Dynamic abnormal grain growth (DAGG) is a phenomenon that produces abnormal grain growth at elevated temperatures during plastic deformation. It is distinct from classically studied static abnormal grain growth phenomena in that it only occurs during plastic deformation. Previous investigations of DAGG in a Mo sheet material produced using powder metallurgy techniques observed DAGG grains to grow more rapidly near the sheet surface than near the sheet center. This phenomenon is explored in the present study. A Mo sheet material produced using arc melting techniques is also studied to determine the morphology of DAGG grains. A preference for growth near the sheet center is observed in this material. The through-thickness variations in texture and grain size for both the arc-melted and powder-metallurgy Mo sheet materials are investigated. The preference for growth near the surface in the powder-metallurgy material is due to a through-thickness variation in grain size, with smaller grains near the surface and larger grains near the center. The preference for DAGG grain growth at the center of the arc-melted sheet material is because of very large grains that grow near the sheet surface. These large grains may be the product of multiple abnormal grains occurring near the sheet surface because of texture variation through the sheet thickness. Regardless, the DAGG grain cannot consume these large grains and leaves them as island grains decorating the region near the sheet surface. These results suggest that DAGG is driven primarily by grain boundary curvature. Microstructures that include DAGG grains are investigated with electron backscatter diffraction (EBSD). A new method to evaluate geometrically necessary dislocation densities using EBSD data is derived. DAGG grains are relatively undeformed compared to the polycrystalline microstructure. DAGG grains are not oriented either favorably or unfavorably for slip. Results of the analysis of the grain boundaries between DAGG grains and normal grains do not indicate any special character preference for these grain boundaries. / text

Philosophiae Doctor - PhD / Nanocrystalline silicon (nc-Si:H) is an interesting type of silicon with superior electrical properties that are more stable compared to amorphous silicon (a-Si:H). Silicon nitride (SiNₓ) thin films are currently the dielectric widely applied in the microelectronics industry and are also effective antireflective and passivating layers for multicrystalline silicon solar cells. Research into the synthesis and characterization of nc-Si:H and SiNₓ thin films is vital from a renewable energy aspect. In this thesis we investigated the film growth mechanisms and the filament stability during the hot-wire chemical vapour deposition (HWCVD) of nc-Si:H and SiNₓ thin films. During the HWCVD of nc-Si:H, electron backscatter diffraction (EBSD) revealed that the tantalum (Ta) filament aged to consists of a recrystallized Ta-core with Ta-rich silicides at the hotter centre regions and Si-rich Ta-silicides at the cooler ends nearer to the electrical contacts. The growth of nc-Si:H by HWCVD is controlled by surface reactions before and beyond the transition from a-Si:H to nc-Si:H. During the transition, the diffusion of hydrogen (H) within the film is proposed to be the reaction controlling step. The deposition pressure influenced the structural, mechanical and optical properties of nc-Si:H films mostly when the film thickness is below 250 nm. The film stress, optical band gap, refractive index and crystalline volume fraction approached similar values at longer deposition times irrespective of the deposition pressure. Filament degradation occurred during the HWCVD of SiNₓ thin films from low total flow rate SiH₄ / ammonia (NH₃) / H₂ gas mixture. Similar to the HWCVD of nc-Si:H, the Ta-core recrystallized and silicides formed around the perimeter. However, Tanitrides formed within the filament bulk. The extent of nitride and silicide formation, porosity and cracks were all enhanced at the hotter centre regions, where filament failure eventually occurred. We also applied HWCVD to deposit transparent, low reflective and hydrogen containing SiNₓ thin films at total gas flow rates less than 31 sccm with NH₃ flow rates as low as 3 sccm. Fluctuations within the SiNₓ thin film growth rates were attributed to the depletion of growth species (Si, N, and H) from the ambient and their incorporation within the filament during its degradation.

Understanding the plastic deformation mechanisms in polycrystals is a long-standing fundamental problem and its improvement has significant potential impact on the increase in materials resistance to typical failure modes such as fatigue cracking and stress corrosion cracking and hence the increase in the materials strength. However many deformation models are yet to be validated as quantitative experimental results at mesoscale to correlate dislocations and microstructure features are limited. This thesis furthers the High Resolution EBSD (HR-EBSD) technique in Geometrically Necessary Dislocation (GND) density measurement from qualitative analysis with a typical map size of 100 μm x100 μm to quantitative analysis with a map of 500 μm x500 μm by determining the optimised scanning step size (0.5 μm) and detector binning level (4x4 binning). This allows a statistically large number of grains to be sampled. Combining with obtained crystallographical information from a conventional EBSD system, systematic studies on GNDs behaviours with respect to a range of microstructure features such as grain boundaries and triple junctions were conducted on monotonically deformed polycrystal copper samples under tension. Relatively high GND density points were found near triple junctions and some grain boundaries whereas the low GND density points tend to appear near the grains’ interiors. These tendencies are particularly profound in low and moderately deformed samples. Hence more detailed analyses were performed to investigate the relations of GND density and the properties of grain boundaries and triple junctions. These quantitative analyses were complemented with direct visual assessment. The visual inspection provides interesting findings such as the strong GND structure dependence on grain orientations and GND structure development through increasing deformation; grain-grain interaction influences on GND structure development and GND structures near triple junctions. These GND density studies provide experimental results to validate some of the existing plastic deformation models for instance Ashby’s model of hardening and Hall-Petch relation. However, some of the new observations on GND structures at mesoscale cannot be fully rationalised by existing proposed mechanisms. Hence new models have been proposed that these GND structures might be generated from the intersections of different slip systems which occurred in various parts of a grain, or by the dislocation piling-up at some microstructural features e.g. triple junctions and twin boundaries.

