Ingenieurwissenschaften und zugeordnete Tätigkeiten
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Organisationseinheit der BAM
- 9 Komponentensicherheit (175)
- 6 Materialchemie (158)
- 7 Bauwerkssicherheit (139)
- 8 Zerstörungsfreie Prüfung (133)
- 5 Werkstofftechnik (117)
- 9.3 Schweißtechnische Fertigungsverfahren (99)
- 7.6 Korrosion und Korrosionsschutz (89)
- 8.5 Röntgenbildgebung (66)
- 9.4 Integrität von Schweißverbindungen (54)
- 6.6 Physik und chemische Analytik der Polymere (49)
Eingeladener Vortrag
- nein (443)
Die neue Crosslinking-Methode ist hilfreich, um Immunglobuline des Isotyps G ortspezifisch an ihrer Bindungsstelle mit Protein A oder G zu konjugieren. Die Kopplungen von Protein A und G konnten erfolgreich an Maus- und Human-IgG durchgeführt, sowie die Bedingungen untersucht und optimiert werden. Die Aktivierung von Protein G mit Glutaraldehyd erfolgt am besten bei pH 8 und die anschließende Kopplung mit Maus-IgG1 bei einem pH-Wert von 6. Jedoch wurden mit SIAB und Sulfo-SIAB als Crosslinker im Vergleich zu Glutaraldehyd noch höhere Signale erhalten. Für die Kopplung von SIAB sind 40% DMSO im Reaktionspuffer günstig, währenddessen Sulfo-SIAB gut wasserlöslich ist daher keine Lösungsvermittler benötigt. Es ergab sich ein optimaler pH-Wert von 7,4 um Protein A mit SIAB zu aktivieren und den gleichen pH-Wert um die Kopplung mit Maus-IgG1 durchzuführen. Für die Kopplung von Protein G mit Maus-IgG1 hingegen zeigten die Experimente, dass ein leicht saurer pH-Wert bei pH 6 für den IgG-Kopplungsschritt am günstigsten ist. Während die Inkubationszeit von Maus-IgG1 mit Protein G bei 16 h liegt, muss mit Protein A bis zu 40 h inkubiert werden, um das Kopplungsmaximum zu erreichen. Des Weiteren wurde das Crosslinking von Human-IgG (Herceptin) mit SIAB untersucht. Dabei zeigte sich, wie in der Abbildung 47 zu sehen ist, dass Protein A und G vergleichbar gut an Human-IgG zu koppeln sind. Für das Crosslinking von Protein G mit Maus-IgG1 ist dagegen ein deutlich besserer Umsatz im Vergleich zu Protein A zu erkennen (Abbildung 48). Heterobifunktionale Linker können mit der reaktiveren Gruppe die erste Bindung eingehen, um erst nach Zugabe eines weiteren Reagenzes die zweite Bindung auszubilden und zudem intramolekulare Reaktionen möglichst zu vermeiden.
Im Vergleich zu anderen Proteinen ist die Identifizierung von Antikörpern anhand ihrer Sequenz zum Beispiel mittels "peptide mass fingerprinting" schwierig. Da die Sequenzinformation eines Antikörpers aufgrund der hypersomatischen Mutation während der Affinitätsreifung nicht im Genom eines Organismus gespeichert ist, kann die Aminosäuresequenz nicht auf einfachem Weg der DNA-Sequenzierung gewonnen werden. Das ist nur in seltenen Fällen möglich, wenn dem Endanwender der Zellklon der Antikörper-produzierenden Zelle zugänglich ist. Eine Sequenzierung auf Protein-Ebene ist sehr aufwändig und teuer und wird daher fast nie für die Charakterisierung von analytischen Antikörpern verwendet. Der Mangel an Validierung dieser analytischen Antikörper, die bei Experimenten verwendeten werden, löst aber eine Reihe Probleme aus, die die Wiederholbarkeit dieser Experimente schwierig und in einigen Fällen unmöglich macht. Das sorgt jährlich für verschwendete Forschungsgelder in Milliardenhöhe und hindert den wissenschaftlichen Fortschritt.
Ziel der vorliegenden Arbeit war die Entwicklung einer einfachen und schnellen Methode, die es trotzdem ermöglicht, die Identifikation von Antikörpern sicherzustellen. Dazu wurde eine Methode basierend auf dem "peptide mass fingerprinting" gewählt. Das Problem der unbekannten Aminosäuresequenz der Antikörper wurde gelöst, indem lediglich die Peptidmuster der entstehenden Fingerprint-Spektren zur Identifikation herangezogen wurden. MALDI wurde dabei als Ionisationsmethode für die Massenspektrometrie gewählt, da die resultierenden Spektren im Gegensatz zu ESI-MS einfach auszuwerten sind. Auch kann auf eine vorige Trennung der Peptide mittels LC verzichtet werden, was zusätzlich Analysenzeit spart. Für die Proteinspaltung wurde eine simple saure Hydrolyse mittels Ameisensäure gewählt. Im Vergleich zum herkömmlichen Trypsin-Verdau konnten auf zeitraubende Arbeitsschritte wie Denaturierung, Reduktion und Alkylierung der Antikörper verzichtet werden. Die Hydrolyse mittels Ameisensäure wurde bisher nur auf kleine und mittelgroße Proteine angewendet, sodass im ersten Teil dieser Arbeit mehrere Schritte optimiert wurden bevor zufriedenstellende Fingerprint-Spektren von Antikörpern erhalten wurden.
