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Thesis (Ph.D.); Submitted to Iowa State Univ., Ames, IA (US); 19 Dec 2004. / Published through the Information Bridge: DOE Scientific and Technical Information. "IS-T 2309" Mangui Han. US Department of Energy 12/19/2004. Report is also available in paper and microfiche from NTIS.

Submitted by Pedro Silva Filho (pfsilva@ipen.br) on 2017-11-17T17:43:50Z No. of bitstreams: 0 / Made available in DSpace on 2017-11-17T17:43:50Z (GMT). No. of bitstreams: 0 / A zircônia tetragonal estabilizada por ítria (Y-TZP) têm sido utilizada na área odontológica para próteses livres de metais devido à estética associada ao alto desempenho mecânico. Porém, a presença de ambiente úmido pode causar a transformação acelerada da fase tetragonal para monoclínica e consequente falha catastrófica deste material, processo este conhecido como degradação a baixa temperatura ou envelhecimento. A cinética desta transformação é função da composição química da cerâmica e sua microestrutura. Tendo em vista que métodos químicos permitem a síntese de pós cerâmicos à base de zircônia de dimensões nanométricas, cuja microestrutura da cerâmica sinterizada é constituída por grãos submicrométricos quimicamente homogêneos, e que a presença de alumina é indicada para evitar a degradação de fases da zircônia, o objetivo deste estudo foi verificar a degradação a baixa temperatura e ambiente úmido de cerâmicas de zircônia estabilizada com 3 mol% de ítria (Y-TZP) e do compósito Y-TZP/Al2O3, proveniente de pós sintetizados pela rota de coprecipitação. A concentração de alumina na Y-TZP foi estudada na faixa de 0,05 a 20% em massa. A eficiência do processo desenvolvido foi verificada pela avaliação das características físicas dos pós obtidos (granulometria, área de superfície específica, estado de aglomeração e estrutura cristalina). As amostras cerâmicas foram prensadas, sinterizadas e avaliadas quanto à densidade aparente e microestrutura. Após a caracterização inicial das cerâmicas a degradação das amostras foi estudada in vitro em reator hidrotérmico pressurizado a 150°C. As amostras (n=4) foram submetidas à análise de difração de raios X de acordo com o tempo de envelhecimento, acompanhando a curva cinética de transformação de fase. A porcentagem de cada fase cristalina foi determinada pelo Método de Rietveld. A relação entre o tempo de envelhecimento e a concentração de fase monoclínica foi determinada pela equação de Avrami modificada por Kolmogorow (Johnson-Mehl- Avrami-Kolmogorow JMAK). Após envelhecimento a 150°C por 70 horas, todas as amostras contendo alumina apresentaram menor concentração de fase monoclínica, comparativamente à cerâmica Y-TZP, que apresentou 66,5% dessa fase. Menores porcentagens de fase monoclínica após o envelhecimento hidrotérmico foram obtidas com a adição de 10 e 20% em massa de alumina na matriz de zircônia, sendo esses valores 59,1 e 52,9%, respectivamente. Deve-se considerar, no entanto, que a diminuição da degradação total é consequência da menor porcentagem de zircônia na matriz em função da adição de alumina. Neste contexto, o efeito benéfico da adição de alumina ocorre apenas no início do envelhecimento. / Dissertação (Mestrado em Tecnologia Nuclear) / IPEN/D / Instituto de Pesquisas Energéticas e Nucleares - IPEN-CNEN/SP

En conditions de stockage définitif, la désintégration a des radionucléides (produits en réacteur) induit desdommages dans le combustible nucléaire usé. Cet endommagement, et les déformations associées, doivent êtreétudiés pour évaluer correctement la tenue et l'évolution à long terme des pastilles de combustible. La démarcheproposée dans cette thèse pour réaliser cette étude consiste :- à simuler la désintégration a par une implantation d'ions hélium dans une couche fine, en surface depolycristaux d'U02 j- à mesurer les déformations qui en résultent par des techniques de diffraction aux rayons X : la macrodiffractionpour une mesure moyenne dans la couche implantée, la microdiffraction, produite par un rayonnementsynchrotron, pour des mesures très localisées, à l'intérieur des grains d'un polycristal d'U02.L'étude des déformations en fonction de la dose implantée permet de d'évaluer les effets des dégâts d'irradiationsur des durées de stockage de plusieurs milliers d'années.De nouvelles méthodes d'analyse ont été mises au point pour interpréter automatiquement les milliers de clichésde microdiffraction et en déduire la mesure des déformations dans la couche implantée. Un modèle mécaniquea été construit pour rendre compte des mesures avec une grande précision, équivalente à la précision expérimentale.Ce modèle permet de mesurer le gonflement induit par les dommages d'irradiation pour des endommagementsallant jusqu'à 0,77 dpa. Les valeurs mesurées sont comparables à des résultats de la littérature, obtenus sur despastilles auto-irradiées. Il a également permis de quantifier l'augmentation avec l'endommagement de l'anisotropieélastique de l'U02.La microdif / During long term storage of spent nuclear fuel, the a-decays of radionuclides produced by the in-pile irradiationinduces damages in pellets. These damages, and the resulting strains, must be studied in order to assess correctlythe long term evolution of fuel pellets. The approach chosan here is :- to simulate the a-decays by He ion implantation j- to measure the resulting straÏns using X ray diffraction techniques : macrodiffraction for average measurements,and synchrotron radiation based micro diffraction for local measurements inside grains.The study of strains as a function of ion implantation Huency enables to evaluated irradiation damages overthousands of storage yearB.New analytical methods have been developed to automatically interpret thousands of microdiffraction patterns,and to deduce strain into the implanted layer. Mechanical modeling bas been used to accurately predictmeasurements. This model enables to measure the isotropie swelling induced by helium implantation in a lowdamage range (below 0.77 dpa). Measured values are close to results previously reported in literature on selfirradiated pellets. This model also allowed to quantify the increase with damage of U02 elastic aniBOtropy.X ray microdiffraction is a powerful technique to map the strRin fields within grains. This enables to study theinfluence of neighboring grains on the measured straÏns. This influence remains negligible (below the measurementaccuracy) for low depth helium implantation (60 keV). For deeper belium implaotations (500 aod 1500 keV), thisis not anymore the case : strains are very heterogeneous in the vicinity of gYRin boundaries.

