance with time due to physical aging. The initial microporous structures approach a denser state via local chain rearrangements, leading to a dramatic reduction in permeability. As chain packing during film casting and physical aging are the key factors determine the performance in separation applications, characterization of the molecular mobility in these materials has been proved to provide valuable information. In recent research on PIM-1 the archetypal PIM, a molecular relaxation process with high activation energy together with a significant conductivity in the glassy state has been found and explained with the formation of local intermolecular agglomerates due to interaction of π-electrons in aromatic moieties of the polymer backbone. In this work, the dielectric behavior of the polymeric films and their response upon heating (aging) were measured by isothermal frequency scans during different heating/cooling cycles in a broad temperature range down to 133K for the first time. Multiple dielectric processes following Arrhenius behavior were observed. Local fluctuations, Maxwell-Wagner-Sillars (MWS) polarization and structural relaxations were discussed correlating to structural-properties of PIM-1. Up to now, no other work has studied the role of porosity and thermal history of PIM-1 film in dielectric processes. The goal is by eliminating thermal history and considering storing conditions provide better understanding on aging and plasticizing in high free volume glassy polymer PIM-1.
Especially now in times of the energy revolution, the demand for energy-efficient separation processes promotes the advancement of new high-performance materials for use as highly selective separation membranes. Polymers with intrinsic microporosity (PIMs) are of high interest in the field of gas separation membranes. Currently the application of PIMs for membrane technology is still restrained by their strong tendency to physical aging involving a significant loss of their good gas separation properties. Physical aging phenomenon is related to the molecular mobility of PIMs which was investigated by broadband dielectric spectroscopy (BDS) previously [1]. In this work, covalent phosphinine-based framework (Eto-CPSF) was used as a nanofiller (0-10 wt %) in a PIM-1 matrix to potentially enhance the gas transport properties and prevent physical aging. Since molecular mobility is a fundamental parameter determining gas transport as well as physical aging in such a material, our study includes dielectric investigations by BDS of pure PIM-1 and PIM-1/Eto-CPSF mixed matrix membranes to establish a correlation between molecular mobility and gas transport properties. In addition, gas permeability was determined by the time-lag method (0-10 bar pressure) at 35 °C for N2, O2, CH4 and CO2 for all MMMs.
The dielectric behavior of the polymeric films and their response upon heating were measured by isothermal frequency scans during different heating/cooling cycles in a broad temperature range up to 250 °C. Multiple dielectric processes following Arrhenius behavior were observed. Local fluctuations, Maxwell-Wagner-Sillars (MWS) polarization and structural relaxations were discussed correlating to structural-properties of PIM-1. As main result for MMMs, the permeability of PIM-1 for CH4 and CO2 gases were increased significantly with only 5 wt% of nanofiller within the polymer matrix. However, this is not observed for Eto-CPSF concentrations higher than ca. 7 wt% probably due to a microphase separated morphology of the nanocomposite system. Furthermore, the permselectivity of membranes for pair gases O2/N2 and CO2/N2 show enhancement up to a concentration of about 7 wt% Eto-CPSF filler.
The first documentation of fuel biodeterioration dates back to the late 19th century. However, extensive studies concerning the microbial fuel contamination started in 1980’s. Polymeric fuel storage tanks containing diesel and biodiesel provide environmental conditions for microbial growth. Several studies demonstrated that bacteria, which were found in contaminated fuel systems, can use fuels as macronutrient; but such bacteria can also cause microbiologically influenced corrosion and fouling.
The aim of this study is to investigate the initial attachment behavior of bacteria, isolated from a diesel contamination, on neat and photooxidized high-density polyethylene (PE-HD). Two common PE-HD’s, less- and biodiesel-stabilized, were radiated to UV light representing a tank exposed to sunlight. The effect of photooxidiation on PE-HD’s surface were characterized chemically by Fourier-transform infrared spectroscopy (FTIR). The attached bacteria Pseudomonas aeruginosa and Bacillus subtilis on the polymer surface were evaluated by fluorescence microscopy and colony-forming unit tests (CFU).
PE-HD as a polymeric fuel storage tank material: Photooxidation, fuel sorption and long-term storage
(2018)
High-density polyethylene (PE-HD) is a commodity thermoplastic polymer which is typically used for packing of dangerous goods. Its good resistance against photooxidation, fuels, chemicals and other environmental factors in addition to low production costs makes PE-HD attractive for fuel storage applications. Typical engine fuels stored in polymer tanks are petrol, diesel and biodiesel that receives increasing attention as proper alternative to fossil fuels. One of the major problems with biodiesel is its susceptibility to oxidize due to its chemical composition of unsaturated fatty acids which also can cause polymer degradation.
The aim of this study is to investigate the influence of different environmental factors, UV radiation and commonly stored fuels, on the mechanical, physical and chemical properties of two types of PE-HD polymers (stabilized and non-stabilized). The influence on the mechanical properties was tested by Charpy and tensile tests, chemical and physical properties were evaluated by Fourier-transform infrared spectroscopy (FTIR) and by dynamical mechanical analysis (DMA) tests. Samples were characterized after varying exposure time of UV radiation and after fully and partially immersion in biodiesel. In addition, similar experiments were conducted using diesel for comparison.
A commercially available bio epoxy resin with kenaf fibers and halogen free inorganic and organic flame retardants, respectively, is investigated concerning its thermal stability and fire performance. Particular attention has been paid to the difference of short fibers, fiber mats and woven
materials.
Renewable alternatives for common thermoset resins are demanded to go for sustainability. The objective is to create a flame retarded epoxy resin from a commercial bio epoxy resin with halogen free inorganic and organic flame retardants, respectively. Alumina trihydrate, aluminum diethyl phosphinate, a DOPO-based phosphonamidate and ammonium polyphosphate seem to have promising performances. Properties are enhanced with different bio fillers: pyrolyzed cocoa shells and plant waste (provided by Otto A. Müller Recycling GmbH, thanks!), short fibers and nonwovens of the natural fiber kenaf, hydroxypropyl-ß-cyclodextrin and sulfobutylether-ß-cyclodextrin.
Fire performance is investigated by cone calorimeter examinations, LOI and UL-94 ratings. Thermal analysis is given by TG-FTIR and DSC measurements.
Combinations of flame retardants and bio-fillers lead to reduced PHRR and THR, reach V0 in UL-94 and have a significant increase in LOI of up to 37 vol.-%. 10 % ammonium polyphosphate with 10 % pyrolyzed cocoa shell performs best, builds a magnificent protective layer, and shows good intumescence.
Mit additiven Fertigungsverfahren hergestellte Bauteile und Produkte aus Kunststoffen werden zunehmend nicht mehr nur als Prototypen, sondern als voll funktionsfähige Bauteile und Produkte gefertigt. Bedingt durch die Fertigungsprozesse und den schichtweisen Aufbau resultieren physikalische Materialeigenschaften, die stark von den Fertigungsparametern abhängen und zudem anisotrop sind. Von den Fertigungsparametern werden auch die Oberflächeneigenschaften beeinflusst, sodass zu erwarten ist, dass sich die Beständigkeit gegenüber äußeren Umwelteinflüssen bei additiv gefertigten Bauteilen von der konventionell gefertigter unterscheiden kann. Nachfolgend wird daher die Entwicklung eines Qualitätssicherungskonzeptes basierend auf spektroskopischen und zerstörungsfreien Prüfverfahren vorgestellt, in dem der Alterungsprozess von mittels Fused Deposition Modelling (FDM) und mittels Lasersintering (LS) hergestellten Probekörpern untersucht wird.
Mit additiven Fertigungsverfahren hergestellte Bauteile und Produkte aus Kunststoffen werden zunehmend nicht mehr nur als Prototypen, sondern als voll funktionsfähige Bauteile und Produkte gefertigt. Bedingt durch die Fertigungsprozesse und den schichtweisen Aufbau resultieren physikalische Materialeigenschaften, die stark von den Fertigungsparametern abhängen und zudem anisotrop sind. Von den Fertigungsparametern werden auch die Oberflächeneigenschaften beeinflusst, sodass zu erwarten ist, dass sich die Beständigkeit gegenüber äußeren Umwelteinflüssen bei additiv gefertigten Bauteilen von der konventionell gefertigter unterscheiden kann. Nachfolgend wird daher die Entwicklung eines Qualitätssicherungskonzeptes basierend auf spektroskopischen und zerstörungsfreien Prüfverfahren vorgestellt, in dem der Alterungsprozess von mittels Fused Deposition Modelling (FDM) und mittels Lasersintering (LS) hergestellten Probekörpern untersucht wird.
Bei der Bestrahlung und Bewitterung von polymeren Werkstoffen wird die Degradation durch eine Absorption von Strahlung initiiert und meistens durch weitere Klimagrößen, wie z.B. Wärme, Feuchte und atmosphärische Gase beeinflusst. Die Messung einer effektiven Bestrahlungsstärke und ihre zeitliche Integration sind deshalb von großer Bedeutung.
Photochemische Prozesse werden beim Sehen oder allgemeiner bei Farbstoffen schon durch sichtbare (VIS) Strahlung, dagegen bei der Erythembildung der Haut und der Photodegradation von Polymeren erst durch die energiereicheren Photonen der ultravioletten (UV) Strahlung initiiert. Die spektrale Empfindlichkeit des Auges und die Erythembildung sind im VIS- bzw. UV-Bereich sehr stark wellenlängenabhängig, was durch die Angabe der mit der spektralen Hellempfindlichkeit V() des Auges bewerteten VIS-Strahlung in Lux (lx) bzw. die mit der Erythem-Wirkfunktion bewertete UV Strahlung als dimensionsloser UV-Index berücksichtigt wird. Spektrale Empfindlichkeiten.
