Electron microscopy was first conducted in the 1930s with the advent of theTEM and later the STEM. In 1969, the first commercial SEM was released,with the possibility of retrofitting it to behave like a STEM following soonafterwards. In 1979, Danilatos and Robinson advanced electron microscopyby creating a new type of SEM which allowed a controlled quantity of gasinto the sample chamber, termed ESEM. The most recent evolution in thisline was the combination of ESEM and STEM in 2005, a procedure termedWet STEM.The focus of this work is on investigating applications of this new technique,along with the contrast mechanisms involved in forming an image. Tothat end, a wide variety of samples will be imaged. Clay and paint suspensions(colloids) are used to test Wet STEM’s capacity to image submergedobjects, as well as thin objects which are stacked together. Diblock copolymerfilms are used to test Wet STEM’s ability to distinguish chemically similarmaterials without staining, the physical effects of heavy metal staining andto demonstrate the necessity of gas for the purpose of charge neutralisation. Single cell biological samples are also investigated. Internal contrast inmammalian cells is visible without recourse to staining, but chemical fixationis required despite maintaining a high relative humidity. Bacteria are moreresilient and as such are easier to image than animal cells, requiring no priortreatment. When exposed to low relative humidity, bacteria are found tocollapse. The collapse pattern is observed to differ between wild-type andcytoskeletal-deficient bacteria of the same species and strain, so it is likelythat dehydration-induced collapse offers information about the position andshape of the bacterial cytoskeleton.

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Le bois est un matériau complexe, hétérogène et anisotrope. Ses propriétés mécaniques varient fortement en fonction de l'essence et de l'échelle considérées. Pour mieux comprendre le comportement du bois en fonction de sa structure, nous proposons dans le cadre de cette thèse une étude expérimentale à l'échelle des tissus qui est réalisée sur plusieurs types de bois : bois de peuplier, y compris bois de tension et bois d'épicéa. Compte tenu des faibles dimensions des échantillons testés, les mesures de déformation sont effectuées « sans contact » afin de s'assurer de ne pas perturber l'échantillon en cours de l'essai.Les premières séries de mesures sont réalisées sur les trois zones (tendue, normale, opposée) et selon les 3 directions matérielles (longitudinale, radiale et tangentielle) d'une tige de peuplier inclinée. Les résultats obtenus permettent de comparer des comportements mécaniques du bois de peuplier dans toutes les zones considérées en fonction de ses propriétés microscopiques.Les deuxièmes séries de mesures sont réalisées en compression, grandes déformations, dans la chambre d'un ESEM (Microscope électronique à balayage environnemental) sur du bois feuillu (peuplier) et sur du bois résineux (épicéa). Grâce aux images obtenues en période d'essai, du domaine élastique jusqu'à la densification, la réponse de chaque type du bois à la même sollicitation est illustrée.Enfin, une partie de la modélisation numérique par la MPM (Materiel Point Method) est proposée dans notre projet envisagé comme prolongement de ce travail. Il permettra de simuler le comportement mécanique du bois en grande déformation. / Wood is a complex, heterogeneous and anisotropic material. Its mechanical properties are highly variable according to the species and scale considered. In order to better understand the behaviour of wood in relation to its structure, this PhD work proposes an experimental study at the tissue scale. This work is performed on several types of wood: poplar, including tension wood and spruce. Considering the small dimensions of the tested samples, a “non-contact” method is used to limit perturbations, therefore ensuring the measurement precision.The first series of measurements were realised in the three zones (tension, normal, opposite) and for the three material directions (longitudinal, radial and tangential) of an inclined poplar tree. The results obtained allowed us to compare the mechanical properties of poplar wood in all zones in relation to their microscopic features.The second series of tests were performed in the chamber of an ESEM (Environmental Scanning Electron Microscope) on hardwood (poplar) and softwood (spruce). With the images obtained during the test, from the elastic zone to the densification, the response of each type of wood to the same solicitation is presented and commented.Finally, some numerical modelling by the MPM (Material Point Method) is proposed as prospects of the present work. It will allow the mechanical behaviour of wood in large deformation to be predicted.

