The main goal of this dissertation was to show that the principle of atomic layer deposition (ALD) can be applied to “endless” fibers. A reactor of atomic layer deposition has been designed, especially for coating depositions onto meter long bundles of fibers. Aluminum oxide (alumina), titanium oxide (titania), double layers of alumina and titania, as well as aluminium phosphate have been deposited onto bundles of carbon fibers using the home-built reactor. Scanning electron microscopic (SEM) and transmission electron microscopic (TEM) images indicate that the coatings were uniform and conformal onto fiber surface. There was a good adhesion of the coatings to the fibers. Alumina has been deposited using two separate aluminum sources (aluminum trichloride and trimethylaluminum), and water as a source of oxygen. In case of alumina deposition using aluminum trichloride and water, initial deposition temperature was 500 °C. In these conditions, a part of the fiber bundle has been damaged. Thus, the deposition temperature was decreased to 300 °C and the fibers were unaffected. In addition, during this process hydrochloric acid is formed as a byproduct which is a corrosive substance and affects the reactor and there was a chloride impurity in the coatings. Thus, aluminum trichloride precursor was replaced by trimethylalumium. Alumina deposition onto carbon fibers using trimethylaluminum and water was carried out at a temperature of 77 °C. SEM images revealed that the fibers were unaffected and the coatings were uniform and conformal. Oxidation resistance of the carbon fibers was improved slightly after alumina deposition. Oxidation onset temperature of the uncoated fibers was about 630 °C. The resistance was linearly increased with the coating thickness (up to 660 °C) and getting saturated over a thickness of 120 nm. Titania coatings have been deposited using titanium tetrachloride and water. The physical appearances of the titania coatings were similar to the alumina coatings. The oxidation onset temperature of the titania coated carbon fibers was similar to the uncoated fibers but the rate of oxidation was decreased than the uncoated fibers. Two double layer coatings were deposited, alumina followed by titania (alumina/titania), and titania followed by alumina (titania/alumina). If the fibers were coated with the double layer of alumina/titania, they had almost same oxidation onset as alumina coated fibers but the rate of oxidation was decreased significantly compared to alumina coated fibers. This feature is independent of the thickness of the titania layers, at least in the regime investigated (50 nm alumina followed by 13 nm and 40 nm titania). On the other hand, the oxidation onset temperature of fibers coated with titania/alumina (20 nm titania /30 nm alumina) was approximately 750 °C. The fibers were burned completely when temperature was further increased to 900 °C and held another 60 minutes at 900 °C. This is significantly better than any other coating used in this dissertation. ALD of titania and alumina in principle was known beforehand, this dissertation here applies this knowledge for the first time to endless fibers. Furthermore, this dissertation shows for the first time that one can deposit aluminum phosphate via ALD (planar surface as well as fibers). Aluminum phosphate might be special interest in the fiber coating because it is a rather soft material and thus might be used to obtain a weak coupling between fiber and matrix in composites. Aluminum phosphate was deposited using trimethylaluminum and triethylphosphate as precursors. Energy dispersive X-ray spectroscopy and solid state nuclear magnetic resonance spectra confirmed that the coating comprises aluminum phosphate (orthophosphate as well as other stoichiometries). Scanning electron microscopic images revealed that coatings are uniform and conformal. In cases of alumina and titania, it was observed that the coatings were delaminated from the ends of cut fibers and thus formed of clear steps. On the other hand, for aluminum phosphate coating it was observed that the border between coating and underlying fiber often being smeared out and thus formed an irregular line. It seems in case aluminum phosphate cohesion is weaker than adhesion, thus it might be act a weak interface between fiber and matrix. Alumina, titania, and double layer microtubes have been obtained after selective removal of the underlying carbon fibers. The carbon fibers were selectively removed via thermal oxidation in air at temperatures exceeding 550 °C. SEM and TEM images indicate that the inner side of the tube wall has the same morphology like the fibers. In addition, it was observed that the individual microtubes were separated from their neighbors and they had almost uniform wall thicknesses. The longest tubes had a length of 30 cm. / Das Hauptziel dieser Dissertation bestand darin nachzuweisen, dass die Atomlagenabscheidung (engl. atomic layer deposition (ALD)) auf „endlose“ Fasern angewendet werden kann. Es wurde ein Reaktor zur Atomlagenabscheidung gestaltet, der speziell für die Beschichtung meterlanger Faserbündel geeignet ist. Aluminiumoxid, Titanoxid, Doppelschichten aus Aluminiumoxid und Titanoxid sowie Aluminiumphosphat wurden mit Hilfe des selbstgebauten Reaktors auf Kohlefaserbündel abgeschieden. Rasterelektronenmikroskopische (REM) und transmissionselektronenmikroskopische (TEM) Aufnahmen zeigten, dass die Beschichtung auf den Fasern einheitlich und oberflächentreu war. Des Weiteren wurde eine gute Adhäsion zwischen Beschichtung und Fasern beobachtet. Das Prinzip der Beschichtung mit Titanoxid und Aluminiumoxid mit Hilfe der ALD war bereits vorher bekannt und im Rahmen dieser Dissertation jedoch erstmals auf "endlose" Fasern angewendet. Des Weiteren wird in dieser Dissertation erstmals gezeigt, dass es möglich ist, Aluminiumphosphat mittels ALD abzuscheiden (sowohl auf planaren Oberflächen als auch auf Fasern). Aluminiumphosphat könnte von besonderem Interesse in der Faserbeschichtung sein, da es ein relativ weiches Material ist und könnte daher als eine Art „schwacher“ Verbindung zwischen Faser und Matrix in Kompositen dienen. Die Oxidationsbeständigkeit von beschichten Kohlefasern wurde im Vergleich zu unbeschichteten Fasern bis zu einem gewissen Grad erhöht. Monoschichten von Aluminiumoxid und Titanoxid waren dafür wenig effektiv. Aluminiumphosphatbeschichtete Fasern waren deutlich besser geeignet als die beiden anderen. Eine Doppelschicht aus Titanoxid gefolgt von Aluminiumoxid verbesserte die Oxidationsbeständigkeit nochmals deutlich gegenüber allen anderen Beschichtungen, die in dieser Dissertation verwendet wurden. Mikroröhren aus Aluminiumoxid, Titanoxid und Doppelschichten wurden durch die selektive Entfernung der zugrunde liegenden Kohlefasern erhalten. Einzelne Mikroröhren waren von benachbarten Röhren getrennt und sie weisen eine nahezu einheitliche Wanddicke auf.