Die Photodegradation von Polymeren ist im UV-Bereich ebenfalls stark wellenlängenab-hängig, was bisher nicht berücksichtigt wurde. Seit Mitte der 70er Jahre, als die lx- bzw lxh- Messung bei der Strahlungsbeanspruchung langsam durch die Ermittlung der radiometrischen UV-Bestrahlungsstärke bzw. der UV-Bestrahlung im gesamten UV-Bereich abgelöst wurde, gab es hier bei der Bewitterungsprüfung keine weiteren Fortschritte auf dem Gebiet der Charakterisierung der Strahlungsbeanspruchung im UV-Bereich.
Seit Jahren liegen zahlreiche Ergebnisse über die spektrale Empfindlichkeit von Photo-degradationsprozessen vor, die zeigen, dass die spektrale Empfindlichkeit im Bereich der Globalstrahlung bei ca. 300 nm, am größten ist und im langwelligen UV-Bereich bei ca. 400 nm gegen Null geht. Die Messungen der radiometrischen Größen UV-Gesamt-bestrahlungsstärke und UV-Gesamtbestrahlung erfasst deshalb über weite Wellen-längenbereiche Strahlungsanteile, die für die Photodegradation bedeutungslos sind und mittelt über potenziell bedeutsame Änderungen im kurzwelligen UV-Bereich hinweg.
Es wird das Konzept eines neuen UV-Radiometers vorgestellt, dessen spektrale Empfindlichkeit einer mittleren spektralen Empfindlichkeit der Photodegradation von Polymeren entspricht. Die effektive UV-Bestrahlungsstärke und UV-Bestrahlung kann dadurch wesentlich genauer erfasst werden.
Weathering reference materials are used to characterize the harshness of an exposure, aiming on either reproducibility of a specific exposure or on the comparability between various kinds of weathering exposure.
The materials that are used as weathering reference materials differ in their sensitivities (as well as in interactions and interferences of the latter), conditioned by the different processes which lead to the respective property change. It is also essential to take into account the necessary measurement equipment for the respective property change, in order to allow timely intervention.
What are the key issues on choosing a weathering reference material?
What can be learned from the weathering reference materials, investigated so far?
Possibilities and limitations are discussed on the basis of existing weathering reference materials. Conclusions are drawn, for establishing new weathering reference materials.
Die Umweltwirkungen auf ein Material werden als Überlapp der Funktionskurven von Materialempfindlichkeit und einwirkenden Umweltparametern betrachtet. Wenn entweder die Empfindlichkeit oder die Beanspruchungen Null sind, ergibt sich auch keine Umweltwirkung und bei beidseitig Werten größer Null das jeweilige Produkt der beiden. Die Akkumulation der nicht-reversiblen Effekte über die Zeit und allen Eigenschaftsänderungen entspricht der Alterung des Materials für den jeweiligen Expositionszeitraum.
Die digitale Umweltsimulation gliedert sich hier in drei Teilaspekte. Ein erster, rein materialwissenschaftlicher Teil hat die Aufgabe, alle relevanten Materialempfindlichkeiten experimentell zu quantifizieren. Ein zweiter – unter Umständen numerischer Teil – hat die Aufgabe, das Bauteil und seine Einbaulage zu digitalisieren und aus den makroskopischen Umgebungsbedingungen die relevanten mikroklimatischen Umweltparameter für alle Oberflächen- oder Volumenelemente zu bestimmen. In einem dritten Teil werden die Einwirkungen über den betrachteten Zeitraum berechnet und kumuliert. Dieses Konzept, das auf den so genannten Expositions-Reaktions-Funktionen (ERF) basiert, wird an Beispielen der Photoxidation erläutert. Dieses Vorgehen wurde schon beim ViPQuali-Projekt als Numerische Umweltsimulation umgesetzt.
Überprüft werden muss das Modell unbedingt an einer realitätsnahen Validierungsbeanspruchung. Hier werden die ermittelten ERFs mit über den kompletten Beanspruchungszeitraum geloggten Umweltparametern gekoppelt, um die berechnete mit der experimentell erfahrenen Alterungswirkung zu vergleichen. Nur so kann sichergestellt sein, dass alle für die Anwendungsumgebung relevanten Materialempfindlichkeiten einbezogen wurden.
Weathering reference materials (WRMs) are used to characterize the harshness of an exposure, aiming on either reproducibility of a specific exposure or on the comparability between various kinds of natural or artificial weathering exposure.
The materials that are used as weathering reference materials differ in their sensitivities (as well as in interactions and interferences of the latter), conditioned by the different processes which lead to the respective property change. It is also essential to take into account the necessary measurement equipment for the respective property change, in order to allow timely intervention.
What are the key issues on choosing a weathering reference material?
What can be learned from the weathering reference materials, investigated so far?
Possibilities and limitations are discussed on the basis of existing weathering reference materials. Conclusions are drawn, for establishing new weathering reference materials.
Aufgrund des tieferen Eindringens der solaren Strahlung treten bei transparenten und bei transluzenten (durchscheinenden) Kunststoffen veränderte Bedingungen gegenüber opaken Proben auf. Dies kann zu speziellen Effekten und damit zu einem abweichenden Bewitterungsverhalten führen. Auch aus Mangel an geeigneten Normen werden diese Effekte häufig vernachlässigt. Deshalb initiiert der DIN-FNK auf ISO-Ebene ein entsprechendes Dokument.
Die Norm ist in der Form eines Technical Reports geplant. In einem ersten Teil sollen die Besonderheiten transparenter oder transluzenter Kunststoffe erläutert werden, um den Nutzer für mögliche Probleme zu sensibilisieren. Im zweiten Teil werden Empfehlungen für Bestrahlung oder Bewitterung herausgearbeitet. In einem dritten Teil geht es dann um Besonderheiten bei der Messung von Eigenschaftsänderungen transparenter bzw. transluzenter Kunststoffe. In informativen Anhängen sollen verschiedene Beispiele die Thematik illustrieren.
Laboratory studies with pedestrians could depend strongly on Initial conditions. Comparisons of the results of such studies require to distinguish carefully between homoge neous and heterogeneous populations.
A series of well-controlled laboratory studies were performed with participants with and without impairments. Individual pedestrian movement through a corridor and a bottleneck of all participants was recorded by wide-angle HD-cameras and the trajectories of each participant was extracted automatically by using PeTrack.
This contribution shows that considering participants with impairments in laboratory studies of pedestrian movement is feasible and reports preliminary the inuences of movement. Preliminary analyses imply two main conclusions and a preliminary forecast: _rst, social behaviour in laboratory studies is considerately and respectful; we did not observe altruistic behaviour; but considerately behaviour may encourage a reduced capacity at bottlenecks. Second, technical devices to improve movement require space and reduce capacity.
Studien zur Erforschung von Kenngrößen der Bewegung von Personen wurden in der Vergangenheit meistens mit jungen und fitten Menschen durchgeführt. In Folge des demographischen Wandels und der Anforderungen an barrierefreies Bauen stellt sich die Frage, ob die so ermittelten Kenngrößen der Bewegung auch auf heterogene Personengruppen übertragen werden können. Da bei der Berechnung von Räumungszeiten zunehmend Ingenieurmethoden eingesetzt werden, deren Ergebnisse ganz wesentlich von den zu Grunde gelegten Bewegungsparametern, wie z. B. der freien Gehgeschwindigkeit, abhängen, hat die Validität der Kenngrößen maßgeblichen Einfluss auf die sicherheitstechnische Evaluation von Gebäuden und Versammlungsstätten.
In diesem Artikel wird anhand aktueller Forschungsergebnisse aus Bewegungsstudien, an denen Menschen mit und ohne Beeinträchtigungen teilgenommen haben, der Einfluss der Heterogenität auf Kenngrößen der Bewegung vorgestellt. Darüber hinaus werden die Besonderheiten des Studienablaufs und die Möglichkeiten und Grenzen der Untersuchungsmethode dargestellt. Die Untersuchungen bestätigen, dass die Berücksichtigung besonderer Personengruppen signifikanten Einfluss auf die Kenngrößen der Bewegung hat und daher die Ergebnisse der Ingenieurmethoden beeinflusst und zukünftig bei heterogenen Personengruppen beachtet werden muss.
Emergency exits as bottlenecks in escape routes are important for designing traffic facilities. Especially the fundamental diagram is a crucial performance criterion for assessment of pedestrians' safety in facilities and an important basis for calculation methods. For this reason, several studies were performed during the last decades which focus on the quantification of movement through bottlenecks. These studies were usually conducted with populations of homogeneous characteristics to reduce influencing variables and for reasons of practicability.
Studies which consider heterogeneous characteristics in performance parameters are rarely available. In response and to reduce this lack of data a series of well-controlled large-scale movement studies considering pedestrians with different disabilities was carried out.
Evakuierungsübung Werkstatt: positives Ergebnis
Evakuierungsübung Wohnbereich: Optimierungspotential identifiziert
•Lange Evakuierungszeiten
•Vorzeitige Rückkehr in das Gebäude / Freigabe
•Gefährdungsbeurteilungen
•Einweisung / regelmäßige Übung Assistenzmittel
•Intensivierung der Zusammenarbeit / Abstimmung mit örtlicher Feuerwehr
Understanding movement in heterogeneous groups is important for a meaningful evaluation of evacuation prediction and for a proper design of buildings. The understanding of interactions and influencing factors in heterogeneous groups on key performance figures is fundamental for a safe design. This contribution presents results of experimental studies on movement of a crowd through a bottleneck involving participants with and without disabilities. High precise trajectories of the attendees extracted from video recordings were used to calculate density and velocity of the participants. Besides the well-established fundamental diagram new insights into the individual relation between density and velocity are discussed. A complex structure and considerate behaviour in movement implicates a strong influence of the heterogeneity on key performance values of safe movement.