The presented thesis focuses on designing a cryogenic cell for the study of water ice in an environmental scanning electron microscope (ESEM). This cell allows the study ice in the temperature range 80 K – 300 K in a nitrogen gas environment with a pressure of up to 400 Pa. The cell is cooled by a flow cooling system, where liquid or gaseous nitrogen is used as a refrigerant. The cell consists of a double-walled vessel with vacuum insulation, a flow-through heat exchanger, a sample well, and a cooled cell lid. The heat exchanger was designed to be able to dissipate the heat load at the level of 1 W. The exchanger is equipped with an electric resistance heater with an output of approximately 60 W, enabling heating of the sample at speeds of up to 100 K·min-1. The design also includes an LN2 gateway located on the door of the vacuum chamber of the microscope, to which the capillaries of the heat exchanger for the intake and outlet of refrigerant are connected. During the experimental verification of the cryogenic cell in the test vacuum chamber with a pressure of GN2 ~ 400 Pa, the limit temperature of 77.5 K on the sample well was reached.

<p>The work presented in this thesis is concerned with the microstructure of zinc oxide varistor materials used in surge protecting devices. This class of material has been characterised with special emphasis on the functional microstructure and the development of the microstructure during sintering. Several different techniques have been used for the analysis, especially scanning electron microscopy (SEM) in combination with electron beam-induced current (EBIC) analysis and <i>in-situ</i> studies of heat-treatment experiments and transmission electron microscopy (TEM) in combination with energy dispersive X-ray spectrometry (EDS) and electron holography. </p><p>Detailed TEM analyses using primarily centred dark-field imaging of grain boundaries, especially triple and multiple grain junctions, were used to reveal the morphological differences between the various Bi₂O₃ phases. The triple and multiple grain junctions were found to exhibit distinct differences in morphology, which could be attributed the difference in structure of the crystalline Bi₂O₃ polymorphs present in the junctions. </p><p>Electrical measurements were performed on individual ZnO/ZnO grain boundaries using EBIC in the SEM. The EBIC signal was found to depend strongly on the geometric properties of the interface and also on the symmetry of the depletion region at the interface. A symmetric double Schottky barrier was never observed in the experiments, but instead barriers with clear asymmetry in the depletion region. Experimental results together with computer simulations show that reasonably small differences in the deep donor concentrations between grains could be responsible for this effect.</p><p>Electron holography in the TEM was used to image the electrostatic potential variation across individual ZnO/ZnO interfaces. The sign of the interface charge, the barrier height (about 0.8 eV) and the depletion region width (100 to 150 nm) were determined from holography data. Asymmetries of the depletion region were also found with this technique. </p><p>The full sintering process of doped ZnO powder granules was studied <i>in-situ</i> in the environmental SEM. The densification and grain growth processes were studied through the sintering cycle. The formation of a functional microstructure in ZnO varistor materials was found to depend strongly on the total pressure.</p>

Macroscopic “carbonaceous” fossils such as Grypania, Katnia, Chuaria, and Tawuia play a critical role in our understanding of biological evolution in the Precambrian and their environmental implications. Unfortunately, understanding of these fossils remains limited by their relative simplicity of form, mode of preservation, and broad taphonomic variability. As a result, debate continues as to even the fundamental taxonomic affinity of the organisms. Megascopic coiled forms (i.e. Grypania and Katnia), for instance, have been interpreted as trace fossils, multicellular algae, prokaryotic filaments, macroscopic bacteria, cyanobacteria, or a transitional form from macroscopic to megascopic bacterial life. Similarly, Chuaria and Tawuia have been interpreted as compressed prokaryotic colonies, algae or algal reproductive stages, and multicellular plant material. Accessibility of new material and increasingly sophisticated means of analysis warrant a new look at these ancient fossils. Understanding the biological affinity of Grypania, in particular, is critical because current opinion is split as to whether these megascopic structures are more likely represent either multicellular bacteria or multicellular algae. Confirmation of either a bacterial or algal affinity would strongly influence fundamental understanding of biospheric evolution, particularly in terms of ocean oxygenation and the availability of bioessential trace metals. Although estimates for the degree of oxygenation required for a Grypania-like multicellular algae are only about 10 % present atmospheric levels (PAL), this estimate is still substantially higher than estimates based on geochemical data suggesting that oxygen levels may not have reached 10% PAL until the latter Neoproterozoic. It has been hypothesized that protracted oxygen of the Proterozoic biosphere may have played a critical role in the availability of redox-sensitive nutrients necessary for bacterial nitrogen fixation and the limiting of eukaryotic evolution. Within this context, our understanding of the taxonomic affinity of Grypania may profoundly affect our understanding of Earth’s biospheric evolution. This thesis provides morphological and geochemical analyses of Grypania spiralis from more than 100 newly collected specimens from the Belt Supergroup for comparison to previously collected specimens from all other known Grypania-bearing localities. Data is used to explore questions regarding the morphology, structural complexity, mode of preservation, and chemistry of fossil material, and to hypothesize on the taxonomic affinity of Grypania spiralis and its implications for biospheric evolution.