The current dissertation, titled “Fire Response of Composite aerostructures” deals with a crucial subject of the aeronautics industry that is the fire response of composite aerostructures, more specifically the issue of interest in this work is the fuselage fire burnthrough from an external liquid jet-fuel pool fire. Other fire issues that “bother” the aeronautics industry are the fire spread inside the cabin, smoke generation and toxicity of the fumes, but these are not handled in the current dissertation. Aircraft structures are designed to withstand various loading scenarios during their operational life. These loading scenarios are associated to a great extent with normal aircraft operation (flight manoeuvres, take-off and landing). However there are situations where the aircraft structures are required to assure the safety of the passengers and crew. In the case of an emergency crash landing, the threat of an external jet-fuel fire always exists. Considering that the aircraft structure survives the impact, the survivability of the passengers and crew onboard the aircraft depends solely on the fire resistance of the aircraft structure. A measure of the fire resistance of an aircraft structure is the time needed for the flames to penetrate the fuselage and spread inside the cabin, the so-called, burn-through time. So far, the aircraft fire resistance has been extensively studied by conducting lab, medium and full scale tests. The early lab scale tests were performed by the Federal Aviation Administration (FAA) and involved the Bunsen-burner flammability test of coupons for developing fire safe interior materials. As the application of polymer materials on aircrafts kept increasing, the problem of fire burn-through due to external fire emerged. Marker was one of the first to perform full-scale fuselage burn-through tests to access the insulating performance of materials. Also a statistical analysis was performed by Cherry and Warren that accessed and analyzed data from past accidents and their work resulted in proving the importance of fuselage fire hardening and the passengers’ lives that could be saved using low-cost solutions. These works led the FAA to proposed new fire testing procedures for aircraft materials. The scope of this dissertation was to assess the performance of various structural materials in a pool-fire scenario. A simplified approach is made, approximating the pool-fire conditions with a flat panel burn-through test in accordance to the ISO2685:1998(E) Standard. The originality of the present work comes from the fact that it incorporates a multistage approach in order to investigate the behaviour and response of composite aircraft structures in the possibility of a fire event. The current approach goes down on material level in order to investigate and model the deterioration (decomposition) of the polymer composite. Thus, it investigates and proposes a methodology of how the thermophysical properties of the composite are deteriorated due to the fire event. It proceeds into developing a progressive-damage material model (material properties varying with the deterioration degree) and finally implementing this custom material model into a commercial FE package and solving the loading scenarios. Being more specific the current work begins with a quick review of the literature where incidents and work done on the burnthrough event for the past 20-30 years are summarized. It progresses then to presenting the various types of polymers used in the aircraft industry and their basic decomposition mechanisms, from the unsaturated polyesters to the epoxies and phenolics and in the end reference to the thermoplastics is made. Every organic material, hence, polymers used in aerospace applications, present a set of response characteristics when subjected to fire, specifically the heat release rate, thermal stability index, limiting oxygen index, flammability index, time-to-ignition, surface flame spread, mass loss, smoke density and smoke toxicity. Following is the backbone of this dissertation, the kinetics modelling. Two approaches are made, one simplified using single stage kinetics where the decomposition degree a is calculated based on the Arrhenius reaction theory and using the kinetic triplets (kinetic parameters) extracted from thermogravimetry, TGA, data using the Friedman multi-curve method. The second approach is more complicated and considers multi-stage decomposition of the polymer composite. Specifically a 3-stage reaction network is considered for every material, the LY-Ref, and the two modified batches, one with ammonium polyphosphate AP423 and the other both with AP423 and multi-wall carbon nanotubes MWCNT. Again the kinetic parameters, activation energy EA, frequency factor A, and reaction order n, are extracted for every step using the van Krevelen methodology. In the end using the reaction rates equations the reconstruction of the TGA curves is achieved with an error of less than 5% from the test data. Correlations that consider the material deterioration and affect the thermophysical properties of the materials are proposed. Those expressions are being developed for both of the two kinetic approaches, the single and multi stage. Another crucial part of this work is the measurement and calibration of the applied fire load. Again two fire load approaches are used, one according to the ISO2685 Standard where a propane burner was manufactured and calibrated according to the Standard for medium scale samples testing and a lab scale butane burner for small samples. The ISO2685 burner was also CFD simulated and the models calibrated against analytical expressions, ISO requirements and real measurements. The CFD simulations were performed so the heat flux or heat transfer coefficient to be extracted and used as input for the later thermal FE burnthrough models. The heat flux distribution of the lab-scale AML burner on the specimen surface was measured via a water cooled Schmit-Boelter SBG01 heat flux sensor manufactured by Hukseflux. Manufacturing and material details are presented concerning the samples used for every test campaign. Metallic (AL2024-T3) samples, CFRP neat and modified, and hybrid GLARE ones where manufactured. Also the experimental work performed is described. Cone calorimetry testing data are available, results from thermogravimetry tests, differential scanning calorimetry, and finally the burnthrough tests with both the testing apparatuses, the ISO2685 one and the AML lab-scale burner. The modelling