Avec l’avènement des NEMS, MEMS, films minces et autres revêtements, la caractérisation des propriétés mécaniques à uneéchelle locale est primordiale. A cet effet, l’essai d’indentation instrumentée permet l’acquisition continue de la réponse (courbeforce – profondeur de pénétration) d’un matériau à la pénétration d’un indenteur de géométrie donnée. Le post-traitement d’unetelle courbe permet la détermination de propriétés telles que le module d’indentation ou la dureté. Cette analyse est basée surla théorie du contact élastique, qui suppose une géométrie axisymétrique parfaite de la pointe d’indentation, un comportementpurement élastique du matériau, et la non-prise en compte des déplacements radiaux dans la zone de contact. En pratique, ceshypothèses sont souvent mises en défaut : les indenteurs sont généralement des pyramides à 3 pans (Berkovich, Cube Corner)ou 4 pans (Vickers, Knoop) présentant un émoussement de la pointe, et le comportement mécanique des matériaux est souventcomplexe. La correction de la relation de Sneddon, utilisée dans la méthode d’Oliver et Pharr pour l’analyse des essais denanoindentation, est donc nécessaire. Dans le cadre de cette thèse, nous nous sommes intéressés à la détermination de ce facteurde correction, qui n’est pas une valeur universelle ni unique comme le préconisent certains auteurs. Il dépend notamment de lapression exercée par la pointe d’indentation et du matériau sollicité. Cette étude s’est faite sur la base de la détermination de laloi de comportement d’un des matériaux standards utilisés pour la calibration de l’essai de nanoindentation, la silice fondue.Ce matériau présente un comportement mécanique spécifique : sa déformation anélastique s’effectue par un mécanisme dedensification. Dans un premier temps, les paramètres de cette loi de comportement sont identifiés par une approche inversecombinant la simulation numérique 3D de l’essai d’indentation à l’optimisation de la fonction objectif au moyen d’unalgorithme génétique. Le facteur de correction est ensuite déterminé pour deux géométries de pointes et à différentes valeursdu rapport adimensionnel "profondeur de pénétration/rayon de pointe". La méthodologie proposée a été appliquée à ladétermination du module d’indentation d’un acier inox. / With the advent of NEMS, MEMS, thin films and other coatings, the characterization of local mechanical properties is achallenge. For this purpose, the instrumented indentation test allows for the continuous acquisition of the response (loadpenetration depth) of the material using an indenter of given geometry. The post-processing of such a curve allows thedetermination of the indentation modulus or the hardness of that material. This analysis relies on the elastic contact theory,which assumes an axisymmetric and perfect indenter, a purely elastic behaviour, and no radial displacements in the contactarea. In practice, those assumptions are defeated: indenters shapes are rather three-sided (Berkovich, Cube Corner) or foursided (Vickers, Knoop) pyramids, with blunted tips. Furthermore, mechanical behaviour is rather complex. The introductionof a correction factor in the Sneddon’s relationship, on which is based the Oliver and Pharr method for the analysis ofnanoindentation data is then necessary. Whithin the scope of this work, we aimed at determining this correction factor, whichhas not a unique nor a universal value, as recommended by some authors. It depends on the pressure distribution beneath theindenter and on the tested material. This study is based on the identification of the constitutive law of one of the referencespecimen used for calibration of the nanoindentation test, namely fused silica. The latter exhibits a specific mechanicalbehaviour, its anelastic deformation being achieved by a densification mechanism. In a first step we have determined the modelparameters by an inverse approach combining the 3D numerical simulation of the indentation test with the optimization of theobjective function using a genetic algorithm. The correction factor is then determined for two tip geometries and at severalpenetration depth over tip radius adimensional ratios. The proposed methodology was applied to the determination of theindentation modulus of an inox steel.

