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Paper des Monats
- ja (1)
Chemiluminescence (CL) is a sensitive method of investigating the thermo-oxidative stability of polymers in the early stages of degradation. Therefore, CL measurements were applied to different automotive coatings to evaluate their degradation behavior during artificial weathering. In this work, CL measurements were carried out for different automotive coatings to follow their degradation behavior during artificial weathering. The CL emission depends on sample-specific parameters like stabilizer, matrix, or hardener; experimental parameters like the oxygen partial pressure; and exposure parameters like the duration of weathering. The potential of CL could be demonstrated by classifying materials into categories of good, medium, and low degradation performance at a much earlier stage of weathering exposure than in combination with the usual visual detection of weathering effects.
Thermally stimulated luminescence (TL) can be used to detect damage in the early stages of degradation after artificial weathering, and to analyze the efficiency of stabilizers used in automotive coatings. TL is particularly suitable for this task due to its inherent high sensitivity to structural, morphological, and chemical changes in macromolecular chains. In this work, TL measurements were carried out for different automotive coatings to follow their degradation progression during artificial weathering. The TL results demonstrate high sensitivity to parameters like stabilizers, matrices, hardeners, and weathering time, and provide an opportunity to monitor the early stages of damage in polymers, which therefore reduce the time required for further outdoor weathering tests.
Degradation effects of automotive coatings after weathering as detected by thermoluminescence
(2004)
Angesichts der spezifischen Bedeutung der Aushärtung von Phenolharzen für ihre Eigenschaften als Ingenieurwerkstoffe besteht großes Interesse an deren quantitativer Charakterisierung. Mittels DSC-Messungen unter hohem Druck (HP-DSC) kann die Vernetzungsreaktion der Phenolharzformmassen durch die Unterdrückung der Verdampfung niedermolekularer Substanzen ohne störende Überlagerungen verfolgt werden. Mittels verschiedener Vernetzungsgrade können die Einflussparameter der Aufheizrate und der Nachtemperung optimiert werden. Die Messergebnisse ermöglichen eine Modellierung der Reaktionskinetik mit dem Ziel einer verbesserten Prozessführung und Qualitätskontrolle in der industriellen Praxis.
Censorship of parts of written text was and is a common practice in totalitarian regimes. It is used to destroy information not approved by the political power. Recovering the censored text is of interest for historical studies of the text. This paper raises the question, whether a censored postcard from 1942 can be made legible by applying multispectral imaging in combination with laser cleaning. In the fields of art conservation (e.g. color measurements), investigation (e.g. Analysis of underdrawings in paintings), and historical document analysis, multispectral imaging techniques have been applied successfully to give visibility to information hidden to the human eye.
The basic principle of laser cleaning is to transfer laser pulse energy to a contamination layer by an absorption process that leads to heating and evaporation of the layer. Partial laser cleaning of postcards is possible; dirt on the surface can be removed and the obscured pictures and writings made visible again. We applied both techniques to the postcard. The text could not be restored since the original ink seems to have suffered severe chemical damage.
Optical fibers made of fused silica are a common method of transmitting high laser pulse energies. Failure of those fibers is a significant risk. The determination of laser-induced damage thresholds (LIDT) on fiber end facets according to ISO 21254 standard is needed. In the past, single pulse nanosecond laser experiments showed an improvement of LIDT with increasing fiber core diameter for 1064 nm wavelength and a constant beam diameter of 50 µm.
This paper pays particular attention to the influence of the laser beam diameter on damage resistance. All-silica fiber types (LEONI) with different core diameters (100–600 µm) were investigated using beam diameters in a range from 30 µm to 100 µm. For comparison experiments on fused silica preform material (Heraeus F300) were performed. On one hand, surface LIDT of fused silica preform material decreases significantly with increasing beam size. A model considering a random distribution of point defects explains the experimental data qualitatively. On the other hand, LIDT of fiber end facets stays constant. White light microscopy results suggest that the point defect density on fiber end facets is lower compared to the preform surface due to an excellent surface polish quality.
Mixtures of hexamethyldisiloxane (HMDSO) and oxygen have been used for deposition of SiO2-like layers by plasma polymerization under low-pressure conditions onto polyethylene and polystyrene used as basecoat. Water glass was cast onto these 0.5 µm plasma thick siloxane-like layers with a thickness of 5 to 40 µm. The adhesion of these bilayer systems and their flame resistance were tested.
The effect of different plasma parameters such as monomer/gas ratio, pressure and power input into the discharge on the deposition rate and the composition of the formed layers was studied. Characterization and chemical composition of the formed films were performed using infrared, X-ray photoelectron and solid state nuclear magnetic resonance spectroscopy.
Peel strengths of composites were measured and the locus of peel front propagation was detected. Thermal properties of composites were analyzed by thermo-gravimetric analysis. Finally, the fire-retardant properties of thick coated polymers were determined by exposure to flames and the behavior of coatings on the polymers during flaming was observed visually.
Laser cleaning of delicate biological composite materials such as ancient parchment manuscripts from the 15th and 16th century and printed paper from the 19th century is demonstrated with an ultraviolet excimer pulsed laser at 308 nm. Laser fluence levels must stay below the ablation and destruction threshold of the parchment or paper substrate, and have to surpass the threshold of the contaminant matter. Foreign layers to be removed must exhibit a higher optical density than the artifact substrates. Synthetic carbonaceous dirt modelled by water-soluble black crayons showed a characteristically weak featureless laser-induced plasma spectroscopy spectrum near the noise limit. It turned out that laser-induced plasma spectroscopy is of limited use in monitoring halting points (or etch-stops) because it relies on the destruction not only of the laterally inhomogenously distributed contaminant but also of pigment phases on a microscopically rough parchment substrate. Laser-induced fluorescence spectroscopy, however, promises to be a valuable non-destructive testing technique for etch-stop monitoring.
Cleaning of paper is a challenging task due to the fact that a contamination should be removed and a fragile organic original material has to be preserved. Pulsed laser cleaning of artificially soiled Whatman© filter paper samples serving as models for historical paper was performed. Different cleaning strategies employing 8-ns laser pulses at 532 nm wavelength were applied to clean paper avoiding undesired effects like discoloration (yellowing) and mechanical deterioration of the substrate. Multi shot experiments with low-energy pulses were compared with single pulse investigations utilizing high pulse energies achieving a constant energy load incident on the samples in both cases. The cleaning efficiency and possible yellowing effects were evaluated by means of a multi spectral imaging system. An extensive microscopic analysis of the cleaned parts of the samples provided insight into the remaining soiling on the surface and in the bulk of the paper material after laser treatment. As a reference, a hard and a soft eraser were used to clean the samples.
