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This understanding of nanocellulose can be directly applied in future formulation design to use nanocellulose in polymer nanocomposites, foams, emulsions, latexes, gels and biomedical materials. / In this study, the potential of nanocellulose as a reinforcing agent in composite materials was investigated using atomic force microscopy (AFM). AFM was used to probe the mechanical properties of nanocelluloses and to investigate their interactions and adhesion in liquid media. Amplitude modulated-frequency modulated AFM was used to map the mechanical properties of cellulose nanocrystals (CNCs) and cellulose nanofibrils (CNFs). Results showed Young’s moduli of 90 GPa and 120 GPa for CNCs and CNFs, respectively, which are comparable to literature values determined using other methods. Additionally, colloid probe AFM was implemented to observe the interactions (attractive, repulsive, steric, adhesive) between cellulose and silica colloid probes with anionic CNCs (containing either a Na+ or H+ counterion) and cationic CNCs. Colloid probe AFM measurements were carried out in five different liquid media: two salt solutions (NaCl and CaCl2) and three surfactant solutions (cationic cetyltrimethylammonium bromide, CTAB; anionic sodium dodecyl sulfate, SDS; and nonionic Triton X100). It was found that low salt concentrations resulted in electrostatic repulsion and high adhesion, whereas the reverse was observed at high salt concentrations. On the contrary, an increased surfactant concentration and increased number of surfactant aggregates (micelles, bilayers, etc.) resulted in increased adhesion. Surprisingly, the interactions were strongly dependent on the CNC counterion as surfactant adsorption seemed to be primarily driven by electrostatic interactions; CTAB adsorbed more to anionic CNCs, SDS adsorbed more to cationic CNCs and Triton X100 adsorbed minimally to all CNCs. Electrophoretic mobility and particle size data showed complementary results to colloid probe AFM, indicating that interactions between surfactants and CNC films and CNCs in suspension are closely related. This research suggests that CNCs have potential as reinforcing agents due to their high strength and the tunability of their interactions through the simple addition of salts or surfactants. This understanding can be directly applied in future formulation design to use nanocellulose in polymer nanocomposites, foams, emulsions, latexes, gels and biomedical materials. / Thesis / Master of Applied Science (MASc) / Nanocellulose is a sustainable nanomaterial most commonly extracted from plants and trees. In recent research, nanocellulose has been shown to have potential as a reinforcing agent for materials such as plastics, foams, paints and adhesives. In this study, the potential of nanocellulose was investigated using atomic force microscopy (AFM). As predicted, AFM measurements indicated that nanocellulose has a high stiffness, supporting the substitution of this biobased material in the place of metals and synthetic fibres. AFM was also used to examine particle interactions in salt and soap-like (surfactant) solutions; changes in nanocellulose size and charge were used to support the findings. Negatively charged nanocellulose interacted more with positively charged surfactants and vice versa. Low salt and high surfactant concentrations led to high adhesion and better material compatibility, which is preferred. This understanding can help us design better nanocellulose materials for future applications.

Digital twins have found increased interest in the recent years with articles being published at an increased rate in the years 2018-2020. with digital twins it is possible to achieve an efficient and responsive planning and control over of facility management. A digital twin by JTH has been implemented for some of the rooms in a corridor, a structured literature study is performed to bridge the knowledge gap, the aim is to review scientific literature regarding digital twins’ in facilities management and assess different concepts dig-ital twins in facility management. The method used is a mixed qualitative-quantitative systematic review that follows the Preferred Reporting Items for Systematic Reviews (PRISMA). The systematic review defines digital twins in facility management and identifies categories as well as digital twins applications in facility management and how digital twins can be used to evaluate building performance and room experience.