Evaluation of evacuation process is common separated by two phases: pre-movement and movement-phase. Individual capabilities of pedestrians have an impact on both and therefore on the time required for safe escape. In view of evaluating the evacuation process, characteristics of realistic movements of pedestrians involved are needed, but so far such data are mainly available for individuals with unrestricted evacuation capabilities only.
Due to the lack of available data, parameter studies in an assisted living for people with disabilities were performed to explore the movement during evacuation. Preparation times for assistance (n=10), unimpeded walking speeds (n=34) depending on the assistance devices in the plane as well as walking speeds on stairs (n=11) were focussed.
Time to prepare an assistance device for utilisation depends significantly on the kind of device type. Further on, practical experience in handling the devices for assistance has an impact on the preparation time. In contrast to the results of the preparation times, any relation on assistance devices were investigated for the unimpeded walking speed in the plane. A remarkable decrease of walking speed on stairs was observed which is independent from the utilised assistance device.
The presented data improve and extend the insufficient engineering data base and raised up questions regarding the complexity of considering pedestrians movement with impairments in evacuation planning.
In der Vergangenheit wurden Kenngrößen der Bewegung von Menschen zumeist in Studien gewonnen, die mit jungen und fitten Menschen durchgeführt wurden (z. B. Studierende oder Soldaten). Aufgrund des demographischen Wandels und aktueller Entwicklungen im Kontext der Barrierefreiheit stellt sich jedoch die Frage, ob die in diesen Studien gewonnen Kenngrößen, z. B. freie Gehgeschwindigkeiten, ohne weiteres auch auf heterogene Personengruppen übertragen werden können.
Bei der Bewertung der Sicherheit von Menschen, z. B. in Wohneinheiten, Verwaltungsgebäuden und Versammlungsstätten, kommen heute Ingenieurmethoden zum Einsatz, welche auf den oben genannten Kenngrößen basieren. Insofern ist es erforderlich, Menschen mit und ohne Beeinträchtigungen bei den Bewegungsstudien zu berücksichtigen. Im vorliegenden Artikel werden aktuelle Ergebnisse solcher Studien vorgestellt. Zudem werden Besonderheiten sowie Grenzen und Möglichkeiten der Untersuchungsmethode herausgearbeitet.
Evaluation of evacuation process is common separated by two phases: pre-movement and movement-phase. Individual capabilities of pedestrians have an impact on both and therefore on the time required for safe escape. In view of evaluating the evacuation process, characteristics of realistic movements of pedestrians involved are needed, but so far such data are mainly available for individuals with unrestricted evacuation capabilities only.
Due to the lack of available data, parameter studies in an assisted living for people with disabilities were performed to explore the movement during evacuation. Preparation times for assistance (n=10), unimpeded walking speeds (n=34) depending on the assistance devices in the plane as well as walking speeds on stairs (n=11) were focussed.
Time to prepare an assistance device for utilisation depends significantly on the kind of device type. Further on, practical experience in handling the devices for assistance has an impact on the preparation time. In contrast to the results of the preparation times, any relation on assistance devices were investigated for the unimpeded walking speed in the plane. A remarkable decrease of walking speed on stairs was observed which is independent from the utilised assistance device.
The presented data improve and extend the insufficient engineering data base and raised up questions regarding the complexity of considering pedestrians movement with impairments in evacuation planning.
Studien zur Erforschung von Kenngrößen der Bewegung von Personen wurden in der Vergangenheit meistens mit jungen und fitten Menschen durchgeführt. In Folge des demographischen Wandels und der Anforderungen an barrierefreies Bauen stellt sich die Frage, ob die so ermittelten Kenngrößen der Bewegung auch auf heterogene Personengruppen übertragen werden können. Da bei der Berechnung von Räumungszeiten zunehmend Ingenieurmethoden eingesetzt werden, deren Ergebnisse ganz wesentlich von den zu Grunde gelegten Bewegungsparametern, wie z. B. der freien Gehgeschwindigkeit, abhängen, hat die Validität der Kenngrößen maßgeblichen Einfluss auf die sicherheitstechnische Evaluation von Gebäuden und Versammlungsstätten.
In diesem Artikel wird anhand aktueller Forschungsergebnisse aus Bewegungsstudien, an denen Menschen mit und ohne Beeinträchtigungen teilgenommen haben, der Einfluss der Heterogenität auf Kenngrößen der Bewegung vorgestellt. Darüber hinaus werden die Besonderheiten des Studienablaufs und die Möglichkeiten und Grenzen der Untersuchungsmethode dargestellt. Die Untersuchungen bestätigen, dass die Berücksichtigung besonderer Personengruppen signifikanten Einfluss auf die Kenngrößen der Bewegung hat und daher die Ergebnisse der Ingenieurmethoden beeinflusst und zukünftig bei heterogenen Personengruppen beachtet werden muss.
Evaluation of evacuation process is common separated by two phases: pre-movement and movement-phase. Individual capabilities of pedestrians have an impact on both and therefore on the time required for safe escape. In view of evaluating the evacuation process, characteristics of realistic movements of pedestrians involved are needed, but so far such data are mainly available for individuals with unrestricted evacuation capabilities only.
Due to the lack of available data, parameter studies in an assisted living for people with disabilities were performed to explore the movement during evacuation. Preparation times for assistance (n = 10), unimpeded walking speeds (n = 34) depending on the assistance devices in the plane as well as walking speeds on stairs (n = 11) were focussed.
Time to prepare an assistance device for utilisation depends significantly on the kind of device type. Further on, practical experience in handling the devices for assistance has an impact on the preparation time. In contrast to the results of the preparation times, any relation on assistance devices were investigated for the unimpeded walking speed in the plane. A remarkable decrease of walking speed on stairs was observed which is independent from the utilised assistance device.
The presented data improve and extend the insufficient engineering data base and raised up questions regarding the complexity of considering pedestrians movement with impairments in evacuation planning.
Emergency exits as bottlenecks in escape routes are important for designing traffic facilities. Especially the fundamental diagram is a crucial performance criterion for assessment of pedestrians' safety in facilities and an important basis for calculation methods. For this reason, several studies were performed during the last decades which focus on the quantification of movement through bottlenecks. These studies were usually conducted with populations of homogeneous characteristics to reduce influencing variables and for reasons of practicability.
Studies which consider heterogeneous characteristics in performance parameters are rarely available. In response and to reduce this lack of data a series of well-controlled large-scale movement studies considering pedestrians with different disabilities was carried out.
Understanding movement in heterogeneous groups is important for a meaningful evaluation of evacuation prediction and for a proper design of buildings. The understanding of interactions and influencing factors in heterogeneous groups on key performance figures is fundamental for a safe design. This contribution presents results of experimental studies on movement of a crowd through a bottleneck involving participants with and without disabilities. High precise trajectories of the attendees extracted from video recordings were used to calculate density and velocity of the participants. Besides the well-established fundamental diagram new insights into the individual relation between density and velocity are discussed. A complex structure and considerate behaviour in movement implicates a strong influence of the heterogeneity on key performance values of safe movement.
Products and by-products of the invertebrate and vertebrate farming, respectively, are shown to be promising bio-based flame retardant adjuvants in epoxy thermosets. While the addition of bone meal results in the formation of an inorganic shield, protein-based powders from insects provide an intumescent behavior under forced flaming conditions. Combining the latter with a common flame retardant such as ethylene diamine phosphate, the charring efficiency and self-extinguishing properties can be further enhanced.
Intumescent coatings for fire protection offer advantages over (non-intumescent) cementitious coatings and boards regarding speed of construction, architectural aesthetics, sometimes costs, and other features. However, conventional organic intumescent coatings as well as soluble silicate (waterglass) coatings form foams with low mechanical stability, and the latter coatings generally suffer from low resistance against humidity. Therefore, the search for novel intumescent coatings for more demanding conditions (e.g., abrasive environments) is a necessity in the context of steadily increasing requirements of society and industry.
In this contribution, we present results on intumescent aluminosilicate coatings for fire protection that form foams with significantly increased mechanical strength. Two base formulations, a metakaolin/silica-based mix, adapted from Krivenko et al., and a silica/corundum-based mix, developed at Curtin University, as well as formulations modified with additives (Al(OH)3, Mg(OH)2, B2O3, Na2B4O7), were applied to steel plates (75 mm × 75 mm) and exposed to simulated fire conditions (fire curve according to ISO 834-1:1999). Temperature-time curves were recorded to assess the degree at which the coatings insulated the substrate. In addition, XRD, TG, oscillatory rheometry, and SEM were employed to characterise the coatings.
The coatings were observed to partly expand during hardening due to H2 formation. When the hardened coatings were exposed to elevated temperatures they intumesced as expected, with the degree and nature of expansion dependent on the formulation. Oscillatory rheometry provided insights into the intumescent processes in an apparently brittle material. It revealed that the hardened aluminosilicate coatings became viscous (loss factor > 1) at 75–225 °C, in the temperature range of major water release, as opposed to a “standard” metakaolin-based geopolymer, which continued to behave as a solid. This explains the intumes¬cent behavior of the coatings, i.e. further expansion and foam formation. Microstructural analysis confirmed pore expansion and coalescence; XRD showed that the phases formed after heating (max. temperature ~840 °C) were of ceramic-type.