Thin plasma polymer films were deposited using the pulsed plasma mode. These plasma polymers should possess a more regular structure than those produced by the conventional continuous-wave (cw) mode, because of lower monomer fragmentation caused by the plasma pulses and the chemical chain propagation during the plasmaless (free!) periods. The thermoluminescence method was applied to functional groups carrying plasma polymer layers which are used in medical technology. Examples are formation of biocompatible, biosensoric and bioactive coatings or in metal polymer composites such as adhesion-promoting interlayers.
In addition to the use of the conventional X-ray Photoelectron Spectroscopy for thin film characterization, the new method of thermoluminescence was applied to characterize undesired defects and structural specifics produced in the polymer films by pp or cw plasma mode. The main areas of focus were oxygen-containing groups produced by post-plasma oxygen introduction via auto-oxidation, oxidation of implemented unsaturations and trapped radical sites known as typical irregular structures in plasma polymers.
Chemical-analytical investigation of fire products in intermediate storages of recycling materials
(2012)
Organic materials like paper, cardboard, textiles or plastics are mostly flammable. In intermediate storages for recycling products, these materials are stored in large amounts. If fire occurs in these stores, large emissions of smoke and other potentially harmful products are likely. In the present study, the gaseous products released from fires of such materials—for example, because of self-ignition—were investigated. Different fractions (paper/cardboard, textiles and plastics) were crushed at low temperatures (about 80 K) and subsequently allowed to smoulder at different temperatures using the German standard Deutsches Institut für Normung 53436. The gases produced were sampled and analysed using Fourier transform infrared spectroscopy. The chemical composition of these gases differed considerably depending on fuel type. For flammable materials without heteroatom, the gases consisted predominantly of toxic compounds like carbon monoxide and carbon dioxide. Smouldering of materials containing heteroatoms showed, in addition to carbon monoxide, carbon dioxide and water vapour, further toxic components containing the heteroatom. Materials containing chlorine produced hydrogen chloride, and materials containing nitrogen produced ammonia and hydrogen cyanide.
The chemical analysis of fire debris represents a crucial part in fire investigations to determine the cause of a fire. A headspace solid-phase microextraction (HS-SPME) procedure for the detection of ignitable liquids in fire debris using a fiber coated with a mixture of three different sorbent materials (Divinylbenzene/Carboxen/Polydimethylsiloxane, DVB/CAR/PDMS) is described. Gasoline and diesel fuel were spiked upon a preburnt matrix (wood charcoal), extracted and concentrated with HS-SPME and then analyzed with gas chromatography/mass spectrometry (GC/MS). The experimental conditions—extraction temperature, incubation and exposure time—were optimized. To assess the applicability of the method, fire debris samples were prepared in the smoke density chamber (SDC) and a controlled-atmosphere cone calorimeter. The developed methods were successfully applied to burnt particleboard and carpet samples. The results demonstrate that the procedure that has been developed here is suitable for detecting these ignitable liquids in highly burnt debris.
Um Stahlbauteile im Brandfall vor einer zu schnellen Erwärmung zu schützen, wird häufig auf reaktive Brandschutzsysteme (RBS) zurückgegriffen. Die Produkte eigenen sich besonders aufgrund der profilfolgenden Applikationsmöglichkeit und der vergleichsweise geringen Beschichtungsdicken. Bei einer Brandbeanspruchung schäumt das RBS auf und bildet eine thermische Schutzschicht um das Stahlprofil aus. Dadurch wird die Erwärmung des Stahls verlangsamt und der temperaturbedingte Festigkeitsverlust verzögert, wodurch sich die Feuerwiderstandsdauer des Stahlbauteils verbessert. Aus Brandversuchen ist bekannt, dass die Leistungsfähigkeit von RBS auf Stahlprofilen mit gekrümmter Oberfläche meist schlechter ausfällt als bei vergleichbaren Bauteilen mit ebener Oberfläche. Zum Einfluss der Oberflächenkrümmung auf die thermische Schutzwirkung von RBS werden in dem folgenden Beitrag sowohl theoretische Hintergründe als auch die Ergebnisse aus Brandversuchen an kleinformatigen Probekörpern vorgestellt. Die systematischen Untersuchungen zeigen, dass mit zunehmender Oberflächenkrümmung die Leistungsfähigkeit des RBS tendenziell abnimmt. Bei der Beurteilung der thermischen Schutzwirkung eines RBS sollte die Oberflächenkrümmung eines Bauteils berücksichtigt werden. Die alleinige Fokussierung auf den Profilfaktor eines Stahlprofils ist im Allgemeinen nicht ausreichend. Die Untersuchungen bilden die Grundlage für die Entwicklung von Screening-Tests zur Beurteilung der Eignung von RBS für gekrümmte Oberflächen, wodurch eine Vorauswahl von Produkten für diesen Einsatzzweck ermöglicht wird.
The inhalationof smoke gases is awell-established cause of poisoning and leads to the death of fire victims. Carbonmonoxide(CO) and Hydrogen cyanide (HCN) are two of the main noxious gases,whereby HCN is formed by an incomplete combustion of materials containing nitrogen. These materials may be natural materials, such as wool, silk and feathers or synthetic plastics, such as polyacrylonitrile (PAN), polyamide and polyurethane. These materials are very common in modern household furnishings; therefore, notonlyCObutalsoHCN can be produced during home fires. Up tonowonly a fewstudieshave been carried out on the generation of HCN as the fire proceeds, e. g. by Crewe et al. The data from such analyses are useful for forensic purposes. This enables the possibility to more accurately assess the events at the fire location, the Situation in which the fire victims are found as well as the cause of death. One way to analyze the gas composition of smoke is to perform bench scale fire tests, where various fire scenarios can be simulated on a smaller scale (e. g. using a smoke density chamber). The results from such experiments were compared with the results obtained in an enclosed room fire test.
