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Eingeladener Vortrag
- nein (659)
Methanotrophs in the rhizosphere of rice field ecosystems attenuate the emissions of CH4 into the atmosphere and thus play an important role for the global cycle of this greenhouse gas. Therefore, we measured the activity and composition of the methanotrophic community in the rhizosphere of rice microcosms. Methane oxidation was determined by measuring the CH4 flux in the presence and absence of difluoromethane as a specific inhibitor for methane oxidation. Methane oxidation started on day 24 and reached the maximum on day 32 after transplantation. The total methanotrophic community was analysed by terminal restriction fragment length polymorphism (T-RFLP) and cloning/sequencing of the pmoA gene, which encodes a subunit of particulate methane monooxygenase. The metabolically active methanotrophic community was analysed by stable isotope probing of microbial phospholipid fatty acids (PLFA-SIP) using 13C-labelled CH4 directly added to the rhizospheric region. Rhizospheric soil and root samples were collected after exposure to 13CH4 for 8 and 18 days. Both T-RFLP/cloning and PLFA-SIP approaches showed that type I and type II methanotrophic populations changed over time with respect to activity and population size in the rhizospheric soil and on the rice roots. However, type I methanotrophs were more active than type II methanotrophs at both time points indicating they were of particular importance in the rhizosphere. PLFA-SIP showed that the active methanotrophic populations exhibit a pronounced spatial and temporal variation in rice microcosms.
In recent years, femtosecond lasers matured from sensitive research setups to turnkey systems for an increasing number of applications. Now that running an ultra-short pulse laser system needs no longer a specialized scientist, safety issues become more crucial. Ultrashort laser pulses have extremely high peak powers and even scattered radiation may possess severe risks to the unprotected eye. Accordingly,
special protection schemes are necessary for these unique laser systems.
Plasma deposited ethylene/allylamine and styrene/allylamine copolymer films were prepared and analyzed using XPS, NEXAFS and ToF-SIMS. The relative partial flow rate of the each monomer was used as the variable deposition parameter, while the other deposition parameters were kept constant at optimized values for the retention of functional groups. The effect of the variation in the relative partial flow rates of co-monomers on various chemical aspects of the films like unsaturation, nitrogen retention and branching was investigated revealing several non-linear correlations. This observation is taken as an indication for chemical copolymerization processes during film deposition. An attempt is made to compare these non-linear correlations with approaches which have been developed for classic radical copolymerization processes. The aging behavior of these plasma copolymer films was also studied; the results indicated a stabilization against oxidation in comparison to the aging of allylamine plasma homopolymers.
Propane/air deflagrations and CTA measurements of turbulence inducing elements in closed pipes
(2008)
The current paper presents experimental investigations on several influence parameters of deflagrations in long closed pipes. The experiments were carried out with different propane/air mixtures, various length-to-diameter ratios (up to L/D=143, D=0.159 m) and miscellaneous initial pressures. Maximum values of explosion pressures and flame speeds were found at stoichiometric propane/air compositions. With increasing L/D, the explosion pressures decreased while higher flame speeds were determined. In addition, elevated initial pressures led to rising explosion pressures. Furthermore, it is well known that turbulence inducing elements in pipes, ducts or vessels enhance the heat and mass transfer during reactive flows. This may lead to a significant acceleration of ongoing gaseous reactions and could finally cause a deflagration to detonation transition (DDT) aligned with much higher pressures and flame speeds. Therefore, constant temperature anemometry (CTA) measurements were carried out to describe the influence of frequently used flange assemblies and baffles on the velocity and turbulence distributions of air flows in steel pipes similar to those in the explosion measurements. The experiments showed that in contrast to flange assemblies, baffles caused a significant increase of the turbulence intensity in pipe flows.
Influence of pressure and chromium content on corrosion reactions at 600 C in a CO2-H2O atmosphere
(2008)
Inorganic-organic nanocomposites are synthesised from polyethylene glycol with an average molar mass of 600 g/mol containing colloidal silica (silicic acid) and diphenyl methane diisocyanate as compact and foamed materials according to the European patent EP1414880. Beside the macroscopic properties, the pore structure and the structure of the polymer matrix of the silica/polyurethane nanocomposites with varying silica contents were studied.
Glass bricks are important transparent building materials. They are produced by joining two halves of glass pressings at 600700 °C. During this production process alkali oxides evaporate and are redeposited at the cooler inner front surfaces of the bricks. This surface layer reacts with H2O and CO2 from the residual brick atmosphere, leading to the formation of an alkali-rich silicate-hydrate layer of ≥50 nm thickness, which could be evidenced leading to a reduced nano-hardness of similar thickness, and from which NaHCO3 crystals can finally grow. Climate chamber experiments (repeated cooling between at -8 and -14 °C and reheating to 0 to 15 °C) resulted in reversible NaHCO3 crystallization and redissolution, presumably influenced by water evaporation or condensation and driven by the NaHCO3 supersaturation of the silicate-hydrate layer. Depending on the timetemperature schedule, different crystal morphologies became visible in this closed system, e.g. isolated spherical crystals, crystals arranged in chains and in double-chains, respectively, which can limit already the transmittance of the glass bricks. When a crack occurs or the brick is opened, the hygroscopic NaHCO3 crystals take up more H2O from the ambient, react irreversibly with the glass surface, finally leading to a total loss of transmittance.
Ultra-high performance concrete (UHPC) is characterised by compressive strengths above 150 MPa and an outstanding durability. These properties are achieved by optimisation of the mixture composition, the mixing procedure as well as the curing conditions of the concrete. Heat curing as well as the use of vacuum mixers may contribute to the high strength. The very high brittleness of UHPC can be compensated by the addition of steel or polymer fibres.
UHPC is produced using a very low water/cement ratio of 0.25 or smaller in combination with adding of polycarboxylate ether based superplasticisers. Furthermore, finest cements with contents of 500 kg/m³, defined selections of coarse and fine aggregates with a maximum grain size between 0.5 and 8 mm and fine pozzolanic (silica fume, fly ash) and inert additives (quartz filler) are used. In doing so, the aim is to obtain a very high packing density of the cement paste matrix and the aggregate/paste interface while a very homogeneous microstructure with a high calcium silicate hydrate (CSH) portion is formed.
In the case of optimal mixing and curing conditions, UHPC contains almost no pores and microcracks. Therefore, studies of porosity and pore structure are very important to characterise UHPC materials in connection with the mixture optimisation. Here, the experimental results for UHPC are presented in comparison with those of high-strength concrete (100 MPa) and normal-strength concrete (35 MPa), respectively.
Nanocomposites of bisphenol A polycarbonate with 2, 4, 6, and 15 wt% multiwall carbon nanotubes (MWNT) and their use in fire retardancy are investigated. Their thermal behavior and pyrolysis are characterized using thermogravimetry, differential scanning calorimeter, oscillatory shear rheology, and dynamic mechanical analysis. The flammability is addressed using LOI and UL 94; the fire behavior, with a cone calorimeter using different irradiation. With increasing MWNT content the storage modulus is increased (10-20%) and melt viscosity increases by several orders of magnitude, particularly for low shear rates. The melt flow, dripping, and deformation during fire are hindered, which influences UL 94 and cone calorimeter results. The peak heat release rate is reduced up to 40-50% due to an improved barrier for small amounts (2 wt%) of MWNT and for low irradiation, whereas the effect is reduced for increasing irradiation and nearly vanishes for increasing filling. Adjuvant but also deleterious mechanisms result in the complex dependency on the MWNT content. Significant flame retardancy effects are specific and limited to only some fire properties. This study allows the materials' potential for implementation in different fire scenarios and tests to be assessed and provides insight into active mechanisms.
A practical method for the quantification of
total purgeable organic sulfur (POS) in highly contaminated
groundwater is described. Volatile organic sulfur
compounds (VOSC) are purged from the water samples by
a stream of oxygen and combusted. The emerging sulfur
dioxide is absorbed in H2O2 and converted to sulfate which
is quantified by ion chromatography and reported as mass
sulfur equivalent. The overall limit of quantification is
0.03 mg l1. The content of POS is balanced with the total
VOSC determined by GC-AED after liquidliquid extraction.