work in this dissertation involved thermal models that were developed into a commercial FE package. It was not part of this work to develop a thermal solver so a commercial one was selected and all the developed methodology was adapted to its requirements and specifications. The boundary conditions on the models are presented both for the ‘hot’ front surface and the rear ‘cooling’ one. For the ‘hot’ one the heat flux distribution is used and for the ‘cooling’ one an equivalent convection is applied that accounts for both convective and radiative cooling. The decomposing material model is implemented into to FE solver via user defined subroutines for the single stage kinetics and the multi-stage approach. Finally the simulations were run and the results and models were compared against the available experimental results. Since so far the burnthrough response of aerostructures was limited to coupon, samples and medium size flat panels. A more realistic approach was performed by developing a mathematical model of a real size test. The certification tests conducted by the FAA are for full size fuselage sectors under the fire load of a burning jet-fuel pan pool-fire. A burning jet-fuel pool fire is a complex phenomenon on its own, combining it with a decomposing fuselage structure make the modeling approach even more difficult to simulate if not impossible. Required data for the pool-sizes under investigation were not available, so data for large external hydrocarbon pool fires from literature were used. Also, because the main characteristic of a jet-fuel (kerosene) pool fire is that the flames are not clear, on the contrary, great amount of shoot is produced making combustion modeling and radiative heat transfer to the fuselage even more of a challenge to model, it was decided to try and tackle this full-scale approach by a simplified the modeling approach. Instead of liquid fuel combustion, an equal hot air stream with mass flow, velocity and temperature properties extracted from literature correlation data was performed. Conclusively, in terms of completeness the benefit analysis performed by Cherry and Warren is presented in brief. The objective of their analysis was to assess the potential benefits, in terms of reduction of fatalities and injuries, resulting from improvements in fuselage burnthrough resistance to ground pool fires. Fire hardening of fuselages will provide benefits in terms of enhanced occupant survival and may be found to be cost beneficial if low-cost solutions can be found. The maximum number of lives saved per year in worldwide transport aircraft accidents, over the period covered by the data, if hardening measures were applied, was assessed to be 12.5 for the aircraft in its actual configuration (when the accidents occurred) and 10.5 for the aircraft configured to later airworthiness requirements. These figures are completely significant and give an extra confirmation that this work on investigating the fire response of composite aerostructures is on the right track. As the work of Cherry and Warren concluded, the fire hardening measures in order to be applicable need to be cost efficient. The concept under which this whole dissertation stepped on was to investigate the fire response of composite aerostructures and the possibility of hardening the structure itself without the use of extra protective layers that add cost and weight to the overall aircraft and its maintenance. In the end it was concluded that there is the possibility of hardening the fuselage structure by design and by material. Incorporating composites into the structure it is possible to prolong the burnthrough time at least for 4-5 minutes before auto ignition occurs on the inner side of the fuselage. Auto ignition of the inner side fuselage cabin materials is mentioned since in NONE of the burnthrough tests of the CFRP composites and the GLARE samples flame penetration was observed. / Στην παρούσα διατριβή με τίτλο «Ανάλυση της απόκρισης σύνθετων πολυμερών υλικών υπό συνθήκες φωτιάς. Εφαρμογή σε αεροπορικές κατασκευές» πραγματοποιείται εργασία στην αριθμητική προσομοίωση και πειραματική διερεύνηση της συμπεριφοράς αεροπορικών κατασκευών σε συνθήκες φωτιάς. Στην μέχρι τώρα βιβλιογραφία οι διάφοροι έλεγχοι για πιστοποίηση των αεροπορικών υλικών αλλά και των αεροσκαφών στο σύνολό τους αποτελούνταν από εκτενείς πειραματικές δοκιμές σε μεσαία κλίμακα καθώς και σε πλήρους κλίμακας κατασκευές. Οι προδιαγραφές των ελέγχων ορίζονται από την Ομοσπονδιακή Διεύθυνση Αεροπλοΐας των Ηνωμένων Πολιτειών της Αμερικής, Federal Aviation Administration FAA. Όπως γίνεται αντιληπτό πλήρους κλίμακας δοκιμές είναι χρονοβόρες αλλά και οικονομικά ασύμφορες, για τον λόγο αυτό τα τελευταία χρόνια πραγματοποιούνται προσπάθειες από την FAA για καθιέρωση Προτύπων ελέγχου μικρής κλίμακας τα οποία σε συνδυασμό με αριθμητικά μοντέλα θα είναι σε θέση να προβλέπουν την συμπεριφορά των αεροπορικών κατασκευών σε συνθήκες φωτιάς από την φάση του σχεδιασμού τους. Θα εξασφαλίζεται έτσι καλύτερη διαχείριση οικονομικών και υλικών πόρων. Στην βιβλιογραφία ο μεγαλύτερος όγκος αριθμητικής μοντελοποίησης έχει πραγματοποιηθεί στους τομείς της ναυπηγικής και των θαλάσσιων κατασκευών καθώς επίσης και τα τελευταία χρόνια στον τομέα της αστικής δόμησης. Αριθμητική δουλεία πάνω στην συμπεριφορά των αεροπορικών κατασκευών είναι υπερβολικά περιορισμένη και εκεί στοχεύει να συμβάλει η παρούσα διατριβή. Οι αεροπορικές κατασκευές εκτός των περιορισμών και προδιαγραφών που θέτουν οι άλλες εφαρμογές απαιτούν την ελαχιστοποίηση του προστιθέμενου βάρους στην κατασκευή. Διάφοροι τύποι πολυμερών συνθέτων υλικών χρησιμοποιούνται στην βιομηχανία, διακρινόμενα σε θερμοσκληρυνόμενα και θερμοπλαστικά. Αρχικά παρουσιάζονται τα θερμοσκληρυνόμενα ξεκινώντας από τους ευρέως χρησιμοποιούμενους πολυεστέρες και βινυλεστέρες, στις φαινολικές και εποξικές ρητίνες καταλήγοντας στους υψηλής θερμοκρασίας κυανεστέρες. Εν συνεχεία γίνεται αναφορά στα συνήθη χρησιμοποιούμενα θερμοπλαστικά, πολυπροπυλένιο PP, Poly-ether ether-ketone PEEK και polyphenylene Sulphide PPS. Φυσικά δεν παραλείπεται να γίνει σύντομη αναφορά και στις τυπικές διεργασίες θερμικής αποσύνθεσης των προαναφερθέντων πολυμερών. Η συμπεριφορά των σύνθετων πολυμερών υλικών σε συνθήκες φωτιάς περιγράφεται από κάποια χαρακτηριστικά μεγέθη τα οποία χρησιμοποιούνται για την ποιοτική και ποσοτική σύγκριση των διαφόρων υποψήφιων αεροπορικών υλικών. Συγκεκριμένα τα μεγέθη αυτά είναι: Heat Release Rate HRR, Thermal Stability Index TSI, Limited Oxygen Index LOI, Extinction