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The lap shear strength of chromic acid anodized, primed, Ti-6Al-4V alloy bonded with a high performance FM-5 polyimide adhesive has been investigated as a function of thermal treatment for selected times at various temperatures in air. The research findings indicate that the lap shear strength decreases with the increase in duration of the thermal treatment at constant temperature and with the increase in temperature at constant time. The bond fails increasingly in the oxide coating with increasing treatment temperature and time of treatment. Surface analysis results for debonded specimens suggest that the process leading to failure is the formation of fluorine-containing materials within the oxide, which weakens the adherend-adhesive bond. The formation of the fluorine components is facilitated by treatment at elevated temperatures. This study suggests that the presence of fluoride ions in the anodic oxide coating, prior to bonding, is detrimental to the bond strength of adhesively bonded Ti-alloy when exposed to high temperatures. The wedge test configuration was used to investigate the influence of temperature on the bond durability of adhesively bonded chromic acid anodized Ti-6Al-4V alloy in air. Based on the average crack length vs. exposure time data, the bond durability varied in the order -25°C > 24°C > 177°C. In each case, the bonded joint failed cohesively within the adhesive, irrespective of the temperature of exposure. XPS analysis and scanning electron photomicrographs of failure surfaces revealed that the failure occurred at the scrim cloth/adhesive interface. The influence of thermal treatment history on the bond durability of adhesively bonded chromic acid anodized Ti-6Al-4V alloy immersed in boiling water was also investigated. The average crack length vs. immersion time indicated no significant differences for specimens that were thermally treated and then bonded compared to the non-thermally treated specimens. In addition, the failure mode was cohesive within the adhesive for specimens prepared using various thermal treatment conditions. The crack growths for samples treated for 0.5 hour and 1.0 hour and for non-thermally treated specimens for any given exposure time were equivalent. In addition, cohesive failure (failure within adhesive) was observed for each specimen under each treatment condition. The specimens that were bonded and then thermally treated for 3 hours, failed in the oxide coating immediately upon insertion of the wedge. Surface analysis results for debonded specimens suggest that the process leading to failure is the formation of fluorine-containing materials within the oxide. The measured average activation energy for the formation of aluminum fluoride species is 149 kJ/mol. The high activation energy suggests that the rate of aluminum fluoride formation is substantial only at high temperatures. In summary, the presence of fluorides in the anodic oxide coatings prior to bonding is detrimental to the overall strength and durability of adhesively bonded chromic acid anodized Ti-6Al-4V joints which have been exposed to high temperatures (350°C-399°C). / Ph. D.

The objective of this study was to evaluate and develop an understanding of durability of an adhesive bonded system, for application in a future high speed civil transport (HSCT) aircraft structure. The system under study was comprised of Ti-6Al-4V metal adherends and a thermosetting polyimide adhesive, designated as FM-5, supplied by Cytec Engineered Materials, Inc. An approach based on fracture mechanics was employed to assess Ti-6Al-4V/FM-5 bond durability. Initially, wedge tests were utilized to find a durable surface pretreatment for the titanium adherends. Based on an extensive screening study, chromic acid anodization (CAA) was chosen as the standard pretreament for this research project. Double cantilever beam specimens (DCB) were then made and aged at 150° C, 177° C, and 204° C in three different environments; ambient atmospheric air (14.7 psia), and reduced air pressures of 2 psi air (13.8 KPa) and 0.2 psi air (1.38 KPa). Joints were aged for up to 18 months (including several intermediate aging times) in the above environments. The strain energy release rate (G) of the adhesive joints was monitored as a function of exposure time in the different environments. A 40% drop in fracture toughness was noted over the 18 month period, with the greatest degradation observed in samples aged at 204° C in ambient atmospheric air pressure. The loss in adhesive bond performance with time was attibutable to a combination of physical and chemical aging phenomena in the FM-5 resin, and possible degradation of the metal-adhesive interface(s). Several mechanical and material tests, performed on the bonded joints and neat FM-5 resin specimens, confirmed the above statement. It was also noted that physical aging could be "erased" by thermal rejuvenation, partially restoring the toughness of the FM-5 adhesive material. The FM-5 adhesive material displayed good chemical resistance towards organic solvents and other aircraft fluids such as jet fuel and hydraulic fluid. The results from the FM-5 adhesive and its bonded joints were compared and contrasted with VT Ultem and REGULUS polyimide adhesives. The FM-5 adhesive showed the best performance among the three adhesive systems. The effect of mode-mixity on the fracture toughness of the Ti-6Al-4V/FM-5 adhesive bonded system was also evaluated. DCB tests in conjunction with end-notched flexure (ENF) and mixed-mode flexure (MMF) tests, were used to fracture the bonded joints under pure mode I, pure mode II, and a combination of mode I and II loadings. The results showed that the mode I fracture toughness was twice as large as the mode II toughness. This was a rather surprising find, in sharp contrast to what several researchers have observed in the past. Our current understanding is that the crack path selection during the failure process plays a significant role in explaining this anomalous behavior. Finally, failure envelopes were generated for the titanium/FM-5 bonded system, both prior to and following thermal aging. These envelopes could serve as useful tools for engineers designing with Ti-6Al-4V/FM-5 bonds. / Ph. D.

