Nanoscale ferroelectric materials have numerous possible applications such as actively tunable photonic crystals, terahertz emitters, ultrasound transducers, and energy harvesters. One of most technologically relevant ferroelectric materials is lead zirconate titanate (PZT) due to its large piezoelectric response. However, there are limited methods currently available for creating nanoscale PZT structures. Current top-down patterning methods include material removal via a high energy beam, which damages the piezoelectric's properties, and wet etching, which is an isotropic process that results in poor edge definition. Similarly, current bottom-up approaches such as hard template-growth and hydrothermal processing have limited control over the aspect ratio of the structures produced and lack site specific registry. In this work, a bottom-up approach for creating PbZr₀.₅₂Ti₀.₄₈O₃ nanotubes was developed using soft-template infiltration by a sol-gel solution. This method allows excellent control of the structures produced, overcoming current manufacturing limitations. PZT nanotubes were fabricated with diameters ranging from 100 to 200 nm, aspect ratios (height to diameter) from 1.25:1 to 5:1, and wall thicknesses from 5 to 25 nm. The piezoelectric and ferroelectric nature of the nanotubes was characterized via scanning probe microscopy in order to investigate nanoscale phenomena. Specifically, the effects of lateral constraint, substrate clamping, and critical size on the extrinsic contribution to the piezoelectric response were studied and the results are discussed.

The goal of this research work is to further the understanding of crystal plasticity, particularly at reduced structural and material length scales. Fundamental understanding of plasticity is central to various challenges facing design and manufacturing of materials for structural and electronic device applications. The development of microstructurally tailored advanced metallic materials with enhanced mechanical properties that can withstand extremes in stress, strain, and temperature, will aid in increasing the efficiency of power generating systems by allowing them to work at higher temperatures and pressures. High specific strength materials can lead to low fuel consumption in transport vehicles. Experiments have shown that enhanced mechanical properties can be obtained in materials by constraining their size, microstructure (e.g. grain size), or both for various applications. For the successful design of these materials, it is necessary to have a thorough understanding of the influence of different length scales and evolving microstructure on the overall behavior. In this study, distinction is made between the effect of structural and material length scale on the mechanical behavior of materials. A length scale associated with an underlying physical mechanism influencing the mechanical behavior can overlap with either structural length scales or material length scales. If it overlaps with structural length scales, then the material is said to be dimensionally constrained. On the other hand, if it overlaps with material length scales, for example grain size, then the material is said to be microstructurally constrained. The objectives of this research work are: (1) to investigate scale and size effects due to dimensional constraints; (2) to investigate size effects due to microstructural constraints; and (3) to develop a size dependent hardening model through coarse graining of dislocation dynamics. A discrete dislocation dynamics (DDD) framework where the scale of analysis is intermediate between a fully discretized (e.g. atomistic) and fully continuum is used for this study. This mesoscale tool allows to address all the stated objectives of this study within a single framework. Within this framework, the effect of structural and the material length scales are naturally accounted for in the simulations and need not be specified in an ad hoc manner, as in some continuum models. It holds the promise of connecting the evolution of the defect microstructure to the effective response of the crystal. Further, it provides useful information to develop physically motivated continuum models to model size effects in materials. The contributions of this study are: (a) provides a new interpretation of mechanical size effect due to only dimensional constraint using DDD; (b) a development of an experimentally validated DDD simulation methodology to model Cu micropillars; (c) a coarse graining technique using DDD to develop a phenomenological model to capture size effect on strain hardening; and (d) a development of a DDD framework for polycrystals to investigate grain size effect on yield strength and strain hardening.