Flammability Index ESI, Time-to-Ignition, Surface Flame Spread, Mass Loss, Smoke Density, Smoke Toxicity. Οι διαδικασίες ελέγχου και τα υπολογιζόμενα μεγέθη γίνονται βάσει διεθνών Προτύπων που κυρίως για τον τομέα της αεροναυπηγικής ορίζονται από την Ομοσπονδιακή Διεύθυνση Αεροπλοΐας FAA. Η αριθμητική προσομοίωση προυποθέτει γνώση της συμπεριφοράς των πολυμερών υλικών σε συνθήκες υψηλής θερμοκρασίας, για τον σκοπό αυτό πραγματοποιήθηκαν πειράματα απώλειας μάζας με χρήση θερμογραβιμετρίας TGA κατά την διάρκεια της οποίας η απώλεια μάζας καθώς και ο ρυθμός αυτής παρακολουθούνται και καταγράφονται σαν συνάρτηση του ρυθμού θέρμανσης. Μέσα από αυτά τα δεδομένα μπορεί να πραγματοποιηθεί εκτίμηση του τρόπου αποσύνθεσης του πολυμερούς. Αρχικά πραγματοποιήθηκε η θεώρηση της μονοβάθμιας αντίδρασης (single-stage reaction) που αποτελεί και την πλέον απλουστευμένη προσέγγιση. Στην θεώρηση αυτή θεωρείται πως η πολυμερής μήτρα περνάει από την «παρθένα» κατάσταση στην απανθρακομένη μέσα σε ένα βήμα. Η περιγραφή της αντίδρασης αυτής γίνεται με μια μονοβάθμια αντίδραση τύπου Arrhenius. Σε δεύτερο βήμα χρησιμοποιήθηκε κινητική θεωρία πολλαπλών σταδίων (multi-stage kinetics) σύμφωνα με την οποία πραγματοποιήθηκε ακριβέστερη προσέγγιση της απόσύνθεσης της πολυμερούς μήτρας των συνθέτων υλικών με απόκλιση μικρότερη του 5% από τα πειραματικά δεδομένα της θερμογραβιμετρείας (thermogravimetry). Και στις δύο προσεγγίσεις της αποσύνθεσης υπολογίσθηκαν οι κινηματικές παράμετροι: συντελεστής συχνότητας A (frequency factor), ενέργεια ενεργοποίησης ΕΑ (activation energy), τάξη αντίδρασης n (reaction order) για κάθε στάδιο. Με την ολοκλήρωση αυτού του σταδίου υπήρχε μια αξιόπιστη δυνατότητα αναπαράστασης της διαδικασίας αποσύνθεσης στο πείραμα της θερμογραβιμετρίας. Είναι γνωστό ότι οι διακυμάνσεις της θερμοκρασίας επηρεάζουν της τιμές των θερμοφυσικών ιδιοτήτων των υλικών. Αναλογιζόμενοι ότι στην διαρκεία της επιβολής της φλόγας στα σύνθετα υλικά όχι μόνο η θερμοκρασία αλλά και η σύσταση μεταβάλλεται συνεχώς λόγω της αποσύνθεσης κρίθηκε αναγκαία η ανάπτυξη μιας μεθοδολογίας που θα συμπεριλαμβάνει την επίδραση της αποσύνθεσης στην μεταβολή των θερμοφυσικικών ιδιοτήτων (θερμική αγωγιμότητα, ειδική θερμοχωρητικότητα και πυκνότητα) της πολυμερούς μήτρας και κατά συνέπεια του συνθέτου υλικού. Οι εξαγόμενες μαθηματικές σχέσεις χρησιμοποιήθηκαν στην αριθμητική προσομοίωση που ακολούθησε. Με σκοπό την ορθή αριθμητική μοντελοποίηση κρίνεται αναγκαία η μέτρηση και βαθμονόμηση του θερμικού φορτίου τον πειραματικών δοκιμών. Το μετρούμενο θερμικό φορτίου χρησιμοποιήθηκε εν συνεχεία ως φόρτιση στα αναπτυχθέντα μοντέλα. Χρησιμοποιήθηκαν δύο πειραματικές διατάξεις εφαρμογής φλόγας, μία μεσαίας κλίμακας σύμφωνα με τις διατάξεις του FAA Standard, που περιγράφεται στο ISO2685:1998(E) “Aircraft – Environmental test procedure for airborne equipment – Resistance to fire in designated fire zones” και μίας εργαστηριακής κλίμακος. Πραγματοποιήθηκε μέτρηση με θερμοζεύγη και καλορίμετρο νερού καθώς και αριθμητική μοντελοποίηση με χρήση CFD για την πρώτη διάταξη. Ενώ για την εργαστηριακής κλίμακας έγινε μέτρηση με θερμοζεύγη και ενός αισθητήρα θερμικού φορτίου «water-cooled Hukseflux Schmit-Boelter SBG01 sensor». Εν συνεχεία πραγματοποιήθηκε η κατασκευή των δοκιμίων των υποψήφιων υλικών καθώς και οι πειραματικές δοκιμές και έλεγχοι τους. Συγκεκριμένα πραγματοποιήθηκε: Θερμιδομετρία κώνου (cone calorimetry), Θερμογραβιμετρία (thermogravimetry), Θερμιδομετρία Διαφορικής Ανίχνευσης (Differencial Scanning Calorimetry, DSC), Μέτρηση Θερμικής αγωγιμώτητας, Δοκιμή διείσδυσης φλόγας (Fire burnthrough penetration). Καθώς ο χαρακτηρισμός της αποσύνθεσης των πολυμερών υλικών, η μεταβολή των θερμοφυσικών ιδιοτήτων, η μέτρηση και βαθμονόμηση του επιβαλλόμενου θερμικού φορτίου καθώς και οι πειραματικές δοκιμές έχουν ολοκληρωθεί ακολουθεί η αριθμητική προσομοίωση. Οι συνοριακές συνθήκες θερμικού φορτίου και ψύξης επιλέχθησαν ως εξής. Ως φόρτιση θεωρήθηκε η κατανομή του θερμικού φορτίου (σε kW/m2) στην εμπρός επιφάνεια του πάνελ. Στην ψύξη της πίσω επιφάνειας λήφθηκε υπόψη τόσο η ελεύθερη μεταφορά θερμότητας με επαφή όσο και η ακτινοβολία. Το μοντέλο της συμπεριφοράς του υλικού διαμορφώθηκε κατάλληλα ώστε να γίνει κατανοητό από τις απαιτήσεις ενός εμπορικού κώδικα Πεπερασμένων Στοιχείων επίλυσης θερμικών προβλημάτων και προσομοιώθηκαν οι πειραματικές δοκιμές διείσδυσης φλόγας των δύο πειραματικών διατάξεων, μεσαίας και εργαστηριακής κλίμακος. Πλέον της αριθμητικής προσομοίωσης της συμπεριφοράς σε φωτιά επίπεδων δοκιμίων αεροπορικών κατασκευών, πραγματοποιήθηκε προσπάθεια απλουστευμένης μοντελοποίησης των συνθηκών φλόγας ενός λιμνάζοντος όγκου καυσίμου αεροσκαφών στο εξωτερικό μιας ατράκτου. Δημιουργήθηκε ένα τρισδιάστατο ρευστομηχανικό μοντέλο πρόβλεψης του θερμικού φορτίου στην επιφάνεια μιας τυπικής ατράκτου σύμφωνα με τις προδιαγραφές γεωμετρίας του Προτύπου “Full-scale test evaluation of Aircraft fuel fire burnthrough resistance improvements” DOT/FAA/AR-98/52,1999. Τα ρευστομηχανικά αποτελέσματα συγκρίθηκαν με δεδομένα βιβλιογραφίας για μεγάλες φλεγόμενες δεξαμενές λιμνάζοντος καυσίμου. Εκτός από την μελέτη της απόκρισης των αεροπορικών κατασκευών σε συνθήκες φλόγας σκοπός της παρούσας εργασίας είναι και η παρουσίαση λύσεων οι οποίες θα έχουν την δυνατότητα της βελτίωσης της συμπεριφοράς των υπαρχουσών δομών καθώς και των μελλοντικών σύνθετων δομών. Ενδεικτικά αναφέρεται η δυνατότητα χρήσης νανοεγκλεισμάτων, και βελτιωμένων μονωτικών υλικών, π.χ. aerogels. Όπως έχει ήδη αναφερθεί οι αεροπορικές κατασκευές θέτουν τον περιορισμό της ελαχιστοποίησης του προστιθέμενου βάρους, για τον λόγο αυτό η ενίσχυση των συνθέτων υλικών θα πρέπει να πραγματοποιηθεί σε επίπεδο υλικού και σχεδιασμού. Πρέπει δηλαδή η ίδια η κατασκευή που είναι ικανή να φέρει τα μηχανικά φορτία να εξασφαλίζει και την πιστοποίηση της FAA για συνθήκες φωτιάς. Συνοψίζοντας, η παρούσα διατριβή πραγματοποιεί μια καινοτόμο, γρήγορη και αρκετά ακριβή προσέγγιση του σημαντικότατου ζητήματος της συμπεριφοράς των πολυμερικών σύνθετων αεροπορικών δομών σε συνθήκες φωτιάς Η πολυπλοκότητα του όλου φαινομένου επέβαλε την πραγματοποίηση παραδοχών και απλουστεύσεων. Καθώς όμως με την αυξανόμενη χρήση των συνθέτων υλικών στις αεροπορικές κατασκευές, ο τομέας της ασφάλειας σε συνθήκες φλόγας είναι συνεχώς αυξανόμενος και απαιτητικός. Για αυτό οι παραδοχές και θεωρήσεις της παρούσας διατριβής μπορούν να βελτιωθούν με χρήση νέων υπολογιστικών μεθόδων και πειραματικών δεδομένων με στόχο την ακόμα ακριβέστερη πρόβλεψη της συμπεριφοράς τον αεροπορικών δομών σε συνθήκες φλόγας.