The fire protection (defined here as the time for the steel substrate to reach the critical temperature of 500 °C) depended mainly on the thick¬ness of the fully expanded coating, i.e. after intumescence. An alumino¬silicate coating free of additives with an original thickness of 12 mm was able to protect the steel for >30 min. The addition of 10 % anhydrous borax (Na2B4O7) caused a significant improvement, such that an original coating thickness of only 6 mm was sufficient to protect the steel for ~30 min. This was caused by the formation of sodium metaborate dihydrate (NaB(OH)4) in the coating that led to a significantly extended dehydration plateau in the temperature-time curve at ~100 °C during the fire exposure.
Brände zerstören immer wieder wichtige Kulturgüter und gefährden nationales Kulturerbe. Das Projekt BRAWA erarbeitet neue Strategien und innovative Technologien, um die Brandsicherheit historischer Gebäude zu erhöhen. Dabei basiert das Konzept auf der Vernetzung von Sensoren, die bereits beim Auftreten bestimmter Gase in der Frühphase der Brandentstehung Alarm auslösen. Durch ein neuartiges Helferkonzept soll eine frühe Branderkennung und -bekämpfung ermöglicht werden.
Im Rahmen des BMBF geförderten Verbundprojekts „TEBRAS – Konzepte und Techniken zur Branderkennung, Bekämpfung und Selbstrettung in der frühesten Brandphase“ arbeiten sechs Partner aus der Wissenschaft und der Industrie gemeinsam an Lösungen zur schnelleren Branddetektion und Bekämpfung. Ausgehend von Brandschadenstatistiken werden zunächst häufige Brandentstehungsszenarien, Brandursachen und die beteiligten Objekte und Materialien identifiziert. Auf dieser Basis wird ein Testszenario entwickelt, das es erlaubt, einen repräsentativen Entstehungsbrand unter definierten Testbedingungen zu untersuchen. Typische Brandkenngrößen werden anhand der ausgewählten Referenzszenarios des Schwelbrands einer Mischbrandkrippe vorgestellt. Der Fokus liegt dabei auf den freigesetzten Brandgasen.
A promising approach for the further improvement of fire detection techniques is the inclusion of fire gases in the characteristics used to detect a fire. A screening of sample materials representative for common first burning items and their gas release under different ignition conditions was performed to gain an overview of possible target gas candidates. Different fire scenarios were investigated to evaluate fire gases produced in early stages of fire development, their time of appearance and concentration development using the vitiated mass loss calorimeter and a heating plate setup in the single burning item test chamber.
Im Rahmen des BMBF geförderten Verbundprojekts „TEBRAS – Konzepte und Techniken zur Branderkennung, Bekämpfung und Selbstrettung in der frühesten Brandphase“ arbeiten sechs Partner aus der Wissenschaft und der Industrie gemeinsam an Lösungen zur schnelleren Branddetektion und Bekämpfung. Ausgehend von Brandschadenstatistiken werden zunächst häufige Brandentstehungsszenarien, Brandursachen und die beteiligten Objekte und Materialien identifiziert. Auf dieser Basis wird ein Testszenario entwickelt, das es erlaubt, einen repräsentativen Entstehungsbrand unter definierten Testbedingungen zu untersuchen. Typische Brandkenngrößen werden anhand der ausgewählten Referenzszenarios des Schwelbrands einer Mischbrandkrippe vorgestellt. Der Fokus liegt dabei auf den freigesetzten Brandgasen.
Avoiding antimony – effect of Ca(H2PO2)2 on smoke emission and fire behaviour in brominated ABS
(2023)
The replacement of antimony trioxide (Sb2O3) in brominated flame-retardant ABS (ABS/FR) is of great interest. This study investigates the influence of calcium hypophosphite (CaP) in ABS/FR on flame retardancy and smoke emission. Different amounts of talc are added to ABS/FR/CaP to evaluate the influence of an inorganic barrier on smoke emission and flame retardancy. The cone calorimeter unveiled a reduction by 46% in PHRR for ABS/FR/CaP. Additional 8 wt.-% talc (ABS/FR/CaP/8Talc) reduced the PHRR by 61%. ABS/FR/CaP exhibited a more condensed phase action, which resulted in less smoke emission. The study investigates the influence of CaP in ABS/FR on the smoke toxicity, smoke density and the smoke particles distribution in the smoke density chamber (ISO 5659-2) coupled to a FTIR spectrometer and electrical low pressure cascade impactor (ELPI).
Replacing antimony trioxide (ATO) in flame retardant formulations is an urgent task due to its toxicity. There are indications that calcium hypophosphite (CaP) may be a promising replacement. This study investigates the decomposition, fire behavior, and smoke release of brominated flame-retarded acrylonitrile butadiene styrene (ABS) under various fire scenarios like ignition, developing fire and smoldering, while replacing ATO with CaP and CaP/talc. Adding 4 wt.-% of talc to CaP formulations showed beneficial effects on flammability due to changes in the viscosity and barrier properties. Synergism between 8 wt.-% talc and CaP improved the protective layer in the developing fire scenario, resulting in a ∼60 % decrease in the peak of heat release rate and reduction of ∼21 % in total smoke production (ref. ABS+Br+ATO). With a conventional index of toxicity (CIT) of below 0.75, ABS+Br+CaP passes the highest requirements according to EN 45545-2. Overall, the CaP/talc materials improve flame retardancy, show less smoke emission under forced flaming conditions, and prevent chronic intoxication and environmental pollution through smoke particles contaminated with antimony.
This work investigates the fire phenomena of rigid polyurethane foams (RPUFs) in detail. To elucidate structure-property relationships, systematically varied sets of materials were prepared covering polyurethane, polyisocyanurate-polyurethane and flame retarded polyurethane foams. Advanced cone calorimeter investigations provide insight into the fire behavior under forced flaming conditions. Thermocouples inside specimens give information about the temperature gradient during combustion. Furthermore, fire phenomena were characterized using cross sections of quenched samples and the scanning electron microscope. By using a Multi methodological approach and systematically varied sets of foam materials, new insights into the burning of RPUFs were won. For the flame retarded foams, the dominant flame retardant mode of action changed with density. PIR foams exhibited a cellular structure in the residue leading to the superior fire performance compared to polyurethane foams. The understanding of fire phenomena contributes to future development of tailored flame retardant strategies for RPUFs.
This work investigates the fire phenomena of rigid polyurethane foams (RPUF) in detail. Rigid polyurethane foams (RPUF) are widely used in industry and daily life because of their outstanding mechanical and thermal insulating properties. In case of fire, cellular polymers like RPUF behave differently from bulk materials, the reason for this is their low thermal inertia. The aim of this study is to investigate the fire phenomena of RPUF in detail. Characterized by simultaneous physical and chemical processes which interact, depend, and compete with each other, the combustion of RPUF is a highly complex occurrence. Therefore it is necessary to study all aspects in detail. The fire phenomena that were examined are gasification, liquefaction, charring and structural integrity as well as collapse. The comprehensive understanding of the processes taking place during combustion is the foundation of customized development of successful flame retardant approaches. Advanced cone calorimeter investigations provide insight into the fire behavior under forced flaming conditions. Thermocouples in the inside of specimens give information about the temperature gradient and temperature of the pyrolysis zone during combustion. Changes in the morphology and thickness of the pyrolysis zone were examined using a hot-stage microscope, as well as SEM images of cross-sections of quenched foam specimens. Furthermore, fire phenomena were characterized using LOI and thermal analysis. By using a multimethodological approach and systematically varied sets of Polyurethane and Polyisocyanurate foams, new insights into the burning of RPUF were won. The detailed knowledge of fire phenomena is essential for future development of tailored flame retardant strategies for RPUF.
Brandsicherheit von Bussen
(2021)
Grundsätzlich lässt sich sagen, dass Busbrände relativ häufig auftreten, auch wenn sich das im öffentlichen Bewusstsein nicht unbedingt widerspiegelt. In Deutschland gibt es keine einheitliche Brandstatistik, nach einer eigenen Internetrecherche brennt im Schnitt aber etwa an jedem zweiten Tag ein Bus in Deutschland.
Auch eine interne Umfrage eines Verbands von Busbetreibern bestätigte die Häufigkeit von Bränden: Ungefähr 1 Prozent der Busse hatte im Jahr einen Brandfall – wobei hier auch kleinere Ereignisse mitgezählt wurden. Die britische Statistik bestätigt diese Zahlen. Sie führt für die letzten 10 Jahre ca. 11900 Brände pro Jahr in Fahrzeugen, davon ca. 315 pro Jahr in Bussen auf. Brände in Bussen sind für die Passagiere eine große Gefährdung, da sie sich meist sehr schnell ausbreiten.
Zwei schwere Brände ereigneten sich in Deutschland 2008 und 2017.
In this study included:
The consideration of a façade kit as a construction product
The consideration of a façade as a part of a specific building. In some national regulations this would mean that detailing such as
window openings may also need to be considered.
Fire scenario identification for each of the Member States that regulate for the fire performance of the façade system based on alternative assessment methods.
