Previous studies on very high-cycle fatigue behavior of thin silicon films suggest a strong environmental dependence of the degradation mechanism, the precise nature of which is still subject to debate. In the present study, 2-micron-thick polycrystalline Si notched cantilever beam structures were used to investigate fatigue degradation in a high-temperature (80°C), high-humidity (90%RH) environment. The specimens were subjected to fully reversed sinusoidal loading at resonance (~40kHz) with stress amplitudes ranging from 1.46 to 1.6GPa, resulting in life-spans between 10⁶ and 10⁹ cycles. Comparison to a reference set of S-N data obtained at moderate environmental conditions (30°C and 50%RH) reveals a strong tendency for faster degradation with increasing temperature and humidity. The obtained damage accumulation rates in the 80°C, 90%RH environment exceed the reference by two orders of magnitude. Transmission electron microscopy (TEM) on vertical through-thickness slices reveals oxide thickening after cycling. The influence of ~20nm Al[subscript2]O₃ deposited on the surface of the fatigue specimens using Atomic Layer Deposition (ALD) technique was also studied. The presence of the alumina coating results in a higher fatigue resistance at 30°C and 50%RH, as well as a drastically different frequency evolution behavior. No oxide thickening was observed in the TEM for coated run-out specimens. A model is proposed to explain the different degradation behavior of the ALD-alumina coated samples. Thickened oxides after cycling appear consistent with the reaction-layer fatigue mechanism. Finite element modal analysis incorporating surface oxide layers and cracking was employed to relate the damage observed in TEM to the experimentally measured changes in resonant frequency. In conclusion, the reaction-layer mechanism seems capable of describing micron-scale polysilicon fatigue, even though the critical processes such as room-temperature, stress-assisted oxidation remain elusive.

To better understand consequences of classical assumptions regarding deformation mechanisms at the mesoscale, experimental observations of mesoscale deformation are presented. In light of actual micrographics of deformed polycrystals, the Von Mises criterion which states that 5 independent plastic deformation sources are needed at each material point to satisfy compatibility is studied, and the consequences of violating this assumption are presented through comprehensive parametric studies. From these studies, it can be concluded that not only are 5 independent plastic deformation sources not needed or observed at each point, but if less than 5 sources are allowed to be active a new physical understanding of a mechanism for kinematic hardening emerges. Furthermore, for enhanced subgrain rotation and evolution the Von Mises criterion must be violated. The second focus of this work is looking at studies, experiments, and models of mesoscale deformation in order to better understand controlling deformation length scales, so that they can be fed into a combined top-down, bottom-up, non-uniform crystal plasticity model that captures the variability provided by the mesoscale during deformation. This can in turn be used to more accurately model the heterogeneity provided by the response of each grain. The length scale intuited from insight into mesoscale deformation mechanisms through observation of experiments and analytical models is the free slip line length of each slip system, which informs non-uniform material parameters in a crystal plasticity model that control the yielding, hardening, and subsequent softening of each individual slip system. The usefulness of this non-uniform multiscale crystal plasticity model is then explored with respect to its ability to reproduce experimentally measured responses at different strain levels for different size grains. Furthermore, a "Mantle-Core" type model which combines both the non-uniform material parameter model and the limited slip model is created, in which the majority of plastic deformation is accommodated near the grain boundary under multi-slip, and uniform plastic deformation occurs in the bulk dominated by double or triple slip. These models are compared for similar levels of hardening, and the pole figures that result from their deformation are compared to experimental pole figures. While there are other models that can capture the heterogeneity introduced by mesoscale deformation at the grain scale, this combined top-down, bottom-up multiscale crystal plasticity model is by far one of the most computationally efficient as the heterogeneity of the mesoscale is does not emerge by introducing higher order terms, but rather by incorporating the heterogeneity into a simple crystal plasticity formulation. Therefore, as computational power increases, this approach will be among the first that will be able to perform accurate polycrystal level modeling while retaining the heterogeneity introduced by non-local mesoscale deformation mechanisms at the sub-grain scale.

