Microbial-Induced Calcium Carbonate (CaCO3) Precipitation (MICP) is a biological process in which microbial activities alter the surrounding aqueous environment and induce CaCO3 precipitation. Because the formed CaCO3 crystals can bond soil particles and improve the mechanical properties of soils such as strength, MICP has been explored for potential engineering applications such as soil stabilisation. However, it has been difficult to control and predict the properties of CaCO3 precipitates, thus making it very challenging to achieve homogeneous MICP-treated soils with the desired mechanical properties. This PhD study investigates MICP at both micro and macro scales to improve the micro-scale understandings of MICP which can be applied at the macro-scale for improving the homogeneity and mechanical properties of MICP-treated sand. A microfluidic chip which models a sandy soil matrix was designed and fabricated to investigate the micro-scale fundamentals of MICP. The first important finding was that, during MICP processes, phase transformation of CaCO3 can occur, which results in smaller and less stable CaCO3 crystals dissolving at the expense of growth of larger and more stable CaCO3 crystals. In addition, it was found that bacteria can aggregate after being mixed with cementation solution, and both bacterial density and the concentration of cementation solution affect the size of aggregates, which may consequently affect the transport and distribution of bacteria in a soil matrix. Furthermore, bacterial density was found to have a profound effect on both the growth kinetics and characteristics of CaCO3. A higher bacterial density resulted in a quicker formation of a larger amount of smaller crystals, whereas a lower bacterial density resulted in a slower formation of fewer but larger crystals. Based on the findings from micro-scale experiments, upscaling experiments were conducted on sandy soils to investigate the effect of injection interval on the strength of MICP treated soils and the effects of bacterial density and concentration of cementation solution on the uniformity of MICP treated soils. Increasing the interval between injections of cementation solution (from 4 h to 24 h) increased the average size of CaCO3 crystals and the resulting strength of MICP-treated sand. An optimised combination of bacterial density and cementation solution concentration resulted in a relative homogeneous distribution of CaCO3 content and suitable strength and stiffness of MICP-treated sand. This thesis study revealed that a microfluidic chip is a very useful tool to investigate the micro-scale fundamentals of MICP including the behaviour of bacteria and the process of CaCO3 precipitation. The optimised MICP protocols will be useful for improving the engineering performance of MICP-treated sandy soils such as uniformity and strength.

The factors influencing senescence in white clover (Trifolium repens L.) are of considerable importance to the pastoral sector of New Zealand’s economy. The plant hormones, ethylene and the cytokinins, have been implicated as having opposing influences on senescence. This project focused on the cytokinins. The rate limiting step in cytokinin biosynthesis is catalysed by isopentenyl transferase (IPT) and the primary enzyme in the degradation of cytokinins is cytokinin oxidase/dehydrogenase (CKX). Both IPT and CKX genes are present as multi-gene families. A reduction in the level of active cytokinins either via a decrease in IPT expression, or an increase in CKX expression, or both, would implicate the cytokinins in developmental leaf senescence in white clover. White clover grows in a sequential pattern with leaves at all stages of development making it a good model for studying leaf development and senescence. A decrease in leaf chlorophyll is used as a marker for the onset of senescence. A micro-scale chlorophyll analysis was developed using the NanoDrop™ thus allowing tissue from the same leaflet to be used for gene expression and chlorophyll measurements. The pattern of chlorophyll changes was similar to that shown by Hunter et al.(1999) and Yoo et al.(2003) in white clover stolons used for ethylene research. Reverse transcriptase PCR (RT-PCR) and BLAST analysis was used to identify five putative IPT genes and seven putative CKX genes from white clover. RT-PCR demonstrated the expression of seven of these genes (TrIPT1. TrIPT13, TrIPT15 TrCKX1, TrCKX2, TrCKX6). Analysis with quantitative real-time PCR showed expression of TrCKX2 increased markedly during leaf expansion and was consistently high during senescence, suggesting a potential role for CKX in facilitating the progression of senescence.

