Carbonfaserverstärkten Kunststoffen (CFK) erzielen ihre herausragende Festigkeit und Steifigkeit durch exakte Anpassung der Faserverläufe im Bauteil an die im Einsatz wirkenden Belastungen. Für eine Qualitätskontrolle und eine Optimierung der Fertigungsverfahren ist daher ein Verfahren notwendig, das in der Lage ist, die Faserorientierung in 3D-Preforms (mehrlagigen, drapierten Vorformlingen aus trockenen Carbonfasern) und 3D-CFK zerstörungsfrei zu messen und mit der Soll-Faserorientierung zu vergleichen. Die derzeit für die Faserorientierungsmessung eingesetzten optischen bzw. Röntgen-CT-Verfahren sind hierfür nur beschränkt geeignet, da optische Verfahren auf die oberste Lage und Röntgen-CT-Verfahren auf Kleinproben beschränkt sind. In dieser Arbeit wird daher ein Verfahren entwickelt, das die Faserorientierung in mehrlagigen 3D-Carbonfaserpreforms und -CFK zerstörungsfrei messen kann. Grundlage hierfür ist die Hochfre-quenz-Wirbelstromprüfung, die eine Darstellung der Verläufe der leitfähigen Carbonfäden in den einzelnen, übereinander gestapelten Lagen des CFK erlaubt. Um hierauf aufbauend eine vollauto-matische Faserorientierungsmessung zu schaffen, wird in einem ersten Schritt ein Roboter-Bahnplanungsverfahren zur vollständigen Erfassung komplex geformter 3D-Oberflächen entwi-ckelt. Aus dem erhaltenen 3D-Wirbelstrombild der Oberfläche wird anschließend über einen auf lokaler Abwicklung und Fouriertransformation beruhenden Algorithmus die lokale Faserorientie-rung in den einzelnen Lagen gemessen und die 3D-Verläufe einzelner Fäden werden rekonstruiert. Die Messunsicherheit des Verfahrens wird anhand systematischer experimenteller Untersuchungen an 2-, 4-, 6- und 8-lagigen 2D-Gelegestapeln quantifiziert. Untersucht wird hierbei auch der Einfluss der Materialparameter (Gelegetyp) sowie der Messparameter (Spulenanordnung, Spulendurch-messer, Sensororientierung, Messfrequenz) auf die sich ergebende Messunsicherheit, woraus Empfehlungen für die Wahl von Sensor und Messfrequenz abgeleitet werden. Das entwickelte Messverfahren wird anschließend an zwei 3D-Anwendungsfällen validiert. Als erster Anwendungsfall wird ein vierlagiges, komplex geformtes CFK-Bauteil betrachtet. Es wird gezeigt, wie mithilfe des entwickelten Messverfahrens die Faserorientierung aller vier Lagen zerstörungsfrei erfasst werden kann. Verschiedene Exemplare desselben Bauteils werden hinsicht-lich der Faserorientierung verglichen. Anschließend wird im zweiten Anwendungsfall ein automati-scher Drapierprozess zu einer Halbkugel betrachtet, bei dem verschiedene, ein-, zwei und vierlagi-ge textile Halbzeuge hinsichtlich der sich ausbildenden Faserorientierung nach der Drapierung verglichen werden, mit dem Ziel, das Verformungsverhalten mehrlagiger Strukturen besser zu verstehen und Empfehlungen für die Halbzeugauswahl abzuleiten. In einem abschließenden Schritt werden Schnittstellen geschaffen, um die Faserorientierungsmes-sung in den CFK-Entwicklungsprozess zu integrieren. Zum einen wird durch eine Schnittstelle zur Drapiersimulation ein quantitativer Vergleich zwischen vorausgesagter und Ist-Faserorientierung möglich, zum anderen wird gezeigt, wie die gemessenen Faserorientierungen der Einzellagen direkt zur Parametrierung von Struktursimulationen verwendet werden können. Das entwickelte Verfah-ren ermöglicht damit eine fundierte Festigkeits- und Steifigkeitsanalyse mit den zerstörungsfrei gemessenen Faserorientierungen nach dem Umformprozess.:1 Einleitung 2 Grenzen bestehender Verfahren zur Faserorientierungsmessung bei der CFK-Herstellung 3 Stand der Technik zur Wirbelstromprüfung von Carbonfasermaterialien 4 Entwicklung einer Roboter-Bahnplanung zur vollständigen Erfassung einer 3D-Oberfläche 5 Entwicklung einer Faserorientierungsmessung aus 3D-Wirbelstromdaten 6 Experimentelle Untersuchung der Messunsicherheit an 2D-Gelegestapeln 7 Verfahrenserprobung an mehrlagigen 3D-Preforms und CFK 8 Integration der Faserorientierungsmessung in den CFK-Entwicklungsprozess 9 Zusammenfassung und Ausblick / The superior strength and stiffness of carbon fiber reinforced plastics (CFRP) results from an exact adaptation of the component’s fiber orientation to the external loads during service. Quality control, as well as development and optimization of the production processes, thus require a method to non-destructively measure the fiber orientation in 3D preforms (draped multilayer stacks made of dry carbon fibers) and CFRP. Currently, this fiber orientation measurement is done by optical or X-ray computer tomography methods, which are limited, however to the uppermost, optical visible fabric layer (optical methods) or to small sample sizes (X-ray computer tomography). Therefore, this thesis develops a method to non-destructively measure the 3D fiber orientation in multi-layer 3D preforms and CFRP. The starting point for this development is the technique of high-frequency eddy current testing, which allows an imaging of the individual carbon yarn courses in multiple stacked textile layers. In order to develop a fully-automated fiber orientation measure-ment process with this technique, in a first step a robot path planning is developed that allows the complete scanning of a complexly-shaped 3D surface with an eddy current sensor. From the resulting 3D eddy current image of the surface, the local fiber orientation of the individual layers is measured by local development (flattening) of the surface and a Fourier transformation. The uncertainty of measurement for this method is quantified from experiments with 2-, 4-, 6- and 8-layer 2D non-crimp fabric stacks. The influence of the material parameters (type of fabric) as well as of the measurement parameters (sensor type, coil diameter, sensor orientation, measure-ment frequency) is evaluated. Recommendations for the choice of sensor and measurement frequency are derived. The developed measurement method is subsequently validated with two different 3D application cases. As a first application case, a four-layer, complexly-shaped CFRP component is analyzed. It is shown how the developed measurement method can be used to non-destructively measure the fiber orientation of all four layers. Different specimen of the same CFRP component are compared regarding fiber orientation. The second application case is an automated draping process to a hemispherical shape, for which one-, two- and four-layer textile fabrics are compared regarding the fiber orientation after draping, in order to better understand the forming properties of multi-layer structures and derive recommendations for the choice of textile. In the final step, software interfaces are developed to integrate the fiber orientation measurement into the CFRP design and development process. It is integrated with a draping simulation, to allow a quantitative comparison of the predicted and the measured fiber orientations. Furthermore, it is shown how the measured fiber orientation of the individual fabric layers can be used for the parametrization of finite element structural simulations. The developed measurement method thus lays the base for a substantiated strength and stiffness analysis based on the component’s actual as-is fiber orientation after the draping process.:1 Einleitung 2 Grenzen bestehender Verfahren zur Faserorientierungsmessung bei der CFK-Herstellung 3 Stand der Technik zur Wirbelstromprüfung von Carbonfasermaterialien 4 Entwicklung einer Roboter-Bahnplanung zur vollständigen Erfassung einer 3D-Oberfläche 5 Entwicklung einer Faserorientierungsmessung aus 3D-Wirbelstromdaten 6 Experimentelle Untersuchung der Messunsicherheit an 2D-Gelegestapeln 7 Verfahrenserprobung an mehrlagigen 3D-Preforms und CFK 8 Integration der Faserorientierungsmessung in den CFK-Entwicklungsprozess 9 Zusammenfassung und Ausblick

Ermüdungsrissbildung ist ein gefährliches und kostenintensives Phänomen, welches frühzeitig erkannt werden muss. Weil kleine Fehlstellen jedoch hohe Testempfindlichkeit erfordern, wird die Prüfzuverlässigkeit durch Falschanzeigen vermindert. Diese Arbeit macht sich deshalb die Diversität unterschiedlicher zerstörungsfreier Oberflächenprüfmethoden zu Nutze, um mittels Datenfusion die Zuverlässigkeit der Fehlererkennung zu erhöhen. Der erste Beitrag dieser Arbeit in neuartigen Ansätzen zur Fusion von Prüfbildern. Diese werden durch Oberflächenabtastung mittels Wirbelstromprüfung, thermischer Prüfung und magnetischer Streuflussprüfung gewonnen. Die Ergebnisse zeigen, dass schon einfache algebraische Fusionsregeln gute Ergebnisse liefern, sofern die Daten adäquat vorverarbeitet wurden. So übertrifft Datenfusion den besten Einzelsensor in der pixelbasierten Falscherkennungsrate um den Faktor sechs bei einer Nutentiefe von 10 μm. Weiterhin wird die Fusion im