Polycrystal models, beginning with the work of Sachs (1928) and Taylor (1938), have been used to predict very complex material behavior. The basis of these models is single crystal plasticity theory, which is then extended to model an actual (polycrystalline) material composed of a large number of single crystals or grains. Crystal plasticity models are formulated at the scale of the individual grain, which is viewed as a fundamental material element. To first order this is a reasonable approximation, and results in qualitatively good predictions. However, it is also well known that the grain is not a uniform entity, and that a great deal of non-uniform activity, including the development of well-defined dislocation structures, occurs within individual grains. The goals of this research are to complete an experimental data set for validation of material modeling, and to then improve the physical basis of predictive polycrystal plasticity models. Preferred orientations (textures) of oxygen free high conductivity (OFHC) copper were measured using reflection x-ray diffraction techniques. Monotonic strain paths included a variety of strain levels for both compression and torsion. One of the significant contributions of this research was the measurement of textures resulting from non-monotonic deformation histories, specifically compressive prestrain (to two different levels) followed by torsion to an effective plastic strain of 1.00. We also concluded synchrotron radiation experiments to map Laue images to examine subgrain microtexture formation at various stages of finite deformation. The second major contribution is to polycrystal plasticity modeling. Improvements to the plasticity model were achieved by including the effects of gradually developing, sub-grain scale microstructures, without explicitly modeling the structures, in terms of both crystallographic texture formation and work hardening. The effects of these microstructures were incorporated through the use of new internal state variables. They result in a broadening of the peaks of the macroscopic texture and a reduction of the rate of texture formation. Predictions of crystallographic orientation distributions were verified by plotting stereographs, which were shown to match measured crystallographic textures. The microstructural hardening law was introduced through a new form of latent hardening, which was shown to match experimental stress-strain behavior more closely than the basic model of Pierce, Asaro, and Needleman (1982). This latent hardening form augmented a Taylor-type term, which reflected statistically stored dislocations in the slip system hardness. Significantly, this improvement was also noted in the case of non-monotonic loading, which the standard model could not predict even to first order. Also, in the course of this research a planar double slip model was used as a precursor to the full three-dimensional modeling. The objective was to use the planar model to test various formulations, at least qualitatively, since it is a simpler model. As a result of comparisons between the three-dimensional simulations and the planar ones, the planar model was shown to be an insufficient tool for developing new texture and hardening evolution schemes as compared to the three-dimensional models. The planar model was unsuitable for modeling any but the most basic crystal plasticity relations and most simple deformation paths in a qualitative manner.

Material properties of polycrystalline aggregates should manifest the influence of crystallographic texture as defined by the orientation distribution function (ODF). A representation theorem on material tensors of weakly-textured polycrystals was established by Man and Huang (2012), by which a given material tensor can be expressed as a linear combination of an orthonormal set of irreducible basis tensors, with the components given explicitly in terms of texture coefficients and a number of undetermined material parameters. Man and Huang's theorem is based on the classical assumption in texture analysis that ODFs are defined on the rotation group SO(3), which strictly speaking makes it applicable only to polycrystals with (single) crystal symmetry defined by a proper point group. In the present study we consider ODFs defined on the orthogonal group O(3) and extend the representation theorem of Man and Huang to cover pseudotensors and polycrystals with crystal symmetry defined by any improper point group. This extension is important because many materials, including common metals such as aluminum, copper, iron, have their group of crystal symmetry being an improper point group. We present the restrictions on texture coefficients imposed by crystal symmetry for all the 21 improper point groups and we illustrate the extended representation theorem by its application to elasticity.

Thesis (Ph. D.)--University of Missouri-Columbia, 1997. / Typescript. Vita. Includes bibliographical references (leaves 114-122). Also available on the Internet.

Thesis (Ph. D.)--University of Missouri-Columbia, 1997. / Typescript. Vita. Includes bibliographical references (leaves 114-122). Also available on the Internet.

