The effect of thermo-mechanical processing by deformation and annealing on the grain boundary configuration of commercially pure Ni-200 is reported in this thesis. Ni-200 is unalloyed, thus avoiding the complex effects associated with alloying elements on the formation and development of different types of grain boundaries. One step strain-recovery with strain levels in the range of 3% to 7.5% (with 1.5% intervals) and annealing temperatures in the range of 800ºC to 1000ºC (with 100ºC intervals) were used in processing. The effects of parameters such as strain level, annealing temperature, annealing time and grain growth on grain boundary configurations were studied. Using Orientation Image Microscopy (OIM) it was found that the Fsp (fraction of special grain boundaries) value of strained samples annealed in the range of 800ºC to 1000ºC began to increase after a critical length of time, after which the Fsp value increased quickly and becoming a maximum in 2~4 minutes. The length of the critical annealing time for the increase of Fsp was shorter in the material with the higher levels of strain at a constant annealing temperature. Also the critical annealing time was shorter when annealed at higher temperatures under a fixed level of strain. The Fsp value increased to 80% from an as received value of about 30% in the samples with varying strain levels. However, the Fsp values only increased from 30% to 45% in the material without strain. Due to grain boundary migration, the Fsp values increased with grain size and became a maximum during the heat treatment of the strained material. In the material without strain however even when grain growth occurred, limited improvement in Fsp values occurred showing that contribution of strain is very important to the formation of special boundaries. By varying the strain levels, annealing temperatures and times, material with high Fsp values in a wide range of grain size can be obtained. Under the present processing conditions used however, multi-cycle was not helpful to the improvement of Fsp. TEM observations indicated dislocation tangles occurred near the grain boundary of the 1x6% strained samples. These dislocation tangles decreased with time at 800˚C and were reduced considerably after 20 minutes. Thermodynamic and kinetic models were used in the calculations of twin density-grain size relationships. The results indicated that the contribution of strain is equivalent to the increase of grain boundary energy, which provided an extra driving force and improved probability of twin embryo formation.

We have investigated several topics in the area of manganites including oxygen disorder, grain boundaries, low field magnetoresistance, magnetoresistive anisotropy and magnetic properties. Studied materials were in the form of polycrystalline samples and epitaxial thin films. The studied compounds were Sm(1-x)Sr(x)MnO3 (SSMO) and La(1-x)Ca(x)MnO3 (LCMO). 1-We have studied the effects of oxygen disorder and grain boundary disorder in the SSMO system close to half hole doping level. The temperature dependencies of resistivity and magnetoresistance were measured as a function of the vacuum annealing time. We observed a logarithmic increase of the resistivity as a function of vacuum annealing time. We have shown that an increasing grain boundary disorder softens the magnetic phase transition from a first order phase transition into a second order transition. Furthermore, the peaks in the resistivity and specific heat are broadened and there is an increase in the charge-carrier scattering rates in the metallic state. On the other hand, the polaronic hopping activation energies in the insulating state changed slightly as a function of grain boundary disorder. The origin of these phenomena is discussed. Magnetoresistive anisotropy has been studied as a function of the grain size. Results showed a strong grain size dependence of anisotropic electrical transport in granular samples of manganites. 2-We investigated the anisotropic magnetoresistance (AMR) in ultrathin LCMO films grown on various substrates. It was found that depending on the strain state, the AMR in some of these systems exceeds 100% and can even change sign. These changes are dramatic when compared to the few percent change in AMR in conventional ferromagnets. The mechanism behind these changes in the AMR is discussed. We have also studied the effects of strain on resistive peak broadening with a simple percolation model. We have shown that strain associated with a lattice mismatched substrate in thin films can cause new electronic behavior, not found in bulk materials or thicker films of the same chemical composition. Resistivity of the ultra thin films exhibit strong relaxation effects when measured as a function of time in a constant magnetic field.