Separate determination of the non-volatile organic
sulfur compounds by direct combustion of the water sample
and adsorption to charcoal yielded a mass balance of
the total sulfur content. Semi-quantitative GC-MS after
purge & trap accumulation revealed that the VOSC mixture
is composed of C1C4 alkyl sulfides. The implementation
of the developed methodology for the quantification of
VOSC as potential catalyst poison in a cleaning plant
for groundwater contaminated with volatile haloorganics
(VOX) is presented.
Die Koordinierungsstelle für Informationen zur Behälterabfertigung (KOBAF): Aufgaben und Erfahrungen
(2008)
The purpose of this work is modelling of the behaviour of a metal matrix (Ti-6242) that governs the nonlinear time-dependent response of the metal matrix composite (SiC/Ti-6242). For this purpose two different viscoplastic constitutive models are applied. First, it is the two-layer viscoplasticity model available in the finite element method (FEM)-based code ABAQUS. Second, it is the model of Chaboche implemented as a user material subroutine into another FEM-based code ANSYS and additionally into the package Mathematica. Parameters of both the models are obtained based on the available results of experimental tests carried out at different temperatures and strain rates. Utilisation of matrix models for simulation of the thermomechanical fatigue behaviour of the undamaged composite is discussed by a comparison with quasi-static tensile and high-temperature creep experimental tests.
A molecular modeling investigation of dilation effects induced by sorbed gas molecules in two glassy polymers is presented. As experimental reference, integral sorption of CO2 and CH4 was measured for polysulfone (PSU) and a polyimide (6FDA-TrMPD, PI4) at 308 K and a pressure of 10 bar. Simultaneously, the gas induced swelling effect was measured with a dilatometer based on a capacitive distance sensor recorded. The experimental evidence of the (on the observed time scale and concentration levels) elastic nature of the gas induced dilation is supported by the dilation and contraction behavior observed in molecular dynamics (MD) simulations of respective detailed atomistic packing models. These models were constructed in accordance with gas concentration levels obtained from the experimental sorption results. Quantitative deviations between simulated and measured dilations are discussed as a consequence of an anelastic response of the polymer matrix which is too fast to be resolved in the experiments whose kinetics is dominated by diffusional processes. In the simulation, the initial insertion of penetrant molecules into equilibrated packing models circumvents the slow diffusional process of the experiment and allows a reasonable representation of the dilation process as well as a closer investigation. Our simulation approach reveals a different behavior for PSU and PI4 on the corresponding time scale. Most likely, the different chain mobility of the two polymers is responsible for the respective response to the inserted amount of gas molecules which is discussed in terms of the different chain mobilities of the two polymers.
Werkstoffe
(2008)
Constitutive modelling of creep degradation due to rafting in single crystal Ni-base superalloys
(2008)
The aim of this research was to investigate the influence of nominal temperature errors on test results and to develop the nominal temperature tolerance for TMF-tests. This concept was confirmed with series of specially developed TMF-tests with defined temperature errors, performed on one test material (NIMONIC 90) in a temperature range of 400850 °C. These tests should show the influence of temperature errors on test results with an emphasis on lifetime in comparison with reference tests. It is shown that with a limited number of specimens and only one test material, it is possible to propose a reasonable general temperature tolerance for TMF-tests, valid for a wide range of materials and test conditions.
In the paper, a model typical for contact situations of automotive brakes is established based on the method of movable cellular automata. The processes taking place at local contacts in an automotive brake system are analysed. Based on microscopic and micro-analytical observations, the following contact situations were simulated: (i) a couple of ferritic steel against pearlitic steel, both covered by an oxide layer mixed with graphite nanoparticles and (ii) the same situation but without oxide layers. The results of calculated mean coefficients of friction of the oxide-on-oxide contact correspond well to expected values for a real braking system, whereas steel-on-steel contact are twice as high. This allows one to make some conclusions; for example, oxide formation will take place more quickly than friction layer elimination, and finally this is responsible for the stabilisation of the coefficient of friction.
Die BAM wurde vom Industriegaseverband (IGV) zur Beantwortung der Frage, ob eine positive Neubewertung von in Deutschland zugelassenen Bauarten im Sinne der europäischen Richtlinie über ortsbewegliche Druckgeräte (RL 1999/36/EG) möglich ist, mit der Erstellung eines Gutachtens beauftragt. Es soll insbesondere die systematische Entwicklung der Zulassungsanforderungen für diese Art von Druckgefäßen in Deutschland berücksichtigen.
Explizit sind im Rahmen des Auftrages zu betrachten: Bauarten von nahtlosen Gasflaschen aus Stahl mit einer Zugfestigkeit (Rm) von weniger als 1.100 MPa für Industriegase, deren Zulassung ohne jedwede Art von Auflagen oder Einschränkungen auf der Basis der Druckgasverordnung (vom 20. Juni 1968) und nachfolgend der Druckbehälterverordnung erteilt wurde.
Aufgrund der systematischen Betrachtung können Bauarten, deren Zulassungen unter irgendeiner Art von Betriebsauflagen oder sonstigen Einschränkung erteilt worden sind, nicht mit diesem Gutachten erfasst werden.
Dies Gutachten analysiert die Unterschiede in den Beschaffenheitsanforderungen nach Druckgas- bzw. Druckbehälterverordnung gegenüber dem geltenden RID/ADR 2007. Es soll den benannten Stellen nach Richtlinie 1999/36/EG (TPED) eine Vereinfachung ihrer Bewertungsarbeit zur Neubewertung von in Deutschland zugelassenen Gasflaschen ermöglichen.
Für die Anwendung dieses Gutachtens wird auf die sog. „Flaschen-Negativliste“ der EIGA
(Doc. 86/02 „Gas cylinders with restricted use in the EU“) und ggf. auf weitere zukünftig verfügbare Erkenntnisquellen verwiesen. Die dort beschriebenen Flaschen, u. a. aus Deutschland, werden unabhängig von der formalen Konformität mit der Richtlinie 1999/36/EG von den Mitgliedern der EIGA bzw. des IGV nicht den benannten Stellen zur wiederkehrenden Prüfung und damit auch nicht zur Neubewertung vorgestellt.
Dieses Gutachten ersetzt das Gutachten zur Neubewertung von vorhandenen und in Deutschland ohne Auflagen oder Einschränkungen zugelassenen Bauarten von nahtlosen Stahlflaschen, Gutachten der BAM vom 21. August 2001; Gutachter: Mair, G. W. und Müller, H.-J. und die gleichnamige Überarbeitung (Rev. 1) vom 20. Juli 2007.
Determining a pore structure’s mechanical and chemical data on lime rendering exposed
outdoors and including masonry in the laboratory, with regard to their behaviour on moisture
transport and weathering was the objective. In search of clues for a dose-response relation -
i.e. upon a connection between the emission rate of SO2 and NOx on one hand and the degree
of damage to mainly plaster having a lime component on the other - it has been of interest to
what extent their structural characteristics including pore space are modified and so
consequently also physico-technical properties and chemical composition. For determining
corresponding criteria, a widely diversified spectrum of test methods such as to obtain data
concerning porosity and moisture transport, mechanical behaviour, and chemistry as well is
available. A description of the manufacture of plate-shaped rendering specimens with lime
putty, industrially hydrated lime and dolomitic hydrate (the last two also having a cement
admixture) and also hydraulic lime as binding agents is included. First deposition velocity and
absorption rate for SO2 were determined in laboratory tests on these materials in dry and
moist states. After their exposure on outdoor racks at six locations in the Berlin region with
differing SO2 atmospheric contents over at least 5 years, the samples of course show timedependent
modifications of chemical and physical qualities which are especially reflected in
the form of profiles of structure, strength and concentration, e.g. for sulphate. Local climatic
differences, however, partly exert a greater influence on material than emissions. Similar
investigations were performed on samples of comparable composition exposed 4 and 17
years. But the real surprise is furnished by the renderings’ behaviour depending upon
orientation and upon height at a building. Since weathering behaviour and moisture transport
(absorption, storage, release) are directly interdependent, further criteria are necessary for a
critical assessment of a plasters’ pore structure. Starting from sands, plasters were
characterized. The structural parameters were lastly influenced by the respective contents of
sand, binder and mixing water. These results and those gained from bricks naturally find their
expression in masonry sections manufactured there from, and above all in their capillary and
evaporative behaviours, and also when applying different test liquids. Summary and cited
literature is given at the end of this report.