The work presented in this thesis is concerned with the microstructure of zinc oxide varistor materials used in surge protecting devices. This class of material has been characterised with special emphasis on the functional microstructure and the development of the microstructure during sintering. Several different techniques have been used for the analysis, especially scanning electron microscopy (SEM) in combination with electron beam-induced current (EBIC) analysis and in-situ studies of heat-treatment experiments and transmission electron microscopy (TEM) in combination with energy dispersive X-ray spectrometry (EDS) and electron holography. Detailed TEM analyses using primarily centred dark-field imaging of grain boundaries, especially triple and multiple grain junctions, were used to reveal the morphological differences between the various Bi2O3 phases. The triple and multiple grain junctions were found to exhibit distinct differences in morphology, which could be attributed the difference in structure of the crystalline Bi2O3 polymorphs present in the junctions. Electrical measurements were performed on individual ZnO/ZnO grain boundaries using EBIC in the SEM. The EBIC signal was found to depend strongly on the geometric properties of the interface and also on the symmetry of the depletion region at the interface. A symmetric double Schottky barrier was never observed in the experiments, but instead barriers with clear asymmetry in the depletion region. Experimental results together with computer simulations show that reasonably small differences in the deep donor concentrations between grains could be responsible for this effect. Electron holography in the TEM was used to image the electrostatic potential variation across individual ZnO/ZnO interfaces. The sign of the interface charge, the barrier height (about 0.8 eV) and the depletion region width (100 to 150 nm) were determined from holography data. Asymmetries of the depletion region were also found with this technique. The full sintering process of doped ZnO powder granules was studied in-situ in the environmental SEM. The densification and grain growth processes were studied through the sintering cycle. The formation of a functional microstructure in ZnO varistor materials was found to depend strongly on the total pressure.

Condensation of water vapor is an everyday phenomenon which plays an important role in power generation schemes, desalination applications and high-heat flux cooling of power electronic devices. Continuous dropwise condensation is a desirable mode of condensation in which small, highly-spherical droplets regularly form and shed off the surface before a thick liquid is formed, thereby minimizing the thermal resistance to heat transfer across the condensate layer. While difficult to induce and sustain, dropwise condensation has been shown to achieve heat and mass transfer coefficients over an order of magnitude higher than its filmwise counterpart. Superhydrophobic surfaces have been extensively studied to promote dropwise condensation with mixed results; often surfaces that are superhydrophobic to deposited droplets formed in the gas phase above the surface do not retain this behavior with condensed droplets nucleated and grown on the surface. Recently, nanostructured superhydrophobic surfaces have been developed that are robust to vapor condensation; however, these surfaces still are not ideal for condensation heat transfer due to the high thermal resistance of the vapor layer trapped underneath the droplets and the reduced footprint of direct contact between the highly-spherical droplets and the underlying substrate. This work has two main objectives. First, a comprehensive free energy based thermodynamic model is developed to better understand why traditional superhydrophobic surfaces often lose their properties when exposed to condensed droplets. The model is first validated using data from the existing literature and then extended to analyze the suitability of amphiphilic (e.g. part hydrophobic and part hydrophilic) nanostructured surfaces for condensation applications. Secondly, one of the promising amphiphilic surfaces identified by the thermodynamic model is fabricated and tested to observe condensation dynamic behavior. Two complementary visualization techniques, environmental scanning electron microscopy (ESEM) and optical (light) microscopy, are used to probe the condensation behavior and compare the performance to that of a traditional superhydrophobic surface. Observations from the condensation experiments are used to propose a new mechanism of coalescence that governs the temporal droplet size distribution on the amphiphilic nanostructured surface and continually generates fresh sites for the droplet nucleation and growth cycle that is most efficient at heat transfer.