Melamine and melamine resins are widely used as fire retardants for polymer materials used in pharmaceutical, plastic, textile, rubber, and construction industry. Melamine-based flame retardants act by blowing off intumescent layers, char formation, and emission of quenching ammonia gas and diluent molecular nitrogen. Special advantages are: low cost, low smoke density and toxicity, low corrosive activity, safe handling, and environmental friendliness. Methylated poly(melamine-co-formaldehyde) (mPMF) was used as thick (≥40 µm) fire-retardant coating for plasma pretreated polymers. A combined low-pressure plasma pretreatment consisting of oxygen plasma exposure followed by deposition of thin poly(allylamine) (ppAAm) and poly(allyl alcohol) (ppAAl) plasma polymers as adhesion promoters have improved the adhesion of thick mPMF coatings strongly. Chemical structure and composition of deposited polymer films were characterized by infrared-attenuated total reflectance and X-ray photoelectron spectroscopy (XPS). After peeling, the peeled layer surfaces were also investigated for identification of the locus of failure and their topography using optical microscopy and XPS. Often the adhesion promotion was so efficient that the peeling of coating was not possible. Thermal properties of plasma polymers and dip-coating films were analyzed by thermogravimetric analysis. Significant improvement of fire-retardant properties of coated polymers was confirmed by flame tests.
Laser-induced periodic surface structures (LIPSS, ripples) were generated on stainless steel (100Cr6) and titanium alloy (Ti6Al4V) surfaces upon irradiation with multiple femtosecond laser pulses (pulse duration 30 fs, central wavelength 790 nm). The experimental conditions (laser fluence, spatial spot overlap) were optimized in a sample-scanning geometry for the processing of large surface areas (5 × 5 mm²) covered homogeneously by the nanostructures. The irradiated surface regions were subjected to white light interference microscopy and scanning electron microscopy revealing spatial periods around 600 nm. The tribological performance of the nanostructured surface was characterized by reciprocal sliding against a ball of hardened steel in paraffin oil and in commercial engine oil as lubricants, followed by subsequent inspection of the wear tracks. For specific conditions, on the titanium alloy a significant reduction of the friction coefficient by a factor of more than two was observed on the laser-irradiated (LIPSS-covered) surface when compared to the non-irradiated one, indicating the potential benefit of laser surface structuring for tribological applications.
Cleaning of artificially soiled paper using nanosecond, picosecond and femtosecond laser pulses
(2010)
Cleaning of cultural assets, especially fragile
organic materials like paper, is a part of the conservation
process. Laser radiation as a non-contact tool offers
prospects for that purpose. For the studies presented here,
paper model samples were prepared using three different paper
types (pure cellulose, rag paper, and wood-pulp paper).
Pure cellulose serves as reference material. Rag and woodpulp
paper represent essential characteristics of the basic
materials of real-world artworks. The papers were mechanically
soiled employing pulverized charcoal. Pure and artificially soiled paper samples were treated with laser pulses of
28 fs (800 nm wavelength) and 8–12 ns (532 nm) duration in
a multi pulse approach. Additionally, the cellulose reference
material was processed with 30 ps (532 nm) laser pulses.
Damage and cleaning thresholds of pure and soiled paper
were determined for the different laser regimes. Laser working
ranges allowing for removal of contamination and avoiding
permanent modification to the substrate were found.
The specimens prior and after laser illumination were characterized
by light-optical microscopy (OM) and scanning
electron microscopy (SEM) as well as multi spectral imaging
analysis. The work extends previous nanosecond laser
cleaning investigations on paper into the ultra-short pulse
duration domain.
Reconstructing the course of a fire and performing chemical analysis of ignitable liquids in fire debris is an important tool to conduct fire investigations in suspected arson cases. Here, a total of five fire tests has been performed to investigate the effect of fire accelerants on the fire development of a room fire and to prove the capability of analytical methods. Different experimental scenarios have been realized (no accelerant, accelerant applied at different positions, and different amounts of fire accelerant). Each test room was equipped with an identical set of living room furnishing. The location and amount of the fire accelerant applied löschen varied in four of five tests. One experiment was carried out without fire accelerant. Fire quantities such as mass loss (of the entire room), gas temperatures (at several locations in the room), and heat release were determined during the experiments, and chemical-analytical studies were carried out. A headspace solid phase micro extraction procedure, using gas chromatography–mass spectrometry, was used to analyze fire debris samples to potentially detect ignitable liquids. Beside the analysis of fire debris samples, swipe soot samples were analyzed and the detectability of the fire accelerant used was demonstrated. Results show that it is possible to provide evidence of ignitable liquids in soot samples collected from walls. This allows an additional sampling strategy at potential crime scenes, besides taking fire debris samples.
Melamine resins were used as 50-µm-thick fire retardant coatings for polypropylene (PP). Preceding deposition, low-pressure plasma polymer films of allyl alcohol were coated onto PP to improve the adhesion between PP and melamine resin coatings. The efficiency of such fire retardant coatings was confirmed by flame tests. The plasma-deposited polymer and the dip-coated melamine resin films were characterized by Fourier transform infrared-attenuated total reflectance spectroscopy and X-ray photoelectron spectroscopy (XPS). The adhesion of coatings was measured using a 90° peel test with a doubled-faced adhesive tape. To detect the locus of failure, the peeled layer surfaces were inspected using optical microscopy and XPS. Thermal properties of PP thick melamine resin-coated films were analyzed by thermogravimetric analysis.
First developments of a new test to evaluate the fire behavior of photovoltaic modules on roofs
(2015)
A new test for photovoltaic (PV) modules exposed to an external fire source on roofs is proposed, and first results are presented. This is a simplification of the standards commonly in use for testing PV modules as roofing parts, roofing components or building components. Most of the tests required different fire scenarios and the use of burning brands such as wood cribs. In our study we proposed replacing wooden burning brands with a propane burner, the output of which is close to the one that can be observed in the burning of wooden cribs 500 g and 2 kg in size. The fire behavior was assessed by measuring smoke evolution, burning drips, flaming debris, and the time to burn-through of monocrystalline, polycrystalline and amorphous silicon panels. Two different configurations of the burner were tested, with the fire source on the top of the module or under the tilted module, respectively. The fire behavior of the modules was dependent on the burner output (16 to 46 kW), but also on the construction type of the panel (glass/glass or glass/plastic sheet) and on the position of the fire source (top or bottom). These preliminary tests for further development of the procedure yielded encouraging results for the evaluation of PV panels on roofs.