Recent bus fires in Europe, such as the bus fire in France 2015 with 43 fatalities and the bus fire in Germany 2017 with 19 fatalities, show that these fires can be very hazardous and time for escape can be too short. Recently, several fire safety measures came into force for busses. Engine compartment suppression systems will be mandatory for all busses in Europe. This is a big step in fire safety as about 80 % of fires start in the engine compartment. However, in several recent bus fires a time of less than 5 minutes has been reported from detection of the fire to a fully developed fire. As normally many people are on board of a bus, a bus fire is not comparable to fire in a home. Especially for people with reduced mobility or for fires after a collision the available times for escape are too short. When the fire service is on scene the transition to a fully developed fire might have happened already. Passengers who are not able to escape in this short period of time mostly cannot be rescued by the fire service even with quick response times because of the dramatic fire development. Fires that do not start in the engine compartment but develop in the cabin are rarer but extremely dangerous because fire and smoke spread very rapidly. The reason for the fast fire and smoke development in the cabin are the materials which are used. Over the last tens of years materials in busses had major developments. The amount of plastic in the cabin has grown significantly. In a modern coach the biggest fire load often is not the fuel anymore but the interior materials.
Bus fire safety is mainly regulated by ECE regulations R 118 and R 107. A comparison with European standards for trains shows that for trains, in contrast to busses, a holistic fire concept exists. Fire scenarios as well as escape scenarios and passenger behaviour are taken into account, resulting in fire safety regulations on a high level compared with bus regulations. In contrast to regulations for train materials no limits for heat or smoke production are given for bus materials. Larger heat release values promote more rapid fire spread. Also smoke production and toxicity are key factors in fires. The smoke reduces the visibility in the case of fire, and together with the toxicity of the smoke can make escape from the vehicle impossible. Figure 1 shows the remains of the bus from the recent severe bus fire in Germany in 2017.
As a result of experience with real cases and results from research projects we think it is necessary to develop a holistic fire safety concept for busses as it exists for other transport means like railways. The fire safety concept should include vehicle configuration and design as well as areas of use, e.g. use in cities, use in long-distance traffic on motorways and use in tunnels.
Das EU Projekt EU FireStat SI2.830108, das vom Europäischen Parlament finanziert und von der DG GROW der Europäischen Kommission in Auftrag gegeben wurde, hat aufgearbeitet, welche Terminologie in den europäische Mitgliedsstaaten verwendet wird und die von den Mitgliedstaaten erhobenen Daten über Gebäudebrände zu analysieren. Dabei wurden die Schwierigkeiten bei der Erfassung und die Unterschiede bei der Auslegung ermittelt und eine gemeinsame Terminologie sowie eine Methode zur Erfassung der erforderlichen Daten vorgeschlagen.
Folgende Schwerpunkte wurden bearbeitet: Zunächst erfolgte eine Diagnose von Terminologie-, Datenerhebungs- und Auslegungsproblemen, Erhebung der Terminologie und der Datenerfassung, Identifizierung der für die Entscheidungsfindung benötigten Daten, Analyse der Methoden zur Datenerhebung Definition einer gemeinsamen Terminologie, Methodik der Kosten-/Nutzenbewertung zur Unterstützung politischer Entscheidungen, Fallstudie zur Anwendung der Methode der Kosten-/Nutzenbewertung, Beschreibung einer zukünftigen Datenerhebungsmethode.
Das Ergebnis des Projekts ist eine Empfehlung, welche Daten in den Mitgliedstaaten erhoben werden sollten, um wissensbasierte Entscheidungen in Bezug auf den Brandschutz zu ermöglichen. Damit wird die Grundlage für Maßnahmen und Initiativen geschaffen, die den Brandschutz und die Brandverhütung der Mitgliedstaaten unterstützen, so dass knappe Ressourcen gezielt eingesetzt werden können.
Das EU Projekt EU FireStat SI2.830108, das vom Europäischen Parlament finanziert und von der DG GROW der Europäischen Kommission in Auftrag gegeben wurde, hat aufgearbeitet, welche Terminologie in den europäische Mitgliedsstaaten verwendet wird und die von den Mitgliedstaaten erhobenen Daten über Gebäudebrände zu analysieren. Dabei wurden die Schwierigkeiten bei der Erfassung und die Unterschiede bei der Auslegung ermittelt und eine gemeinsame Terminologie sowie eine Methode zur Erfassung der erforderlichen Daten vorgeschlagen.
Folgende Schwerpunkte wurden bearbeitet: Zunächst erfolgte eine Diagnose von Terminologie-, Datenerhebungs- und Auslegungsproblemen, Erhebung der Terminologie und der Datenerfassung, Identifizierung der für die Entscheidungsfindung benötigten Daten, Analyse der Methoden zur Datenerhebung Definition einer gemeinsamen Terminologie, Methodik der Kosten-/Nutzenbewertung zur Unterstützung politischer Entscheidungen, Fallstudie zur Anwendung der Methode der Kosten-/Nutzenbewertung, Beschreibung einer zukünftigen Datenerhebungsmethode.
Das Ergebnis des Projekts ist eine Empfehlung, welche Daten in den Mitgliedstaaten erhoben werden sollten, um wissensbasierte Entscheidungen in Bezug auf den Brandschutz zu ermöglichen. Damit wird die Grundlage für Maßnahmen und Initiativen geschaffen, die den Brandschutz und die Brandverhütung der Mitgliedstaaten unterstützen, so dass knappe Ressourcen gezielt eingesetzt werden können.
Brandschutz
(2022)
Die Präsentation gibt einen Überblick über die Arbeiten im German Pilot des EU-Projekts TREEADS. Es werden klein-, mittel- und großskalige Versuche an Waldboden mit einheimischer Vegetation durchgeführt. Begleitend werden numerische Untersuchungen durchgeführt, die eine Variation der Parameter, wie Bodenfeuchte, Temperaturen und Wind über die Experimente hinaus erlauben. Die gemessenen Materialparameter dienen als Input für die numerischen Berechnungen. Die numerischen Modelle werden mit den mittel- und großskaligen Experimenten validiert.
Several attempts have been made in the past to develop a European harmonized testing and assessment method for façades before the European commission decided to publish a call for tender on the topic. A project consortium from five countries (Sweden, UK, France, Germany and Hungary) applied to the call for tender and was contracted to develop a European approach to assess the fire performance of façades. 24 sub-contractors and 14 stakeholder entities were part of the project.
The objective of the European project was to address a request from the Standing Committee of Construction (SCC) to provide EC Member States regulators with a means to regulate the fire performance of façade systems based on a European approach agreed by SCC. In addressing this objective, the project team was asked to consider a number of issues which are presented and discussed.
Motor Vehicles
(2021)
The amount of plastic and synthetic materials is still growing in all sectors of everyday life. In the automotive industry, plastic materials are now widely used in vehicles because of their excellent mechanical properties and their light weight combined with low production costs. However, plastic materials are flammable and can generate toxic smoke gases which can endanger passengers’ lives in the event of fire.
Recent facade fires worldwide have driven change in regulations for façade fire safety in different parts of the world. The Grenfell Tower fire 2017 in London triggered a thorough investigation of many aspects of the fire. One investigation was about the UK building regulations from Dame Judith Hackett 1,2. This investigation compares the UK with the situation other parts of the world.
The influence of pressure sensitive adhesive (PSA) tapes as adhesive layers on the burning behaviour of bonded materials has been investigated. Single-sided tapes as an outer connection between construction materials have large influence on flammability, flame spread and fire resistance. In contrast, double sided tapes only take a small impact on the flammability but can drasticly change the burning behaviour in developing fires.
Im Rahmen des laufenden IGF Projektes 20762 N wurde der Einfluss von Haftklebebändern auf das Brandverhalten von Klebverbunden Untersucht. Dabei wurden sowohl kommerziell verfügbare Klebebänder mit unterschiedlichem Brandverhalten als auch Modellhaftklebebänder mit neuartigen Flammschutzmitteln eingesetzt.
Zunächst wurde das Brandverhalten der Klebebänder adressiert und anschließend der Einfluss jenes Brandverhaltens auf Brandeigenschaften von entsprechend geklebten Verbunden analysiert.
Im Bezug auf die Entflammbarkeit besitzt das Klebeband im Inneren eines Klebverbundes nur einen geringen Einfluss auf das Brandverhalten und die Eigenschaften des Substrates dominieren.
Im sich entwickelnden Brand, hier simuliert durch das Cone Calorimeter, sind deutliche Unterschiede zwischen massivem und geklebten Bauteil zu erkennen. Dabei wirkt die Klebfuge je nach Substrat und Klebebandbeschaffenheit unterschiedlich.
Weitere Untersuchungen zu flammgeschützten Haftklebstoffen sollen erfolgen und somit neue Wege in der Haftklebstoffentwicklung aufzeigen.
In the recent years, more and more products in construction and automotive industry are bonded by adhesive tapes instead of mechanical fasteners but there is no sufficient understanding of how these bonded, layered materials behave in fires. Our research project gives an insight of how adhesives and substrates interact with each other in different fire scenarios and how flame retardants function in pressure sensitive adhesive (PSA) tapes. A systematic investigation on the burning behavior of PSA tapes as free-standing films, as top layers on different substrates and as sandwich-like adhesive joints was performed. The burning behavior of free-standing PSA tapes and those used as a coating was significantly improved by using phosphorus-based flame retardants. Furthermore, it was shown that, depending on tape structure and substrate, the PSA tape can lower the fire risk by acting as an intermediate protection layer in bonded materials.