Un microscope à force atomique (AFM) est utilisé pour caractériser des matériaux isolant ou semi-conducteur avec une résolution pouvant atteindre l'échelle atomique. Ce microscope est constitué d'un capteur de force couplé à une électronique de contrôle pour pouvoir correctement caractériser ces matériaux. Parmi les différents modes (statique et dynamique), nous nous focalisons essentiellement sur le mode dynamique et plus particulièrement sur le fonctionnement sans contact à modulation de fréquence (FM-AFM). Dans ce mode, le capteur de force est maintenu comme un oscillateur harmonique par le système d'asservissement. Le projet ANR Pnano2008 intitulé : ”Cantilevers en carbure de silicium à piézorésistivité métallique pour AFM dynamique à très haute fréquence" a pour objectif d'augmenter significativement les performances d'un FM-AFM en développant un nouveau capteur de force très haute fréquence. Le but est d'augmenter la sensibilité du capteur et de diminuer le temps nécessaire à l'obtention d'une image de la surface du matériau. Le système de contrôle associé doit être capable de détecter des variations de fréquence de 100mHz pour une fréquence de résonance de 50MHz. Etant donné que les systèmes présents dans l'état de l'art ne permettent pas d'atteindre ces performances, l'objectif de cette thèse fut de développer un nouveau système de contrôle. Celui-ci est entièrement numérique et il est implémenté sur une carte de prototypage basée sur un FPGA. Dans ce mémoire, nous présentons le fonctionnement global du système ainsi que ses caractéristiques principales. Elles portent sur la détection de l'écart de fréquence de résonance du capteur de force. / An atomic force microscope (AFM) is used to characterize insulating materials or semiconductors with a resolution up to the atomic length scale. The microscope includes a force sensor linked to a control electronic in order to properly characterize these materials. Among the various modes (static and dynamic), we focus mainly on the dynamic mode and especially on the frequency modulation mode (FM-AFM). In this mode, the force sensor is maintained as a harmonic oscillator by the servo system. The research project ANR Pnano2008 entitled: "metal piezoresistivity silicon carbide cantilever for very high frequency dynamic AFM" aims to significantly increase the performance of a FM-AFM by developing new very high frequency force sensors. The goal is to increase the sensitivity of the sensor and to decrease the time necessary to obtain topography images of the material. The control system of this new sensor must be able to detect frequency variations as small as 100mHz for cantilevers with resonance frequencies up to 50MHz. Since the state-of-the-art systems doe not present these performances, the objective of this thesis was to develop a new control system. It is fully digital and it is implemented on a FPGA based prototyping board. In this report, we present the system overall functioning and its main features which are related to the cantilever resonant frequency detection. This detection is managed by a phase locked loop (PLL) which is the key element of the system.