Les semiconducteurs organiques (OSC) tels que les composés organiques photovoltaïques (OPVs), les diodes électroluminescentes organiques (OLEDs) ou encore les transistors organiques à effet de champ (OFETs) constituent un domaine de recherche très attractif en raison de leur potentiel en tant que couches actives dans les dispositifs optoélectroniques. Les composés aromatiques polycycliques ainsi que les hétéroaromatiques sont considérés comme des matériaux prometteurs pour les OSC en raison de leurs conductivités électriques potentielles, de leurs propriétés optiques ainsi que de leurs assemblages géométriques. Ces deux systèmes et leurs propriétés photophysiques ont été étudiés dans les trois chapitres de cette thèse. Dans le premier chapitre, une étude sur un ensemble d'acènes linéaires, angulaires et condensés consistant en des liens hétéroatomes avec des agrégations uniques a été décrite et analysée. Les hétéroacènes N-fusionnés angulaires et π-étendus sont la classe principale étudiée dans le deuxième chapitre. Leurs synthèses sont basées sur la réaction de couplage de Suzuki-Miyaura et la réaction de Cadogan. Outre les acènes et les hétéroacènes N-fusionnés, les N-hétéroaromatiques ont fait l'objet d'une attention particulière dans le domaine de matériaux. L'un d'entre eux est la classe des quinazolines utilisées comme partie acceptrice d'électrons dans les structures push-pull pour le transfert de charge intramoléculaire (TCI). L'étude des relations entre les structures dérivées du motif quinazoline de type donneur d'électron-accepteur-donneur (D-A-D) et leurs propriétés de photoluminescence est le principal travail mentionné dans le troisième chapitre. / Organic semiconductors (OSCs) are a highly attractive research field due to their potentials as active layers in optoelectronic devices such as organic field-effect transistors (OFETs), organic photovoltaic (OPVs) and organic light emitting diodes (OLEDs). Polycyclic aromatic compounds as well as heteroaromatics are considered as promising materials for OSCs due to their semi conductivity properties, optical properties and geometric structures. The mentioned systems and their photophysical properties were investigated in three chapters of my thesis. In the first chapter, a study on a set of linear, angular and condensed acenes consisting of heteroatom linkages with unique aggregations was described and analyzed. The angular and π-extended N-fused heteroacenes are the main class studied in the second chapter. Their synthesis is based on the Suzuki-Miyaura coupling and the Cadogan reactions. Besides acenes and N-fused heteroacenes, N-heteroaromatics have gained attention in material area. One of them is the quinazoline class that is known as an electron withdrawing unit in push-pull structures for intramolecular charge transfer (ICT). The investigation of the relationships between the electron donor-acceptor-donor (D-A-D) quinazoline-based structures and their photoluminescence properties is the main work mentioned in the third chapter.

The project explores the possibilities of using additive manufacturing (3d-printing) to build architecture. Through a combination of theoretical research and practical experiments a building system has been developed which has the capabilities to create houses with great geometric flexibilities to a affordable price today. The construction system Perimeter is demonstrated in a pavilion situated at Norra Djurgården in Stockholm. / Projektet undersöker möjligheterna att använda additiv tillverkning (3d-printning) för att bygga arkitekturen. Genom en kombination av teoretisk forskning och praktiska experiment har ett byggsystem utvecklats som har kapacitet att skapa hus med stora geometriska flexibilitet till ett överkomligt pris i dag. Konstruktionssystemet Perimeter demonstreras i en paviljong belägen på Norra Djurgården i Stockholm.