Nowadays, the need for three-dimensional miniaturized components is increasing in many areas, such as electronics, biomedics, aerospace and defence, etc. To support the demands, various micro-scale fabrication techniques have been further introduced and developed over the last decades, including micro-electric-mechanical technologies (MEMS and LIGA), laser ablation, and miniature machine tools (mMTs). Each of these techniques has its own benefits, however miniature machine tools are superior to any others in enabling three-dimensional complex geometry with high relative accuracy, and the capability of dealing with a wide range of mechanical materials. Thus, mMTs are emerging as a promising fabrication process. In this work, various researches have been carried out based on the mMTs. The thesis presents micro-machining, in particular, micro-milling force model and three relevant subsystems for miniature machine tools (mMTs), to enhance machining productivity/efficiency and dimensional accuracy of machined parts. The comprehensive force model that predicts micro-endmilling dynamics has been developed. Unlike conventional macro-machining, the cutting mechanism in micro-machining is complex with high level of non-linearity due to the combined effects of edge radius, size, and minimum chip thickness effect, etc., resulting in no chip formation when the chip thickness is below the minimum chip forming thickness. Instead, part of the work material deforms plastically under the edge of a tool and the rest of the material recovers elastically. The developed force model for micro-endmilling is effective to understand the micro-machining process. As a result, the micro-endmilling force model is helpful to improve the quality of machined parts. In addition, three relevant subsystems which deliver maximum machining productivity and efficiency are also introduced. Firstly, ultrasonic atomization-based cutting fluid application system is introduced. During machining, cutting fluid is required at the cutting zone for cooling and lubricating the cutting tool against the workpiece. Improper cutting fluid application leads to significantly increased tool wear, and which results in overall poor machined parts quality. For the micro-machining, conventional cooling methods using high pressure cutting fluid is not viable due to the potential damage and deflection of weak micro-cutting tools. The new atomization-based cutting fluids application technique has been proven to be quite effective in machinability due to its high level of cooling and lubricating. Secondly, an acoustic emission (AE)-based tool tip positioning method is introduced. Tool tip setting is one of the most important factors to be considered in the CNC machine tool. Since several tools with different geometries are employed during machining, overall dimensional accuracy of the machined parts are determined by accurate coordinates of each tool tip. In particular, tool setting is more important due to micro-scale involved in micro-machining. The newly developed system for tool tip positioning determines the accurate coordinates of the tool tip through simple and easy manipulation. At last, with the advance of the 3D micro-fabrication technologies, the machinable miniaturized components are getting complex in geometry, leading to increased demand on dimensional quality control. However, the system development for micro-scale parts is slow and difficult due to complicated detection devices, algorithm, and fabrication of a micro-probe. Consequently, the entire dimensional probing system tends to become bulky and expensive. A new AE-based probing system with a wire-based probe was developed to address this issue with reduced cost and size, and ease of application. / Graduate

The mechanical properties of crystalline metals are strongly affected when the sample size is limited to the micron or sub-micron scale. At these scales, the mechanical properties are enhanced far beyond classical predictions. Besides, the surface to volume ratio significantly increases. Therefore surfaces and interfaces play a big role in the mechanical properties of these micro-samples. The effect of different interfaces on the mechanical properties of micro-samples is not yet well understood. The aim of this project is to characterize, understand, and predict the effect of confinement on deformation mechanisms at micro-scale. In this study, micro-pillars were fabricated by Focused Ion Beam (FIB). Micro-pillars were homogeneously coated with thin films by magnetron sputtering and cathodic arc deposition. The mechanical properties of carbon-coated-, chromium coated-, naked-, annealed- and non-annealed micro-pillars were measured. Afterwards, the results of micro-compression tests and Automated Crystal Orientation Mapping on Transmission electron microscopy (ACOM TEM) were compared and led to some surprising new findings.Dislocations are blocked by amorphous- and even crystalline coating in the deformed