For thin epitaxial metal films, when the thickness is on the order of the Fermi wavelength, [lambda subscript F], quantum confinement can dramatically alter the physical properties of the film. These so-called Quantum Size Effects (QSE) can dramatically alter the morphology of thin films by an intricate interplay between kinetics and surface energy driven thermodynamics. These effects lead to rich growth-related phenomena in Pb(111) films grown on semiconductor substrates such as Si(111). For example, QSE can drive flat film formation when growth is dominated by surface energy oscillations. This is rather surprising for Pb/Si systems because of a rather high lattice mismatch. However, these films are not defect free, but rather show common occurrences of three defect types. Low Temperature Scanning Tunneling Microscopy (LT-STM) was utilized to characterize these defects on the atomic scale. Furthermore, these defects create modulations in the electron density resulting in fluctuations in QWS near defect sites. Another topic of recent interest is how QSE affect adsorption of as well as how adsorbates modify QSE for these Pb films. In this thesis, LT-STM and first principles calculations were utilized to study Cs adsorbates on Pb film surfaces, defects, and step edges. Cs adsorption is intricately related to the electronic structure of the surface, especially the defect sites which can act as surface traps. These Cs adsorbates, which are assumed to be ionized, enhance elastic surface scattering of empty-state electrons. This results in observable wave interference patterns near Cs impurities. Furthermore, Cs adsorbates, by an overall step energy reduction, can promote QSE-related nanostructures, which are otherwise too weak when kinetic effects cannot be ignored. This enhancement of "quantum stability" is driven by favorable Cs step binding and can be explained within the contexts of Density Functional Theory (DFT). / text

Porous tungsten is used to manufacture dispenser cathodes due to it refractory properties. Surface porosity is critical to functional performance of dispenser cathodes because it allows for an impregnated ceramic compound to migrate to the emitting surface, lowering its work function. Likewise, surface roughness is important because it is necessary to ensure uniform wetting of the molten impregnate during high temperature service. Current industry practice to achieve surface roughness and surface porosity requirements involves the use of a plastic infiltrant during machining. After machining, the infiltrant is baked and the cathode pellet is impregnated. In this context, cryogenic machining is investigated as a substitutionary process for the current plastic infiltration process. Along with significant reductions in cycle time and resource use, surface quality of cryogenically machined un-infiltrated (as-sintered) porous tungsten has been shown to significantly outperform dry machining. The present study is focused on examining the relationship between machining parameters and cooling condition on the as-machined surface integrity of porous tungsten. The effects of cryogenic pre-cooling, rake angle, cutting speed, depth of cut and feed are all taken into consideration with respect to machining-induced surface morphology. Cermet and Polycrystalline diamond (PCD) cutting tools are used to develop high performance cryogenic machining of porous tungsten. Dry and pre-heated machining were investigated as a means to allow for ductile mode machining, yet severe tool-wear and undesirable smearing limited the feasibility of these approaches. By using modified PCD cutting tools, high speed machining of porous tungsten at cutting speeds up to 400 m/min is achieved for the first time. Beyond a critical speed, brittle fracture and built-up edge are eliminated as the result of a brittle to ductile transition. A model of critical chip thickness (hc) effects based on cutting force, temperature and surface roughness data is developed and used to study the deformation mechanisms of porous tungsten under different machining conditions. It is found that when hmax = hc, ductile mode machining of otherwise highly brittle porous tungsten is possible. The value of hc is approximately the same as the average ligament size of the 80% density porous tungsten workpiece.

This research work is aimed at understanding the electronic properties of Bi(110) nanostructures. This study chiefly uses Scanning Tunneling Microscopy (STM), Scanning Tunneling Spectroscopy (STS) and Non Contact Atomic Force Microscope (NCAFM) to investigate the geometric and electronic structure of Bi(110) islands on highly oriented pyrolytic graphite (HOPG) substrate. STM measurements are the primary focus of the thesis which involves imaging the bismuth islands and study of its atomic structure. STM images of the Bi(110) islands reveal a ‘wedding cake’ profile of the bismuth islands that show paired layers on top of a base. I(V) (Current vs voltage) data was acquired via STS techniques and its first derivative was compared to DFT calculations. The comparison implied the presence of a dead wetting layer which was present only underneath the bismuth islands. We observed bilayer damped oscillations in the surface energy that were responsible for the stability of paired layers in Bi(110) islands. Interesting Moiré pattern arising out of misorientation between the substrate and the overlayer are also observed in STM images on some bismuth islands. Bright features pertaining to enhanced LDOS (local density of states) were observed on the perimeter of the bismuth islands and stripes in the STM images and STS dI/dV maps which appear at energies around the Fermi level. The bright features which we termed as ‘bright beaches (BB)’ are also observed on grain boundaries and defects that suggest that they are related to termination of the chain of bismuth atoms. The Bi(110) islands and stripes were observed to form preferred widths with a well defined periodicity. This peculiar phenomenon was attributed to a lateral quantum size effect (QSE) that results from a Fermi wave vector with appropriate shifts in Fermi energy. The widths of the islands prefer to adjust themselves at the nodes of this in-plane Fermi wavelength. NaCl deposited on a HOPG substrate forms cross shaped islands which were used as spacers to limit the interaction between the bismuth films and the underlying HOPG substrate. The NaCl islands are transparent to the flow of tunneling current and allow STS measurements. The LDOS of Bi/HOPG was very similar to the LDOS of Bi deposited on NaCl/HOPG which suggests that the wetting layer underneath the bismuth islands plays an important role in decoupling the film from the underlying substrate.