Steel tension rod systems consist of tension rods, fork connectors and associated intersection or connecting plates. They are used for truss systems, bracings or suspensions owing to slender design and increased economic efficiency. In case of fire, beside the tension rods themselves, the connection parts require appropriate fire protection. The use of intumescent fire protection coatings prevents a rapid heating of the steel and helps to ensure the load-carrying capacity of the structures. Because the connection components of the tension rod systems feature surface curvature as well as a complex geometry, high demand is placed on the intumescence and thermal protection effectiveness of the reactive fire protection coatings. Experimental studies were carried out to investigate the performance of intumescent coatings applied to the components of tension rod systems. The examined aspects include the foaming and cracking behaviour of the intumescent coatings, the influence of different dry film thicknesses (DFT), the heating rate of the steel connecting parts in comparison to the tension rods, as well as the mounting orientation of the tension rods together with their associated fork connectors. The results show that a decrease in the surface curvature and/or an increase in the mass concentration of the steel components lead to a lower heating rate of the steel. Moreover, the performance of the intumescent coating on tension rod systems is influenced by the mounting orientation of the steel components.
For intumescent coatings durability is an important aspect. Due to ageing, which is caused by climatic conditions, the thermal protection performance of intumescent coatings can be reduced during the working life. The national German and the European procedures to assess the durability of intumescent coatings presume a working life of 10 years. For a longer period, additional investigations are required. However, the European assessment procedure does not provide specific information how to prove a durability of more than 10 years. In addition to this formal reason, also from a scientifical position, it is necessary to investigate the degradation of intumescent coatings in detail to propose a corresponding test concept for a durability of more than 10 years.
The presentation summarises the existing knowledge about the degradation behaviour and ageing of intumescent coatings. Furthermore, the results of different approaches from a recently conducted research project are presented. Starting from a water-based and an epoxy-based guide formulation, in a first approach a degradation of the intumescent coating was carried out directly during the production process, i.e. by reducing the concentration of functionally relevant chemical components. In another approach, the duration of the short-term weathering tests was significantly extended, i.e. by multiple repetition of the artificial weathering. The thermal protection performance of the intumescent coating was assessed by fire tests and tests with electrical heating source. In addition, small-scale tests were carried out to determine the thermal material properties of the intumescent coating and thermo-analytical methods were applied to characterise the degradation. Derived from this knowledge, possibilities to test and assess a working life for a period of more than 10 years are proposed.
Steel tension rod systems consist of tension rods, fork connectors and associated intersection or connecting plates. They are used for truss systems, bracings or suspensions owing to slender design and increased economic efficiency. In case of fire, beside the tension rods themselves, the connection parts require appropriate fire protection. The use of intumescent fire protection coatings prevents a rapid heating of the steel and helps to ensure the load-carrying capacity of the structures. Because the connection components of the tension rod systems feature surface curvature as well as a complex geometry, high demand is placed on the intumescence and thermal protection effectiveness of the reactive fire protection coatings. Experimental studies were carried out to investigate the performance of intumescent coatings applied to the components of tension rod systems. The examined aspects include the foaming and cracking behaviour of the intumescent coatings, the influence of different dry film thicknesses (DFT), the heating rate of the steel connecting parts in comparison to the tension rods, as well as the mounting orientation of the tension rods together with their associated fork connectors. The results show that a decrease in the surface curvature and/or an increase in the mass concentration of the steel components lead to a lower heating rate of the steel. Moreover, the performance of the intumescent coating on tension rod systems is influenced by the mounting orientation of the steel components.
Fire resistance of fiber-reinforced polymers (FRPs) has been an important area of research for many years since FRPs are mainly used in the transportation and construction sectors. This study presents the fire behavior, and mechanical performance between the flame retarded pure epoxy resin and flame retarded glass-fiber composites before, during, and after a fire event. This enables a deeper understanding of the transferability of flame retardants on composite materials.
This study presents the processability, fire behavior, and mechanical performance between the flame retarded pure epoxy resin and flame retarded glass-fiber-reinforced plastic before, during, and after a fire event. This enables a deeper understanding of the transferability of flame retardants, modes of action, char enhancement, and flame inhibition on composite materials
Several investigation groups have studied the flame-retardancy modes of action and properties of epoxy resins in the past; nevertheless, the selection of suitable flame retardants for epoxy resins remains challenging, and the transfer to fiber composites is difficult. The addition of flame retardants and glass fibers (GFs) to a polymeric system in a fire scenario changes the polymer's pyrolytic path and burning characteristics, reduces the heat released in the combustion, and suppresses the modes of action in the condensed and gas phase. In this study, the thermal analysis, flammability, fire behavior, residue analysis, fire stability, and quantification of modes of action of three different systems with three halogen-free flame retardants (melamine polyphosphate (MPP), ammonium polyphosphate (APP), and silane ammonium polyphosphate (SiAPP)) and three different types of GFs (unidirectional (UD), bidirectional (BD), and woven roving (WR)) will be compared with pure epoxy resin as a reference.
Zur Bedarfsplanung von Feuerwehren in Städten in der Bundesrepublik Deutschland wurden im Jahr 1998 die Qualitätskriterien Hilfsfrist, Funktionsstärke und Erreichungsgrad für ein standardisiertes Schadensereignis erarbeitet. Das standardisierte Schadensereignis basiert auf Ergebnissen der O.R.B.I.T.-Studie aus dem Jahr 1978. Der dort dargestellte Rauchgas-temperaturverlauf für einen standardisierten Wohnungsbrand stellt Ergebnisse von Brandversuchen in einer Wohnung aus dem Jahr 1939 dar. Die zur Untersuchung herangezogenen Einrichtungsgegenstände bestanden dabei überwiegend aus cellulosehaltigen Materialien wie Holz und Papier. Die zunehmende Verwendung von Werkstoffen auf der Basis von Holz und Polymeren führt jedoch zu einer veränderten stofflichen Zusammensetzung von Einrichtungsgegenständen in Wohnungen. Im Rahmen der vorliegenden Dissertation wurde der Einfluss dieser veränderten stofflichen Zusammensetzung von gegenwärtigen Einrichtungsgegenständen auf den Verlauf von Raumbränden sowie auf die damit verbundene Stoff- und Energiefreisetzung während der Brandentstehungs- und Brandausbreitungsphase untersucht. Im Fokus der Untersuchung stand der Raum der Brandentstehung sowie ein angrenzender Raum.
Die Ergebnisse zeigen, dass gegenwärtige Einrichtungsgegenstände sowohl im Raum der Brandentstehung als auch in dem angrenzenden Raum zu höheren Rauchgastemperaturen und -konzentrationen führen. Grund hierfür sind neben den höheren Wärmefreisetzungsraten auch die höheren Stoffausbeuten der in den gegenwärtige Einrichtungsgegenständen verwendeten Materialzusammensetzungen. Vor diesem Hintergrund zeigt sich, dass sich die auf Basis der O.R.B.I.T.-Studie definierten Standards nicht mehr als Grundlage zur Bedarfsplanung von Feuerwehren eignen. Diese können mit Hilfe der vorliegenden Ergebnisse einer Prüfung unterzogen werden, um den veränderten Brandverläufen im Rahmen einer zukünftigen Bedarfsplanung gerecht zu werden.
In recent years, fire safety requirements for bus interior materials have been increased and introduced into international regulations. Fire safety requirements for the burning rate, melting and dripping behaviour of interior materials already exist for many years. However, it remains unclear to what extent the release of smoke, combustion products and their toxicity should be limited. Therefore, a research and development project 82.0723 funded by BASt (Federal Highway Research Institute) was initiated to develop a simplified procedure for testing the toxicity and smoke development in case of fire of interior materials used in buses. The scope of the research included calculations to assess the toxicity of fire gases and the derivation of specifications for the formation of practicable limit values for smoke toxicity. Further investigations are needed to derive these limit values for smoke toxicity in order to be applicable for real fire scenarios in buses.
Crisis management, particularly the evacuation of handicapped people during a fire scenario presents a highly demanding challenge for nursing staff and rescue forces on site. The German research Project SiME is an interdisciplinary cooperation of university and non-university research institutions as well as medium-sized companies, which work together to develop strategies to manage such critical scenarios. In the SiME project, which is funded by the German Federal Ministry of Education and Research, evacuation characteristics of pedestrians with physical, mental or age-related disabilities are investigated to fit consisting numerical evacuation models with data. One of the major tasks of the OvGU was to set up a database of scenarios related to fire, explosion or substance releases in the working and living environment of handicapped people. Therefore, more than 463 fire Events occurring over the last decade in Germany were documented in this database and categorized by a suitable assignment of characteristics e.g. location of fire, ignition source, number of fatalities and injured.
Crisis management, particularly the evacuation of handicapped People during a fire scenario presents a highly demanding challenge for nursing staff and rescue forces on site. The German research Project SiME is an interdisciplinary cooperation of university and non-university research institutions as well as medium-sized companies, which work together to develop strategies to manage such critical scenarios. In the SiME project, which is funded by the German Federal Ministry of Education and Research, evacuation characteristics of pedestrians with physical, mental or age-related disabilities are investigated to fit consisting numerical evacuation models with data. One of the major tasks of the OvGU was to set up a database of scenarios related to fire, explosion or substance releases in the working and living environment of handicapped people. Therefore, more than 463 fire Events occurring over the last decade in Germany were documented in this database and categorized by a suitable assignment of characteristics e.g. location of fire, ignition source, number of fatalities and injured.
The evaluated data were the basis for carrying out a quantitative risk analysis. Thus event trees were set up for different integrative infrastructures with which occurrence probabilities for different scenarios could be calculated for each path. The extent of damage, as a quantity describing the impact, was assumed to be personal injury or death or serious injury. By a risk assessment critical Scenarios could be derived from the risk analysis.