Die BAM untersucht regelmäßig Statistiken über Unfälle mit wassergefährdenden Stoffen sowie Datenerhebungen zu Gefahrgutunfällen. Ziel ist es, Hinweise zu Tendenzen und Lücken abzuleiten, die möglicherweise Anlass für weitere Aktivitäten und Maßnahmen geben, z. B. im rechtlichen Bereich oder in der Praxis. Regelmäßig beobachtete Unfallstatistiken über Jahre geben einen guten Überblick über das Unfallgeschehen in Deutschland. Dieser Bericht betrachtet das Jahr 2005 im Vergleich zu den Vorjahren.
Das ZfP Verfahren Impulsradar wird bei der Untersuchung des Schotterunterbaus von Schienen wegen unterstützend eingesetzt, um deren Struktur und Materialeigenschaften zu bestimmen. Eingesetzt werden kann dieses Verfahren sowohl für die Qualitätskontrolle beim Neubau von Schienenwegen als auch für die Bedarfsermittelung von Instandsetzungsarbeiten aufgrund von Schotterverunreinigungen. Kosten können eingespart werden durch eine Verlängerung der Reinigungszyklen und der Lebensdauer des Schotters. Ein Antennenarray für die Ermittlung der Ausbreitungsgeschwindigkeit wurde entwickelt und aufgebaut. Ergebnisse von Schottermessungen im Labor werden vorgestellt.
Das Tabellenwerk "Sicherheitstechnische Kenngrößen" ist in zwei Bänden herausgegeben worden. Während im ersten Band "Brennbare Flüssigkeiten und Gase" vorrangig die sicherheitstechnischen Kenngrößen reiner Stoffe im Gemisch mit Luft behandelt werden, stehen im Band 2 "Explosionsbereiche von Gasgemischen" die Eigenschaften von Gemischen aus Brenngas, Oxidator und Inertgas im Mittelpunkt. Damit soll erstmals dem Wunsch von Industrie und Behörden entsprochen werden, in einem Tabellenwerk komplette Datensätze zu den Explosionsbereichen von Stoffgemischen in gedruckter Form zur Verfügung zu stellen. Den Explosionsdiagrammen kann man die Zusammensetzung von explosionsfähigen Gemischen entnehmen. Sie sind damit Grundlage für Maßnahmen des primären Explosionsschutzes, z. B. für die Inertisierung.
Die Daten für die Explosionsdiagramme wurden überwiegend der Datenbank CHEMSAFE, Update 2008, entnommen. Diese Datenbank, die gemeinsam von der Gesellschaft für Chemische Technik und Biotechnologie e. V. (DECHEMA), der Bundesanstalt für Materialforschung und -prüfung (BAM) sowie der Physikalisch-Technischen Bundesanstalt (PTB) herausgegeben wird, enthält von Fachleuten bewertete sicherheitstechnische Kenngrößen. Die Kenngrößen brennbarer Flüssigkeiten werden traditionell von der PTB, die Kenngrößen brennbarer Gase und Stäube sowie die entsprechenden Explosionsdiagramme werden von der BAM bearbeitet, die auch den zweiten Band dieses Tabellenwerkes herausgibt.
Geophysikalische Verfahren zur Strukturerkundung und Schwachstellenanalyse von Flussdeichen – ein Handbuch ISBN: ISBN 978-3-981 07 - 4 Vor dem Hintergrund der seit Mitte der 90er Jahre in Deutschland gehäuft auftretenden Hochwasserereignisse (Rhein 1993/1995, Saale 1994, Oder 1997, Donau, Elbe und Mulde 2002/2005/2006) und den damit verbundenen umfangreichen Schäden, die ursächlich auf das Versagen von Hochwasserschutzanlagen (Deichbrüche) zurückzuführen waren, wird deutlich, dass die teilweise mehrere hundert Jahre alten Flussdeiche den Belastungen, bedingt durch ihre Bauart, die eingesetzten Baustoffe und die Bauhöhen, zum Teil nicht mehr gewachsen sind. Vor einer schutzzielabhängigen Entscheidung, ob eine Deichanlage künftigen Belastungen standhält oder ggf. zu ertüchtigen bzw. neu zu errichten ist, bedarf es als grundlegender Voraussetzung einer detaillierten Untersuchung des Tragsystems Bauwerk (Deich) und Untergrund. Ziel dieser Untersuchungen ist es, Schwachstellen des Tragsystems nach Umfang und Lage zu ermitteln, um daraus gezielt mögliche Sanierungsstrategien ableiten zu können. Für eine systematische Schwachstellenanalyse bieten sich in Kombination mit konventionellen geotechnischen Untersuchungsmethoden geophysikalische Messverfahren an. Einschlägige Normen und Richtlinien (DWA-M 507, DIN 19712) empfehlen zwar den Einsatz von geophysikalischen Verfahren, geben aber kaum praktische Hinweise für die Anwendung dieser Methoden. So erfolgt der Einsatz zerstörungsfreier geophysikalischer Verfahren zur Strukturerkundung an Deichen in Kombination mit geotechnischen Untersuchungen bisher regional differenziert und teilweise unsystematisch. Zudem werden von den für den Hochwasserschutz verantwortlichen Behörden zumeist keine oder sehr unterschiedliche Anforderungen an derartige Untersuchungen formuliert. Dadurch mangelt es den mit der Ausführung beauftragten Dienstleistern (Ingenieurbüros) zumeist an eindeutigen Vorgaben. Dies führt in der Regel dazu, dass die Qualität der aus diesen Untersuchungen abgeleiteten Aussagen höchst unterschiedlich ausfällt und vielfach nicht als optimal bezeichnet werden kann. Eine Hilfe zur Methoden- und Parameterwahl sowie eine systematische Bewertung der Eignung geophysikalischer Verfahren zur Strukturerkundung von Deichen gab es bisher nicht. Nach den Hochwasserereignissen des Jahres 2002 an Elbe und Mulde initiierte das Bundes- ministerium für Bildung und Forschung (BMBF) das Forschungsprogramm „Rimax“ (Risi- komanagement extremer Hochwasserereignisse). Mit diesem Programm werden zahlreiche Projekte auf ganz unterschiedlichen Gebieten der Hochwasserforschung gefördert [8]. Eines dieser Projekte ist das Verbundprojekt „Systematische Evaluierung existierender und innovativer Methoden zur Schwachstellenanalyse und Strukturerkundung von Deichen“ (DEISTRUKT). Ziel war es, möglichst viele erfolgversprechende oberflächen- und bohrlochgeophysikalische Methoden auf ihre Eignung für die Deichstrukturerkundung und Schwachstellenanalyse zu prüfen. Besondere Aufmerksamkeit wurde dabei auf die Umsetzung in geotechnisch verwertbare Ergebnisse gelegt. Mit dem Vorhaben DEISTRUKT sollte die Grundlage für einen effektiven Einsatz dieser Verfahren gelegt werden. Behörden und ausführende Ingenieurbüros sollen ein Werkzeug für die Entscheidungsfindung bei Konzeption, Ausschreibung, Durchführung und Bewertung geophysikalischer Messungen in Verbindung mit den geotechnischen Untersuchungsergebnissen erhalten. Basierend auf einer intensiven Recherche und praktischen Tests wurde eine systematische Evaluierung durchgeführt. Die Darstellung der Ergebnisse erfolgt als Richtlinie in diesem Handbuch. Berührungsfreie Methoden der Aerogeophysik oder der Fernerkundung waren nicht Gegenstand der Untersuchungen und bleiben daher im vorliegenden Handbuch unberücksichtigt. Das vorliegende Handbuch soll sowohl dem Praktiker aus Geophysik und Geotechnik als auch Behördenvertretern, die geophysikalische Leistungen zu beauftragen haben, als Hilfe zur Auswahl geeigneter Methoden und Messparameter dienen. Insoweit ist es auch als Ergänzung zu den Richtlinien DIN 19712, DIN 4020 und DWA-M 507 zu sehen. Sinngemäß können die in diesem Handbuch gegebenen Empfehlungen und Hinweise auch für die Erkundung von Trassen für den Deichneubau bzw. für Deichrückverlegungen, Seedeiche sowie für Flussseiten- bzw. Kanalseitendämme im Sinne von [36] gelten. Im Kapitel 2 werden insbesondere die Bauweise (Struktur) von Flussdeichen und die damit verbundenen Schwachstellen des Tragsystems sowie die daraus abgeleiteten Untersuchungsmethoden beschrieben. Kapitel 3 behandelt die Anforderungen und den Ablauf der geophysikalischen Deicherkundung und zeigt die Verknüpfungen zu den geotechnischen Untersuchungen auf. Eine kurze Beschreibung der wichtigsten bei der Deicherkundung eingesetzten geophysikalischen Methoden enthält Kapitel 4. In Kapitel 5 erfolgt die Bewertung der Eignung dieser Methoden. Schließlich werden im Anhang Hinweise zur Ausschreibung geophysikalischer Leistungen gegeben.