samples. Parallel slip systems were detected in the chromium layer and the copper micro-pillar. Even though the chromium layer has parallel slip systems, dislocation pile-up at the interface was found after deformation. The most significant finding in this study concerns the back stress of the dislocation pile-up, which affects the dislocation sources and causes an increase of the flow stress to generate new dislocations from these sources. Thermal annealing increases the strength and flow stress of FIB fabricated micro samples. The annealing treatment restores the lattice that was damaged by the FIB fabrication process. A higher stress is required to initiate the dislocation nucleation in a pristine lattice. Techniques of fabrication and investigation were developed to study the role of confinement and interfaces on the mechanical properties of materials at micro scale. Mechanisms of deformation were unraveled and a better understanding of the key parameters was reached. / Doctorat en Sciences de l'ingénieur et technologie / info:eu-repo/semantics/nonPublished

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La thèse a été réalisée dans le cadre d’un partenariat entre le laboratoire d’accueil (C2MA, IMT Mines d’Alès), l’entreprise Renault et un contrat Cifre. La prise de conscience de la dégradation de la qualité de l’air s’étend à tous les environnements, que ce soit à l’intérieur ou à l’extérieur. En Asie, cette prise de conscience se traduit par de très strictes réglementations de la qualité de l’air dans l’habitacle automobile. Les constructeurs se doivent de respecter ces nouvelles réglementations afin de pouvoir vendre leurs véhicules dans ces pays où le marché automobile est en pleine croissance (principalement en Chine). C’est dans ce contexte que Renault a décidé d’améliorer la prise en compte de la qualité de l’air habitacle dans le développement de ses véhicules. Les contraintes techniques et la numérisation des outils de travail ont orienté le travail de thèse vers la modélisation de cette qualité de l’air habitacle. Afin de pouvoir tendre vers cet objectif, plusieurs points ont été traités. Tout d’abord, l’émission des matériaux d’habitacle a été caractérisée afin de comprendre quels composés organiques volatils et quels matériaux étaient responsables de la dégradation de la qualité de l’air dans le véhicule. Ensuite, une nouvelle approche expérimentale a été développée permettant une caractérisation plus représentative de l’émission des matériaux dans l’habitacle. Ces travaux ont permis de confirmer l’importance de l’impact des conditions environnementales sur l’émission des matériaux qui avait été observé dans la littérature. L’étude de ces paramètres environnementaux a été traitée tant dans l’application de modèles présentées dans la littérature que de détermination de facteurs expérimentaux permettant une extrapolation maitrisée de la mesure de l’émission des matériaux à la qualité de l’air dans l’habitacle du véhicule. Enfin, une première méthodologie de modélisation a pu être proposée et appliquée à des systèmes simplifiés permettant de montrer la cohérence de la démarche empruntée. / The thesis is the result of a partnership between the C2MA (IMT Mines Alès) laboratory and Renault, a car manufacturer, as part of a Cifre contract. The awareness of air quality pollution spread among all indoor or outdoor environments. In Asia, strict regulations about vehicle interior air quality have been released to answer this social realisation. The car manufacturers must fulfil these requirements to be able to market their products in these countries (mainly in China). In these circumstances, Renault decided to improve the way they consider the vehicle interior air quality during the design of the vehicles. The thesis work concerns the modelling of vehicle interior air quality because of the technical obligations and the digitalisation. Different research question came up to follow this objective. First of all, the emission of passenger compartment’s materials has been characterised to understand what Volatile Organic Compounds (VOC) are responsible of the degradation of air quality inside a car and what are the sources. Then, a new characterisation approach of emission has been developed allowing to get a better toughness and representativeness of the results. These studies showed the significance of environmental conditions on the emission ofmaterials that had been studied in the scientific literature. The study of the impact of these environmental factors on the material’s emission was the next step and two different research axes has been explored: the study and development of the modelling available in the literature and the establishment of experimental factors leading to a mastered extrapolation of the characterisation of material’s emission to vehicle interior air quality. Finally, a first methodology has been proposed and applied to simplified systems showing the consistency of the developed process.