The increasing demand for powerful miniaturized products for all industrial applications has prompted the industry to develop new and innovative manufacturing processes to fabricate miniature parts. One of the major challenges facing the industry is the dynamic market which requires continuous improvements in design and fabrication techniques. This means providing products with complex features while sustaining high functionality. As a result, microfabrication has gained a wide interest as the technology of the future, where tabletop machine systems exist. Microforming processes have the capability of achieving mass production while minimizing material waste. Microforming techniques can produce net-shape products with intricacy in fewer steps than most conventional microfabrication processes. Despite the potential advantages, the industrial utilization of microforming technology is limited. The deformation and failure modes of materials during microforming is not yet well understood and varies significantly from the behavior of materials in conventional forming operations. In order to advance the microforming technology and enable the effective fabrication of microparts, more studies on the deformation and failure of materials during microforming are needed. In this research work, an effort to advance the current status of microforming processes for technologies of modern day essentials, is presented. The main contribution from this research is the development of a novel method for characterizing thin sheet formability by introducing a micro-mechanical bulge-forming setup. Various aspects of analyzing microscale formability, in the form of limiting strains and applied forces, along with addressing the well known size effects on miniaturization, were considered through the newly developed method. A high temperature testing method of microformed thin sheets was also developed. The aim of high temperature microforming is to study the material behavior of microformed thin sheets at elevated temperatures and to explore the capability of the known enhancement in formability at the macroscale level. The focus of this work was to develop a better understanding of tool-sheet metal interactions in microforming applications. This new knowledge would provide a predictive capability that will eliminate the current time-consuming and empirical techniques that, and this in turn would be expected to significantly lower the overall manufacturing cost and improve product quality.

Les effets d’échelle sur la résistance mécanique des matériaux, i.e. le fait que plus un échantillon de matière est grand, plus, en moyenne, sa contrainte à rupture sera faible, déjà soulignées par Leonardo da Vinci et Edmée Mariotte il y a des siècles, demeurent de nos jours un problème crucial pour établir des règles de sécurité et de conception de grandes structures à partir de données de laboratoire. Ces effets d’échelle sont généralement expliqués soit par une approche déterministe qui prédit une résistance asymptotique non nulle mais, par construction, ne tient pas compte des fluctuations de la résistance moyenne et de leur dépendance vis-à-vis de la taille, ou d'une approche statistique basée sur la théorie du maillon le plus faible qui implique une résistance nulle pour un système de taille infini.Récemment, un cadre alternatif a été proposé sur la base d’une interprétation de la rupture en compression des matériaux hétérogènes comme une transition de phase critique entre un état intact et un état rompu. Cette interprétation libère les hypothèses de base de la théorie du maillon le plus faible comme la fragilité extrême et l’indépendance entre évènements de microfracturation et prédit qu’un système de taille infinie conservera une résistance mécanique non nulle (σ_∞ ) mais une variabilité associée de la résistance nulle. En appliquant ce cadre critique, les effets d’échelle statistique sur la résistance en compression du béton, un matériau quasi-fragile typique et important en génie civil, sont étudiés dans cette thèse.A partir d’une importante série d’expériences de compression uniaxiale (527 essais) qui a été réalisée sur des échantillons du béton de quatre tailles différentes et trois microstructures différentes, nous démontrons (i) l’échec de la théorie du maillon le plus faible dans ce cas ; et au lieu de cela (ii) la pertinence du cadre critique pour tenir compte des effets d’échelle sur la résistance à rupture en compression du béton, en termes de valeur moyenne, de fluctuation associées et de probabilité de défaillance. A partir d’une analyse détaillée de la microstructure de nos matériaux, nous montrons que la structure des pores, plutôt que les aggrégats, joue un rôle important sur les effets d’échelle sur la résistance à rupture en compression. Dans ce cadre, la résistance asymptotique (σ_∞ ) représente la véritable résistance caractéristique en compression (f_ck ), qui est une propriété essentielle pour la conception de structures à grande échelle et pour le contrôle de la qualité du béton.En conséquence du rôle important de la structure des pores sur les effets d’échelle sur la résistance en compression des bétons à faible porosité, lors