Laser-induced periodic surface structures (LIPSS, ripples) were processed on steel (X30CrMoN15-1) and titanium (Ti) surfaces by irradiation in air with linear polarized femtosecond laser pulses with a pulse duration of 30 fs at 790 nm wavelength. For the processing of large LIPSS covered surface areas (5 mm × 5 mm), the laser fluence and the spatial spot overlap were optimized in a sample-scanning geometry. The laser-processed surfaces were characterized by optical microscopy (OM), white light interference microscopy (WLIM) and scanning electron microscopy (SEM). Spatial LIPSS periods between 450 and 600 nm were determined. The nanostructured surface regions were tribologically tested under reciprocal sliding conditions against a 10-mm diameter ball of hardened 100Cr6 steel. Paraffin oil and engine oil were used as lubricants for 1000 sliding cycles at 1 Hz with a normal load of 1.0 N. The corresponding wear tracks were analyzed by OM and SEM. In particular cases, the laser-generated nanostructures endured the tribological treatment. Simultaneously, a significant reduction of the friction coefficient and the wear was observed in the laser-irradiated (LIPSS-covered) areas when compared to the non-irradiated surface. The experiments reveal the potential benefit of laser surface structuring for tribological applications.
The Federal Institute for Risk Assessment (BfR) DocCenter has received more and more reports of cases of carbon monoxide (CO) poisoning, some even with fatal outcomes after indoor use of charcoal grills. CO is odorless, colorless, non-irritant and does not produce any other warning effect perceptible to humans. The BfR and the Federal Institute for Materials Research and Testing (BAM) have completed a cooperative research project to investigate the toxic concentrations of CO that are reached when charcoal grills or open fires are used indoors.
Durch die Verwendung von Grillgeräten in geschlossenen Räumen, wie Gartenlauben, Wohnungen oder Garagen kam es in den vergangenen Jahren zu einer Vielzahl von Unfällen mit schweren Vergiftungen und Todesfällen. Seit 2008 scheint das Auftreten von Kohlenmonoxid (CO) Intoxikationen innerhalb Deutschland wieder zu zunehmen. Die Hauptursachen sind dabei der unsachgemäße Gebrauch von Holzkohlegrills, schlecht gewartete Gasthermen und Kamine. Zum Schutz der Bevölkerung ist deshalb eine Aufklärung über mögliche Gefahren wichtig.
Im Rahmen dieser Arbeit wurden diese Gefahren bewertet. Es wurden verschiedene Brandszenarien mit Grillgeräten, mit unterschiedlichen Grillkohlearten und –mengen in geschlossenen Räumen realisiert und die entsprechenden Konzentrations-Zeit-Verläufe ermittelt. Bei den Brandversuchen wurden zudem notwendige Eingabeparameter für numerische Simulationen ermittelt, um die Verwendung von Holzkohlegrills in geschlossenen Räumen zu simulieren. Die Auswirkungen für Menschen beim Grillen in geschlossenen Räumen wurden quantifiziert, indem die Eintrittszeitpunkte der Handlungsunfähigkeit und des Todes mittels Fractional Effective Dose (FED)-Konzept bestimmt wurden. Die Ergebnisse zeigen deutlich, dass eine frühzeitige Detektion der toxischen Gase zur Warnung von Personen dringend notwendig ist. In den durchgeführten Brandversuchen zeigte sich, dass die gebräuchlichen Rauchmelder auf Streulichtbasis keine rechtzeitige Warnung ermöglichen. Deshalb sind für solche Brandszenarien andere Branddetektoren erforderlich. Entsprechende Versuche mit CO-Brandmeldern zeigten, dass das freigesetzte CO beim Grillen in geschlossenen Räumen frühzeitig detektiert werden kann und Personen somit rechtzeitig gewarnt werden können.
Zur frühzeitigen Erkennung von Schwelbränden wurde weiterhin ein neuer Wasserstoffdetektor getestet. Die Entstehung von Wasserstoff in einer sehr frühen Brandphase kann zur frühzeitigen Erkennung von Schwelbränden genutzt werden. Bei ersten Schwelbrandexperimenten mit Holzproben konnte Wasserstoff in einer geschlossenen Kammer (0,5 m3) nachgewiesen werden, noch bevor es zu einer erhöhten CO-Emission kam. Die Ergebnisse der Schwelbrandversuche werden vorgestellt und die Verwendbarkeit von CO- und Wasserstoff-Detektoren erörtert und diskutiert.
Melamine and melamine resins are widely used as fire-retardants for polymer building materials. Cured melamine systems are used in heat-sensitive items, such as furniture and window frames and sills. In this work, differently cured methylated poly(melamine-co-formaldehyde) (cmPMF) resins were used as fire-retardant coverage for poly(styrene) (PS) and poly(ethylene) (PE) building materials. Such polymer layers should have several tenths of micrometers thickness to produce sufficient fire retardancy. These thick layers were produced by dip-coating. To promote sufficient adhesion of such thick coating to the polyolefin substrates, also in the case of high temperatures occurring at fire exposure, the polymer substrates were firstly coated with a few hundred nanometer thick adhesion-promoting plasma polymer layer. Such thin plasma polymer layers were deposited by low-pressure plasma polymerization of allyl alcohol (ppAAl). It was assumed that the hydroxyl groups of ppAAl interact with the melamine resin; therefore, ppAAl was well suited as adhesion promoter for thick melamine resin coatings. Chemical structure and composition of polymer films were investigated using infrared-attenuated total reflectance and X-ray photoelectron spectroscopy (XPS). Peel strengths of coatings were measured. After peeling, the peeled polymer surfaces were also investigated using optical microscopy and XPS the layers for identification of the locus of peel front propagation. Thermal properties were analyzed using TGA (thermo-gravimetric analyses). Finally, the fire-retardant properties of such thick coated polymers were evaluated by exposure to flames.
This study evaluates the efficacy of compressed air foam (CAF) in comparison to common fire extinguishing media. Newly developed mixed-material burning cribs were used as a normative fire load for extinguishing tests to accurately represent the significantly elevated utilization of synthetic materials in everyday life. A series of outdoor experiments was carried out to analyze the effectiveness of the fire extinguishing medium CAF using synthetical class-A foaming agents from two different manufacturers, and compared them to water and waterfoam solution as a function of the extinguishing distance. In a second series, performed inside a fire room, the efficiency of CAF-usage in indoor fires was evaluated. Moreover, the results of the indoor test series provided information about the composition of smoke gases based on the kind of extinguishing tactic used to suppress the fire. The results showed that under the tested conditions CAF suppressed fire more effectively than both water and water with foaming agents. CAF was able to wet areas hardly accessible to other extinguishing media, and due to its various simultaneously occurring effects and its compact jet with high kinetic energy, it cooled down temperatures more efficiently than water or water-foam solution.