Reinforced cement concrete (RCC) structures have become an important aspect in most of the buildings in our society around the world. Most of the multistoried reinforced concrete buildings house important institutions such as hospitals, schools, government establishments, defense establishments, business centers, sports stadiums, super markets and nuclear power plants. The cost of construction of such multistoried RCC structures is very high, and these structures need to be maintained and restored based on their functionality and importance using repair and retrofit strategies when these structures undergo damage. The steps involved in restoring RCC structures that have damages using repair / retrofit measures consists of identifying the source or cause of damage, assessment of the degree or extent of damage that has taken place using nondestructive techniques. Based on the assessment of degree of damage suitable repair / retrofit strategy using the appropriate repair material is applied to achieve the required load carrying capacity or strength. The present work involves assessing the efficacy of carbon fibre reinforced polymer (CFRP) based system applied on pre-damaged structural members to restore the member’s strength and stiffness through experimental investigations and finite element predictions. To validate the macrolevel properties of predamaged concrete micromechanical analysis, microscale studies and analytical investigations have been conducted. Plain and reinforced concrete test specimens: cylinders, square prisms and rectangular prisms having 25MPa and 35MPa cylinder compressive strengths pre-damaged due to mechanical (monotonic and cyclic loading) and thermal loading (exposure to different temperature and time durations) with applications of CFRP repair subjected to compression is investigated to study the behavior and enhancement in the compressive strength and stiffness after application of repair. Non destructive testing of thermally damaged concrete (exposed to different temperature and exposure time) is conducted using ultrasonic pulse velocity and tomography methods to understand the degradation in the strength and stiffness of thermally damaged concrete. The results of the non destructive testing helps in assessing the amount of repair that can be applied. To validate the macro scale behavior of thermally damaged concrete micro scale studies was performed adopting micro indentation, petrography, Raman spectroscopy, scanning electron miscroscopy (SEM) and Electron probe micro analysis (EPMA). During the event of a fire in RC structures which have been retrofitted. The high temperature caused due to fire tends to make the concrete to deteriorate and the repair material to delaminate. Loss of strength/ stiffness in concrete and delamination of the repair material in a retrofitted structural component in a structure causes instability which results in partial collapse or complete collapse of the structure. Thermal insulation of concrete and the repair material (CFRP) using geo-polymer mortar and simwool thermal fibre blanket exposed to high temperature and different exposure time are experimentally investigated. This is to evaluate the effectiveness of the thermal insulation in protecting epoxy based structural repair material(CFRP) from thermal damage and to minimize the delamination of the repair material when exposed to high temperatures. Slender columns when loaded eccentrically fail at a load much lesser than their actual load carrying capacity. In RC buildings where additional floors need to be added, in those situations slender columns which are already eccentrically loaded tend to get damaged or fail due to additional load which act on them. Therefore to restore such columns experimental and finite element investigations on reinforced concrete slender columns having 25MPa cylinder compressive strength subjected to eccentric monotonic compressive loading with applications of CFRP repair is studied to understand the behavior and the enhancement in load carrying capacity after application of repair. Experimental investigations are conducted to study fracture and fatigue properties of thermally damaged concrete geometrically similar notched plain and reinforced concrete beams having 25MPa cylinder compressive strength exposed to different combinations of temperature and durations with application of repair (CFRP). Nonlinear fracture parameters of thermally damaged concrete is computed which help in understanding the fracture behavior of thermally damaged concrete and application of repair. Effectiveness of CFRP repair and failure behaviour of these beams are studied when these thermally damaged notch concrete beams are subjected to monotonic and cyclic (fatigue) loading. Reinforced concrete slender beams when subjected to unexpected loads such as earthquakes get damaged. The increase in load carrying capacity and fatigue life of reinforced concrete slender beams having 25MPa cylinder compressive strength in flexure subjected to monotonic and cyclic loading with applications of CFRP repair is investigated using experimental and finite element investigations. Finite element analysis of concrete specimens pre-damaged due to mechanical (monotonic and cyclic loading) / thermal loading (exposure to different temperature and time durations) with applications of CFRP repair and assessment of amount of repair required is investigated. Analytical (empirical) models are developed to assess the mechanical properties of concrete (elastic moduli, compressive strength and split tensile strength) exposed to different temperatures and time durations. Nonlinear fracture parameters of geometrically similar plain concrete notch beams exposed to different temperature and time durations are determined. Fracture parameters (stress intensity factor) of thermally damaged plain and reinforced concrete notched beams with application of CFRP have been determined. Effect of size and shape of thermally damaged plain concrete compression members with application of CFRP wrap have been studied. Crack mouth opening displacements (CMOD), strains and crack lengths of thermally damaged plain concrete (PC) notched beams using digital image correlation has also been determined.

Il est prévu d’augmenter la durée de vie des centrales nucléaires actuellement opérationnelles. Le vieillissement des structures en béton armé telles que les tours aéroréfrigérantes doit être évalué, son incidence sur la capacité portante calculée. Dans le cas de fortes dégradations, le renforcement doit être envisagé, afin d’assurer la pérennité de ces tours face aux sollicitations extrêmes telles que les tempêtes de vent et les séismes. Ce travail vise à quantifier les effets néfastes que peut générer la réduction de section des aciers induite par la corrosion, en particulier sur la capacité portante des tours dans des conditions de sollicitations extrêmes monotones ou cycliques de types vent et séisme. Ces sollicitations sont certainement les plus sévères, entrainant la structure dans le domaine non linéaire, elles sont susceptibles d’induire des endommagements de type fissuration qui dans le cas de sollicitation cycliques peuvent s’avérer néfastes. Des modélisations numériques sont proposées pour déterminer la réponse quasi-statique ou dynamique de la structure, en tenant compte des apparitions de fissures dans le béton et de leur évolution via des lois de comportement appropriées du matériau béton, ainsi que la plastification des aciers. Dans le cas d’une sollicitation sismique, dans le but de comparer les approches de modélisation du séisme et d’évaluer la robustesse des résultats, les réponses dynamiques sont évaluées par trois méthodes différentes de calcul : l’approche dynamique temporelle non linéaire, la méthode spectrale et la méthode modale temporelle. Des études paramétriques portant sur l’amortissement, les combinaisons de charges et les configurations structurales, sont aussi menées. Dans le cas d’une sollicitation de type vent, la technique de renforcement à l’aide de matériaux composite, tel que le tissu de fibres de carbone (TFC) est modélisée. Le comportement de la structure endommagée présentant un taux de corrosion avancée, est évalué dans le régime pré- et post-fissuration, comparativement à la structure intègre. La perte de capacité portante est quantifiée, un renforcement permettant de restaurer l'intégrité et donc d’augmenter la durée de vie de la structure est proposé. / The authorities have planned to increase the lifetime of currently operating nuclear power plants. The ageing of reinforced concrete structures such as cooling towers should be evaluated and its impact on the bearing capacity calculated. In the case of significant damage, the strengthening must be considered to ensure the sustainability of these towers facing the risk of storms and earthquakes becoming more and more frequent. This work aims to quantify the adverse effects that can generate concrete cracks and rebar section loss induced by corrosion, especially on the bearing capacity of nuclear power plant cooling towers under monotonic or cyclic extreme load conditions (wind and earthquake). These loads are certainly the most severe, since they take the structure into the nonlinear domain and can induce or amplify cracking damage. Numerical simulations are proposed to determine the quasi-static or dynamic response of the structure, taking into account appearance of concrete cracks and their evolution via an appropriate material concrete law and rebar's yielding. In the case of a seismic load, the responses are evaluated by three different methods; the nonlinear response history analysis (NLRHA), the response spectrum analysis and the modal response history analysis (MRHA) in order to compare the earthquake modeling approaches and to evaluate the robustness of the results. Parametric studies on damping, load combinations and structural configurations, are also performed. In the case of a wind load, the strengthening technique using composite materials, such as carbon fiber reinforced plastic (CFRP) is modeled. The behavior of the damaged structure with an advanced corrosion rate is estimated in the pre- and post-cracking regime, compared to the undamaged structure. The drop of bearing capacity is quantified, a reinforcement designed is proposed to restore the integrity and thus increase the lifetime of the structure.