Um zu klären unter welchen Umständen eine Gefährdung von Spannstählen beim Kontakt mit verzinkten Bauteilen gegeben ist, wurden umfangreiche Laborversuche in alkalischen Lösungen und verschiedenen Betonen sowie Zeitstandversuche an Spannbetonprobekörpern durchgeführt. Dabei zeigte sich, dass Abstandsvariationen im Nahbereich nur einen geringen Einfluss auf die Polarisation des Stahles haben. Ein praxisrelevanter, unkritischer Abstand für den indirekten Kontakt des Spannstahls, z. B. über die Bewehrung, konnte daher nicht definiert werden. Aus den Versuchsreihen wurde deutlich, dass ein wesentlicher Einfluss durch das Flächenverhältnisses Stahl: Zink gegeben ist. Hier konnte eine praxisrelevante Grenze ermittelt werden. Danach führen Flächenverhältnisse größer 10 : 1 nicht zu einer Polarisation des Spannstahls in den Bereich der Wasserstoffentwicklung. Die im Labor gewonnen Ergebnisse konnten durch Untersuchungen zunächst an realen Betonfertigteilen, später auch an Spannbetonfertigteilen bei der Fa. Rekers verifiziert werden. Auf der Grundlage dieser Untersuchungen wurde für eine spezielle Spannbetonbinderausführung, bei der die Flächenverhältnisse in unkritischen Breichen lagen, für die Verwendung von verzinkten Einbau- teilen im indirekten Kontakt mit Spannstählen eine Zustimmung im Einzelfall gegeben. Während der Vorhabensbearbeitung wurde von den beteiligten Firmen eine weitere Problematik angesprochen. Dabei ging es um den Einsatz von verzinkten Einbauteilen in Spann- betonfertigteilen aus Stahlfaserbeton. Auch hier war die Frage, ob eine Gefährdung der Spannstähle durch indirekten Kontakt über die nicht verzinkten Stahlfasern möglich ist. Durch Untersuchungen an realen Fertigteilabschnitten bei den Firmen Rekers und Max Bögl konnte gezeigt werden, dass ein Kontakt über die Stahlfasern selbst über sehr kurze Entfernungen nicht vorliegt. Auf der Grundlage dieser Ergebnisse wurden für derartige Fertigteile beim Deutschen Institut für Bautechnik entsprechende bauaufsichtliche Zulassungen unter Verwendung verzinkter Einbauteile beantragt. Um eine sichere Gefährdungsabschätzung bei indirektem Kontakt für Flächenverhältnisse vornehmen zu können, bei denen eine Polarisation der Spannstähle in den Bereich der Wasserstoffentwicklung erfolgt, wurden Zeitstandversuchsreihen unter Wasserstoffbeladung durchgeführt. Diese führten an zugelassenen Spannstählen nicht zu Brüchen während der Versuchszeit. Die anschließend ermittelten mechanischen Kennwerte zeigten keine signifikanten Änderungen. Aus den Ergebnissen dieser Untersuchungen, die bezüglich der Bela- dungsmenge, der Beladungszeiten und der gewählten Vorspannung sehr konservativ ausgelegt wurden, ist ein indirekter Kontakt von Spannstählen zu verzinkten Einbauteilen als unkritisch zu bewerten. Eine entsprechende Änderung der Norm ist anzustreben. Aus grundsätzlichen Gründen der direkte Kontakt durch Einhaltung des in der DIN 1045-1 geforderten Mindestabstandes von 2 cm aber weiterhin sicher auszuschließen. Dies stellt für die Anwender aus praktischer Sicht kein Problem dar. Durch die in enger Zusammenarbeit mit der Industrie durchgeführten Forschungsarbeiten wird es den Anwendern ermöglicht, zukünftig verzinkte Einbauteile in Spannbetonfertigteilen einzusetzen. Teilweise konnte der Einsatz durch Zustimmungen im Einzelfall bzw. durch bauaufsichtliche Zulassungen bereits unmittelbar in der Praxis umgesetzt werden. Damit wurde das Ziel des Vorhabens erreicht.
The ability to reliably predict the amount and type of salts within a wet masonry is one of the most important and challenging subjects in the field of non-destructive combat of salt attack and preserving buildings and monuments of historical or archaeological value. To investigate the potential value of complex resistivity (CR) measurements for the early detection of salt and moisture related stone altering, a controlled salt type and concentration experiment series has been performed and a new procedure of an image based effective impedance modelling developed. Complex resistivity magnitude and phase measurements in the frequency range of 1 mHz to 100 Hz were acquired on a wide variety of wholly and partially brine saturated building stone samples. Deteriorating agents NaCl, Na2SO4, CaCl2 and MgSO4 were used. Since water and salt are not measured directly, the method is incapable of deducing possible building damages lacking a priori information. In the case of saturated materials, and provided thorough calibration data are available, a reliable estimate of salt concentration is possible from the measured resistivity magnitude. Additional indication on the dominant cation in the solution can be obtained from the measured resistivity phase, which is significantly higher the lower its valency. Furthermore, the measurements reported in this study give an important guide to the limitations of CR in obtaining pore surface area and pore throat estimates. For wet porous materials, in which polarization occurs due to complex surface conduction, the dominant pore throat and amount of specific surface affect its polarizability. Sandstones, sand-limestones and aerated concretes are more qualified observation objects (pore throats between 20 and 100 μm), whereas for bricks (pore sizes often < 5 μm) the method seems far less favorable. For those materials, which exhibit a Cole-Cole (C-C) type of relaxation, the phase peak is observed to decrease significantly with pore throat size and to occur at higher frequencies. The predicted power-law correlation between the C-C relaxation time and characteristic length scale (pore throat size for consolidated materials) is supported by the presented data. The experimental salinity study reveals how responsive polarization (in terms of imaginary conductivity) is to changing the ionic concentration or composition of the pore fluid. The properties of the electrical double layer and particularly its chemical composition are most likely the crucial controlling factors. The imaginary conductivity is observed to increase for most materials up to fluid salinities of about 1 S/m - a fact, that may be attributed to a mechanism of ion saturation within the electrical double layer; further ion supply seems to counteract this leading to ion-ion interactions, which decrease ionic mobility. CR measurements on partially saturated samples demonstrate the method’s sensitivity to water content. For most materials the imaginary conductivity component decreased significantly faster than the real component. Independent of the pore fluid and even though its salinity naturally increased during the evaporative drying procedure, the normalized saturation exponent of the quadrature component was about twice as high as the real one especially for clay-rich sandstones. The results revealed diverse behavior such as decreases and increases in relaxation time with saturation. In some cases a suppression of a distinctive relaxation curve at low saturations was observed. The results indicate, that contrary to conclusions from recent related studies, the correlation between a C-C relaxation time and hydraulic properties may be limited. In order to infer information on the charge distributions within the EDL, zeta-potentials and surface charge densities were obtained from electroacoustic measurements on particle suspension containing the same amounts and types of salt like used in the brine saturation CR study. The results add weight to the assumption that there is some universal positive relationship between zeta-potential and imaginary conductivity. A notable dependence of imaginary conductivity on diffuse layer surface charge was only observed in case of one sandstone (Cottaer), this being the material with the most abundant clay content. An image based effective impedance modelling approach revealed the fact that, even though it is not able to factor scale effects in, it is helpful to study general microstructural implications on CR responses. It was observed, that an increasing salt concentration (that creates a shrinking electrical double layer) reduces the peak phase and moves it towards higher frequency. The same effect would have an increasing fluid conductivity for a otherwise fixed microstructure. For some combinations of material and salt, however, in the experimental work the peak phase was observed to shift towards lower frequency: a phenomenon that could not be explained with the modelling. Therefore, it is assumed that chemical properties, like ion mobilities or other surface chemistry properties (ionexchange processes) must be regarded to conclusively explain surface conductivity mechanisms. Other experimental observations like the alteration of CR spectra at desaturation could likewise be modelled. If these models truly mimic the effective electrical properties, the results give new implications on the effective medium behavior. Concluding, the author values the complex resistivity method as a possible effective non-destructive testing (NDT) tool for a wide range of building stones. Depending on pore size and saturation important additional information can be obtained. In all cases, a priori information and calibration data are essential, that is, CR should not be treated as a stand-alone method. Further measurements are needed to develop a more complete model of the electrical double layer and its alteration with changing salinity and ion types.