de l'estimation de la résistance caractéristique à partir d'une série d'essais avec une seule taille d'échantillon, une condition sur cette taille par rapport à la taille caractéristique de la structure des pores est proposée. / Size effects on mechanical strength, i.e. the fact that larger structures fail under lower stresses than smaller ones, already highlighted by Leonardo da Vinci and Edmée Mariotte centuries ago, remain nowadays a crucial problem to establish structural design rules and safety regulations from an upscaling of laboratory data. These size effects are generally explained either from a deterministic energetic approach that predicts a non-vanishing asymptotic strength but, by construction, does not account for fluctuations around the mean strength and their size dependence, or from a statistical approach based on the weakest-link theory that implies a vanishing strength towards large scales.Recently, an alternative framework has been proposed based on an interpretation of compressive failure of heterogeneous materials as a critical transition from an intact to a failed state. This critical interpretation releases the underlying hypotheses of the weakest-link theory, pure brittleness and the independence of damage events, while predicting a non-vanishing asymptotic mean strength (σ_∞ ) but vanishing intrinsic fluctuations at large scales. The application this framework to the statistical size effects on compressive strength of concrete, a typical quasibrittle material of tremendous importance in civil engineering, is investigated in this thesis.From an extensive series of uniaxial compression experiments (527 tests) carried out on concrete samples with four different sizes and three different microstructures, we demonstrate (i) the failure of the weakest-link theory in this case, and instead (ii) the pertinence of the critical framework to account for size effects on compressive strength of concrete, in terms of average strength, associated fluctuations, and probability of failure. From a detailed analysis of the microstructural disorder of our materials, we show that the pore structure, rather than the concrete mix, plays a significant role on size effects on strength. In this framework, the asymptotic strength (σ_∞ ) represents the genuine characteristic compressive strength (f_ck ) of the material, a key property for the dimensioning large-scale structures from an upscaling of small-scale laboratory mechanical tests and for the quality control of concrete.As a consequence of the leading role of the pore structure in controlling the size effects on compressive strength of low-porosity concretes, when estimating the characteristic (asymptotic) strength from a series of tests with a single sample size, a condition on this size with respect to the characteristic scale of pore structure is proposed to be fulfilled.

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No. of bitstreams: 1 filenga_d_me_bauru.pdf: 7092752 bytes, checksum: 39027609a3847f35afe9186806ee8144 (MD5) Previous issue date: 2016-04-04 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / Na presente dissertação realizou-se o estudo das forças críticas e do comportamento dinâmico dos vórtices magnéticos de fitas supercondutoras do tipo II com arranjos conformes de centros de aprisionamento (pinning), bem como de diversos outros tipos de arranjos e também de diferentes trechos de arranjos. Além dos efeitos da geometria finita e aprisionamento, foi analisado o comportamento do sistema ao variar parâmetros externos como força de transporte e campo magnético. Os sistemas simulados correspondem a supercondutores bidimensionais, finitos na direção transversal e infinitos na direção longitudinal. A descrição das interações existentes no sistema pôde ser feita através de um conjunto de equações de Langevin, as quais foram resolvidas utilizando a técnica de Dinâmica Molecular. As soluções destas equações permitiram, dentre outros resultados, a obtenção das trajetórias e velocidades dos vórtices. Através das trajetórias, foi possível determinar o comportamento dinâmico das linhas de fluxo, e através das velocidades, os valores de força crítica. Para obter as posições iniciais dos vórtices, foi utilizado um algoritmo de Recozimento Simulado Generalizado (Generalized Simulated Annealing), o qual permitiu obter as configurações de menor energia do sistema. Os cálculos realizados foram feitos para 154 diferentes sistemas, que consistiram na análise do comportamento das interações neles existentes ao variar o campo magnético externo (H) aplicado nas amostras, bem como na análise dos efeitos de tamanho das fitas supercondutoras, utilizando diferentes arranjos e trechos de arranjos de centros de aprisionamento. Para o estudo da influência do campo magnético aplicado, foi feita uma varredura com diferentes valores de H e um valor fixo de largura de fita, tanto para o arranjo conforme quanto para os arranjos quadrado, aleatório, hexagonal e conforme deformado de centros de aprisionamento, a fim de realizar comparações. Para o estudo dos efeitos de tamanho, foram utilizados valores fixos de campo magnético externo aplicado e diferentes