In laser machining with ultrashort laser pulses unwanted X-ray radiation in the keV range can be generated when a critical laser intensity is exceeded. Even if the emitted X-ray dose per pulse is low, high laser repetition rates can lead to an accumulation of X-ray doses beyond exposure safety limits. For 925 fs pulse duration at a center wavelength of 1030 nm, the X-ray emission was investigated up to an intensity of 2.6 × 10^14 W/cm2. The experiments were performed in air with a thin disk laser at a repetition rate of 400 kHz. X-ray spectra and doses were measured for various planar target materials covering a wide range of the periodic table from aluminum to tungsten. Without radiation shielding, the measured radiation doses at this high repetition rate clearly exceed the regulatory limits. Estimations for an adequate radiation shielding are provided.
Reaktive Brandschutzsysteme können die Feuerwiderstandsdauer von Stahlbauteilen signifikant erhöhen. Im Brandfall schäumt das reaktive Brandschutzsystem auf und bildet um das Stahlbauteil eine thermische Schutzschicht aus. Dadurch wird die Erwärmung des Stahls verlangsamt und der temperaturbedingte Festigkeitsverlust verzögert. Reaktive Brandschutzsysteme werden überwiegend in drei Bereichen angewendet: Hochbau, Offshore bzw. maritimer Sektor sowie Tank- bzw. Behälterbau. Insbesondere bei Stahltanks und -behältern sind häufig einfach oder auch doppelt gekrümmte Bauteiloberflächen anzutreffen. Aufgrund des meist begrenzten seitlichen Expansionsvermögens von reaktiven Brandschutzsystemen kann es bei Bauteilen mit konvexer Oberflächenkrümmung zu einer Intensivierung der Rissbildung im Schaum kommen, wodurch sich häufig die thermische Schutzwirkung verschlechtert. Da zum Thema des Einflusses der Oberflächenkrümmung auf die Leistungsfähigkeit reaktiver Brandschutzsysteme bisher kaum Untersuchungen vorliegen, wurden exemplarisch zwei Tankböden mit zwei verschiedenen Trockenschichtdicken eines reaktiven Brandschutzsystems einer Brandprüfung unterzogen. Bei gleicher Trockenschichtdicke des reaktiven Brandschutzsystems zeigten die Tankböden eine wesentlich schnellere Erwärmung als ebene Stahlplatten mit vergleichbarem Profilfaktor. Die Brandprüfungen und die Ergebnisse zum Einfluss der Oberflächenkrümmung werden im Beitrag ausführlich vorgestellt und diskutiert.
A great number of Central Asian wall paintings, archeological materials, architectural fragments, and textiles, as well as painting fragments on silk and paper, make up the so called Turfan Collection at the Asian Art Museum in Berlin. The largest part of the collection comes from the Kucha region, a very important cultural center in the third to ninth centuries. Between 1902 and 1914, four German expeditions traveled along the northern Silk Road. During these expeditions, wall paintings were detached from their original settings in Buddhist cave complexes. This paper reports a technical study of a wall painting, existing in eight fragments, from the Buddhist cave no. 40 (Ritterhöhle). Its original painted surface is soot blackened and largely illegible. Grünwedel, leader of the first and third expeditions, described the almost complete destruction of the rediscovered temple complex and evidence of fire damage. The aim of this case study is to identify the materials used for the wall paintings. Furthermore, soot deposits as well as materials from conservation interventions were of interest. Non-invasive analyses were preferred but a limited number of samples were taken to provide more precise information on the painting technique. By employing optical and scanning electron microscopy, energy dispersive X-ray spectroscopy, micro X-ray fluorescence spectroscopy, X-ray diffraction analysis, and Raman spectroscopy, a layer sequence of earthen render, a ground layer made of gypsum, and a paint layer containing a variety of inorganic pigments were identified.
The adhesion of thick poly(allylamine)-polyphosphate layers (1 µm) deposited by the wet-chemical layer-by-layer technique (LbL) onto polyethylene or polystyrene (each 100 µm) was very low. To promote the adhesion of these LbL layers the polyolefin substrates were oxidized at the surface by short exposure to the oxygen plasma (2 or 5 s) and subsequently coated with an interlayer of plasma-deposited poly(allylamine) or poly(allyl alcohol) (100 nm). The plasma polymer interlayers have improved strongly the adhesion between polyolefin substrates and polyphosphate coatings. Such phosphate coatings are interesting for life sciences (nucleotide formation) but also for fire retardancy in combination with N-rich compounds such as melamine.
The intention was to prefer chemical and hydrogen bonds for adhesion promoting because of their high binding energy. Therefore, the introduced oxygen-containing groups at the polyolefin surface could interact with the OH or NH2 groups of the adhesion-promoting plasma polymer interlayer. These groups were also able to interact strongly with the poly(allylamine)-polyphosphate topcoating.
The coated polyolefins were investigated using Fourier Transform Infrared Spectroscopy in Attenuated Total Reflectance mode (FTIR-ATR), X-ray Photoelectron Spectroscopy (XPS), Thermo-Gravimetric Analyses (TGA) and Atomic Force Spectroscopy (AFM) and 90° peel test.
Sub-100-nm laser-induced periodic surface structures (LIPSS) were processed on bulk titanium (Ti) surfaces by femtosecond laser pulse irradiation in air (30 fs pulse duration, 790 nm wavelength). The laser peak fluence, the spatial spot overlap, and the number of overscans were optimized in a sample-scanning geometry in order to obtain large surface areas (5 mm × 5 mm) covered homogeneously by the LIPSS. The laser-processed regions were characterized by optical microscopy (OM), white light interference microscopy (WLIM) and scanning electron microscopy (SEM). The friction coefficient of the nanostructured surfaces was tested during 1000 cycles under reciprocal sliding conditions (1 Hz, 1.0 N normal load) against a 10-mm diameter ball of hardened 100Cr6 steel, both in paraffin oil and in engine oil used as lubricants. Subsequently, the corresponding wear tracks were qualified by OM, SEM, and energy dispersive X-ray analyses (EDX). The results of the tribological tests are discussed and compared to that obtained for near wavelength-sized fs-LIPSS, processed under somewhat different irradiation conditions. Some constraints for a beneficial effect of LIPSS on the tribological performance are provided.