The objective of this work is to demonstrate the practical application and sensitivity of ultrasound as a high frequency Dynamic Mechanical Analysis DMA technique for the characterisation of polymers. Conventional DMA techniques are used to determine thermo mechanical behaviour of polymers by typically employing dynamic shear or tensile loading modes at defined frequencies between 0.1 and 50 Hz. Sound waves may also be employed for DMA applications and depending on type of wave propagated, shear G´, G´´ and longitudinal L´, L´´ storage or loss modulus and tan (δ) may be determined from the measured acoustic parameters sound velocity and amplitude. The primary advantage of ultrasound DMA is that due to the compact sensor size it can easily be integrated into most manufacturing processes. To demonstrate the sensitivity of ultrasound to variations in the viscoelastic properties of polymers, the acoustic properties of a cured epoxy with an observed glass transition temperature of 86 °C (tan(δ) peak, 1Hz) were monitored in a temperature range from 20 to 200 °C and compared to conventional DMA results. The influence of measurement frequency, dispersion, hysteresis, reflections at material boundaries, and changes in material density on the measured sound velocity and amplitude were taken into account. To support conclusions a wide range of experimental data was evaluated using sensors operating in the frequency ranges 400 to 800 kHz and 3 to 6 MHz. The ultrasound results are compared to the tensile moduli E´, E´´ and tan(δ) measured using a conventional DMA technique operating at 0.1 to 33 Hz. Using different evaluation strategies such as the Williams Landel Ferry WLF equation it was possible to study the sensitivity of wave propagation to variations in the viscoelastic behaviour of a polymer. Taking advantage of this background knowledge, further experimental results are presented with the aim of demonstrating the sensitivity of this technique for cure monitoring applications and to the material transformations: gelation and vitrification. For this purpose an epoxy resin was cured at a range of constant temperatures whereby the curing reaction and the corresponding change in viscoelastic properties were monitored. Analysis techniques employed included ultrasound at 3 to 6 MHz, Differential Scanning Calorimeter DSC and Rheometry at 1 Hz. All results were summarised and presented graphically. Additionally an Arrhenius relationship was employed enabling direct comparison of results obtained from analysis techniques based on different working principles. Using this information, it was possible to demonstrate the practical application and the sensitivity of this technique to even small changes in viscoelastic properties of polymers.
In der vorliegenden Arbeit wurden Untersuchungen an Rückständen von thermisch abgebauten, flammgeschützten Polymeren vorgenommen, mit dem Ziel, die Struktur und den Phasenbestand der eingebauten Flammschutzmittel und der Polymere sowie deren Wechselwirkungen als Funktion der Temperatur und umgebenden Atmosphäre (N2 und Luft) zu charakterisieren. Ein wichtiges Werkzeug, das Informationen über den amorphen Zustand der Abbauprodukte und deren thermisch bedingte Phasenumwandlungen in andere amorphe oder kristalline Strukturen sowie Aussagen über die Nahordnungen der betrachteten Kernspinsorte liefert, stellt in dieser Arbeit der Einsatz der Festkörper-NMR-Spektroskopie dar. Hierbei sind neben Einzelimpuls-(SP), rotor-synchronisierte Spin-Echo- (RSE) und Kreuzpolarisationstechniken (CP) auch REDOR- (Rotational echo double resonance) und TRAPDOR- (Transfer of population in double resonance) Messungen zur Anwendung gekommen. Zusätzlich konnten aus den 11B- und 31P-NMR- Experimenten quantitative Aussagen über den relativen Borat- und Phosphor bzw. Phosphat-Anteil im festen Rückstand getroffen werden, wobei insbesondere für die 31P-Kerne eine quantitative Erfassung der kristallinen und amorphen Phosphatphasen durchgeführt wurde. Im ersten System wurden die Flammschutzmittel roter Phosphor (Prot) und Mg(OH)2 in HIPS kombiniert. Aus den Ergebnissen umfangreicher NMR-Experimente konnte abgeleitet werden, dass der größte Teil des eingesetzten Prot hauptsächlich in amorphen (Mg-Ortho-, -Di-, -Ketten und Ringphosphaten) und weniger in kristallinen Phosphatphasen verbleibt. Zudem konnte für den Parameter der Temperatur und aus der Verfügbarkeit von Sauerstoff (N2-Atmosphäre/Luft) einen deutlicher Einfluss auf den Abbauprozess und die Bildung der Phosphatphasen (kristallin/amorph) nachgewiesen werden. Aus dem Vergleich der Ergebnisse der Temperversuche mit den Ergebnissen der Verbrennungsversuche im Cone Calorimeter konnte ein anaerober Abbauweg bestätigt werden. In einem zweiten System wurden die thermischen Reaktionen zwischen den Flammschutzadditiven BDP und Zinkborat sowie ihren Einfluss auf den thermischen Abbau eines PC/ABS-Blends untersucht. Der thermisch belastete Rückstand wird unabhängig von der Atmosphäre von amorphen Phosphatgruppen dominiert. Dabei konnten die während der Temperprozesse gebildeten Verbindungen α-Zn3(PO4)2 und BPO4 als Folge einer Festphasenreaktion zwischen den eingesetzten Flammschutzadditiven identifiziert werden, wobei das α-Zn3(PO4)2/BPO4 Verhältnis als Indikator für einen aeroben bzw. anaeroben Abbauprozess dient, der für die Feuerrückstände eindeutig einen anaeroben Abbau liefert.