This project explores the fundamental mechanisms of grain boundary sliding (GBS) with an emphasis on its role in superplasticity, using both micro- and macro-mechanical testing methods. GBS plays an important role in the deformation of polycrystalline materials, especially at high homologous temperatures (above half of the melting point). Classical models for GBS (Rachinger sliding and Lifshitz sliding) assume that all grains and grain boundaries undergo the same process, but recent research has shown this is not true. Individual grain boundaries differ in their ability to participate in sliding and diffusion. Therefore, it is important to investigate the response of individual grain boundaries to stress. This project uses microcantilevers, loaded using a nanoindenter, to investigate the response to stress of individual grain boundaries in Sn-1%Bi, which is expected to exhibit GBS at room temperature. The response of individual grain boundaries are correlated with grain boundary characters determined using electron backscattered diffraction (EBSD). On the macroscopic scale, both in-situ and ex-situ shear tests are conducted to investigate the superplastic behaviour of this material. The strain rate sensitivity index of the material with a grain size of 8.5 μm is found to be around 0.45. Surface marker lines have quantitatively revealed grain boundary sliding. The investigation from surface studies is expanded to the interior of bulk material in 3D by conducting an in-situ tensile test coupled with diffraction contrast tomography (DCT) at a synchrotron facility. The microcantilever tests enable grain boundary sliding and diffusion creep to be investigated separately by varying the normal and shear stresses on the grain boundary plane. GBS is dependent on grain boundary structure (misorientation angle, rotation axis and grain boundary plane orientation). The microcantilever size is similar to the grain size used in the macro-mechanical tests. It is demonstrated that the shear stress for steady-state GBS is comparable in micro- and macro-tests. Grain neighbour switching events have been identified in the interior of bulk material in 3D for the first time.

At the microscopic level, many materials are made of smaller and randomly oriented grains. These grains are separated by grain boundaries which tend to decrease the electrical and thermal conductivity of the material. The motion of grain boundaries is an important phenomenon controlling the grain growth in materials processing and synthesis. Mathematical modeling and simulation is a powerful tool for studying the motion of grain boundaries. The research reported in this thesis is focused on the numerical simulation and analysis of a coupled surface and grain boundary motion which models the evolution of grain boundary and the diffusion of the free surface during the process of grain growth. The “quarter loop” geometry provides a convenient model for the study of this coupled motion. Two types of normal curve velocities are involved in this model: motion by mean curvature and motion by surface diffusion. They are coupled together at a triple junction. A front tracking method is used to simulate the migration. To describe the problem, different formulations are presented and discussed. A new formulation that comprises partial differential equations and algebraic equations is proposed. It preserves arc length parametrization up to scaling and exhibits good numerical performance. This formulation is shown to be well-posed in a reduced, linear setting. Numerical simulations are implemented and compared for all formulations. The new formulation is also applied to some other related problems. We investigate numerically the linear stability of the travelling wave solutions for the quarter loop problem and a simple grain boundary motion problem for both curves in two dimensions and surfaces in three dimensions. The numerical results give evidence that they are convectively stable. A class of high order three-phase boundary motion problems are also studied. We consider a region where three phase boundaries meet at a triple junction and evolve with specified normal velocities. A system of partial differential algebraic equations (PDAE) is proposed to describe this class of problems by extending the discussion for the coupled surface and grain boundary motion. The linear well-posedness of the system is analyzed and numerical simulations are performed. / Science, Faculty of / Mathematics, Department of / Graduate

abstract: Shock loading produces a compressive stress pulse with steep gradients in density, temperature, and pressure that are also often modeled as discontinuities. When a material is subject to these dynamic (shock) loading conditions, fracture and deformation patterns due to spall damage can arise. Spallation is a dynamic material failure that is caused by the nucleation, growth, and coalescence of voids, with possible ejection of the surface of the material. Intrinsic defects, such as grain boundaries are the preferred initiation sites of spall damage in high purity materials. The focus of this research is to study the phenomena that cause void nucleation and growth at a particular grain boundary (GB), chosen to maximize spall damage localization. Bicrystal samples were shock loaded using flyer-plates via light gas gun and direct laser ablation. Stress, pulse duration, and crystal orientation along the shock direction were varied for a fixed boundary misorientation to determine thresholds for void nucleation and coalescence as functions of these parameters. Pressures for gas gun experiments ranged from 2 to 5 GPa, while pressures for laser ablation experiments varied from 17 to 25 GPa. Samples were soft recovered to perform damage characterization using electron backscattering diffraction (EBSD) and Scanning Electron Microscopy (SEM). Results showed a 14% difference in the thresholds for void nucleation and coalescence between samples with different orientations along the shock direction, which were affected by pulse duration and stress level. Fractography on boundaries with strong damage localization showed many small voids, indicating they experience rapid nucleation, causing early coalescence. Composition analysis was also performed to determine the effect of impurities on damage evolution. Results showed that higher levels of impurities led to more damage. ABAQUS/Explicit models were developed to simulate flyer-plate impact and void growth with the same crystal orientations and experimental conditions. Results are able to match the damage seen in each grain of the target experimentally. The Taylor Factor mismatch at the boundary can also be observed in the model with the higher Taylor Factor grain exhibiting more damage. / Dissertation/Thesis / Doctoral Dissertation Mechanical Engineering 2020