Η παρούσα διδακτορική διατριβή έχει ως κύριο αντικείμενο μελέτης την μοντελοποίηση και έλεγχο ενός μικρορομποτικού βραχίονα αναλυόμενου σε σφαιρικά πεπερασμένα στοιχεία σε περιβάλλον με εξωτερικές δυνάμεις Van Der Waals και συνυπολογίζοντας την τριβή. Τα κύρια σημεία είναι η εισαγωγή των εξωτερικών δυνάμεων στο μοντέλο του μικρορομπότ, η δημιουργία προσαρμοστικού ελέγχου για την επίτευξη ακολουθίας τροχιάς με αναγνώριση και ακύρωση των ισχυρών μεταβαλλόμενων εξωτερικών δυνάμεων, η αναγνώριση της θέσης και η αποφυγή εμποδίων σε άγνωστο περιβάλλον κλίμακας μικρομέτρων και ο καθορισμός τροχιάς για προσέγγιση σημείων στον χώρο εργασίας του μικρορομπότ. Προτείνεται επίσης ένα σύστημα επενέργησης σε διάταξη τένοντα με νανοκαλώδια και γίνεται μελέτη της αντοχής του σε σχέση με τις μέγιστες δυνάμεις-ροπές που παρουσιάζονται κατά τον έλεγχο. Για την αναγνώριση των εξωτερικών δυνάμεων δοκιμάζονται διαφορετικά είδη εκτιμητών και εξετάζεται η απόδοσή τους στο συνολικό σύστημα. / The present PhD thesis has a key object the modeling and control of a micro robotic manipulator, represented by spherical particles in an environment with external Van Der Waals forces and taking friction into account. The main points are a) the insertion of the external forces in the micro robot model, b) the adaptive control used in order to follow a desired trajectory, with identification and cancellation of the external forces, the position identification and avoidance of obstacles in an unstructured micrometer scale environment and the trajectory planning towards a target point in the task space of the microrobot. Also a tendon like actuation system is proposed, using nanowires and its mechanical properties are studied in order to determine the viability of its use in relation to the required torques during the control process. For the external force identification scheme, various types of estimators are proposed and their efficiency in the system is studied.

Vibratory gyroscopes have gained immense popularity in the microsystem technology because of their suitability to planar fabrication techniques. With considerable effort in design and fabrication, MEMS (Micro-electro-mechanical-system) vibratory gyroscopes have started pervading consumer electronics apart from their well known applications in aerospace and defence systems. Vibratory gyroscopes operate on the Coriolis principle for sensing rates of rotation of the r tating body. They typically employ capacitive or piezoresistive sensing for detecting the Coriolis force induced motion which is, in turn, used to determine the impressed rate of rotation. Interestingly, Nature also uses vibratory gyroscopes in its designs. Over several years, it has evolved an incredibly elegant design for vibratory gyroscopes in the form of dipteran halteres. Dipterans are known to receive mechanosensory feedback on their aerial rotations from halteres for their flight navigation. Insect biologists have also studied this sensor and continue to be fascinated by the intricate mechanism employed to sense the rate of rotation. In most Diptera, including the soldier fly, Hermetia illucens, the halteres are simple cantilever like structures with an end mass that probably evolved from the hind wings of the ancestral four-winged insect form. The halteres along with their connecting joint with the fly’s body constitute a mechanism that is used for muscle-actuated oscillations of the halteres along the actuation direction. These oscillations occur in the actuation plane such that any rotation of the insect body, induces Coriolis force on the halteres causing their plane of vibration to shift laterally by a small degree. This induced deflection along the sensing plane (out of the haltere’s actuation plane) results in strain variation at the base of the haltere shaft, which is sensed by the campaniform sensilla. The goal of the current study is to understand the strain sensing mechanism of the haltere, the nature of boundary attachments of the haltere with the fly’s body, the reasons of asymmetrical geometry of the haltere, and the interaction between both wings and the contralateral wing and haltere. In order to understand the haltere’s strain sensing mechanism, we estimate the strain pattern at the haltere base induced due to rotations about the body’s pitch, roll, and yaw axes. We model the haltere as a cantilever structure (cylindrical stalk with a spherical end knob) with experimentally determined material properties from nanoindentation and carry out analytical and numerical (finite element) analysis to estimate strains in the haltere due to Coriolis forces and inertia forces resulting from various body rotations. From the strain pattern, we establish a correlation between the location of maximum strain and the position of the campaniform sensilla and propose strain sensing mechanisms. The haltere is connected to the meta thoracic region of the