<p>Additive manufacturing (AM) can be an advantageous substitute to various traditional manufacturing techniques. Due to the ability to rapidly create products, AM has been traditionally used to prototype more efficiently. As the industry has progressed, however, use cases have gone beyond prototyping into production of complex parts with unique geometries. Amongst the most popular of AM processes is fused deposition modeling (FDM). FDM fabricates products through an extrusion technique where plastic filament is heated to the glass transition temperature and extruded layer by layer onto a build platform to construct the desired part. The purpose of this research is to elaborate on the potential of this technology, while considering environmental impact as it becomes more widespread throughout industry, research, and academia.</p> <p>Although AM consumes resources more conservatively than traditional methodologies, it is not free from having environmental impacts. Several studies have shown that additive manufacturing can affect human and environmental health by emitting particles of a dynamic size range into the surrounding environment during a print. To begin this study, chapters investigate emission profiles and characterization of emissions from FDM 3D printers with the intention of developing a better understanding of the impact from such devices. Background work is done to confirm the occurrence of particle emission from FDM using acrylonitrile butadiene styrene (ABS) plastic filament. An aluminum bodied 3D printer is enclosed in a chamber and placed in a Class 1 cleanroom where measurements are conducted using high temporal resolution electrical low-pressure impactor (ELPI), scanning mobility particle sizer (SMPS), and optical particle sizer (OPS), which combined measure particles of a size range 6-500nm. Tests were done using the NIST standard test part and a honeycomb infill cube. Results from this study show that particle emissions are closely related to filament residence time in the extruder while less related to extruding speed. An initial spike of particle concentration is observed immediately after printing, which is likely a result of the long time required to heat the extruder and bed to the desired temperature. Upon conclusion of this study, it is theorized that particles may be formed through vapor condensation and coagulation after being released into the surrounding environment.</p> <p>With confirmation of FDM ultrafine particle emission at notable concentrations, an effort was consequently placed on diagnosing the primary cause of emission and energy consumption based on developed hypotheses. Experimental data suggests that particle emission is mainly the result of condensing and agglomerating semi-volatile organic compounds. The initial emission spike occurs when there is dripping of semi-liquid filament from the heated nozzle and/or residue left in the nozzle between prints; this supports the previously stated hypothesis regarding residence time. However, the study shows that while printing speed and material flow influence particle emission rate, the effects from these factors are relatively insignificant. Power profile analysis indicates that print bed heating and component temperature maintaining are the leading contributors to energy consumption for FDM printers, making time the primary variable driving energy input.</p> <p>To better understand the severity of FDM emissions, further investigation is necessary to diligence the makeup of the process output flows. By collecting exhaust discharge from a Makerbot Replicator 2x printing ABS filament and diffusing it through a type 1 water solution, we are able to investigate the chemical makeup of these compounds. Additional exploration is done by performing a filament wash to investigate emissions that may already be present before extrusion. Using solid phase micro-extraction, contaminants are studied using gas chromatography mass spectrometry (GCMS) thermal desorption. Characterization of the collected emission offers more comprehensive knowledge of the environmental and human health impacts of this AM process.</p> <p>Classification of the environmental performance of various manufacturing technologies can be achieved by analyzing their input and output material, as well as energy flows. The unit process life cycle inventory (UPLCI) is a proficient approach to developing reusable models capable of calculating these flows. The UPLCI models can be connected to estimate the total material and energy consumption of, and emissions from, product manufacturing based on a process plan. The final chapter focuses on using the knowledge gained from this work in developing UPLCI model methodology for FDM, and applying it further to the second most widely used AM process: stereolithography (SLA). The model created for the FDM study considers material input/output flows from ABS plastic filament. Energy input/output flows come from the running printer, step motors, heated build plate, and heated extruder. SLA also fabricates parts layer by layer, but by the use of a photosensitive liquid resin which solidifies when cured under the exposure of ultraviolet light. Model material input/output flows are sourced from the photosensitive liquid resin, while energy input/output flows are generated from (i) the projector used as the ultraviolet light source and (ii) the step motors. As shown in this work, energy flow is mostly time dependent; material flows, on the other hand, rely more on the nature of the fabrication process. While a focus on FDM is asserted throughout this study, the developed UPLCI models show how conclusions drawn from this work can be applied to different forms of AM processes in future work.</p>