Une approche couplée prenant en compte l’interaction de la plasticité cristalline et de la diffusion d’hydrogène a été établie et utilisée pour étudier le transport de l’hydrogène dans les agrégats polycristallins synthétiques de l’acier 316L avec des géométries de grains and des orientations cristallographiques différentes. Les champs mécaniques calculés à l’aide du code ZeBuLoN sont transférés dans un code de diffusion développé dans le cadre de ce travail. Une nouvelle formulation associée à un nouveau schéma numérique permet un calcul qui présente une bonne convergence. Les résultats des simulations montrent la redistribution de l’hydrogène dans les polycristaux due à la présence des hétérogénéités des contraintes hydrostatiques à l’échelle intragranulaire. L’effet de la vitesse de déformation a été quantitativement obtenu. Afin d’enrichir l’approche continue, un intérêt particulier est porté sur le rôle des joints de grains. Des simulations numériques d’un modèle atomique plan par plan ont été développées et appliquées aux bicristaux et aux structures de type ”bambou”. Les effets de puits ou de barrière induits par la présence des joints de grains sont clairement démontrés dans le cas du nickel pur. Pour reproduire ces effets dans les simulations de diffusion avec le modèle continue, une approche originale de simulation”multi-échelles” de la diffusion au joint de grain a été développée, et un nouveau régime de diffusion au joint de grain a été modélisé. / In the present work, we establish a one-way coupled crystal plasticity – hydrogen diffusion analysis and use this approach to study the hydrogen transport in artificial polycrystalline aggregates of 316L steel with different grain geometries and crystallographic orientation. The data about stress/strain fields computed at the microstructure scaleutilizing the crystal plasticity concept are transferred to the in-house diffusion code which was developed using a new numerical scheme for solving parabolic equations. In the case of initial uniform hydrogen content, the heterogeneity of the mechanical fields is shownto induce a redistribution of hydrogen in the microstructure. The effect of strain rate is clearly revealed. In the second part, hydrogen transport across grain boundaries is investigatedconsidering the specific diffusivity and segregation properties of these interfaces. Using a discrete atomic layer model, the retarding impact of grain boundaries is demonstrated on bicrystals and bamboo type membranes with and without external mechanical loading. To reproduce the effects observed in the atomistic simulations into the crystal plasticity – hydrogen diffusion model, a new physically based multi-scale method is proposed. Using this new approach we study the effect of grain boundary trapping kinetics on hydrogen diffusion and reveal a new grain boundary diffusion regime which has notbeen reported before.

A study was done to determine the temperature and load interaction effects on the fatigue crack growth rate of polycrystalline superalloy IN100. Temperature interaction testing was performed by cycling between 316°C and 649°C in blocks of 1, 10 and 100 cycles. Load interaction testing in the form of single overloads was performed at 316°C and 649°C. After compiling a database of constant temperature, constant amplitude FCGR data for IN100, fatigue crack growth predictions assuming no load or temperature interactions were made. Experimental fatigue crack propagation data was then compared and contrasted with these predictions. Through the aid of scanning electron microscopy the fracture mechanisms observed during interaction testing were compared with the mechanisms present during constant temperature, constant amplitude testing. One block alternating temperature interaction testing grew significantly faster than the non-interaction prediction, while ten block alternating temperature interaction testing also grew faster but not to the same extent. One hundred block alternating testing grew slower than non-interaction predictions. It was found that as the number of alternating temperature cycles increased, changes in the gamma prime morphology (and hence deformation mode) caused changes in the environmental interactions thus demonstrating the sensitivity of the environmental interaction on the details of the deformation mode. SEM fractography was used to show that at low alternating cycles, 316°C crack growth was accelerated due to crack tip embrittlement caused by 649°C cycling. At higher alternating cycles the 316°C cycling quickly grew through the embrittled crack tip but then grew slower than expected due to the possible formation of Kear-Wilsdorf locks at 649°C. Overload interaction testing led to full crack retardation at 2.0x overloads for both 316°C and 649°C testing. 1.6x overloading at both temperatures led to retarded crack growth whereas 1.3x overloads at 649°C created accelerated crack growth and at 316°C the crack growth was retarded.