In this work we introduce the Voronoi fundamental zone octonion (VFZO) interpolation framework for grain boundary (GB) structure-property models and surrogates. The VFZO framework offers an advantage over other five degree-of-freedom (5DOF) based property interpolation methods because it is constructed as a point set in a Riemannian manifold. This means that directly computed Euclidean distances approximate the original octonion distance with significantly reduced computation runtime (∼7 CPU minutes vs. 153 CPU days for a 50000×50000 pairwise-distance matrix). This increased efficiency facilitates lower interpolation error through the use of significantly more input data. We demonstrate grain boundary energy (GBE) interpolation results for a non-smooth validation function and simulated bi-crystal datasets for Fe and Ni using four interpolation methods: barycentric interpolation, Gaussian process regression (GPR) or Kriging, inverse-distance weighting (IDW), and nearest neighbor (NN)interpolation. These are evaluated for 50000 random input GBs and 10000 random prediction GBs. The best performance was achieved with GPR, which resulted in a reduction of the root mean square error(RMSE) by 83.0% relative to RMSE of a constant, average model. Likewise, interpolation on a large, noisy, molecular statics (MS) Fe simulation dataset improves performance by 34.4 % compared to 21.2 %in prior work. Interpolation on a small, low-noise MS Ni simulation dataset is similar to interpolation results for the original octonion metric (57.6 % vs. 56.4 %). A vectorized, parallelized, MATLAB interpolation function (interp5DOF.m) and related routines are available in our VFZO repository (github.com/sgbaird-5dof/interp) which can be applied to any of the 32 crystallographic point groups1. The VFZO framework offers advantages for computing distances between GBs, estimating property values for arbitrary GBs, and modeling surrogates of computationally expensive 5DOF functions and simulations.

In this work we introduce the Voronoi fundamental zone octonion (VFZO) interpolation framework for grain boundary (GB) structure-property models and surrogates. The VFZO framework offers an advantage over other five degree-of-freedom (5DOF) based property interpolation methods because it is constructed as a point set in a Riemannian manifold. This means that directly computed Euclidean distances approximate the original octonion distance with significantly reduced computation runtime (∼7 CPU minutes vs. 153 CPU days for a 50000×50000 pairwise-distance matrix). This increased efficiency facilitates lower interpolation error through the use of significantly more input data. We demonstrate grain boundary energy (GBE) interpolation results for a non-smooth validation function and simulated bi-crystal datasets for Fe and Ni using four interpolation methods: barycentric interpolation, Gaussian process regression (GPR) or Kriging, inverse-distance weighting (IDW), and nearest neighbor (NN)interpolation. These are evaluated for 50000 random input GBs and 10000 random prediction GBs. The best performance was achieved with GPR, which resulted in a reduction of the root mean square error(RMSE) by 83.0% relative to RMSE of a constant, average model. Likewise, interpolation on a large, noisy, molecular statics (MS) Fe simulation dataset improves performance by 34.4 % compared to 21.2 %in prior work. Interpolation on a small, low-noise MS Ni simulation dataset is similar to interpolation results for the original octonion metric (57.6 % vs. 56.4 %). A vectorized, parallelized, MATLAB interpolation function (interp5DOF.m) and related routines are available in our VFZO repository (github.com/sgbaird-5dof/interp) which can be applied to any of the 32 crystallographic point groups1. The VFZO framework offers advantages for computing distances between GBs, estimating property values for arbitrary GBs, and modeling surrogates of computationally expensive 5DOF functions and simulations.

No description available.

A method for the retrieval of grain boundary inclination parameters of the grain boundary character distribution by oblique double-sectioning is proposed. The method, which is similar to the recovery of the orientation distributions from sets of incomplete pole-figures, is described along with a framework for implementation. The method directly measures grain boundary inclinations in a manner similar to serial sectioning while statistically sampling the microstructure comparably to stereological methods. Computer simulations of the method were used to confirm the mathematical framework. Additional simulations, where the grain boundary normal distributions were recovered by both oblique double-sectioning and stereological methods, showed that results recovered by 3 orthogonal double-sections from oblique double-sectioning proved to be just as accurate as the 25 section-cuts required for stereology in resolving the finer details in the recovered distribution.

No description available.