La caractérisation des contraintes internes présentes dans les matériaux de structure ou fonctionnels est primordiale pour une optimisation de leurs propriétés et de leur tenue en service. Ce travail de thèse est une contribution au développement d'une technique de microscopie par diffraction des rayons X, appelée "Differential Aperture X-ray Microscopy", (DAXM, permettant la caractérisation 3D et non-destructive de la microstructure de matériaux cristallins et des contraintes internes présentes dans le matériau. Cette technique est basée sur l'utilisation du rayonnement synchrotron; nous avons utilisé la ligne CRG BM32 du synchrotron européen ESRF. Le faisceau de rayons incident est polychromatique (5-25keV) et fortement focalisé (section sub-micrométrique). En raison la pénétration du faisceau dans le matériau, qui est typiquement de quelques dizaines de microns, l'image de diffraction collectée est une superposition des diagrammes de Laue de tous les cristaux situés sur le trajet du faisceau incident. La DAXM utilise, en supplément de la microdiffraction Laue "classique", un masque mobile (ici un fin fil de tungstène) qui absorbe une partie des faisceaux diffractés. L'analyse de l'évolution des niveaux de gris des pixels de l'image en fonction de la position du masque permet non seulement de reconstruire la microstructure du matériau en profondeur mais aussi d'accéder à la distribution 3D des déformations élastiques (et des contraintes associées). L'un des avantages de la DAXM est sa résolution spatiale, de l'ordre du micromètre, qui permet d'envisager l'analyse des concentrations de contraintes dans les matériaux polycristallins, dans le cadre des approches micromécaniques expérimentales.Le travail mené dans cette thèse avait pour but d'améliorer le dispositif expérimental existant,de mettre en place la formulation théorique du problème, et de développer les outils numériques permettant le traitement des données.Du point de vue expérimental, nous avons notamment développé une machine d'essai mécanique in-situ (flexion 4-points) adaptée à la ligne BM32, et nous proposons un masque multi-fil qui devrait permettre de réduire significativement la durée de l'acquisition des données.Nous avons établi les équations de triangulation reliant la position des pixels du détecteur,la position du fil, et la profondeur de la source le long du faisceau incident. On montre ainsi que la reconstruction 3D nécessite une procédure de dérivation des niveaux de gris; nous nous sommes limités dans ce travail à une dérivation par différence finie d'ordre 1, qui reste sensible au bruit d'image. Ces équations font apparaître la nécessité de déterminer la géométrie du montage avec grande précision. On propose pour cela l'utilisation de la fluorescence de l'échantillon. On adjoint aux équations géométriques une description mathématique simplifiée de l'atténuation du faisceau par l'échantillon, prenant en compte un coefficient d'absorption unique. Le modèle de calibration est testé sur plusieurs matériaux, avec de très bons résultats.La capacité de la DAXM à reconstruire une microstructure est testée sur des échantillons modèles pour lesquels la géométrie 3D de la microstructure est parfaitement connue : empilement de fin fils de GaN sur un substrat, et plan de macle dans un polycristal d'acier inoxydable (316L). On montre que la résolution de la DAXM est variable d'un pixel à l'autre du détecteur; la microstructure peut cependant être reconstruite avec une précision de l'ordre du micromètre.La DAXM est ensuite testée sur un échantillon d'UO2 implanté d'ions Kr, créant une couche de surface d'épaisseur micrométrique fortement déformée (collaboration CEA-Cadarache). On observe que la méthode de reconstruction proposée produit d'importants artefacts, qui sont dus à la transmission variable des faisceaux diffractés dans le masque. Nous mettons en place la formulation permettant de prendre en compte cet effet. / The characterization of the internal stresses present in structural or functional materials is essential for an optimization of their properties and their durability in service. This thesis work is a contribution to the development of the so-called '' Differential Aperture X-ray Microscopy'' (DAXM) technique, allowing 3D and non-destructive characterization of the microstructure of crystalline materials and internal stresses. This technique makes use of synchrotron radiation; we used the beamline CRG BM32 of the European synchrotron ESRF. The polychromatic and highly focused incident beam penetrates the sample, and the collected diffraction image is a superimposition of the Laue diagrams of all the crystals located along the path of the incident beam. The DAXM uses, in addition to the "conventional" Laue microdiffraction technique, a moving mask that absorbs part of the diffracted beams. The analysis of the evolution of the gray levels of the image pixels as a function of the position of the mask makes it possible not only to reconstruct the microstructure of the material at depth but also to access the 3D distribution of the elastic deformations (and associated stress). One of the advantages of the DAXM is its spatial resolution, of the order of a micrometer, which makes it possible to envisage the analysis of stress concentrations in polycrystalline materials, within the framework of experimental micromechanical approaches.The work carried out in this thesis was aimed at improving the existing experimental system,to put in place the theoretical formulation of the problem, and to develop the numerical tools allowing the processing of the data.From an experimental point of view, we have developed an in-situ mechanical test device (4-point bending) adapted to BM32, and we propose a multi-wire mask to significantly reduce the data acquisition time.We have established the geometric equations of the problem. It is thus shown that the 3D reconstruction requires a gray scale derivation procedure. This work is limited to the use of a finite difference derivation method of order 1, which remains sensitive to image noise. These equations show the need to determine the geometry of the setup with great precision. For this purpose, the use of the fluorescence of the sample is proposed, coupled with a simplified description of the beam attenuation by the sample taking into account only a single absorption coefficient. The calibration model is tested on several materials, with very good results.The capacity of the DAXM to reconstruct a microstructure is tested on model samples for which the 3D geometry of the microstructure is perfectly known: a stack of GaN wires on a substrate, and a twin plane in a stainless steel polycrystal. It is shown that the resolution of the DAXM is variable from one pixel to the other of the detector; the microstructure can however be reconstructed with an accuracy of the order of one micrometer.The DAXM is then tested on a sample of UO2 implanted by Kr ions, creating a highly deformed surface layer with micrometric thickness (collaboration with CEA-Cadarache). It is found that the proposed reconstruction method is affected by the variable transmission of the diffracted beams in the mask. We propose a formulation that takes this effect into account.