Additive Manufacturing (AM) in terms of laser powder-bed fusion (L-PBF) offers new prospects regarding the design of parts and enables therefore the production of lattice structures. These lattice structures shall be implemented in various industrial applications (e.g. gas turbines) for reasons of material savings or cooling
channels. However, internal defects, residual stress, and structural deviations from the nominal geometry are unavoidable.
In this work, the structural integrity of lattice structures manufactured by means of L-PBF was non-destructively investigated on a multiscale approach.
A workflow for quantitative 3D powder analysis in terms of particle size, particle shape, particle porosity, inter-particle distance and packing density was established.
Synchrotron computed tomography (CT) was used to correlate the packing
density with the particle size and particle shape. It was also observed that at least about 50% of the powder porosity was released during production of the struts.
Struts are the component of lattice structures and were investigated by means of laboratory CT. The focus was on the influence of the build angle on part porosity and surface quality. The surface topography analysis was advanced by the quantitative characterisation of re-entrant surface features. This characterisation was compared with conventional surface parameters showing their complementary
information, but also the need for AM specific surface parameters.
The mechanical behaviour of the lattice structure was investigated with in-situ CT under compression and successive digital volume correlation (DVC). The Deformation was found to be knot-dominated, and therefore the lattice folds unit cell layer wise.
The residual stress was determined experimentally for the first time in such lattice structures. Neutron diffraction was used for the non-destructive 3D stress investigation. The principal stress directions and values were determined in dependence of the number of measured directions. While a significant uni-axial stress state was found in the strut, a more hydrostatic stress state was found in the knot. In both cases, strut and knot, seven directions were at least needed to
find reliable principal stress directions.
Polyethylen hoher Dichte (PE-HD) wird als Werkstoff für Rohre und Behälter für den Transport und zur Lagerung von Gefahrgütern verwendet. Für die Beurteilung und technische Freigabe dieser Materialien ist insbesondere das Verständnis des Schädigungsmechanismus des langsamen, umgebungsbedingten Spannungsrisses (engl.: „environmental stress cracking“, ESC) essentiell. ESC tritt bei relativ geringen auf einen Werkstoff einwirkenden mechanischen Spannungen auf. An lokalen Fehlstellen (z.B. Defekte, Inhomogenitäten, Kerben) beginnend wächst ein Riss langsam durch das Material und führt nach gewisser Zeit zu einem charakteristischen, pseudo-spröden Bruch. Dabei wird das Risswachstum durch äußere Medieneinwirkung zusätzlich entscheidend beeinflusst. Dieses langsame Risswachstum wird als Hauptursache für das plötzliche und unerwartete Versagen von Polymerwerkstoffen angesehen.
Eine etablierte Prüfmethode zur Bewertung des Materialverhaltens gegenüber dieses Schädigungsmechanismus ist der Full-Notch Creep Test (FNCT), der für PE-HD Behältermaterialien üblicherweise unter Verwendung von wässrigen Netzmittellösungen (Arkopal N 100) durchgeführt wird. Die aus dem FNCT erhaltene Standzeit dient dabei als Bewertungskriterium für verschiedene PE-HD-Werkstoffe. In einer Studie wurden neben einer typischen Arkopal-N-100-Netzmittellösung praktisch relevante, organische Flüssigkeiten wie Biodiesel und Diesel als Testmedien verwendet, um deren Einfluss auf das ESC-Verhalten von PE-HD-Behältermaterialien zu charakterisieren. Neben der klassischen Standzeit-Auswertung erfolgte eine erweiterte Bruchflächenanalyse mittels Licht- (LM), Laserscanning- (LSM) und Rasterelektronenmikroskopie (REM). Insbesondere die LSM erlaubt eine schnelle und einfache Unterscheidung pseudo-spröder und duktiler Bruchbilder, die zur Beurteilung der Repräsentativität des FNCT für das dem Spannungsriss zugrundeliegenden langsamen Risswachstum von Bedeutung ist.
Predictive Methods for Determining the Thermal Decomposition Properties of Hazardous Substances
(2019)
Due to the fast development and availability of computers, predictive approaches are increasingly used in the evaluation process of hazardous substances complementary to experiments. Their use was recommended as alternative to experimental testing by the REACH regulation to complete the lack of knowledge on properties for existing substances that must be registered before 2018 (upon quantities). Among the proposed predictive approaches, Quantitative Structure Property Relationships (QSPR) are powerful methods to predict macroscopic properties from the only molecular structure of substances. In that context, the HAZPRED project (2015-2018, founded by the SAF€RA consortium) aims to develop theoretical models (e.g. QSPR) and small-scale tests to predict complex physico-chemical properties (e.g. thermal stability, explosivity) of hazardous substances to complete the lack of knowledge on these hazardous substances quickly or to understand their decomposition behaviour better. In particular, this contribution will present the work done in this project on the physical hazards of organic peroxides and self-reactive substances: gathering of existing experimental data, new experimental campaigns, review of existing models and proposition of new estimation methods.