Die Suche nach halogenfreien Flammschutzmitteln für Polycarbonat / Acrylnitril- Butadien-Styrol-Copolymerisat (PC/ABS) führte zur Entwicklung von Triphenylphosphat (TPP), Resorcinol-bis(diphenylphosphat) (RDP) und Bisphenol-A- bis(diphenylphosphat) (BDP). Das unvollständige Wissen über die genauen Wirkungsmechanismen dieser Arylphosphate erschwert jedoch eine gezielte Optimierung der Systeme. In der vorliegenden Arbeit wurden die verschiedenen Flammschutzmechanismen von BDP in PC/ABS aufgeklärt. Ein Vergleich zwischen BDP mit RDP und TPP wurde gezogen und der Einfluss weiterer Additive wie Polytetrafluorethylen (PTFE), Böhmit, Zinkborat und Talk auf das Flammschutzverhalten von BDP herausgearbeitet. Dazu wurde das thermische Abbauverhalten mittels TG und TG-FTIR aufgeklärt. Die Entflammbarkeit wurde mit LOI- und UL 94-Tests bestimmt und das Brandverhalten anhand von Messungen im Cone Calorimeter bei unterschiedlichen Bestrahlungsstärken bewertet. Die Verbrennungsrückstände wurden mittels Festkörper-FTIR und Festkörper-NMR-Messungen charakterisiert. BDP wirkt in PC/ABS in der Gasphase durch Flammenvergiftung und in der festen Phase als Vernetzungsinitiator von PC. PTFE beeinflusst das Fließverhalten der Polymerschmelze und ermöglicht so die beste Klassifizierung im UL 94-Test von PC/ABS mit BDP. BDP ist thermisch stabiler als RDP und TPP und deshalb am aktivsten mit PC in der festen Phase. Böhmit verursacht durch eine H2O-Freisetzung Hydrolysereaktionen und wirkt somit leicht antagonistisch bezüglich der Festphasenaktivität von BDP. Zinkborat reagiert mit BDP zu alpha-Zinkphosphat und Borphosphat und unterdrückt so die Wirkung von BDP als Flammenvergifter und Vernetzungsinitiator. Die Zugabe von Talk bewirkt eine Verstärkung des Rückstandes, hat aber einen antagonistischen Effekt bezüglich der Gasphasenaktivität von BDP. Die Ergebnisse dieser Arbeit liefern ein detailliertes Verständnis der Flammschutzmechanismen von BDP und deren Abhängigkeit von der physikalischen und chemischen Umgebung. Mit diesem Wissen kann die Weiterentwicklung von BDP und anderen Arylphosphaten als Flammschutzmittel in PC/ABS gezielt optimiert werden.
Bone diseases, such as osteoporosis and osteoarthritis, are the second most prevalent health problem worldwide. In Germany approximately 5 millions people are affected by arthritis. Investigating biomineralization processes and bone molecular structure is of key importance for developing new drugs for preventing and healing bone diseases. Nuclear magnetic resonance (NMR) [2] was the primary technique used due to its advantages in characterising poorly ordered and disordered materials [3]. Compared to all the diffraction techniques that widely applied in structural investigations, the usefulness of NMR is independent of long range molecular order. This makes NMR an outstanding technique for studies of complex/amorphous materials. Conventional NMR experiments (single pulse, spin-echo, cross polarization (CP) [4], etc.) as well as their modifications and high-end techniques (2D HETCOR [5], REDOR [6], etc.) were used in this work. Combining the contributions from different techniques enhances the information content of the investigations and can increase the precision of the overall conclusions. Also XRD, TEM and FTIR were applied to different extent in order to get a general idea of nanocrystalline hydroxyapatite crystallite structure. Results: - A new approach named “Solid-state NMR spectroscopy using the lost I spin magnetization in polarization transfer experiments” [7] has been developed for measuring the transferred I spin magnetization from abundant nuclei, which is normally lost when detecting the S spin magnetization. - A detailed investigation of nanocrystalline hydroxyapatite core was made to prove that proton environment of the phosphates units and phosphorus environment of hydroxyl units are the same as in highly crystalline hydroxyapatite sample. - Using XRD it was found that the surface of the hydroxyapatite nanocrystals is not completely disordered, as it was suggested before, but resembles the hydroxyapatite structure with HPO4 2-(and some CO3 2-) groups instead of PO4 3- groups and water instead of OH- groups. - The organic-mineral interface of bone was studied in order to clarify which organic molecules are in the closest spatial proximity to the bone mineral phase and to investigate the influence of the organic matrix on the mineral formation. It was found that most probably these molecules are glycosaminoglycan rather than a protein.
The behavior of amorphous polymers in contact with gas atmospheres is still an area of both fundamental scientific and applied industrial research. Applications range from the use as barrier materials or protective coatings to active layers in sensor applications (‘artificial nose’) and the large field of gas separation membranes. In all these applications, high concentrations of small penetrant molecules may lead to a plasticization of the polymer. This effect is utilized in processing applications, where supercritical carbon dioxide (CO2) can be used as a plasticizer.4 The phenomenon of penetrant induced plasticization of glassy polymers is also observed in gas separation membranes.5 In the process of natural gas sweetening, the CO2 content of the gas mixture is reduced by separation of the CO2 from the fuel gas methane (CH4) to avoid corrosion of pipelines and to enhance the fuel value. Solubility and diffusivity of the respective gas determine the separation performance of the membrane material, i.e., the permselectivity. Both parameters are connected to the internal structure of the polymer and its free volume. To achieve high throughputs, e.g. to enhance costeffectiveness, it is desirable to increase the CO2 solubility and mobility. However, the observed plasticization and the associated relaxations in the polymer matrix change its structure and free volume, and thereby affect the selectivity of the material.6 In addition, other properties of the polymer are influenced, e.g. a reduction of glass transition temperature,7 yield stress8 and creep compliance9 have been observed. The origin and mechanism of these structural relaxations are poorly understood, as are the factors that influence solubility and mobility of the plasticizing penetrant. This lack of knowledge leads to a development of new or optimized materials, which is in part determined by trial and error. A deeper understanding of the phenomena that accompany gas sorption on the molecular level is therefore needed to control material properties and enable a targeted design of functional materials. Therefore, in this work, laboratory experiments are combined with detailed atomistic molecular simulations. Modelling. In detailed atomistic molecular modeling, the interactions of an assembly of atoms, e.g. a polymer molecule, are calculated according to known physical laws. Several established analysis methods allow an indirect determination of certain properties of such assemblies, others can even be directly calculated.10 However, CPU-power limits both the size and the simulation time of such assemblies. The size of the simulated packing models used in this work (_ 5000 atoms) ranges among the larger models found in the literature. Forcefield based Molecular Dynamics (MD) simulations are calculated in femtosecond steps, but reliable results are usually not obtained until a nanosecond of net simulation time has been performed. Millions of interactions need to be calculated, making the time effort for these ‘virtual experiments’ comparable to laboratory experiments. However, increasing speed of single processors and the possibility of parallel processing will further reduce the evaluation times for such simulations in the future. The goal of computer simulations is therefore to establish reliable methods to predict material properties. Properties of new materials could then be assessed by simulations first and only the most promising materials need to be synthesized for further testing, reducing the expense of trial and error. Although some methods already exist to predict polymer/gas properties from simulations, which show well agreeing results in ideal circumstances, they frequently fail when applied to less moderate conditions, e.g., high penetrant concentrations, long time scales, large penetrants etc. The aforementioned gas induced plasticization of polymers presents such a case where the gap of time scales between experiment and available simulation time amounts to several orders of magnitude. The time scale of simulations is limited to a few nanoseconds and therefore it is not possible to directly simulate relaxations of the glassy matrix as they are observed experimentally. Experiments, on the other hand, yield results of the real macroscopic system, and though molecular details cannot be observed individually, the accumulated effects permit the analysis through models on a statistical or phenomenological basis. It is the aim of this work to survey new approaches of a combined analysis of experimental and modelling results and to establish, where possible, a convergence of boundary conditions or, alternatively, an identification and isolation of comparable aspects of these seemingly incompatible methods of research. To this effect, phenomenological models are utilized as a means of interpretation of experimental data as well as to construe modelling results.