fly’s body by a complicated hinge mechanism that actuates the haltere into angular oscillations with a large amplitude of 170 ◦ in the actuation plane and very small oscillation in the sensing plane. We aim to understand the reason behind the dissimilar boundary attachments along the two directions. We carry out bending experiments using micro Newton force sensor and estimate the stiffness along the actuation and sensing directions. We observe that the haltere behaves as a rigid body in the actuation direction and a flexible body in the sensing direction. We find the haltere to be a resonating structure with two different kinds of boundary attachments in the actuation and sensing directions. We create a finite element model of the haltere joint based on the optical and scanning microscope images, approximate material properties, and stiffness properties obtained from the bending experiments. We subsequently validate the model with experimental results. The haltere geometry has asymmetry along the length and the cross-section. This specific design of the haltere is in contrast to the the existing MEMS vibratory gyroscope, where the elastic beams supporting the proof mass are typically designed with symmetric cross-sections so that there is a mode matching between the actuation and the sensing vibrations. The mode matching provides high sensitivity and low bandwidth. Hence, we are interested in understanding the mechanical significance of the haltere’s asymmetry. First, we estimate the location of the maximum stress by using the actual geometry of the haltere. Next, by using the stiffness determined from bending experiments and mass properties from the geometric model, we find the natural frequencies along both actuation and sensing directions. We compare these findings with existing MEMS vibratory gyroscopes. The dipteran halteres always vibrate at the wing beat frequency. Each wing maintains 180 ◦ phase difference with its contralateral haltere and the opposite wing. Both wings and the contralateral wing-haltere mechanism exhibit coupled oscillatory motion through passive linkages. These linkages modulate the frequency and maintain the out- of-phase relationship. We explore the dynamics behind the out-of-phase behaviour and the frequency modulation of the wing-wing and wing-haltere coupled oscillatory motion. We observe that the linear coupled oscillatory model can explain the out-of-phase relationship between the two wings. However, a nonlinear coupled oscillator model is required to explain both frequency synchronization and frequency modulation of the wing with the haltere. We also carry out a finite element analysis of the wing-haltere mechanism and show that the out-of-phase motion between the wing and the haltere is due to the passive mechanical linkage of finite strength and high actuation force. The results of this study reveal the mechanics of the haltere as a rate sensing gyroscope and show the basis of the Nature’s design of this elegant sensor. This study brings out two specific features— the large amplitude actuated oscillations and the asymmetric geometry of the haltere structure— that are not found in current vibratory gyroscope designs. We hope that our findings inspire new designs of MEMS gyroscopes that have elegance and simplicity of the haltere along with the desired performance.

Organic Rankine cycles can be integrated with district heating systems and in applications of biogas digestion. Evaluating the performance of the installations by Againity AB in Ronneby and Norrköping, Sweden, is a unique opportunity which can support the establishment of ORC technology in the waste heat recovery market, unveiling its feasibilities and limitations. Operational data gathered from October 2017 until April 2018, provides this thesis with information about the ORC-systems. A method using Coolprop and Matlab has been used to detect steady-state series in the Ronneby installation using moving standard deviation and inclination criteria. By screening the data and selecting these series, analytical equations can be used to determine the performance of the installations and map the linear relationship between variables like pressure and generator power. The largest impact on the system in Ronneby is developed in the condenser. Large coolant volume flow creates large heat sink capacity and higher generator efficiency and power. However, with increasing generator power the condenser pressure decrease. Lower condenser pressure results in a decreased evaporation pressure, which could be maintained if the pump was able to run at higher frequencies. The Plant in Norrköping needs further studies and a review of its sensors. The code in Matlab is a resource to Againity and Linköpings university for future work in performance evaluation. It can be used to detect errors in energy balance, local readings, and picture the machines' performance graphically.