We report dielectric and calorimetric studies on metathesis and addition-type polytricyclononenes, both based on the same monomer bearing three pendant OSiMe3 groups. For the addition-type polymer, dielectric spectroscopy reveals a β*-process related to the microporosity, whereas for its metathesis counterpart, the segmental dynamics manifests as an α-process related to a glass transition. Besides active dielectric processes, a significant conductivity contribution is detected for both samples which for the microporous additiontype polymer is three orders of magnitude greater than for the metathesis polymer. The broadband dielectric spectroscopy is complemented by detailed calorimetric investigations, comprising DSC, FSC, and TMDSC. The calorimetric methods detected the glass transition for the metathesis polymer in agreement with the observed dielectric α-process. Furthermore, the already reported gas transport properties for both polymers are compared, setting them in correlation with the observed molecular mobility and conductivity behavior. The discussed results reflect significant differences in molecular mobility of the two polymers affecting the appearance of microporosity which strongly determines the gas transport properties.
Polyesters with DOPO substituents can be successfully synthesized with 10-[2,5-Bis(2-hydroxyethoxy)phenyl]-9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide(DOPO-HQ-glycolether) and DOPO-substituted dimethyl succinate (PIta). These polyester materials show an effective flame retardancy which can be fine-tuned by the chemical structure of the polyester backbone.
Nanomaterials are a relatively new class of materials for which a regulatory framework still has to be established and regulators require comprehensive datasets of well characterized nanomaterials for the implementation. Especially information about the surface chemistry of nanoparticles is crucial, since it largely determines their biological and environmental fate. How the surface chemistry changes under relevant ageing conditions is of particular interest, because exposure will normally occur not to the pristine material but to a nanoform that underwent some kind of transformation.
In this talk, first a short overview about the contributions of division 6.1 to multiple European-funded projects will be presented, in which surface analytical techniques are used to improve the physical-chemical characterization of nanomaterials. Secondly, a study investigating the surface-chemical transformations of a representative set of titanium dioxide nanoparticles is discussed in more detail. The ageing has partly been performed at the BAM division 7.5, and the surface chemistry was analyzed using time-of-flight secondary ion mass spectrometry (ToF-SIMS) and X-ray photoelectron spectroscopy (XPS). By analyzing the complex mass spectra with principal component analysis (PCA), it was possible to identify even subtle changes that occur upon ageing.
Behälter aus hochdichtem Polyethylen (PE-HD) werden zur Lagerung und für den Transport von Kraftstoffen eingesetzt. Beim Kontakt beider Medien diffundiert der Kraftstoff in das Polymer, erhöht dessen Volumen und Duktilität und ändert damit das Fließverhalten des Polymers unter Zugbelastung. Zudem weist PE-HD in Luft im verstreckten Bereich das sogenannte strain-whitening (Lichtstreuung) auf, während in Diesel gelagertes PE-HD optisch transparent wird. Zur Untersuchung dieses Phänomens wurden ortsaufgelöste Röntgenrefraktion und –diffraktion (Topographie) eingesetzt. Aus Sicht der molekularen Struktur (Diffraktion) weisen die beiden Probentypen keine Unterschiede auf: im verstreckten Bereich liegt eine „Fasertextur“ der Polymerketten in Belastungsrichtung vor, im unverstreckten Bereich nahezu ideale Isotropie. Die für mikroskopische Strukturen empfindliche Röntgenrefraktion zeigt außerdem für die Probe in Luft im verstreckten Bereich eine ausgeprägte Orientierung von Grenzflächen in Zugrichtung, während die in Diesel gelagerte Probe keine Grenzflächen zeigt. In Analogie zum optischen Verhalten bewirken die ähnlichen Brechungsindizes beider Medien im Röntgenbereich, dass eindiffundierter Diesel als Immersionsflüssigkeit die Brechungseigenschaften herabsetzt.
Behälter aus hochdichtem Polyethylen (PE-HD) werden zur Lagerung und für den Transport von Kraftstoffen eingesetzt. Beim Kontakt beider Medien diffundiert der Kraftstoff in das Polymer, erhöht dessen Volumen und Duktilität und ändert damit das Fließverhalten des Polymers unter Zugbelastung. Zudem weist PE-HD in Luft im verstreckten Bereich das sogenannte strain-whitening (Lichtstreuung) auf, während in Diesel gelagertes PE-HD optisch transparent wird. Zur Untersuchung dieses Phänomens wurden ortsaufgelöste Röntgenrefraktion und –diffraktion (Topographie) eingesetzt. Aus Sicht der molekularen Struktur (Diffraktion) weisen die beiden Probentypen keine Unterschiede auf: im verstreckten Bereich liegt eine „Fasertextur“ der Polymerketten in Belastungsrichtung vor, im unverstreckten Bereich nahezu ideale Isotropie. Die für mikroskopische Strukturen empfindliche Röntgenrefraktion zeigt außerdem für die Probe in Luft im verstreckten Bereich eine ausgeprägte Orientierung von Grenzflächen in Zugrichtung, während die in Diesel gelagerte Probe keine Grenzflächen zeigt. In Analogie zum optischen Verhalten bewirken die ähnlichen Brechungsindizes beider Medien im Röntgenbereich, dass eindiffundierter Diesel als Immersionsflüssigkeit die Brechungseigenschaften herabsetzt.
As a potential substitute for currently used halogenated flame retardants we explored the synthesis of dibenzo[d,f][1,3,2]dioxaphosphepine 6-oxide (BPPO) and derivatives. BPPO is a cyclic phosphonate and was synthesized by a simple, three-component condensation using 2,2´-biphenol, phosphorus trichloride and water by improving a procedure given by Natchev. Subsequently, BPPO was employed in phospha-Michael additions in line with the known synthesis of DOPO-compounds to double bonds. These reactions result in novel phosphorus-containing compounds with flame retardant activíty. The chemical structure of the unsaturated compounds was systematically varied yielding non-reactive flame retardants (without functional groups) from acrylates and diesters, and reactive (with functional groups) flame retardants from p-benzoquinone. The use of the phosphonate BPPO and its derivatives as flame retarding additives has not been described yet. The BPPO ring is highly reactive. Therefore, it is supposed that it mainly acts in the gas phase.
The new phosphonates were applied as additives for improving the flame retardancy of rigid PUR/PIR foams with triethyl phosphate (TEP) as plasticizer. The foam characteristics like density, cell integrity, pore size and mechanical properties were investigated. The burning properties of the foams were analyzed in the vertical flame spread according to DIN 4102 and by cone calorimetry. The relevant parameters depended on the phosphorus content, which is illustrated for PIR foams with ethyl 3-(6-oxidodibenzo[d,f][1,3,2]dioxaphosphepin-6-yl)propanoate (X, Z = H; Y = OEt; EA-BPPO) as FR additive.
At comparable P-content, the EA-BPPO additive reached the PHHR-values of the benchmark foam with TEP and triphenyl phosphate as FR additive. With increased P-content the values were further reduced. TML and MARHE parameters showed a similar tendency. The FR additives dispersed well in the formulation and had no significant influence on foam density, cell integrity and pore size compared to the reference sample.
Nowadays, various polymeric materials are used in E&E applications with sufficient flame retardance by adding rather different flame retardants. It doesn’t matter whether cables are used outdoor or are installed indoor as building products, the weathering exposures such as UV radiation, humidity and variation in temperature occur and influence the flame-retardant property. Recently, the lifetime of the flame retardance itself becomes an increasingly important factor. In this work, several devices were used to perform accelerated artificial ageing simulating different environment exposures.
The comprehensive and global understanding of the durability of flame retardance in dependence on the weathering or ageing conditions is still a matter of discussion. Therefore, the weathering resistance of various halogen-free fire-retarded polymers was investigated in this work. Polymeric systems with different kinds of fire retardants were chosen, including various fire retardant mechanisms. Ethylene Vinyl Acetate (EVA) blends with high amounts of inorganic flame retardant such as aluminum hydroxide (ATH), boehmite and synergists, which mainly dilutes the polymer resin work as heat sink and cooling agent, and enhance residue formation was examined. Thermoplastic Polyurethane (TPU) was modified with melamine cyanurate (MC), which mainly acts by changed melt flow and dripping behavior as well as fuel dilution. Additionally, aluminum diethylphosphinate and boehmite are induced as assistant flame retardant. Furthermore, glass fiber reinforced Polyamide 66 (PA) was investigated containing different kinds of aluminum diethylphosphinate based flame retardant mixtures, which acts by flame inhibition and additional char formation.
The degradation of the surface was analyzed after the different weathering conditions. Most of the specimens exhibited an intensive material degradation at the top surface accompanied by a distinct discoloration, e.g. getting darker or showing yellowing. The weathering of the EVA samples lead to numerous cracks (already) after 4000 h. The corresponding changes in the chemical structure was investigated by ATR FT-IR for all materials.
The flammability was investigated by cone calorimeter, UL-94 burning chamber, and oxygen index (LOI) using plate and bar specimens. The flame retardance of most of the materials studied degrades only slightly or were rather stable for the investigated exposure times. Interestingly, also some opposite results were found. EVA modified by different inorganic flame retardants such as ATH achieved higher LOI after exposing in the humidity chamber and the accelerated oxidation under water in the autoclaves. It is suggested that the particle size of ATH and boehmite plays an important role, when these flame retardants agglomerate at the surface during accelerated weathering.