Most of the research on Hydrogen Assisted Cold Cracking (HACC) in high strength steel welds conducted over the last several decades has focused on single-pass welds, especially considering materials with yield strengths of about 700 MPa. Most of the weld procedure specifications, guidelines and standards targeted at HACC avoidance recommend preheating procedures. Application of such regulations to multi-pass welds of modern high strength structural steels with yield strengths of up to 1300 MPa is very limited. Actually there is no decent knowledge and only an empirical experience how to weld such joints in real components subjected to a respective shrinkage restraint. Consequently, an increasing number of failure cases, partly of catastrophic dimensions, have been reported in the present decade. The present contribution is targeted to close this knowledge gap by elucidating the principal effects of various inhomogeneous Hydrogen Removal Heat Treatment (HRHT) procedures on the HACC avoidance in high strength structural steel welds. As a typical representative in the upper yield strength range of this category of materials, a S 1100 QL weld using UNION X96 filler wire has been chosen. The results were achieved by indirectly coupled thermal, structural and hydrogen diffusion finite element modeling of HACC in single-layer and five-layer welded V-bevelled butt joints with plate thicknesses of 20.0 mm and 12.0 mm, respectively, at realistic restraint conditions and have been partly been confirmed by respective Instrumented Restraint Cracking (IRC) Tests. The numerical simulations are based on the interacting three local effects on HACC, i.e. local microstructure, local mechanical load and local hydrogen concentration. HACC has thus been regarded as a cracking phenomenon occurring, if the local mechanical load in a specific microstructure exceeds the limit for the respective hydrogen concentration. The various heat treatments proposed in literature, guidelines, specifications and standards, i.e. sole preheating, controlled interpass temperature, combined preheating and controlled interpass temperature application as well as postheating have been investigated with respect to their effects on the mechanical loading of the butt joints in terms of stresses and strains as well as on the hydrogen removal capabilities. As a particular item, a numerical model for Hydrogen Assisted Stress Corrosion Cracking (HASCC) has been developed further that it can be applied to HACC, in order to study, how such heat treatments influence crack initiation and propagation. By such modeling procedures as the most important results have been achieved: I. Further development and adaptation of a model for hydrogen assisted cracking to HACC and usage validation of the model for this material. II. Evaluation of the effects of pre- and postheating as well as interpass temperature on the stress-strain distribution in multi-pass welds. III. Clarification of the difference between single- and multi-pass welding with respect to stress-strain and hydrogen distribution as well as to HACC initiation and propagation. IV. Establishment of practical hydrogen removal heat treatment diagrams. V. Assessment of the effects of the amount of hydrogen picked up during welding on crack location and propagation.
Die Automobilindustrie sucht nach Lösungen, um Emissionen zu reduzieren, und nach Alternativen zu fossilen Brennstoffen, deren Verfügbarkeit über die nächsten Dekaden abnehmen wird. Aus diesem Grund gewinnen komprimiertes Erdgas sowie Wasserstoff als Energieträger zunehmend an Bedeutung. Um befriedigende Reichweiten mit komprimiertem Gas zu erreichen, wird ein Betriebsdruck von 20 MPa bis zu 70 MPa (nur Wasserstoff) angewandt. Die Hochdruckbehälter müssen die statischen und die dynamischen Innendruck- sowie die thermische Belastung ertragen. Gleichzeitig soll der Behälter eine sichere, aber auch eine wirtschaftliche Leichtbaustruktur sein, welche nur mit Hybridstrukturen (Metall- oder Polymerliner mit Kohlefaser- bzw. Glasfaserumwicklung an der Außenseite) realisiert werden kann. Wegen der Vielzahl an veränderlichen Produktionsparametern zeigen Composite- und speziell Hybridstrukturen große Streuungen in ihrem Strukturverhalten. Die dargestellten Versuchsdaten, welche an industriell gefertigten Composite-Hybriddruckbehältern gemessen wurden, zeigen dieses Problem. Um das Material im Sinne des Leichtbaus effizient zu nutzen und um gleichzeitig einen hohen Grad an Sicherheit mit reproduzierbarem Strukturverhalten zu realisieren, wird ein besseres Verständnis für das Verhalten des Hybriddesigns benötigt. Neben der Betrachtung der Imperfektionen im Composite und der benötigten Messmethoden für die Charakterisierung der Strukturparameter ist das Hauptanliegen der vorliegenden Arbeit die Simulation des Eigenspannungszustandes, resultierend aus der Produktion und dem Betrieb, sowie dessen Auswirkung. Um den Einfluss der verschiedenen Strukturparameter auf das Verhalten des Hochdruckbehälters mittels einer Sensitivitätsanalyse zu untersuchen, wurde ein geschlossen analytisches parametrisiertes Modell erstellt. Für die effektive Parametervariation sind hierfür analytische Modell von Vorteil im Vergleich zu FEM-Modellen. Das vorgestellte nichtlineare analytische Modell berücksichtigt den Einfluss des Eigenspannungszustandes des Autofrettageprozesses, in welchem der Liner kontrolliert durch Innendruck plastifiziert wird. Ebenso werden die Steifigkeitsdegradation infolge von Zwischenfaserbrüchen im Composite bei der Erstbeanspruchung (Degradationsmodell nach Puck), die thermischen Eigenspannungen infolge der verschiedenen Wärmeausdehnungskoeffizienten und der temperaturabhängige E-Modul des Harzsystems berücksichtigt. Die umfangreichen Versuchsdaten validieren die analytische Simulation zufriedenstellend. Die Simulation zeigt, dass der Schichtspannungszustand inklusiv des Eigenspannungszustandes stark von den Parametern Temperatur und Innendruck während der Produktion sowie im Betrieb abhängig sind. Diese Effekte sind bei einer erweiterten Spannungsanalyse der Behälterstruktur zu berücksichtigen.
Hochgeschwindigkeitsbeanspruchungen metallischer Bauteile sind bei einer Vielzahl ingenieurtechnischer Anwendungsbereiche, beispielsweise bei Crash- oder Falltests, bei Umform- oder Spanprozessen mit hohen Belastungsgeschwindigkeiten oder bei Aufprallproblemen von Komponenten schnell rotierender Bauteile auf das umgebende Gehäuse, z. B. bei Flugzeugturbinen, relevant. Dabei treten in dem beanspruchten Bauteil typischerweise Zonen mit großen, lokalisierten Deformationen auf, die auf die Entfestigung des Werkstoffs durch die Entwicklung von Schädigung und durch die Temperaturerhöhung infolge plastischer Dissipation zurückzuführen sind. Die Ausbildung von Scherbändern stellt dabei eine typische Form der Deformationslokalisierung dar. Die kontinuumsmechanische Modellierung solcher Vorgänge erfordert im Allgemeinen die Berücksichtigung einer Vielzahl von Faktoren und Effekten, wie beispielsweise dehnraten- abhängiges Materialverhalten, mit adiabatischer Erhitzung einhergehende thermische Entfestigung, Reibung und Kontakt sowie Schädigung. Darüber hinaus sind die genannten Effekte in dem Rahmen der Theorie großer Deformationen zu betrachten. Dehnratenabhängige ”lokale“ Modelle resultieren dabei nicht zwangsläufig in einer physikalisch sinnvollen Scherbandabbildung, d. h. in einer endlichen Scherbandbreite. Die innere Länge, die eine Begrenzung des Lokalisierungsvolumens darstellt, strebt für verschiedene im Rahmen der Simulation von Hochgeschwindigkeitsbelastungen eingesetzte, nichtlinear dehnratenabhängige Modelle, wie z.B. Potenzgesetz-Modelle oder dem Modell nach JOHNSON&COOK, mit infolge von Entfestigung abnehmender Spannung sowie zunehmender plastischer Dehnrate sehr stark gegen null. Dadurch tritt ein Verlust der lokalisierungsbegrenzenden Wirkung dieser ratenabhängigen Modelle ein, so dass insbesondere jedes, auf diesen Modellen aufbauende Finiten-Element Verfahren eine pathologische Netzabhängigkeit der Ergebnisse aufweist. ”Nicht-lokale“ Gradientenmodelle der Plastizität sind dazu geeignet, die beschriebenen Nachteile zu vermeiden. Die innere Länge dieser Modelle weist eine im Vergleich zu lokalen Modellen deutlich reduzierte Abhängigkeit von dem vorherrschenden Spannungszustand sowie der plastischen Dehnrate auf und wird darüber hinaus wesentlich durch den Wert des nichtlokalen Modellparameters beeinflusst. Die Größenordnung der inneren Länge bleibt dabei selbst für kleine Werte dieses Parameters auch mit Einsetzen von Lokalisierungseffekten zunächst erhalten. Infolge der numerischen Umsetzung nicht-lokaler Modelle mittels der Methode der Finiten- Elemente zeigt sich, dass im Gegensatz zu den auf lokalen Modellen basierenden Verfahren das Volumen der Lokalisierungszone bei stetiger Netzverfeinerung gegen einen endlichen Wert konvergiert. Damit gelingt es durch die Verwendung nicht-lokaler Modelle, die Ausbildung endlicher Scherbanddicken diskretisierungsunabhängig zu simulieren und im Rahmen der Kontinuumsmechanik eine sinnvolle Lösung des zugrunde liegenden physikalischen Problems zu gewährleisten.