The application of lightweight materials for tanks for transportation appears promising. Besides saving weight and therefore transportation costs, new complex geometries that depart from common cylindrical shapes of steel tanks can be manufactured. For transportation of dangerous goods, fire and explosion safety must be maintained to prevent accidents with serious consequences. In this work the fire behavior of lightweight tanks made from glass fiber reinforced plastics (GFRP) with complex geometries is investigated. Pretests on intermediate scale GFRP plates are conducted to identify suitable fire protection systems and surface treatments for composite tanks. The fire resistance is shown to be improved by addition of fire protective coatings and integrated layers. Finally, a complex rectangular GFRP tank with a holding capacity of 1100 liters is fire protected with an intumescent fire coating. The tank is filled up to 80 % with water and burned under an engulfing fully developed fire. It was shown that the intumescent layer could expand before the decomposition of the resin occurred. Furthermore, the adhesion between tank surface and coating was maintained. The structure could withstand a fire for more than 20 min.
Titanium nitride (TiN) was coated on different substrate materials, namely pure titanium (Ti), titanium alloy (Ti6Al4V) and steel (100Cr6), generating 2.5 μm thick TiN layers. Using femtosecond laser pulses (30 fs, 790 nm, 1 kHz pulse repetition rate), large surface areas (5 mm × 5 mm) of laser-induced periodic surface structures (LIPSS) with sub-wavelength periods ranging between 470 nm and 600 nm were generated and characterized by optical microscopy (OM), white light interference microscopy (WLIM) and scanning electron microscopy (SEM). In tribological tests, coefficients of friction (COF) of the nanostructured surfaces were determined under reciprocating sliding conditions (1 Hz, 1.0 N normal load) against a 10-mm diameter ball of hardened 100Cr6 steel during 1000 cycles using two different lubricants, namely paraffin oil and engine oil. It turned out that the substrate material, the laser fluence and the lubricant are crucial for the tribological performance. However, friction and wear could not be significantly reduced by LIPSS on TiN layers in comparison to unstructured TiN surfaces. Finally, the resulting wear tracks on the nanostructured surfaces were investigated with respect to their morphology (OM, SEM), depth (WLIM) and chemical composition by energy dispersive X-ray spectroscopy (EDX) and, on one hand, compared with each other, on the other hand, with non-structured TiN surfaces.
To save weight and resources lightweight tanks with complex geometries made of glass-fibre reinforced plastics (GFRP) are a promising innovation for the transportation of dangerous goods. To realise the use of polymer tanks for such applications, their fire safety must be guaranteed. This paper presents solutions to protect fibre-reinforced plastic tanks from fire. The fire resistance of six GFRP tanks with different fire protection systems was tested in an outdoor full-scale fire test facility according to the regulation stipulated in the ADR (European agreement concerning the national carriage of dangerous goods by road). All tanks feature a complex geometry and a holding capacity of 1100 litres. The fire protection systems are composed of specialised resins as well as two intumescent coatings. All systems had a protective impact. The best results were achieved by the epoxy based intumescent coating, which was able to prolong the time needed to reach 150 °C inside the tank by 20 min. The emergence of a temperature holding point inside the tank due to condensation effects was observed at temperatures around 100 °C.
Zur brandschutztechnischen Ertüchtigung von Stahlkonstruktionen werden reaktive Brandschutzsysteme aufgrund der geringen Beschichtungsdicken und der profilfolgenden Applikation in zunehmendem Maße eingesetzt. Da die für Zugstabsysteme eingesetzten Bauteile meist eine stark konvex gekrümmte Oberfläche aufweisen und der Anschlussbereich über eine vergleichsweise komplexe Geometrie verfügt, stellt dies besonders hohe Anforderungen an die Leistungsfähigkeit von reaktiven Brandschutzsystemen. Anhand von realmaßstäblichen Brandversuchen wurden das Aufschäumungs- und Rissverhalten, der Einfluss der Trockenschichtdicke, die Erwärmung der einzelnen Stahlbauteile sowie der Einfluss der Bauteilorientierung untersucht. Die Ergebnisse zeigen, dass eine Abnahme der Oberflächenkrümmung oder eine Erhöhung der Massenkonzentration der Stahlbauteile zu einer geringeren Aufheizrate des Stahls führt. Darüber hinaus ist festzustellen, dass die Leistungsfähigkeit des reaktiven Brandschutzsystems von der Bauteilorientierung der Zugstabsysteme beeinflusst wird. Die durchgeführten Brandversuche können zur Entwicklung geeigneter Prüfszenarien für die Beurteilung von reaktiven Brandschutzsystemen auf Zugstabsystemen und deren Anschlusskonstruktionen verwendet werden, wodurch eine Erweiterung des zulassungsbasierten Anwendungsbereichs ermöglicht wird.
The thermal degradation behavior of poly(vinyl chloride) (PVC) and poly(N-vinylpyrrolidone) (PVP) blends was investigated using potentiometric measurements of the released HCl gas during the degradation process, estimating the degree of discoloration of the degraded samples and measuring the thermal stability values (Ts) values. The influence of the PVP percentage in the blend and, moreover, the addition of commercial dibasic lead carbonate stabilizer to the blend on its thermal stability was studied. It was found that the dehydrochlorination rate of the blend was promoted by increasing the PVP concentration in the blend.
Various methods have been used for introducing fire retardant additives into polymers. Deposition of thick fire retardant coatings directly onto polymer substrates is an alternative technique. An important advantage of the coating technique is the preservation of the physical and chemical integrity of the polymer material. Moreover, the fire retardancy of the polymer materials can be achieved following their production. Suitable coating materials are inorganics, intumescent, char-forming, oxygendiluting, and cooling or radical quenching layers. The most important problem is to achieve sufficient coating thickness to withstand the direct attack of flame and to protect the polymer bulk from pyrolysis, otherwise blistering of coating, caused by emitted pyrolysis gases, is often observed. To avoid blistering of coating, the adhesion between polyolefin substrate and fire retardant coating has to be extraordinarily high.