The ability to generate three dimensional (3D) microstructures in solids is of great importance in understanding their true nature, as it eliminates speculation about the spatial distribution of features associated with conventional two dimensional (2D) imaging techniques. There are several recently-developed 3D techniques for determining the spatial distribution of microstructural features, each with a given resolution. There is considerable interest in the development of a specific serial sectioning methodology, termed 3D electron backscatter diffraction (3D-EBSD), which combines a focused ion beam (FIB) with EBSD interfaced to a field emission gun scanning electron microscope. Here, FIB is used as a serial sectioning device for cutting parallel slices of single- and multi-phase materials with a site-specific accuracy of up to 50 nm. Each consecutive slice is mapped by EBSD and the complete dataset combined using advanced computer algorithms to generate a volume of a material whereby the true crystallographic features can be analyzed at submicron resolution. The aims of the thesis was to develop 3D-EBSD into a powerful materials analysis tool and use it to resolve several issues concerning the nature of the deformed state and the nucleation and the growth behaviour of recrystallizing grains. The study commenced with an investigation into the effect of material type (restricted to face centred cubic AI, Cu and Au metallic crystals), FIB milling conditions and EBSD software variables on the quality of EBSD patterns generated on ion-milled surfaces of these materials. The effect of material type on EBSD pattern quality following FIB milling was found to be significant with relatively poor quality EBSD patterns obtained for metals of low atomic number. It was demonstrated, particularly for the high atomic number metals, that moderate FIB milling currents (~1-5nA) generated good quality EBSD maps from a given ion-milled surface. This preliminary work was necessary for balancing the time required for serial sectioning during 3D-EBSD and the generation of sufficient quality EBSD maps from each ion-milled surface. The outcomes of this investigation were applied to two major 3D-EBSD investigations on the microstructural and crystallographic characteristics of: (i) deformation features generated in a cold rolled interstitial free (IF) steel, with particular emphasis on the formation of microbands; and (ii) recrystallization of a cold rolled nickel alloy containing coarse (>1 ??m) silica particles, with particular attention given to the generation of particle deformation zones and their influence on nucleation and growth of recrystallizing grains including particle stimulated nucleation (PSN), twin formation during PSN and the growth behaviour of various types of grain boundary into the deformation microstructure. The foregoing 3D-EBSD studies were significant as they revealed various microstructural and crystallographic features not usually clearly evident in conventional 2D micrographs obtained by either EBSD or optical metallography. For example, the technique demonstrated that microbands in cold rolled IF steel consist of irregular curved surfaces that reconcile findings that microbands straight and aligned parallel to slip planes when viewed in normal direction-rolling direction sections but are wavy in transverse direction-rolling direction sections. Three slip planes were found within the angular range of the curved surface of the microband, which indicates that multiple slip planes are operative during deformation. The work also showed the influence of particle diameter on the misorientations generated within particle deformation zones and clearly showed that particle stimulated nucleation (PSN) occurred at particles greater than 1.5-2 ??m. It was observed that PSN in the nickel sample also generates contiguous grains separated by both coherent and incoherent twin boundaries and, on further growth of these grains into the matrix, the coherent boundary dominates and remains parallel to the primary growth direction of the grains.