In recent years the use of carbon fiber reinforcing polymers (CFRP) to repair damaged structural components has become more accepted and practiced. However, the current reference for designing FRP systems to repair and strengthen reinforced concrete (RC) and prestressed concrete (PSC) girders has limitations. Similarly, very few resources address solutions for the debonding problem associated with CFRP laminates or the use of CFRP laminates to repair structural members with pre-existing damage. The included experimental program consists of testing both RC and PSC girders with simulated lateral damage and CFRP repairs. A total of 34 RC beams were statically tested under a 4-point loading until failure and had cross-section dimensions of 5” x 10” (14cm x 25.4cm), were 8’ long (2.44m), and were reinforced with either #3 or #4 mild steel rebar. 13 PSC girders having cross-section dimensions representing a half-scaled AASHTO type II shape, were 20’ long (6.1m), and were prestressed with five 7/16” (11.1mm) diameter low-lax 7-wire strands. Ten of the PSC girders were statically loaded until failure under a 4-point testing setup, but 3 PSC girders were dynamically tested under fatigue loading using a 3-point arrangement. Different configurations of CFRP laminates, number and spacing of CFRP transverse U-wraps, and amount of longitudinal CFRP layers are studied. The results present the flexural behavior of all specimen including load-deflection characteristics, strain characteristics, and modes of failure. Ultimately, results are used to recommend important considerations, needed criteria, and proper design procedures for a safe and optimized CFRP repair configuration.

The diploma thesis focuses on manufacturing carbon fiber and epoxy composite material using filament winding method. Material properties of manufactured composite are ap-proximated using analytical and numerical homogenization models. Calculated material properties are applied to design and evaluate reserve factor of retaining sleeve for high speed brushless permanent magnet synchronous motor. Margin of safety of designed rotor is evaluated using composite failure criteria. Test stand for both static and dynamic testing is designed, static test stand is manufactured and assembled. Static strength test is carried out.

The main goal of this dissertation was to show that the principle of atomic layer deposition (ALD) can be applied to “endless” fibers. A reactor of atomic layer deposition has been designed, especially for coating depositions onto meter long bundles of fibers. Aluminum oxide (alumina), titanium oxide (titania), double layers of alumina and titania, as well as aluminium phosphate have been deposited onto bundles of carbon fibers using the home-built reactor. Scanning electron microscopic (SEM) and transmission electron microscopic (TEM) images indicate that the coatings were uniform and conformal onto fiber surface. There was a good adhesion of the coatings to the fibers. Alumina has been deposited using two separate aluminum sources (aluminum trichloride and trimethylaluminum), and water as a source of oxygen. In case of alumina deposition using aluminum trichloride and water, initial deposition temperature was 500 °C. In these conditions, a part of the fiber bundle has been damaged. Thus, the deposition temperature was decreased to 300 °C and the fibers were unaffected. In addition, during this process hydrochloric acid is formed as a byproduct which is a corrosive substance and affects the reactor and there was a chloride impurity in the coatings. Thus, aluminum trichloride precursor was replaced by trimethylalumium. Alumina deposition onto carbon fibers using trimethylaluminum and water was carried out at a temperature of 77 °C. SEM images revealed that the fibers were unaffected and the coatings were uniform and conformal. Oxidation resistance of the carbon fibers was improved slightly after alumina deposition. Oxidation onset temperature of the uncoated fibers was about 630 °C. The resistance was linearly increased with the coating thickness (up to 660 °C) and getting saturated over a thickness of 120 nm. Titania coatings have been deposited using titanium tetrachloride and water. The physical appearances of the titania coatings were similar to the alumina coatings. The oxidation onset temperature of the titania coated carbon fibers was similar to the uncoated fibers but the rate of oxidation was decreased than the uncoated fibers. Two double layer coatings were deposited, alumina followed by titania (alumina/titania), and titania followed by alumina (titania/alumina). If the fibers were coated with the double layer of alumina/titania, they had almost same oxidation onset as alumina coated fibers but the rate of oxidation was decreased significantly compared to alumina coated fibers. This feature is independent of the thickness of the titania layers, at least in the regime investigated (50 nm alumina followed by 13 nm and 40 nm titania). On the other hand, the oxidation onset temperature of fibers coated with titania/alumina (20 nm titania /30 nm alumina) was approximately 750 °C. The fibers were burned completely when temperature was further increased to 900 °C and held another 60 minutes at 900 °C. This is significantly better than any other coating used in this dissertation. ALD of titania and alumina in principle was known beforehand, this dissertation here applies this knowledge for the first time to endless fibers. Furthermore, this dissertation shows for the first time that one can deposit aluminum phosphate via ALD (planar surface as well as fibers). Aluminum phosphate might be special interest in the fiber coating because it is a rather soft material and thus might be used to obtain a weak coupling between fiber and matrix in composites. Aluminum phosphate was deposited using trimethylaluminum and triethylphosphate as precursors. Energy dispersive X-ray spectroscopy and solid state nuclear magnetic resonance spectra confirmed that the coating comprises aluminum phosphate (orthophosphate as well as other stoichiometries). Scanning electron microscopic images revealed that coatings are uniform and conformal. In cases of alumina and titania, it was observed that the coatings were delaminated from the ends of cut fibers and thus formed of clear steps. On the other hand, for aluminum phosphate coating it was observed that the border between coating and underlying fiber often being smeared out and thus formed an irregular line. It seems in case aluminum phosphate cohesion is weaker than adhesion, thus it might be act a weak interface between fiber and matrix. Alumina, titania, and double layer microtubes have been obtained after selective removal of the underlying carbon fibers. The carbon fibers were selectively removed via thermal oxidation in air at temperatures exceeding 550 °C. SEM and TEM images indicate that the inner side of the tube wall has the same morphology like the fibers. In addition, it was observed that the individual microtubes were separated from their neighbors and they had almost uniform wall thicknesses. The longest tubes had a length of 30 cm.:Bibliographische Beschreibung und Referat 2 Abstract 4 List of abbreviations 10 1. General introduction and outline of this dissertation 12 1.1 References 20 2. Atomic layer deposition: Process and reactor 25 2.1 Introduction 25 2.2 Principle of atomic layer deposition 26 2.3 Materials and methods 29 2.3.1 Precursors 29 2.3.2 Precursors transportation 31 2.3.3 Carrier and purge gas 32 2.3.4 ALD reactors 32 2.4 Flow-Type ALD reactor for fiber coating 33 2.5 Conclusion 35 2.6 References 35 3. Single layer