Both materials, EVA and TPU, were also investigated as cable jackets. While EVA modified with inorganic flame retardants exhibits low-smoke and non-dripping fire behavior, TPU flame-retarded with MC yields cables with pronounced melt-dripping. Cone calorimeter tests were carried out using cable rafts of the size of 100 mm * 100 mm as well as our self-made cable module test, which simulates the vertical full-scale test of a bundle of cables at the bench-scale. Both methods were used to investigate the weathering resistance of the flame retardance in cables. The results of the cable module test for the flame-retarded EVA cables were only slightly affected even when a long time hydrothermal ageing was carried out. This is because of inorganic residue which just delays the fire growth but does not extinguish. However, for the flame-retarded TPU cable jackets, the cable module test exhibited an accelerated fire spread and a melt-dripping behavior which was promoted by weathering exposure.
A well-defined terminology of fire-related variables is important for correct analyses and supporting knowledge-based decisions regarding the evaluation of building fires at the European level. After developing an overview of current practices for fire statistics in Part I, the terminology used and the data collected by the EU Member States and eight other countries regarding fire incidents, property damage and human losses were mapped to increase awareness of their practice and support a comprehensive assessment of several fire statistical datasets. A questionnaire was distributed to relevant authorities responsible for the collection, elaboration/analysis, and fire statistical data publications to define and select the essential variables for an appropriate fire assessment and fire incident description. Based on the results of the questionnaire able to identify the essential fire statistical variables and a detailed analysis of current definitions adopted in the fire statistics of the EU Member States and other countries, a common terminology is proposed to collect the necessary data in the EU Member States and obtain meaningful datasets based on standardised terms and definitions. The results will generate essential outputs to move towards harmonised fire statistics at the EU level and contribute to an appropriate analysis able to improve fire prevention and fire mitigation in building fires.
Flame retardants (FR) are inevitable additives to many plastics. Halogenated organics are effective FRs but are controversially discussed due to the release of toxic gases during a fire or their persistence if landfilled. Phosphorus-containing compounds are effective alternatives to halogenated FRs and have potential lower toxicity and degradability. In addition, nitrogencontaining additives were reported to induce synergistic effects with phosphorus-based FRs. However, no systematic study of the gradual variation on a single phosphorus FR containing both P−O and P−N moieties and their comparison to the respective blends of phosphates and phosphoramides was reported. This study developed general design principles for P−O- and P−N-based FRs and will help to design effective FRs for various polymers. We synthesized a library of phosphorus FRs that only differ in their P-binding pattern from each other and studied their decomposition mechanism in epoxy resins. Systematic control over the decomposition pathways of phosphate (PO(OR)3), phosphoramidate (PO(OR)2(NHR)), phosphorodiamidate (PO(OR)(NHR)2), phosphoramide (PO(NHR)3), and their blends was identified, for example, by reducing cis-elimination and the formation of P−N-rich char with increasing nitrogen content in the P-binding sphere. Our FR epoxy resins can compete with commercial FRs in most cases, but we proved that the blending of esters and amides outperformed the single molecule amidates/diamidates due to distinctively different decomposition mechanisms acting synergistically when blended.
Es wird ein Verfahren zur Charakterisierung der Beständigkeit und Langzeitstabilität von additiv gefertigten Kunststoff-Bauteilen vorgestellt. Dabei sollen die Prüfkörper über 2000 Stunden künstlich bewittert und währenddessen die Änderungen der Eigenschaften der Bauteile zerstörungsfrei untersucht werden. Die Erkenntnisse dienen für die Entwicklung einer Strategie für eine Qualitätskontrolle von additiv gefertigten Kunststoffteilen.
Additiv gefertigte Prüfkörper aus Polyamid 12 (Laser Sinter Verfahren) und Acrylnitril-Butadien-Styrol (Fused Layer Modeling Verfahren) wurden über 2000 Stunden künstlich bewittert und ihr Alterungsverhalten untersucht. Die Ergebnisse wurden anschließend mit denen von Prüfkörpern verglichen, welche auf dieselbe Weise künstlich bewittert, aber mittels konventionellem Kunststoff-Spritzguss hergestellt wurden.
Die Erkenntnisse dienen für die Entwicklung einer Strategie für eine Qualitätskontrolle von additiv gefertigten Kunststoffteilen.
Es wurden mittels Fused Layer Modeling (FLM) Probekörper aus ABS und mittels Laser Sintering (LS) Probekörper aus PA 12 hergestellt, die anschließend für drei Monate einer künstlichen Bewitterung unterzogen wurden. Die dabei erzeugte definierte Alterung wurde nach drei Zeitabschnitten jeweils mit zerstörungsfreien Methoden charakterisiert. Dabei wurde neben den spektroskopischen Standardmethoden auch die aktive Thermografie eingesetzt. Die Ergebnisse zeigen, dass sich mittels der Thermografie sowohl chemische Veränderungen als auch mechanische Schädigungen (Fehlstellen) darstellen lassen. Die Bewitterung beeinflusst die Teiltransparenz der Proben zumindest im sichtbaren Spektralbereich, was bei der Charakterisierung der Fehlstellen, die mittels optisch angeregter aktiver Thermografie detektiert wurden, berücksichtigt werden muss.
Die Erkenntnisse dienen für die Entwicklung einer Strategie für eine Qualitätskontrolle von additiv gefertigten Kunststoffteilen.
Es wurden Prüfkörper aus additiver Fertigung mittels Laser Sinter Verfahren (Polyamid 12, PA 12) und Fused Layer Modeling (Acrylnitril-Butadien-Styrol, ABS) sowie Prüfkörper aus dem Kunststoff-Spritzguss Verfahren (PA 12 und ABS) über 2000 Stunden künstlich bewittert. Vor, während und nach der Bewitterung erfolgte eine zerstörungsfreie Prüfung mittels Thermografie, optischer Mikroskopie und spektralen Methoden (UV/VIS-Spektroskopie und spektrale Reflexion), um den Alterungsfortschritt zu untersuchen und Schäden durch die künstliche Bewitterung sowie eingedruckte Defekte zu identifizieren und zu detektieren.
Zusätzlich wurden zerstörende Zugprüfungen vorgenommen, welche mit einer IR-Kamera verfolgt wurden. Auf diese Weise konnten lokale Temperaturänderungen, hervorgerufen durch elastische sowie plastische Verformungen, zeitaufgelöst erfasst und ausgewertet werden.
Es wird ein Verfahren zur Charakterisierung der Beständigkeit und
Langzeitstabilität von additiv gefertigten Kunststoff-Bauteilen vorgestellt. Dabei sollen die Prüfkörper über 2000 Stunden künstlich bewittert und währenddessen die Änderungen der Eigenschaften der Bauteile zerstörungsfrei untersucht werden.
Das vorgestellte Projekt beschäftigt sich mit den optischen, thermophysikalischen und mechanischen Materialeigenschaften von additiv gefertigten Kunststoffteilen und deren Alterung. Dazu wurden mittels Fused Layer Modeling (FLM) Probekörper aus ABS hergestellt, die anschließend für drei Monate einer künstlichen Bewitterung unterzogen wurden. Die dabei erzeugte definierte Alterung wurde nach drei Zeitabschnitten jeweils mit zerstörungsfreien Methoden charakterisiert. Dabei wurde neben den spektroskopischen Standardmethoden auch die aktive Thermografie eingesetzt. Die Ergebnisse zeigen, dass sich mittels der Thermografie sowohl chemische Veränderungen als auch mechanische Schädigungen (Fehlstellen) darstellen lassen. Die Bewitterung beeinflusst die Teiltransparenz der Proben zumindest im sichtbaren Spektralbereich, was bei der Charakterisierung der Fehlstellen, die mittels optisch angeregter aktiver Thermografie detektiert wurden, berücksichtigt werden muss.
Additiv gefertigte Prüfkörper aus Polyamid 12 (Laser Sinter Verfahren) und Acrylnitril-Butadien-Styrol (Fused Layer Modeling Verfahren) wurden über 2000 Stunden künstlich bewittert und ihr Alterungsverhalten untersucht. Die Ergebnisse wurden anschließend mit denen von Prüfkörpern verglichen, welche auf dieselbe Weise künstlich bewittert, aber mittels konventionellem KunststoffSpritzguss hergestellt wurden.
Es wird ein Verfahren zur Charakterisierung der Beständigkeit und Langzeitstabilität von additiv gefertigten Kunststoff-Bauteilen vorgestellt. Dabei sollen die Prüfkörper über 2000 Stunden künstlich bewittert und währenddessen die Änderungen der Eigenschaften der Bauteile zerstörungsfrei untersucht werden.
From halogenated flame retardants to non-halogenated to nanocomposites, each milestone in flame retardancy research led to an increase in performance and safety. With the rise of ceramic precursors in flame retardants, a new field of applications in extreme fire scenarios has become accessible. Intumescent coatings combined with precursors for ceramics show a high temperature transition to a ceramic foam, which provides much better fire resistance than conventional coatings at temperatures beyond 1200°C. Even a protection at 2000 °C for several minutes can be achieved. Combining the expansion property of traditional intumescent coatings with a ceramification at high temperatures leads to high-performance coatings, whose unique properties may prove useful for emergency insulation systems for re-entry bodies in the aerospace industry or special fire protection applications.
In this study, the protection performance in extreme fire conditions, the development of the expansion and the following ceramic transition of a high-performance coating are investigated. To this end, a small scale high-performance burner setup was created. The coated (2.5/4 mm) steel plates (75 x 75 x 2 mm) were exposed to direct flame treatment of a propane-oxygen-burner controlled by two flow controllers. During the test, temperatures above of 1800 °C were reached and steel and flame temperature were recorded. Fire tests of different durations (1, 2.5, 5, 10 and 20 min) were performed. The residues of the different development stages were analysed with non-destructive µ-computed tomography and scanning electron microscopy. The 3D images of the computed tomography provide an insight into the developing cell structure and state of ceramification of the residues.