I det här utvecklas en reproducerbar polymerisationsmetod för att uppnå en stabil produktion av poly(ε-caprolakton-co-p-dioxanon) (PCLDX), skala upp filamenttillverkningen för att producera 1.75 mm långa filament och optimera 3D-utskriftsprocessen för att tillverka ställningar/anordningar för mjukvävnadsteknik. PCLDX, med högre nedbrytningshastighet och bättre flexibilitet jämfört med poly(ε-caprolactone) (PCL), syntetiserades på ett reproducerbart sätt genom sampolymerisering. Den syntetiserade PCLDX uppvisade önskvärd sammansättning (85 mol% CL : 15 mol% DX), molmassa (cirka 40 kg∙mol-1), dispersitet (cirka 1.8) och relativt låg smältpunkt (cirka 45 ℃). För att tillverka tredimensionella matriser av PCLDX utformades och optimerades två processer, filamenttillverkning och 3D printning. För filamenttillverkningsprocessen användes låg extruderingstemperatur (65 och 80 ℃) och låg extruderingshastighet (100 cm∙min-1) för att spara energi och minimera nedbrytningen. PCLDX-filament med en jämn diameter på 1.75 mm tillverkades genom att använda en passande partikelstorlek (diameter på 3-4 mm) och en kylmetod (blandning av vatten och torris, 0 ℃). De erhållna filamenten uppvisade lägre Youngs modul (25 % lägre än PCL), PCLDX batch oberoende termiska egenskaper, god ytkvalitet och printbarhet. Den termiska nedbrytningen av PCLDX under processen var försumbar och molmassan var nästintill oförändrad. Processen har skalats upp för att producera stora mängder PCLDX-filament, vars produktivitet nådde upp till 140 g∙h-1. Tredimensionella matriser tillverkades genom att printa önskad design genom manuell matning och låg printhastighet (5 mm/s). En isplatta användes för att kyla ner maskinen under printningen för att undvika bucklingproblem. Det optimerade printprotokollet genererade ingen termisk nedbrytning av polymeren, påverkade inte polymerens molmassa eller dispersitet. De producerade matriserna hade samma termiska egenskaper oavsett polymerbatch och god ytkvalitet. Det optimerade printprotokollet användes också framgångsrikt för att skriva ut komplicerade prototyper, t.ex. menisk och knäprotes för potentiella biomedicinska tillämpningar. / In this project, we develop a reproducible polymerization method to achieve stable production of poly(ε-caprolactone-co-p-dioxanone) (PCLDX), scale-up the filament fabrication to produce 1.75 mm filaments and optimize 3D printing process to manufacture scaffolds/devices for soft tissue engineering. PCLDX, with a higher degradation rate and better pliability compared to poly(ε-caprolactone) (PCL), was successfully synthesized by reproducible copolymerization of ε-caprolactone (CL) and p-dioxanone (DX). The synthesized PCLDX exhibited a polymer composition of 85 mol% CL : 15 mol% DX, molar mass around 40 kg∙mol-1, dispersity around 1.8, and relatively low melting point around 45 ℃. From PCLDX particles to final scaffolds, two processes, including filament fabrication and scaffold manufacturing, were designed and optimized. For the filament fabrication process, low extrusion temperature (65 and 80 ℃) and low extrusion speed (100 cm∙min-1) were applied to save energy and minimize degradation. PCLDX filaments with an even diameter of 1.75 mm were fabricated using suitable particle sizes (diameter of 3-4 mm) and a cooling method (mixture of water and dry ice, 0℃). The obtained filaments exhibited lower young’s modulus (25% lower than PCL), consistent thermal properties, good surface quality, and printability. The thermal degradation of PCLDX during the process was negligible, and the molar mass was kept almost unchanged. The process has been scaled up to produce high amounts of PCLDX filaments, whose productivity rate reached up to 140 g∙h-1. For the scaffold manufacturing process, porous scaffolds were manufactured by feeding manually and printing slowly (5 mm/s). The printability was assessed and validated using produced PCL/PCLDX filaments and commercial PCL filaments. The optimized printing protocol maintained the molar mass and dispersity of the material. The produced scaffolds possessed consistent thermal properties independent on polymer batches and good surface quality. The optimized printing protocol was also successfully applied to print complicated prototypes, such as meniscus and knee prosthesis for potential biomedical applications.