Bildtransformationsbereich untersucht. Jedoch werden die theoretischen Vorteile solcher richtungsempfindlichen Transformationen in der Praxis mit den vorliegenden Daten nicht erreicht. Nichtsdestotrotz wird der Vorteil der Fusion gegenüber Einzelsensorprüfung auch hier bestätigt. Darüber hinaus liefert diese Arbeit neuartige Techniken zur Fusion auch auf höheren Ebenen der Signalabstraktion. Ein Ansatz, der auf Kerndichtefunktionen beruht, wird eingeführt, um örtlich verteilte Detektionshypothesen zu integrieren. Er ermöglicht, die praktisch unvermeidbaren Registrierungsfehler explizit zu modellieren. Oberflächenunstetigkeiten von 30 μm Tiefe können zuverlässig durch Fusion gefunden werden, wogegen das beste Einzelverfahren erst Tiefen ab 40–50 μm erfolgreich auffindet. Das Experiment wird auf einem zweiten Prüfkörper bestätigt. Am Ende der Arbeit werden Richtlinien für den Einsatz von Datenfusion gegeben, und die Notwendigkeit einer Initiative zum Teilen von Messdaten wird betont, um zukünftige Forschung zu fördern. / Fatigue cracking is a dangerous and cost-intensive phenomenon that requires early detection. But at high test sensitivity, the abundance of false indications limits the reliability of conventional materials testing. This thesis exploits the diversity of physical principles that different nondestructive surface inspection methods offer, by applying data fusion techniques to increase the reliability of defect detection. The first main contribution are novel approaches for the fusion of NDT images. These surface scans are obtained from state-of-the-art inspection procedures in Eddy Current Testing, Thermal Testing and Magnetic Flux Leakage Testing. The implemented image fusion strategy demonstrates that simple algebraic fusion rules are sufficient for high performance, given adequate signal normalization. Data fusion reduces the rate of false positives is reduced by a factor of six over the best individual sensor at a 10 μm deep groove. Moreover, the utility of state-of-the-art image representations, like the Shearlet domain, are explored. However, the theoretical advantages of such directional transforms are not attained in practice with the given data. Nevertheless, the benefit of fusion over single-sensor inspection is confirmed a second time. Furthermore, this work proposes novel techniques for fusion at a high level of signal abstraction. A kernel-based approach is introduced to integrate spatially scattered detection hypotheses. This method explicitly deals with registration errors that are unavoidable in practice. Surface discontinuities as shallow as 30 μm are reliably found by fusion, whereas the best individual sensor requires depths of 40–50 μm for successful detection. The experiment is replicated on a similar second test specimen. Practical guidelines are given at the end of the thesis, and the need for a data sharing initiative is stressed to promote future research on this topic.

The poly(glycidyl methacrylate)-modified magnetite nanoparticles, Fe3O4-PGMA NPs, were investigated and applied in nondestructive flaw detection of polymeric materials in this research. The Fe3O4 endowed magnetic property to the materials for flaw detection while the PGMA promoted colloidal stability and prevented particle aggregation. The magnetite nanoparticles (Fe3O4 NPs) were successfully synthesized by coprecipitation and then surface-modified with PGMA to form PGMA-modified Fe3O4 NPs by both grafting-from and grafting-to approaches. For the grafting-from approach, the Fe3O4 NPs were surface-functionalized with α-bromo isobutyryl bromide (BIBB) to form BIB-modified Fe3O4 NPs (Fe3O4-BIB NPs) with covalent linkage. The resultant Fe3O4-BIB NPs were used as surface-initiators to grow PGMA by surface-initiated atom transfer radical polymerization (SI-ATRP). For the grafting-to approach, the Fe3O4 NP were surface-functionalized with (3-mercaptopropyl)triethoxysilane (MCTES) to form MCTES-modified Fe3O4 NPs (Fe3O4-MCTES NPs). The PGMA with Br-end group was pre-synthesized by ATRP and then was grafted to the surface of the Fe3O4-MCTES NPs by coupling reaction. Both bare and modified Fe3O4 NPs exhibited superparamagnetism and the existence of iron oxide in the form of Fe3O4 was confirmed. The particle size of individual Fe3O4 NPs was about 8 – 24 nm but they aggregated to form clusters. The PGMA-modified NPs formed stable