In order to achieve such a high level of adhesion, the polymer surface has to be modified with adhesion-promoting functional groups. The deposition of thin plasma polymers as adhesion-promoting layers with NH2, OH or COOH groups has been the most suited method. These functional groups are able to form covalent bonds and other interactions between the fire-resistant coating and the plasma-modified polyolefin substrate. Additionally, the plasma polymer counteracts the strong mechanical stresses in the laminate on exposure to high temperatures by its flexibility.
Until the end of the 1980s many wooden artworks underwent surface treatment by liquid preservatives, e.g. Hylotox-59. DDT (dichlorodiphenyltrichloroethane) crystal structures are formed on the wooden surfaces by the "blooming" of chlorine compounds by time. In addition to an aesthetic disturbance, it is assumed that DDT represents a health risk. Therefore, the removal of DDT crystals from the surfaces is requested. Contaminated wood with natural biocide ageing, gilded and wood carved elements and wooden samples with paint layers were provided by the Schlossmuseum Sondershausen, Germany. Laser cleaning on selected surface areas on the objects was done by means of femtosecond and nanosecond laser pulses. For the same object, cleaning results using 30-fs laser pulses at 800 nm wavelength are compared to findings utilizing 10-ns laser pulses at 1064 nm wavelength. Before and after laser treatment, chlorine measurements at the same surface position were done by X-ray fluorescence analysis (XRF) as an indicator for the presence of DDT. In this way, pointwise chlorine depletion rates can be obtained for the different pulse duration regimes and wavelengths. Additionally, the object surfaces were examined using optical microscopy and multi spectral imaging analysis.
We analysed the hydrogen generation during the smouldering of polymeric materials, which are typically used in the household, in the Smoke Density Chamber coupled to a new developed hydrogen sensor to detect early stages of fires. The results of hydrogen generation were compared with the emission of carbon monoxide and smoke during the fire scenarios. Additionally, the results were compared with parameters used in traditional commercial detection systems. In this scenario, the hydrogen sensor showed encouraging results for the detection of fires in earlier phase compared to traditional detectors. Furthermore, we tested the new developed hydrogen sensor in a real room with different fire scenarios. We have also investigated interferences, e.g. steam and cigarette smoke. The hydrogen sensor could detect hydrogen generation in the earliest stage of fire, even before CO and smoke were developed in detectable amounts. Therefore, the hydrogen sensor can be applied for early fire detection in case of pyrolysis. The sensors are quite good for detecting pyrolysis gases. But when it comes to a fast ignition other techniques are more suitable for it. The sensors are best for combination with other techniques, such as smoke detectors.
Alkali-activated fly ashes have been proposed for various applications where resistance against high temperatures is required, yet several details regarding the response of these materials to heat-exposure need to be clarified. In the present study, heat-induced cracking in fly ash-based alkali-activated pastes and lightweight mortars was analyzed by in-situ acoustic emission (AE) detection during complete heating-cooling cycles (up to ∼1100 °C), augmented by thermogravimetry and ex-situ SEM and XRD analyses. The applicability of the lightweight mortars as passive fire protection coatings was assessed by recording temperature-time curves of mortar-coated steel plates. Cracking during heating was limited and associated exclusively with the dehydration of the materials in the temperature range ∼90–360 °C. However, samples heated to temperatures above ∼600 °C exhibited intense cracking on cooling. This was attributed to differential deformations caused by local sintering and partial melting at the glass transition temperature, and subsequent quenching on cooling.
This paper is intended to be the first study to discuss the fire suppressing performance of the four most common extinguishing media under the same reproducible conditions. The tests were performed in bench-scale and used standardized 5A wood cribs as well as a miniature extinguishing system with a liquid flow rate of 1.4 lmin−1. The tests results present a consistent overview of the fire suppression efficacies of water, water with a foaming agent, nozzle-aspirated foam and compressed air foam. Depending on their jet types, the cooling capabilities of the extinguishing media water and water with a foaming agent were compared to the cooling capability of a full Jet of wet, general and dry foams. The results show that compressed air foam suppressed fire most effectively under the test conditions. Because of the convoluted crib structure, water and water with foaming agents used from a distance are more effective in the form of a full jet rather than a spraying jet. At close range, spraying jets multiply their effectiveness. A slight difference can be observed in the cooling performance of extinguishing foams that use foaming agents from different manufacturers. The paper establishes a link between the foaming agent's cooling capability and its wetting power by relating the results of wood crib fire tests according to DIN EN 3–7 and findings from laboratory immersion tests compliant with DIN EN 1772.
In case of a vehicle fire, an installed LPG (liquefied petroleum gas) tank with a malfunctioning safety device poses severe hazards. To investigate the consequences in case of tank failure, we conducted 16 tests with toroidal shaped LPG vehicle tanks. Three tanks were used for a Hydraulic Burst Test under standard conditions. Another three tanks were equipped with a statutory safety device and were subjected to a gasoline pool fire. The safety device prevented tank failure, as intended. To generate a statistically valid dataset on tank failure, ten tanks without safety devices were exposed to a gasoline pool fire. Five tanks were filled to a level of 20 %; the re-maining five were filled to a level of 100 %. In order to gain information on the heating process, three tem-perature readings at the tank surface, and three nearby flame temperatures were recorded. At distances of l = (7; 9; 11) m to the tank, the overpressure of the shock wave induced by the tank failure and the unsteady tem-peratures were measured. All ten tanks failed within a time of t < 5 min in a BLEVE (boiling liquid expanding vapor explosion). Seven of these resulted directly in a catastrophic failure. The other three resulted in partial failure followed by catastrophic failure. A near field overpressure at a distance of l = 7 m of up to p = 0.27 bar was measured. All ten tests showed massive fragmentation of the tank mantle. In total, 50 fragments were found. These 50 fragments make-up 88.6 % of the original tank mass. Each fragment was georeferenced and weighed. Fragment throwing distances of l > 250 m occurred. For the tanks with a fill level of 20 %, the average number of fragments was twice as high as it was for the tanks that were filled completely.