La microscopie à force atomique (AFM) permet d’étudier à l’échelle nanométrique la surface d’échantillons. Elle offre de nombreux avantages par rapport aux microscopes optiques et aux microscopes électroniques, tout en évitant des étapes de préparation particulières : pas de nécessité de congeler, de métalliser ou de teinter l’échantillon ni de travailler sous vide. La résolution de l'imagerie AFM est principalement déterminée par la morphologie de la sonde utilisée et peut atteindre la résolution moléculaire. Toutefois, les sondes en silicium sont très fragiles. De plus, leur forme pyramidale ou conique génère des artefacts sur l’image résultante. Parmi les sondes actuellement en développement, les sondes à nanotubes de carbone mono-paroi offrent de bonnes caractéristiques en termes de qualité d'imagerie et de longévité. Ces sondes sont plus résistantes et de plus petite taille que les sondes traditionnelles.Cette thèse s’intéresse à la fabrication directe de sondes à nanotubes mono-paroi sur des extrémités de pointes AFM commerciales par la méthode de dépôt chimique en phase vapeur assistée par filament chaud dans un réacteur développé au CBMN. En jouant sur les paramètres de synthèse, tels que la quantité de catalyseur ou la température, nous optimisons le protocole de synthèse originel en collaboration avec son auteur Anne-Marie Bonnot afin de l’adapter à notre réacteur. Les nanotubes obtenus sont caractérisés par les microscopies Raman, électronique à balayage et transmission et à force atomique. La caractérisation montre que les nanotubes obtenus ont une structure mono-paroi. Le rendement d’obtention de sondes nanotubes utilisables est de 30%.Les courbes d’approche-retrait d'AFM nous donnent des informations sur la sonde à nanotube utilisée, telles que sa raideur, le nombre de nanotubes en contact avec la surface. Ces courbes nous permettent de sélectionner les paramètres d’imagerie. Deux échantillons sont testés avec les sondes produites : du graphite pyrolytique haute orientation et des origamis d’ADN rectangulaires. Nous réalisons des expériences d’imagerie avec des sondes à nanotube dans l’air en mode dynamique FM et en milieu liquide en mode Peak Force. Les résultats montrent des images à haute résolution de l’origami d’ADN où la période de 5,8 nm est observable. Les sondes à nanotube présentent également une plus longue durée de vie que les pointes AFM en silicium. / Atomic force microscopy (AFM) is used to study at nanometer scale samples on surfaces. It offers many advantages over conventional optical microscopes and electron microscopes: no freezing, metal coating, vacuum or dye is needed to prepare the sample. The AFM imaging resolution is mostly determined by the sharpness of the used probe and can reach molecular resolution. However, silicon probes are brittle. Additionally, their pyramidal or conical shape generates artifacts on the resulting image. Among the probes currently under development, single-walled carbon nanotube probes offer good characteristics in terms of imaging quality and longevity. These probes are more resistant and smaller in size than traditional probes.This thesis focuses on the direct fabrication of single-wall nanotube probes at the apex of commercial AFM tips by the hot-filament chemical vapor deposition method in a reactor developed at CBMN. By playing on the synthesis parameters, such as the amount of catalyst or the temperature of synthesis, we optimize the original synthesis protocol in collaboration with its author Anne-Marie Bonnot in order to adapt it to our reactor. The nanotubes obtained are characterized by Raman, scanning electron microscopy and transmission electron microscopy and AFM. The characterization shows that the nanotubes obtained have a single-wall structure. The yield of nanotube probes for AFM is 30%.AFM approach-retract curves give us information about the nanotube probe used, such as its stiffness or the number of nanotubes in contact with the surface. These curves allow us to select the imaging parameters. Two samples are tested with the produced probes: highly oriented pyrolytic graphite and rectangular DNA origamis. We image the samples with nanotube probes in both air with dynamical FM mode and in liquid medium with Peak Force mode. The results show high resolution images of DNA origami where the 5.8 nm period is observable. Nanotube probes also have longer life than silicon AFM tips.