oxide coatings 38 3.1 State of the art 38 3.2 Alumina coating using non-flammable precursors 39 3.2.1 Introduction 39 3.2.Result and discussion 39 3.3 Alumina coating using organometallic precursor 46 3.2.1 Introduction 46 3.2.2 Results and discussion 46 3.4 Titania coating using titanium tetrachloride and water 59 3.4.1 Introduction 59 3.4.2 Results and discussion 59 3.5 Experimental Part 67 3.5.1 General experiments 67 3.5.2 Alumina coating using aluminum chloride and water 69 3.5.3 Alumina coating using trimethylalumium and water 69 3.5.4 Titania coating 72 3.6 Conclusions 72 3.7 References 74 4. Coating thickness and morphology 78 4.1 Introduction 78 4.2 Results and discussion 80 4.2.1 Purge time 15 s 81 4.2.2 Purge time 30 s 85 4.2.3 Purge time 45 s to 100 s 85 4.3 Experimental part 88 4.4 Conclusions 89 4.5 References 89 5. Alumina and titania double layer coatings 91 5.1 Introduction 91 5.2 Results and discussion 92 5.3 Experimental part 102 5.4 Conclusions 103 5.5 References 103 6. Atomic layer deposition of aluminum phosphate 105 6.1 Introduction 105 6.2 Results and discussion 106 6.3 Experimental part 113 6.4 Conclusions 114 6.5 References 115 7. Alumina microtubes 117 7.1 Introduction 117 7.2 Results and discussion 118 7.2.1 Fibers before coating deposition 118 7.2.2 Coatings on the carbon fibers 118 7.2.3 Microtubes 121 7.3 Experimental part 127 7.4 Conclusions 128 7.5 References 128 8. Conclusions 131 Acknowledgements 136 Curriculum Vitae 138 Selbständigkeitserklärung 142 / Das Hauptziel dieser Dissertation bestand darin nachzuweisen, dass die Atomlagenabscheidung (engl. atomic layer deposition (ALD)) auf „endlose“ Fasern angewendet werden kann. Es wurde ein Reaktor zur Atomlagenabscheidung gestaltet, der speziell für die Beschichtung meterlanger Faserbündel geeignet ist. Aluminiumoxid, Titanoxid, Doppelschichten aus Aluminiumoxid und Titanoxid sowie Aluminiumphosphat wurden mit Hilfe des selbstgebauten Reaktors auf Kohlefaserbündel abgeschieden. Rasterelektronenmikroskopische (REM) und transmissionselektronenmikroskopische (TEM) Aufnahmen zeigten, dass die Beschichtung auf den Fasern einheitlich und oberflächentreu war. Des Weiteren wurde eine gute Adhäsion zwischen Beschichtung und Fasern beobachtet. Das Prinzip der Beschichtung mit Titanoxid und Aluminiumoxid mit Hilfe der ALD war bereits vorher bekannt und im Rahmen dieser Dissertation jedoch erstmals auf "endlose" Fasern angewendet. Des Weiteren wird in dieser Dissertation erstmals gezeigt, dass es möglich ist, Aluminiumphosphat mittels ALD abzuscheiden (sowohl auf planaren Oberflächen als auch auf Fasern). Aluminiumphosphat könnte von besonderem Interesse in der Faserbeschichtung sein, da es ein relativ weiches Material ist und könnte daher als eine Art „schwacher“ Verbindung zwischen Faser und Matrix in Kompositen dienen. Die Oxidationsbeständigkeit von beschichten Kohlefasern wurde im Vergleich zu unbeschichteten Fasern bis zu einem gewissen Grad erhöht. Monoschichten von Aluminiumoxid und Titanoxid waren dafür wenig effektiv. Aluminiumphosphatbeschichtete Fasern waren deutlich besser geeignet als die beiden anderen. Eine Doppelschicht aus Titanoxid gefolgt von Aluminiumoxid verbesserte die Oxidationsbeständigkeit nochmals deutlich gegenüber allen anderen Beschichtungen, die in dieser Dissertation verwendet wurden. Mikroröhren aus Aluminiumoxid, Titanoxid und Doppelschichten wurden durch die selektive Entfernung der zugrunde liegenden Kohlefasern erhalten. Einzelne Mikroröhren waren von benachbarten Röhren getrennt und sie weisen eine nahezu einheitliche Wanddicke auf.:Bibliographische Beschreibung und Referat 2 Abstract 4 List of abbreviations 10 1. General introduction and outline of this dissertation 12 1.1 References 20 2. Atomic layer deposition: Process and reactor 25 2.1 Introduction 25 2.2 Principle of atomic layer deposition 26 2.3 Materials and methods 29 2.3.1 Precursors 29 2.3.2 Precursors transportation 31 2.3.3 Carrier and purge gas 32 2.3.4 ALD reactors 32 2.4 Flow-Type ALD reactor for fiber coating 33 2.5 Conclusion 35 2.6 References 35 3. Single layer oxide coatings 38 3.1 State of the art 38 3.2 Alumina coating using non-flammable precursors 39 3.2.1 Introduction 39 3.2.Result and discussion 39 3.3 Alumina coating using organometallic precursor 46 3.2.1 Introduction 46 3.2.2 Results and discussion 46 3.4 Titania coating using titanium tetrachloride and water 59 3.4.1 Introduction 59 3.4.2 Results and discussion 59 3.5 Experimental Part 67 3.5.1 General experiments 67 3.5.2 Alumina coating using aluminum chloride and water 69 3.5.3 Alumina coating using trimethylalumium and water 69 3.5.4 Titania coating 72 3.6 Conclusions 72 3.7 References 74 4. Coating thickness and morphology 78 4.1 Introduction 78 4.2 Results and discussion 80 4.2.1 Purge time 15 s 81 4.2.2 Purge time 30 s 85 4.2.3 Purge time 45 s to 100 s 85 4.3 Experimental part 88 4.4 Conclusions 89 4.5 References 89 5. Alumina and titania double layer coatings 91 5.1 Introduction 91 5.2 Results and discussion 92 5.3 Experimental part 102 5.4 Conclusions 103 5.5 References 103 6. Atomic layer deposition of aluminum phosphate 105 6.1 Introduction 105 6.2 Results and discussion 106 6.3 Experimental part 113 6.4 Conclusions 114 6.5 References 115 7. Alumina microtubes 117 7.1 Introduction 117 7.2 Results and discussion 118 7.2.1 Fibers before coating deposition 118 7.2.2 Coatings on the carbon fibers 118 7.2.3 Microtubes 121 7.3 Experimental part 127 7.4 Conclusions 128 7.5 References 128 8. Conclusions 131 Acknowledgements 136 Curriculum Vitae 138 Selbständigkeitserklärung 142

Les enquêtes récentes sur les séismes ont fait ressortir l'importance des murs en béton armé en tant que partie intégrante des structures. L’évolution des règlements prend en compte ces considérations, par contre le bâti existant doit subir des renforcements dans l’objectif de leur mise en conformité. Dans cette thèse une étude expérimentale faite sur douze murs (six élancés et six courts) renforcés par un collage externe en composite a été conduite. Les murs ont été conçus en étant sous-renforcés à la flexion et cisaillement. Quatre de ces six échantillons ont été renforcés par des bandes de PRFC collées. Deux spécimens, un témoin et un renforcé, ont été soumis à un test de chargement statique et quatre échantillons, l'un témoin et trois rénovés, ont été soumis à des essais de charge cyclique. La discussion et l’analyse des tests incluent la description de la fissuration, l’analyse de la rigidité, de la capacité de charge ultime, de la ductilité. / Recent earthquake surveys have revealed the significance of RC walls as an integral part of structures. It reduces the structure damage to some extent. However, like other structural member they too are vulnerable. Researchers on basis of their post eartthquake survey and laboratary experiments have concluded that the RC wall buildings sustained damage, mainly due to design and construction work flaws. In this thesis experimental result of shear walls is discussed. They were designed under-reinforced to fail in shear in ase of short wall and in flexure for slender walls. Three out of these six specimens, in each case, were strengthened externally with CFRP strips bonded to wall panel and mesh anchors installed at wall foundation joint. Two specimens, one RC and one CFRP retrofitted (short and slender wall each), were subjected to static load test and three specimens, one RC and two to three CFRP retrofitted, were subjected to quasi static cyclic load tests. The test result analysis discussion includes failure mode, stiffness, ultimate load capacity, ductility, and energy dissipation.