Meta-analysis of heat release and smoke gas emission during thermal runaway of lithium-ion batteries
(2023)
Herein a meta-analysis of 76 experimental research papers from 2000 to 2021 is given about possible effects on the thermal runaway of lithium-ion battery cells. Data on the hazards of gas emissions and released heat are related to each other and differentiated by cell properties such as, cell geometry, cathode type or state of charge. Quantitative information on the total heat release in the range of 2.0–112.0 kJ Wh−1, the peak heat release rate in the range of 0.006–2.8 kW Wh−1and the smoke gas emission were extracted, normalized in terms of cell energy (Wh), combined in a data library and compared graphically. The total amount of gas emitted (3–48 mmol Wh−1) as well as the released amount of carbon monoxide (1–161 mg Wh−1) and hydrogen fluoride (2–197 mg Wh−1) were investigated as a function of the state of charge and cell geometry. The analysis reveals that the measured values are significantly influenced by the types of calorimeters and smoke gas analyzers used as well as by the type of thermal runaway trigger. This meta-analysis can serve as an important basis for any risk assessment of lithium-ion batteries.
Compressed natural gas (CNG) is a widely used automotive fuel in a variety of countries. In case of a vehicle fire where the safety device also malfunctions, a failure of the CNG automotive cylinder could occur. Such a cylinder failure is associated with severe hazards for the surrounding environment. Firstly, a comprehensive analysis is given below, summarizing various accidents involving CNG automotive cylinders and their consequences. In an extensive experimental program, 21 CNG automotive cylinders with no safety device were tested. Of the 21, burst tests were carried out on 5 Type III and 5 Type IV cylinders. Furthermore, fire tests with 8 Type III and 3 Type IV cylinders were conducted. Apart from cylinder pressure, inner temperature and cylinder mantle temperature, the periphery consequences, such as nearfield blast pressure and fragmentation are documented. The maximum measured overpressure due to a Type III cylinder failure was p = 0.41 bar. Each traceable fragment was georeferenced. All-in-all, fragment throw distances of d > 300 m could be observed. As one key result, it can be stated that the tested Type IV CNG cylinders showed less critical failure behavior then the Type III cylinders under fire impingement.
Commercial grade-1 titanium samples (Ti, 99.6%) were treated using three alternative methods, (i) femtosecond laser processing, (ii) thermal heat treatment, and (iii) electrochemical anodization, respectively, resulting in the formation of differently conditioned superficial titanium oxide layers. The laser processing (i) was carried out by a Ti:sapphire laser (pulse duration 30 fs, central wavelength 790 nm, pulse repetition rate 1 kHz) in a regime of generating laser-induced periodic surface structures (LIPSS). The experimental conditions (laser fluence, spatial spot overlap) were optimized in a sample-scanning setup for the processing of several square-millimeters large surface areas covered homogeneously by these nanostructures. The differently oxidized titanium surfaces were characterized by optical microscopy, micro Raman spectroscopy, variable angle spectroscopic ellipsometry, and instrumented indentation testing. The tribological performance was characterized in the regime of mixed friction by reciprocating sliding tests against a sphere of hardened steel in fully formulated engine oil as lubricant. The specific tribological performance of the differently treated surfaces is discussed with respect to possible physical and chemical mechanisms.
The thermo-oxidative degradation of a polymeric optical cable is investigated by chemiluminescence, The results are reliable and reproducible. Two distinct processes are reported marked by a peak and a plateau behavior versus the time, respectively. Both processes are ruled by thermally activated processes. Beside the dependencies of temperature and time, the influence of absorbed water is discussed. Chemiluminescence is proposed as a promising candidate for a suitable testing method assessing the thermo-oxidative stability of plastic optical fibers and cables. it requires not more than a simple one-day testing procedure and has the advantage that it can be carried out even within the lo cv temperature ranges of the cables' intended use.
The excitation energy transfer (EET) of a bichromophoric cross-shaped molecule was investigated by stationary polarized fluorescence spectroscopy in the solid state. For this purpose 2,2[prime],7,7[prime]-tetrakis(biphenyl-4-yl)-9,9[prime]-spirobifluorene was embedded in a polymeric bisphenol-A-polycarbonate (PC) matrix. The dependence of the fluorescence on concentration and wavelength was determined. The role of the intermolecular and intramolecular EET is dealt with separately and discussed by means of the degree of polarization. The intermolecular excitation energy transfer is described in terms of a Förster transfer mechanism. The intramolecular transfer is prevented for the zero-point vibrational levels by the molecular cross-shaped structure, but is found for a wide range of wavelength, presumably based on vibrationally excited states.
To ensure fire safety, polymers are filled with flame retardants and smoke suppressants. To meet the highest requirements, it is essential to understand the decomposition of those polymeric materials. This study reveals interactions between polymer, smoke suppressants, and flame retardants, and discusses their impact on the materials’ flame retardancy, smoke emission, smoke toxicity, and particle emission in conventional loadings to provide deeper general understanding. Low melting oxide glass, melem, spherical silica, sepiolite, melamine polyphosphate, and boehmite in an aluminum diethylphosphinate flame-retarded polyamide 6.6 were investigated. All smoke suppressants improve the protective layer and act as an adjuvant. Silica and melem performed best under forced flaming conditions. Spherical silica reduces the peak of heat release rate by 39% and the total heat evolved by 14%, whereas 10 wt% melem lowers the total smoke production by 41%. Melem alters the mode of action of aluminum diethylphosphinate from gas to more condensed phase activity. This change reduces flame inhibition and hence smoke toxicity, but further improves the protective layer due to charring reactions in the decomposition mechanism. In addition, the sizes of the smoke particles decrease because of the prolonged time in the pyrolytic zone. This study highlights that interactions between polymer, flame retardants, and smoke suppressants can significantly determine the smoking and burning behavior.
The passive fire protection of steel structures and other load-bearing components will continue to gain importance in future years. In the present contribution, novel intumescent aluminosilicate (geopolymer-bound) composites are proposed as fire-protective coatings on steel. Steel plates coated with these materials were exposed to the standard temperature-time curve as defined in ISO 834 – 1:1999. The coatings partially foamed during curing and expanded further during thermal exposure, demonstrating their intumescent characteristic.Thermogravimetryandoscillatory rheometry determined that the intumescent behavior is attributed to a transition to a viscous state (loss factor > 1) in the temperature range of major water release, differing from conventional geopolymers. XRD and SEM images showed that the coatings had characteristics of ceramic or glass-ceramic foams after fire resistance testing, suggesting superior performance under challenging conditions. The thickness of the coatings influenced their foaming and intumescent behavior and thus the time for the coated steel plates to reach 500 °C. A number of additives were also studied with the best performance obtained from samples containing sodium tetraborate.Acoating of just 6mmwas able to delay the time it takes for a steel substrate to reach 500 °C to more than 30 minutes.