larguras de fita, com arranjos de centros de aprisionamento conforme, aleatório e conforme deformado, bem como diferentes trechos dos arranjos conforme e conforme deformado. Em todos os casos, a densidade de centros de aprisionamento, para efeitos de comparação, foi mantida constante para todos os tipos de arranjos e trechos de arranjos. Os resultados mostram que o arranjo conforme de centros de aprisionamento, e também trechos desse arranjo, apresentam maior estabilidade que os outros tipos de arranjos e trechos de arranjos analisados, revelando, com algumas exceções, maiores valores de força crítica para os valores de campo utilizados. Este resultado também pode ser observado em simulações numéricas que lidam com sistemas supercondutores infinitos. Entretanto, foi possível notar que o aumento na força crítica depende significativamente dos valores de campo magnético aplicados. Enquanto que em sistemas infinitos são reportados acréscimos nas forças críticas, para todos os valores de campo analisados, que podem chegar a até 100% para o arranjo conforme em relação a arranjos aleatórios de centros de aprisionamento, para o caso de fitas supercondutoras encontramos acréscimos nas forças críticas, para todos os valores de campo analisados em sistemas com largura fixa, que chegam a até 65,22%, aproximadamente, para o arranjo conforme em relação a arranjos aleatórios, bem como acréscimos que chegam a até 140% para o arranjo conforme em relação ao arranjo hexagonal de centros de aprisionamento. Ao variar a largura das amostras, encontramos acréscimos de até 81,82%, aproximadamente, para o arranjo conforme e, para trechos do arranjo conforme, um acréscimo de até 127,27%, aproximadamente, na força crítica em relação a arranjos aleatórios de centros de aprisionamento, considerando diferentes valores de H. / In this work we study the critical forces and dynamic behavior of magnetic vortices in type II superconducting tapes with conformal pinning arrays, as well several other types of arrays and also parts of arrays. In addition to the effects of finite geometry and pinning, we analyze system behavior by varying external parameters such as transport force and magnetic field. The simulated systems corresponds a two-dimensional superconductor, finite in the transverse direction and infinite in the longitudinal direction. The description of the interactions existing in the system can be made via a set of Langevin equations which were solved using Molecular Dynamics techniques. The solutions of these equations allowed, among other results, to obtain the trajectories and velocities of the vortices. Through the trajectories, it was possible to determine the dynamic behavior of the vortex lines, and through the velocities, the values of critical force. To obtain the initial positions of the vortices, we use a Generalized Simulated Annealing algorithm, which sought the settings of the lower energy system. Our calculations were made for 154 different systems, consisting in analyzing the interaction behavior contained in the systems by varying the external magnetic field (H) applied in the samples and the analysis of size effects of superconducting tapes using different arrays and parts of arrays of pinning centers. To study the influence of the applied magnetic field, a scan was taken with different values of H and a fixed value of tape width, both the conformal as for square, random, hexagonal and deformed conformal pinning centers, in order to make comparisons. To study the effects of size, were used fixed values of an external applied magnetic field and different widths of tapes, with the conformal, random and deformed conformal pinning centers, as well different parts of the conformal and deformed conformal arrays. In all cases, the density of pinning centers, for the purpose of comparison, were kept constant for all types of arrays, and parts of arrays. The results show that the conformal pinning array, and also parts of this array, exhibit greater stability than other types of arrays and parts of arrays, showing, with some exceptions, higher values of critical forces for the field values used. This result can also be observed in numerical simulations dealing with infinite superconducting systems. However, it was noticeable that the increase in critical force significantly depends on the magnetic field values applied. While in infinite systems are reported increases in critical forces to all field values analyzed which can reach up to 100% for a conformal array of pinning centers in relation to random arrays [1], for the case of superconducting tapes we found increases in critical forces for all field values analyzed in systems with fixed width, which reach up to 65.22%, approximately, to the conformal array in relation to random arrays, and increases to reach up to 140% to the conformal array in relation to the hexagonal array of pinning centers. By varying the width of the samples, there are increases up to 81.82%, approximately, for conformal pinning array, and for parts of a conformal pinning array, an increase of up to 127.27% approximately in critical force in relation to random pinning arrays, considering different H values.