Als eine neue Verfahrensvariante unter den Laserstrahl-Lichtbogen- Hybridschweißverfahren wird das Laserstrahl-Plasma-Hybridschweißen für die Werkstoffgruppe der austenitischen Stähle entwickelt. Neben der Entwicklung eines Hybridschweißkopfes, der für die Kopplung von Plasmalichtbogen und Laserstrahl in einer gemeinsamen Prozesszone ausgelegt ist, liegt ein Schwerpunkt auf der Ermittlung des Einflusses wichtiger Schweißparameter auf das Schweißergebnis und fertigungsrelevanter Kenngrößen wie der erzielbaren Spaltüberbrückbarkeit. Unter Einsatz eines pulverförmigen Zusatzwerkstoffes, der über den Plasmabrenner in die Prozesszone überführt wird, werden dazu Schweißnähte am Stumpfstoß sowie im Überlappstoß angefertigt. Aufbauend auf Ergebnissen aus Schweißversuchen wird ein Modell erstellt, das zu einem besseren Verständnis der Vorgänge im gemeinsamen Schmelzbad von Plasmalichtbogen- und Laserstrahlprozess beitragen soll, indem es die Auswirkung einzelner Schweißparameter auf das Schweißergebnis, wie zum Beispiel die Porenbildung, und somit indirekt die im Schmelzbad wirkenden Kräfte qualitativ einbezieht. Als Basis für die Erstellung des Modells dienen röntgenographische Aufnahmen, metallographische Untersuchungen als auch Hochgeschwindigkeits- aufnahmen des Hybridschweißprozesses. Weiterhin bilden metallurgische Aspekte bzw. die sich einstellenden Erstarrungsgefüge dieser Stähle einen weiteren Untersuchungsschwerpunkt in dieser Arbeit. Die im Schweißgut der Hybridnähte vorliegenden Erstarrungsmodi werden ermittelt und unterschiedliche prozessrelevante Einflüsse auf das Gefüge identifiziert. Darüber hinaus werden der Ferritgehalt sowie die Härte in den unterschiedlichen Zonen des Schweißnahtgefüges bestimmt. Mit der vorliegenden Arbeit liegen Ergebnisse vor, die zur effizienteren Gestaltung von Schweißprozessen im Blechdickenbereich von 5 mm bis 8 mm beitragen können und gleichzeitig auf werkstoffspezifische Besonderheiten der austenitischen Stähle beim Laserstrahl-Plasma-Hybridschweißen mit einem pulverförmigem Zusatzwerkstoff hinweisen.
The objective of the present thesis is to make advancements in understanding solidification crack formation in aluminum welds, by investigating in particular the aluminium 6060/4043 system. Alloy 6060 is typical of a family of Al-Mg-Si extrusion alloys, which are considered weldable only when using an appropriate filler alloy such as 4043 (Al-5Si). The effect of 4043 filler dilution (i.e. weld metal silicon content) on cracking sensitivity and solidification path of Alloy 6060 welds are investigated. Afterwards, cracking models are developed to propose mechanisms for solidification crack initiation and growth. Cracking Sensitivity. Building upon the concept that silicon improves weldability and that weldability can be defined by a critical strain rate, strain rate-composition combinations required for solidification crack formation in the Al- 6060/4043 system were determined using the newly developed Controlled Tensile Weldability (CTW) test utilizing local strain extensometer measurements. Results, presented in a critical strain rate – dilution map, show a crack – no crack boundary which reveals that higher local strain rates require higher 4043 filler dilution to avoid solidification cracking when arc welding Alloy 6060. Using the established crack - no crack boundary as a line of reference, additional parameters were examined and their influence on cracking characterized. These parameter influences have included studies of weld travel speed, weld pool contaminants (Fe, O, and H), and grain refiner additions (TiAl3 + Boron). Each parameter has been independently varied and its effect on cracking susceptibility quantified in terms of strain rate – composition combinations. Solidification Path. Solidification path of the Al-6060/4043 system was characterized using thermal analysis and phase identification. Increasing 4043 filler dilution from 0 to 16% in Alloy 6060 arc welds resulted in little effect on thermal arrests and microstructure, no effect on solidification range, refinement in grain size from 63 to 51 μm, centerline columnar grains disappearance, and decreased cooling rate from 113 to 89 °C/s. Moreover, in order to make direct comparison with literature, castings of controlled mixtures of alloys 6060 and 4043 were also investigated, thereby simulating weld metal composition under controlled cooling conditions. Castings showed a different trend than welds with small increases in silicon content (i.e. increase in 4043 filler dilution) resulting in huge effect on microstructure, no effect on liquidus temperature, drop in solidus temperature from 577°C to 509°C, increase in quantity of interdendritic constituent from 2% to 14%, and different phase formation. Binary β-Al5FeSi, Mg2Si, and Si phases are replaced with ternary β-Al5FeSi, π−Al8FeMg3Si6, and a low melting quaternary eutectic involving Mg2Si, π, and Si. Also, variation of the cooling conditions in castings revealed the existence of a critical cooling rate, above which the solidification path and microstructure undergo a major change. Cracking Model. Implementing the critical conditions for cracking into the Rappaz-Drezet-Gremaud (RDG) model revealed a pressure drop in the interdendritic liquid on the order of 10-1 atm, originating primarily from straining conditions. Since, according to literature, a minimum of 1,760 atm is required to fracture pure aluminum liquid (theoretical), this demonstrates that cavitation as a liquid fracture mechanism is not likely to occur, even when accounting for dissolved hydrogen gas. Instead, a porosity-based crack initiation model has been developed based upon pore stability criteria, assuming that gas pores expand from pre-existing nuclei. Crack initiation is taken to occur when stable pores form within the coherent dendrite region, critical to crack initiation being weld metal hydrogen content. Following initiation, a mass-balance approach developed by Braccini et al. (2000) revealed that crack growth is controlled by local strain rate conditions. Finally, a simplified strain partition model provides a link between critical strain rates measured across the weld and predicted at grain boundaries within the mushy zone. Although based on simplified assumptions, predicted and measured critical strain rate values are of the same order of magnitude. However, because of a longer mushy zone experienced at higher 4043 filler dilution related to a reduction in cooling rate, these models predict a lower weldability with increasing filler dilution, in contradiction with experimental observations. Combining the crack initiation and growth models suggests that hydrogen and strain rate, respectively, determine crack formation. An hypothetical hydrogen – strain rate map defines conceptually the conditions for cracking, suggesting better weldability at low weld metal hydrogen content. With the aid of the modified varestraint test (MVT) and a controlled hydrogen contamination system, results, presented in the form of ram speed – hydrogen map, revealed that hydrogen has little effect on crack growth, providing support to the proposed cracking models. However, a drop in weldability corresponding to the peak in weld metal hydrogen supersaturation suggests a different solidification cracking mechanism, where cavitation supports crack growth.
Jahresbericht 2007
(2008)