dispersion in chloroform and had larger cluster sizes than the unmodified ones because of the PGMA polymer layer. However, the uniformity of the NP clusters could be improved with PGMA surface grafting. The PGMA surface layer of the grafting-from (Fe3O4-gf-PGMA) NPs was thin and dense while that of the grafting-to (Fe3O4-gt-PGMA) NPs was thick and loose. The hydrodynamic diameters (Zave) of Fe3O4-gf-PGMA NP clusters could be controlled between 176 to 643 nm, dependent on the PGMA contents and reaction conditions. During SI-ATRP, side reactions happened and caused NP aggregation as well as increase of size of NP clusters. However, the aggregation has been minimized through optimization of reaction conditions. Oppositely, Zave values of Fe3O4-gt-PGMA NPs had little variation of about 120 – 190 nm. And the PGMA content of the Fe3O4-gt-PGMA NPs was limited to 12.5% because of the spatial hindrance during grafting process. The saturation magnetization (Ms) of the unmodified Fe3O4 NPs was about 77 emu/g, while those of the grafting-from and grafting-to Fe3O4-PGMA NPs were 50 – 66 emu/g and 63 – 70 emu/g, respectively. For Fe3O4-PGMA NPs with similar Fe3O4 contents, the grafting-to NPs had slightly higher Ms than the grafting-from counterparts. In addition, the Ms of both kinds of the Fe3O4-PGMA NPs with higher Fe3O4 content (> 87%) were also higher than that of the fluidMAG-Amine, the commercially available amine-modified MNPs. Besides, both kinds of Fe3O4-PGMA NPs also had much higher Fe3O4 contents and Ms values than most of the reported PGMA-modified MNPs. The magnetic epoxy nanocomposites (MENCs) were prepared by blending the modified Fe3O4 NPs into bisphenol A diglycidyl ether (BADGE)-based epoxy system and the distributions of both kinds of the PGMA-modified NPs were much better than that of the oleic acid-modified Fe3O4 NPs. Similar to the NPs, the MENCs also exhibited superparamagnetism. By cross-section TEM observation, the grafting-to Fe3O4-PGMA NPs formed more homogeneous distributions with smaller cluster size than the grafting-from counterparts and gave higher Ms of the MENCs. Nondestructive flaw detection of surface and sub-surface defects could be successfully achieved by brightness contrast of images given through eddy current testing (ET) method, which is firstly reported. The mechanical properties of the materials were influenced very slightly when 2.5% or lower Fe3O4-gt-PGMA NPs were present while the presence of the Fe3O4-gf-PGMA NPs (1 – 2.5 %) gave mild improvement of the storage modulus and increase of the glass-rubber transition temperature(Tg) of the MENCs. Furthermore, the Fe3O4-PGMA NPs could be evenly coated onto the functionalized ultra-high molecular weight poly(ethylene) (UHMWPE) textiles. The Fe3O4-gt-PGMA NPs were coated on the textile in order to prepare NP-coated textile-reinforced composite. Preliminary result of ET measurement showed that the Fe3O4-gt-PGMA NPs coated on the textiles could visualize the structure of the textile hidden inside and their relative depth. Accordingly, the incorporation of MNPs to polymers opens a new pathway of damage-free structural health monitoring of polymeric materials.

The poly(glycidyl methacrylate)-modified magnetite nanoparticles, Fe3O4-PGMA NPs, were investigated and applied in nondestructive flaw detection of polymeric materials in this research. The Fe3O4 endowed magnetic property to the materials for flaw detection while the PGMA promoted colloidal stability and prevented particle aggregation. The magnetite nanoparticles (Fe3O4 NPs) were successfully synthesized by coprecipitation and then surface-modified with PGMA to form PGMA-modified Fe3O4 NPs by both grafting-from and grafting-to approaches. For the grafting-from approach, the Fe3O4 NPs were surface-functionalized with α-bromo isobutyryl bromide (BIBB) to form BIB-modified Fe3O4 NPs (Fe3O4-BIB NPs) with covalent linkage. The resultant Fe3O4-BIB NPs were used as surface-initiators to grow PGMA by surface-initiated atom transfer radical polymerization (SI-ATRP). For the grafting-to approach, the Fe3O4 NP were surface-functionalized with (3-mercaptopropyl)triethoxysilane (MCTES) to form MCTES-modified Fe3O4 NPs (Fe3O4-MCTES NPs). The PGMA with Br-end group was pre-synthesized by ATRP and then was grafted to the surface of the Fe3O4-MCTES NPs by coupling reaction. Both bare and modified