Cette thèse a pour but d'étudier les effets quantiques apparaissant pour des agrégats métalliques de très petite taille en raison de l'augmentation du ratio surface/volume et de la discrétisation de la structure électronique. Mettre en avant ces effets demande une très grande qualité de fabrication des nanoparticules étudiées, monodisperse dans le cas idéal. Nous fabriquons des nanostructures en encapsulant des agrégats d'argent générés par une source magnétron dans des matrices solides, comme la silice ou l'alumine. Cette technique nous permet de contrôler indépendamment la composition des particules, leur taille, et leur concentration. Un spectre de masse quadripolaire a été mis en place et utilisé comme un filtre en taille pour obtenir une distribution plus étroite et précise.Les échantillons ont été caractérisés par deux techniques complémentaires : par spectroscopie optique à transmission avec des mesures sur des ensembles de particules, et par spectroscopie de perte d'énergie des électrons (EELS) sur des particules uniques, réalisée dans un microscope électronique à balayage par transmission. Bien qu'utilisant deux outils conceptuellement différents, ces deux méthodes mesurent les résonances plasmoniques des particules. Ce travail a donc pour objectif de relier théoriquement et expérimentalement ces deux méthodes dans le but de comprendre comment les propriétés physiques de ces petits agrégats de métaux nobles sont affectées par les effets quantiques / The aim of this thesis is to study quantum effects appearing in very small metallic clusters caused by the increasing surface/volume ratio and the discretization of the electronic structure. Investigating effects such as size dependencies demand a very high quality of the studied nanoparticles, monodisperse in the ideal case. We fabricate nanostructures by embedding silver clusters generated in a magnetron source in solid matrices, such as silica or alumina. This technique gives us full and independent control over the particle composition, size and concentration. A quadrupole mass spectrometer is used as a size filter to obtain a more precise and narrow distribution.Samples have been characterized with two complementary methods: optical transmission spectroscopy of ensembles of particles and electron energy loss spectroscopy (EELS) on single particles using a scanning transmission electron microscope. Although these two tools are conceptually different, they both measure the plasmonic resonances of metal nanoparticles. The objective of this work is to link theory and experiment in these two methods in order to understand how the physical properties of these small noble metal clusters are affected by quantum effects

Most prior investigations of visual working memory (VWM) presented the to-be-remembered items simultaneously in a static configuration (e.g., Luck & Vogel, 1997). However, in everyday situations, such as driving on a busy multilane highway, items (e.g., cars) are presented sequentially and must be retained to support later actions (e.g., knowing if it’s safe to change lanes). In a simultaneous presentation, the relative positions of items are apparent but for sequential presentation, relative positions must be inferred in relation to the background structure (e.g., highway lane markings). To examine sequential encoding in VWM, we developed a novel task in which dots were presented slowly, one at a time, with each dot appearing in one of six boxes (Experiment 1), or in invisible boxes within a visible encompassing outer frame (Experiment 2). Experiment 1 found strong recency effects for judgments of color at the end of the sequence but not for the location of dots. In contrast, without dividing lines, Experiment 2 found strong recency effects for both color and location judgments. These results held true for accuracy, reaction time, and an integrated measure of speed and accuracy. We hypothesize that background structure allows the updating of VWM, slotting each new item into that structure to provide a new configuration that retains both old and new items, whereas in the absence of structure, VWM suffers from severe retroactive interference.