Additive Fertigungsverfahren gewinnen aufgrund der schnellen, flexiblen und kosten-günstigen Fertigung von Bauteilen zunehmend an Bedeutung. Das Laserpulverauf-tragschweißen (LPA) wurde anfangs hauptsächlich als Beschichtungsverfahren ein-gesetzt. Diese Technologie bewerkstelligt aber auch das Reparieren von verschlisse-nen Bauteilen, sodass diese zeitsparend und ressourcenschonend erneuert werden können. Die hohe Aufbaurate, die flexible Pulverzusammensetzung sowie die hohe Endkonturnähe ermöglichen heutzutage die Entwicklung und additive Fertigung von neuen Materialien, wie zum Beispiel Nickel-Titan-Formgedächtnislegierungen.
The determination of mechanical properties of welded Steel structures such as strength or ductility is a subject of high interest for the majority of Companies in the area of metal Processing. The material Parameters can be obtained by performing the tensile test on the samples made from a part of a component. In some cases, it is highly expensive to produce the tensile specimens especially from the weld metal, which contains different type of microstructure such as weld seam or heat affected zone in an extremely small area. Therefore, a method is described in this paper to determine the material Parameters of high strength Steel structures and welded joints locally and without any additional effort to perform the tensile test. In this method, instrumented indentation technique (IIT), an indenter is pushed on the flat surface of a specimen in a certain period of time and simultaneously the applied force and the corresponding indentation path are measured. The data related to the force-indentation diagram is given as input to an artificial neural network (ANN) to obtain the material Parameters. The ANN can be trained by generating the large qualitative data sets with numerical Simulation of the IIT procedure. The Simulation must be run several times with the different material model parameter sets to generate the numerous
force-indentation diagrams as the inputs of ANN. Then, the trained ANN is validated by performing the IIT on the welded joints and comparing the obtained material Parameters from ANN with the tensile test.
Consequently, the mechanical properties of welded joints can be determined by performing the IIT and evaluating the resulting data by the ANN.
To increase the competitiveness of jacket substructures compared to monopiles a changeover from an individual towards a serial jacket production based on automated manufactured tubular joints combined with standardized pipes has to be achieved. Therefore, this paper addresses fatigue tests of automatically welded tubular X-joints focusing on the location of the technical fatigue crack. The detected location of the technical crack is compared to numerical investigations predicting the most fatigue prone notch considering the structural stress approach as well as the notch stress approach. Besides, the welding process of the automated manufactured tubular X-joints is presented.
Chemical effects during the formation of femtosecond laser-induced periodic surface structures
(2019)
The processing of laser-induced periodic surface structures (LIPSS, ripples) on metals and semiconductors in ambient air is usually accompanied by superficial oxidation effects – a fact that is widely neglected in the current literature. In this contribution, chemical, structural, and mechanical alterations in the formation of femtosecond LIPSS are characterized by a variety of surface analytical techniques, including energy dispersive X-ray analyses (EDX), X-ray photoelectron spectroscopy (XPS), micro Raman spectroscopy (µ-RS), and depth-profiling Auger electron microscopy (AEM). Alternative routes of electrochemical and thermal oxidation allow to qualify the relevance of superficial oxidation effects on the tribological performance in oil lubricated reciprocating sliding tribological tests (RSTT). It is revealed that the fs-laser processing of near-wavelength sized LIPSS on metals leads to the formation of a few hundreds of nanometers thick graded oxide layers, consisting mainly of amorphous oxides. Regardless of reduced hardness and limited thickness, this nanostructured surface layer efficiently prevents a direct metal-to-metal contact in the RSTT and may also act as an anchor layer for specific wear-reducing additives contained in the used engine oil.
Mechanochemistry is increasingly used for synthesizing soft matter materials including metal organic compounds and cocrystals. The ever-increasing interest in this method is contrasted by a limited mechanistic understanding of the mechanochemical reactivity and selectivity. Time-resolved in situ investigations of milling reactions provide direct insights in the underlying mechanisms. We introduced a setup enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy. The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. We discuss our recent results investigating the formation of (polymorphic) cocrystals. First investigations of a mechanochemical synthesis under controlled temperature which allow determining the activation barrier are presented.6 Furthermore, X-ray diffraction and in situ Raman spectroscopy coupled with thermography revealed a low temperature increase during milling reactions due to the mechanical impact and clear temperature increases as a result of the reaction heat. Our results indicate that in situ investigation of milling reactions offer a new approach to tune and optimize mechanochemically synthesized compounds.