No description available.

In the present work, we studied the effect of liquid Bi on the microstructure evolution of ultrafinegrained Cu at elevated temperatures.

The excimer-laser annealed (ELA) polycrystalline silicon (p-Si or polysilicon) thin film, which influences more than 100-billion-dollar display market, is the backplane material of the modern advanced LCD and OLED products. The microstructure (i.e. ELA microstructure) and surface morphology of an ELA p-Si thin film are the two main factors determining the material properties, and they significantly affect the performance of the subsequently fabricated thin film transistors (TFTs). The microstructure is the result of a rather complex crystallization process during the ELA which is characterized as far-from-equilibrium, multiple-pulse-per-area and processing-parameter dependent. Studies of the ELA microstructure and the surface morphology closely related to the device performance as well as the microstructure evolution during the ELA process are long-termly demanded by both the scientific research and the industrial applications, but unfortunately have not been thoroughly performed in the past. The main device-performance-related characteristics of the ELA microstructure are generally considered to be the grain size and the presence of the dense grain boundaries. In the work of this thesis, an image-processing-based program (referred to as the GB extraction program) is developed to extract the grain boundary map (GB map) out of the transmission electron microscope (TEM) images of the ELA microstructure. The grain sizes are straightforwardly calculated from the GB map and statistically analyzed. More importantly, based on the GB maps, we propose and perform a rigorous scheme that we call the local-microstructure analysis (LMA) to quantitatively and systematically analyze the spatial distribution of the grain boundaries. The “local area” is mainly defined by the geometry and the location of a TFT. The successful extraction of the GB map and the subsequent LMA are permitted by our unique TEM skills to produce high-resolution TEM micrographs containing statistically significant number of grains for sensible quantitative analysis. The LMA unprecedentedly enables quantitative and rigorous analysis of spatial characteristics of the microstructure, especially the device geometry- and location-related characteristics. Additionally, we present and highlight the benefits of the LMA approach over the traditional statistical grain-size analysis of the ELA microstructure. From the grain-size analysis, we find that grain size across a statistically significant number of grains generally follows the same distribution as in the stochastic grain growth scenario at the beginning of the ELA process when the laser pulse (i.e. shot) number is small. As the shot number increases, the overall grain size monotonically increases while the distribution profile becomes broader. When the scan number reaches the ELA threshold (several tens of laser shots), the distribution profile substantially deviates from the stochastic profile and shows two sharp peaks in grain size around 300nm and 450nm, which is consistent with the previously proposed theory of energy coupling and nonuniform energy deposition during ELA. From the LMA, local nonuniformity of grain boundary density (GB density) at the device length scales and regions of high grain boundary periodicity are identified. More importantly, we find that the local nonuniformity is much more pronounced when p-Si film exhibits some level of spatial ordering, but less pronounced for a random grain arrangement. It is worth noting that the devices of different sizes and orientation have different sensitivity to the local nonuniformity of the ELA-generated p-Si thin film. In addition, based on the analysis results, the connection between the microstructure evolution and the partial melting and resolidification process of the Si film is discussed. Aside from the microstructure, the surface morphology of the ELA films, featuring pronounced surface protrusions, is characterized via an atomic force microscope (AFM). Attempts to planarize those surface protrusions detrimental to the subsequent device performance are conducted. In the attempts, the as-is (oxide-capped) ELA films and the BHF-treated ELA films are subjected to single shots of excimer irradiation. When the results are compared, an anisotropic melting phenomenon of the p-Si grains is identified, which appears to be strongly affected by the presence of the surface oxide capping layer. Conceptual models are developed and numerical simulations are employed to explain the observation of the anisotropic melting phenomenon and the effect of the surface oxide layer. Eventually, 41.8% reduction of root mean square (RMS) surface roughness is achieved for BHF-treated ELA films. The results gained in the systematic analysis of the ELA microstructure and the attempt of surface planarization further our understanding about (1) the device performance-related material microstructure of the ELA p-Si thin films, (2) the microstructure evolution occurring during multiple shots of the ELA process, and (3) the fundamental phase transformations in the far-from-equilibrium melt-mediated excimer-laser annealing processing of p-Si thin films. Such understanding could help engineers when designing the microelectronic devices and the ELA manufacturing process, as well as provide scientific researchers with insights on the melting and solidification of general polycrystalline materials, thus profoundly contributing to both the related scientific society and the technological community. The GB extraction program and the LMA scheme developed and demonstrated in the thesis, as another contribution to the related research filed, could also be generalized to the microstructural study of other polycrystalline materials where grain geometry and arrangement are of concern.