Les aciers inoxydables austéno-ferritiques présentent une microstructure biphasée dans laquelle se mêlent austénite et ferrite. Leurs caractéristiques mécaniques élevées ainsi que leur bonne tenue en corrosion en font un candidat sérieux pour remplacer les aciers inoxydables austénitiques. Malheureusement, la faible forgeabilité de ces alliages rend la fabrication de tôles particulièrement critique. En effet, le phénomène de « crique de rive » est fréquemment rencontré au cours des étapes du laminage à chaud. Par conséquent, cela nécessite des opérations supplémentaires comme le découpage des rives, ce qui aboutit à une augmentation des coûts de production. Les différents facteurs influençant la ductilité à chaud de ces aciers sont passés en revue afin d'identifier quels sont les zones d'ombres. La synthèse bibliographique révèle deux zones d'ombres : d'une part, le manque d'un essai de ductilité à chaud permettant de discriminer différentes microstructures en terme de résistance à la propagation de fissure à haute température ; et d'autre part l'absence de données quantitative concernant la partition de la déformation entre la ferrite et l'austénite lors des étapes de mise en forme à chaud. Le concept de travail essentiel de rupture a été appliqué à hautes températures. Il a été démontré que cette méthode est fiable et discriminante pour quantifier la résistance à la propagation de fissure à haute température. Elle permet également de générer un paramètre physique pertinent pour optimiser les microstructures par rapport à un mode de mise en forme donné. La technique conventionnelle de micro-grilles a été adaptée de manière à cartographier à haute température les déformations à l'échelle de la microstructure. Cette technique fournit en plus des résultats qualitatifs concernant les mécanismes de déformations, des données quantitatives à propos de la partition de la déformation entre la ferrite et l'austénite. Ces données peuvent être utilisées afin de valider les modèles qui prédisent le comportement à chaud des aciers duplex pendant les premières étapes du laminage à chaud. Les deux outils developpés au cours de cette étude permettent de donner des solutions pour éviter le phénomène de « crique de rives ». / The Duplex Stainless Steels (DSS) are defined as a family of stainless steels consisting of a two-phase microstructure involving δ-ferrite and γ-austenite. Exceptional combinations of strength and toughness together with good corrosion resistance under critical working conditions designate DSS a suitable alternative to conventional austenitic stainless steels. Unfortunately, the relatively poor hot workability of these alloys makes the industrial processing of flat products particularly critical. Cracking of the coils during hot rolling along the edges is frequently reported. As a consequence, additional operations like grinding, discontinuous processing or scraping are often required, leading to increased manufacturing costs. The different parameters affecting the hot working of duplex stainless steels have been reviewed in order to identify which are the missing pieces of the puzzle. The bibliographical review reveals that two pieces are missing in the hot workability puzzle. On the one hand, it is necessary to develop a new hot ductility test which allows discriminating microstructures in terms of high temperature tearing resistance, and on the other hand, quantitative data about the strain partitioning between ferrite and austenite during the hot working operations are needed. The Essential Work of Fracture concept has been applied at high temperature. It has been demonstrated that this method is a reliable and discriminating tool for quantifying the high temperature tearing resistance and to generate a physically relevant index to guide the optimization of microstructures towards successful forming operations. A modified micro-grid technique has been developed to experimentally simulate the local state of deformation of different duplex microstructures at high temperature. This technique provides qualitative results about the deformation features as well as quantitative data about the strain partitioning between ferrite and austenite. The micro-strain distributions measured can be used to validate the models predicting the hot deformation of duplex stainless steels during the roughing-mill operations. The two tools developed in this investigation allow suggesting possible remedies for the edge cracking phenomenon.