Fe3O4 NPs exhibited superparamagnetism and the existence of iron oxide in the form of Fe3O4 was confirmed. The particle size of individual Fe3O4 NPs was about 8 – 24 nm but they aggregated to form clusters. The PGMA-modified NPs formed stable dispersion in chloroform and had larger cluster sizes than the unmodified ones because of the PGMA polymer layer. However, the uniformity of the NP clusters could be improved with PGMA surface grafting. The PGMA surface layer of the grafting-from (Fe3O4-gf-PGMA) NPs was thin and dense while that of the grafting-to (Fe3O4-gt-PGMA) NPs was thick and loose. The hydrodynamic diameters (Zave) of Fe3O4-gf-PGMA NP clusters could be controlled between 176 to 643 nm, dependent on the PGMA contents and reaction conditions. During SI-ATRP, side reactions happened and caused NP aggregation as well as increase of size of NP clusters. However, the aggregation has been minimized through optimization of reaction conditions. Oppositely, Zave values of Fe3O4-gt-PGMA NPs had little variation of about 120 – 190 nm. And the PGMA content of the Fe3O4-gt-PGMA NPs was limited to 12.5% because of the spatial hindrance during grafting process. The saturation magnetization (Ms) of the unmodified Fe3O4 NPs was about 77 emu/g, while those of the grafting-from and grafting-to Fe3O4-PGMA NPs were 50 – 66 emu/g and 63 – 70 emu/g, respectively. For Fe3O4-PGMA NPs with similar Fe3O4 contents, the grafting-to NPs had slightly higher Ms than the grafting-from counterparts. In addition, the Ms of both kinds of the Fe3O4-PGMA NPs with higher Fe3O4 content (> 87%) were also higher than that of the fluidMAG-Amine, the commercially available amine-modified MNPs. Besides, both kinds of Fe3O4-PGMA NPs also had much higher Fe3O4 contents and Ms values than most of the reported PGMA-modified MNPs. The magnetic epoxy nanocomposites (MENCs) were prepared by blending the modified Fe3O4 NPs into bisphenol A diglycidyl ether (BADGE)-based epoxy system and the distributions of both kinds of the PGMA-modified NPs were much better than that of the oleic acid-modified Fe3O4 NPs. Similar to the NPs, the MENCs also exhibited superparamagnetism. By cross-section TEM observation, the grafting-to Fe3O4-PGMA NPs formed more homogeneous distributions with smaller cluster size than the grafting-from counterparts and gave higher Ms of the MENCs. Nondestructive flaw detection of surface and sub-surface defects could be successfully achieved by brightness contrast of images given through eddy current testing (ET) method, which is firstly reported. The mechanical properties of the materials were influenced very slightly when 2.5% or lower Fe3O4-gt-PGMA NPs were present while the presence of the Fe3O4-gf-PGMA NPs (1 – 2.5 %) gave mild improvement of the storage modulus and increase of the glass-rubber transition temperature(Tg) of the MENCs. Furthermore, the Fe3O4-PGMA NPs could be evenly coated onto the functionalized ultra-high molecular weight poly(ethylene) (UHMWPE) textiles. The Fe3O4-gt-PGMA NPs were coated on the textile in order to prepare NP-coated textile-reinforced composite. Preliminary result of ET measurement showed that the Fe3O4-gt-PGMA NPs coated on the textiles could visualize the structure of the textile hidden inside and their relative depth. Accordingly, the incorporation of MNPs to polymers opens a new pathway of damage-free structural health monitoring of polymeric materials.:1. Introduction 2. Theoretical section 2.1. Magnetite Nanoparticles (MNPs) 2.2. Applications of MNPs 2.3. Atom transfer radical polymerization (ATRP) 2.4. Magnetic nanocomposites (MNCs) 2.5. Damage-free structural health monitoring (SHM) using MNPs 3. Objective of the work 4. Materials, methods and characterization 4.1. Materials 4.2. Methods 4.3. Formation of polymeric magnetic nanocomposites 4.4. Characterization 5. Results and discussions 5.1. Unmodified magnetite nanoparticles (Fe3O4 NPs) 5.2. Oleic acid-modified (Fe3O4–OA) NPs 5.3. PGMA-modified NPs by grafting-from approach (Fe3O4-gf-PGMA NPs) 5.4. PGMA-modified NP by grafting-to approach (Fe3O4-gt-PGMA NPs) 5.5. Comparison between grafting-from and grafting-to Fe3O4-PGMA NPs 5.6. Magnetic epoxy nanocomposites (MENCs) 5.7. Fiber-reinforced epoxy nanocomposites 6. Conclusions and outlook 7. Appendix 8. List of figures, schemes and tables 9. References Versicherung Erklaerung List of publications