The advent of ultrafast lasers has enabled micromachining schemes that cannot be achieved by other current techniques. Laser direct writing has emerged as one of the possible routes for fabrication of optical waveguides in transparent materials. In this thesis, the advantages and limitations of this technique are explored. Two extended-cavity ultrafast lasers were built and characterized as the laser sources for this study, with improved performance over existing systems. Waveguides are fabricated in oxide glass, chalcogenide glass, and polymers, these being the three major classes of materials for the telecommunication industry. Standard waveguide metrology is performed on the fabricated waveguides, including refractive index profiling and mode analysis. Furthermore, a finite-difference beam propagation method for wave propagation in 3D-waveguides is proposed. The photo-structural modifications underlying the changes in the material optical properties after exposure are investigated. The highly nonlinear processes of the light/matter interaction during the writing process are described using a free electron model. UV/visible absorption spectroscopy, photoluminescence spectroscopy and Raman spectroscopy are used to assess the changes occurring at the atomic level. Finally, the impact of laser direct writing on nonlinear waveguide applications is discussed.

Optical elements are the fundamental components in photonic systems and are used to transform an input optical beam into a desired beam profile or to couple the input beam into waveguides, fibers, or other optical systems or devices. Macroscopic optical elements are easily fabricated using grinding and polishing techniques, but few methods exist for inexpensive fabrication of micro optical elements. In this work we present an innovative technique termed Additive Lithography that makes use of binary masks and controlled partial exposures to sculpt photoresist into the desired optical surface relief profile. We explore various masking schemes for fabricating a variety of optical elements with unprecedented flexibility and precision. These masking schemes used in conjunction with the additive lithographic method allows us to carefully control the photoresist exposure and reflow processes for fabricating complex aspheric lens elements, including aspheric elements whose fabrication often proves highly problematic. It will be demonstrated that employing additive lithography for volume sculpting followed by controlled reflow can also allow us to fabricate refractive beam shaping elements. Finally we will discuss the dry etching techniques used to transfer these optical elements into the glass substrate. Thus the additive lithography technique will be demonstrated as an inexpensive, high throughput and efficient process in the fabrication of micro optical elements.

<p>  </p> <p>This thesis is motivated by the author’s observation that no systematic methodology is available to characterize and model mechanical behaviors of 3D printed parts in terms of their elastic modulus and critical loading capacities. Note that the more controlled and steadier printing process is, the easier the mechanical properties parts can be predicted. This research focuses on the methods for the prediction and validation of mechanical properties of 3D printed parts, and the focus is the responses of the printed parts subjected to tensile loads. The mathematic models are derived to characterize the mechanical properties of a part along three principal directions, and the models are validated experimentally by following the American Society for Testing and Materials (ASTM) D638 testing standards. It is assumed that a unidirectional plane stress occurs to each lamina to (1) simplify a compliance matrix with a size 3 by 3 and (2) characterize the mechanical properties by the elastic modules and strengths in three principal directions. Two mathematical models are developed using the experimental data from the classical laminate theory and finite element analysis (FEA) by the SolidWorks. Both of the developed models are used to predict the ultimate tensile strength and Young’s modulus of the specimens that are printed by setting different raster angles on different layers. This thesis work aims to (1) gain a better understanding of the impact of printing parameters on the strengths of printed parts and (2) explore the feasibility of using the classical laminate theory to predict the mechanical properties of the parts printed with different raster angles and patterns. To validate the proposed mathematic models, parts by FDM are tested by following the ASTM testing standards; moreover, it testifies if the selected ASTM-D638 is suitable to test 3D printed parts by FDM. </p>

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