L’utilisation de composites à matrice thermodurcissable et fibres continues est en constante progression dans le secteur aéronautique, ferroviaire, et automobile. Afin d’améliorer les composites obtenus, notamment leur résistance à l’impact et leur conductivité électrique, des nanocharges organiques ou inorganiques peuvent être ajoutées. Les nanotubes de carbone (CNT) font partie des candidats les plus prometteurs pour le renforcement de composites à multi-échelle. Cependant, il s’avère difficile de contrôler la dispersion, la répartition et l’orientation des CNT, après les avoir mélangés aux prépolymères. Une nouvelle stratégie d’insertion des CNT dans un composite consiste à combiner des fibres de CNT avec des fibres de carbone. L’orientation et l’organisation structurelle des CNT au sein de la fibre permettent d’obtenir d’excellentes propriétés mécaniques et électriques. Dans notre étude, les propriétés de fibres contenant exclusivement des CNT, obtenues par direct spinning, ont été comparées à celles de fibres de carbone (non-ensimées, ensimées, et CNT en surface). Différentes interfaces entre les fibres de CNT, fibres de carbone et deux types de matrices époxy (de TG très différentes) ont été générées et testées par des essais de fragmentation de fibre dans la matrice. La contrainte de cisaillement interfaciale fibre/matrice a été évaluée afin de déterminer l’influence des diverses fibres et ensimages sur les performances mécaniques de composites à matrice organique et à fibres continues. En outre, la nature de l’adhésion et la qualité de l’interphase entre la matrice et la fibre ont été caractérisées par plusieurs techniques d’analyses et d’observations à multi-échelles. / Nowadays, polymer-matrix composites reinforced with carbon fibers are increasingly used in the whole transport sector (aerospace, automotive and railway industries). However, the obtained parts still suffer from low impact resistance and low damage tolerance. To improve these properties, the matrix precursors have to be combined with organic or inorganic compounds to lead to multi-phased matrices. Among them, carbon nanotubes (CNT) are especially promising for targeting multi-scale reinforcement. Since high quality of the parts are required, continuous-fibers-reinforced composites can be produced by resin transfer molding (RTM) which also offers a reduced cost if compared with high temperature- and high pressure-based processes. However, RTM requires a very low viscosity of the polymer precursors and CNT-filled precursors are far too viscous to be injected on dry performs. In addition, this strategy does not allow for a control of the CNT location and orientation in the final part. In this study, innovative ways have been developed to insert CNT in the preform with local positioning and defined orientation. Deliveries of CNT in the matrix, from a neat carbon multi-nanotubes fiber produced by direct spinning, or from a CNT grown on carbon fiber were investigated in two types of epoxy matrices (with very different TG). Different polymer matrix/fiber interfaces have been generated using neat carbon multi-nanotubes fiber, CNT grown on carbon fiber and conventional carbon fiber, with or without sizing. A fine mechanical characterization of various fibers and particularly the measurement of single fiber interfacial properties have been performed in order to determine mechanical performance of continuous fiber reinforced composites. In addition, the nature of adhesion and quality of matrix/fiber interface have been fully evaluated by different multi-scale analyses and suitable microstructural observations.

L’intérêt croissant de l’industrie pour les matériaux composites thermoplastiques est motivé par leurs propriétés de thermoformabilité, de recyclabilité ainsi que leurs capacités de cadences de production élevées. Le développement de matériaux pré-imprégnés thermoplastiques, apparus dès les années 1980, s’est imposé comme un moyen efficace de contourner les fortes viscosités des polymères utilisés en réduisant la distance d’écoulement des polymères à l’état « fondu ». Cette étude s’est plus particulièrement intéressée au développement de composites à base de tissus de verre et de carbone pré-imprégnés par un latex acrylique, le TPREG I. En outre, les propriétés mécaniques élevées des matrices acryliques, alliées à un coût relativement faible, en font un matériau intéressant, de nature à permettre un saut technologique dans la conception et la fabrication de composites structuraux à matrice organique. Notre étude s’est concentrée sur la mesure de l’adhésion à l’interface fibre/matrice acrylique car cette région est au cœur du transfert de charge de la matrice vers les fibres et conditionne donc les propriétés mécaniques du composite. Nous avons choisi d’évaluer l’adhésion interfaciale en combinant des analyses de mouilllage avec des tests mécaniques aux échelles microscopique et macroscopique. Le test micromécanique de la microgoutte permet de mettre en évidence le rôle central de l’ensimage des fibres sur la contrainte de cisaillement interfaciale. L’adhésion thermodynamique, déterminé par des mesures d’énergie de surface, est en accord avec la contrainte de cisaillement et souligne l’influence de la polarité de l’ensimage. A l’échelle macroscopique, les essais de traction hors-axe sur composites unidirectionnels permettant de solliciter l’interface en cisaillement quasi-plan ont mis en exergue une corrélation entre les échelles micro et macro. L’étude a également permis de dégager une forte augmentation de l’adhésion grâce à une modification de la matrice acrylique, ainsi qu’une dégradation des propriétés interfaciales à l’échelle micro par vieillissement hydrolytique. Cette étude constitue une première base de données concernant les propriétés interfaciales de composites thermoplastiques acryliques et démontre l’importance d’une étude multi-échelles dans la conception de nouveaux composites. / The present study was initiated by the development of a new processing route, i.e. latex-dip impregnation, for thermoplastic (TP) acrylic semi-finished materials. The composites resulting from thermocompression of TPREG I plies were studied by focusing of interfacial adhesion. Indeed the fiber/matrix interface governs the stress transfer from matrix to fibers. Thus, a multi-scale analysis of acrylic matrix/fiber interfaces was conducted by considering microcomposites, as models for fiber-based composites, and unidirectional (UD)macro-composites. The study displayed various types of sized glass and carbon fibers. On one hand, the correlation between thermodynamic adhesion and practical adhesion, resulting from micromechanical testing, is discussed by highlighting the role of the physico-chemistry of the created interphase. Wetting and thermodynamical adhesion are driven by the polarity of the film former of the sizing. On the other hand, in-plane shear modulus values from off-axis tensile test results on UD composites are consistent with the quantitative analyses of the interfacial shear strength obtained from microcomposites. More specifically, both tests have enabled a differentiation of interface properties based on the fiber sizing nature for glass and carbon fiber-reinforced (micro-)composites. The study of overall mechanical and interface properties of glass and carbon fiber/acrylic composites revealed the need for tailoring interfacial adhesion. Modifications of the matrix led to successful increases of interfacial adhesion in glass fiber/acrylic composites. An additional hygrothermal ageing study evidenced a significant loss of interfacial shear strength at micro-scale which was not observed for UD composites. The results of this study are a first step towards a database of relevant interface properties of structural TP composites. Finally, the analyses of interfaces/phases at different scales demonstrate the importance of a multi-scale approach to tailor the final properties of composite parts.