In this research, the homogenization relations for elastic properties in isotropic and anisotropic materials are studied by applying two-point statistical functions to composite and polycrystalline materials. The validity of the results is investigated by direct comparison with experimental results. In todays technology, where advanced processing methods can provide materials with a variety of morphologies and features in different scales, a methodology to link property to microstructure is necessary to develop a framework for material design. Statistical distribution functions are commonly used for the representation of microstructures and also for homogenization of materials properties. The use of two-point statistics allows the materials designer to consider morphology and distribution in addition to properties of individual phases and components in the design space. This work is focused on studying the effect of anisotropy on the homogenization technique based on two-point statistics. The contribution of one-point and two-point statistics in the calculation of elastic properties of isotropic and anisotropic composites and textured polycrystalline materials will be investigated. For this purpose, an isotropic and anisotropic composite is simulated and an empirical form of the two-point probability functions are used which allows the construction of a composite Hull. The homogenization technique is also applied to two samples of Al-SiC composite that were fabricated through extrusion with two different particle size ratios (PSR). To validate the applied methodology, the elastic properties of the composites are measured by Ultrasonic methods. This methodology is then extended to completely random and textured polycrystalline materials with hexagonal crystal symmetry and the effect of cold rolling on the annealing texture of near- Titanium alloy are presented.

A novel microstructure-sensitive extreme value probabilistic framework is introduced to evaluate material performance/variability for damage evolution processes (e.g., fatigue, fracture, creep). This framework employs newly developed extreme value marked correlation functions (EVMCF) to identify the coupled microstructure attributes (e.g., phase/grain size, grain orientation, grain misorientation) that have the greatest statistical relevance to the extreme value response variables (e.g., stress, elastic/plastic strain) that describe the damage evolution processes of interest. This is an improvement on previous approaches that account for distributed extreme value response variables that describe the damage evolution process of interest based only on the extreme value distributions of a single microstructure attribute; previous approaches have given no consideration of how coupled microstructure attributes affect the distributions of extreme value response. This framework also utilizes computational modeling techniques to identify correlations between microstructure attributes that significantly raise or lower the magnitudes of the damage response variables of interest through the simulation of multiple statistical volume elements (SVE). Each SVE for a given response is constructed to be a statistical sample of the entire microstructure ensemble (i.e., bulk material); therefore, the response of interest in each SVE is not expected to be the same. This is in contrast to computational simulation of a single representative volume element (RVE), which often is untenably large for response variables dependent on the extreme value microstructure attributes. This framework has been demonstrated in the context of characterizing microstructure-sensitive high cycle fatigue (HCF) variability due to the processes of fatigue crack formation (nucleation and microstructurally small crack growth) in polycrystalline metallic alloys. Specifically, the framework is exercised to estimate the local driving forces for fatigue crack formation, to validate these with limited existing experiments, and to explore how the extreme value probabilities of certain fatigue indicator parameters (FIPs) affect overall variability in fatigue life in the HCF regime. Various FIPs have been introduced and used previously as a means to quantify the potential for fatigue crack formation based on experimentally observed mechanisms. Distributions of the extreme value FIPs are calculated for multiple SVEs simulated via the FEM with crystal plasticity constitutive relations. By using crystal plasticity relations, the FIPs can be computed based on the cyclic plastic strain on the scale of the individual grains. These simulated SVEs are instantiated such that they are statistically similar to real microstructures in terms of the crystallographic microstructure attributes that are hypothesized to have the most influence on the extreme value HCF response. The polycrystalline alloys considered here include the Ni-base superalloy IN100 and the Ti alloy Ti-6Al-4V. In applying this framework to study the microstructure dependent variability of HCF in these alloys, the extreme value distributions of the FIPs and associated extreme value marked correlations of crystallographic microstructure attributes are characterized. This information can then be used to rank order multiple variants of the microstructure for a specific material system for relative HCF performance or to design new microstructures hypothesized to exhibit improved performance. This framework enables limiting the (presently) large number of experiments required to characterize scatter in HCF and lends quantitative support to designing improved, fatigue-resistant materials and accelerating insertion of modified and new materials into service.

In this thesis, we pursue a simulation-based approach whereby microstructure-sensitive finite element simulations are performed within a statistical perspective to examine the VHCF life variability and assess the surface initiation probability. The methodology introduced in this thesis lends itself as a cost-effective platform for development of microstructure-property relations to support design of new or modified alloys, or to more accurately predict the properties of existing alloys.