Following the continually increasing demand for high-density interconnection and multilayer packaging for chips, solder bump size has decreased significantly over the years, this has led to some challenges in the reliability of interconnects. This thesis presents research into the resulting effects of miniaturization on the interconnection with Sn-solder, especially focusing on the full intermetallics (IMCs) micro-joints which appear in the 3D IC stacking packaging. Thereby, systematic studies have been conducted to study the microstructural evolution and reliability issues of Cu-Sn and Cu-Sn-Ni IMCs micro-joints. (1) Phenomenon of IMCs planar growth: The planar IMCs interlayer was asymmetric and composed of (Cu,Ni)6Sn5 mainly in Ni/Sn (2.5~5 μm)/Cu interconnect. Meanwhile, it was symmetric two-layer structure in Cu/Sn (2.5~5 μm)/Cu interconnect with the Cu3Sn fine grains underneath Cu6Sn5 cobblestone-shape-like grains for each IMCs layer. Besides, it is worth noticing that the appearance of Cu-rich whiskers (the mixture of Cu/Cu2O/SnOx/Cu6Sn5) could potentially lead to short-circuit in the cases of ultra-fine ( < 10 μm pitch) interconnects for the miniaturization of electronics devices. (2) Microstructural evolution process of Cu-Sn IMCs micro-joint: The simultaneous solidification of IMCs interlayer supressed the scalloped growth of Cu6Sn5 grains in Cu/Sn (2.5 μm)/Cu interconnect during the transient liquid phase (TLP) soldering process. The growth factor of Cu3Sn was in the range of 0.29~0.48 in Cu-Cu6Sn5 diffusion couple at 240~290 °C, which was impacted significantly by the type of substrates. And the subsequent homogenization process of Cu3Sn grains was found to be consistent with the description of flux-driven ripening (FDR) theory. Moreover, Kirkendall voids appeared only in the Cu3Sn layer adjacent to Cu-plated substrate, and this porous Cu3Sn micro-joint was mechanically robust during the shear test. (3) Microstructural evolution of Cu-Sn-Ni IMCs micro-joint: There was obvious inter-reaction between the interfacial reactions in Ni/Sn (1.5 μm)/Cu interconnect. The growth factor of (Cu,Ni)3Sn on Cu side was about 0.36 at 240 °C, and the reaction product on Ni side was changed from Ni3Sn4 into (Cu,Ni)6Sn5 with the increase of soldering temperature. In particular, the segregation of Ni atoms occurred along with phase transformation at 290 °C and thereby stabilized the (Cu,Ni)6Sn5 phase for the high Ni content of 20 at.%. (4) Micro-mechanical characteristics of Cu-Sn-Ni IMCs micro-joint: The Young s modulus and hardness of Cu-Sn-Ni IMCs were measured by nanoindentation test, such as 160.6±3.1 GPa/ 7.34±0.14 GPa for (Cu,Ni)6Sn5 and 183.7±4.0 GPa/ 7.38±0.46 GPa for (Cu,Ni)3Sn, respectively. Besides, in-situ nano-compression tests have been conducted on IMCs micro-cantilevers, the fracture strength turns out to be 2.46 GPa. And also, the ultimate tensile stress was calculated to be 2.3±0.7 GPa from in-situ micro-bending tests, which is not sensitive with the microstructural change of IMCs after dwelling at 290 °C.

The four pillars of material science and engineering namely structure, processing, properties and performance form the so-called material paradigm. At the heart of the material paradigm is materials characterization, which is used to measure and identify the relationships. Materials Characterization typically reconstructing the conditions giving rise to a measurement, a classic inverse problem. The solutions of these inverse problems are under or over determined and not unique. The solutions of these inverse problems can be greatly improved if accurate forward models exist for these characterization experiments. In this thesis, we will be focusing of developing forward models for electron diffraction modalities. Specifically, four different forward models for electron diffraction, namely the Electron Backscatter Diffraction, Electron Channeling Patterns, Precession Electron Diffraction and Transmission kikuchi Diffraction modalities are presented. Further, these forward models are applied to important materials characterization problems, including diffraction pattern indexing using the dictionary approach and forward model based orientation refinement. Finally, a novel pole figure inversion algorithm using the cubochoric representation and model based iterative reconstruction is also presented.

Being able to predict the evolution of plastic deformation at the microstructural scale is of paramount importance in the engineering of materials for advanced applications. However, this is not straightforward because of the multiscale nature of deformation heterogeneity, both in space and time . The present thesis combines four related studies in a coherent work, which is aimed to develop experimental methods for studying crystal plasticity at the micro and mesoscale. A novel methodology for gold remodelling is initially proposed and used to apply high-density speckle patterns on the surface of stainless steel specimens. The unique proprieties of the speckle pattern enabled plastic deformation mapping with submicron resolution using digital image correlation (HDIC). It was therefore possible to study the concomitant evolution of microbands and transgranular deformation bands in such alloy. High-resolution deformation mapping also enabled comparison with high-resolution electron backscatter diffraction (EBSD) observations. The only partial correspondence of results proved the limits of EBSD in characterizing plastic deformation. The cause of such limitation is later identified in the reduced sensitivity to lattice slip of the EBSD technique. Hence, a novel method of HDIC data analysis is proposed to separate the contributions of lattice slip and lattice rotation from the deformation mapping. The method is adopted to characterize plasticity in austenitic stainless steel and at the plastic deformation zone (PDZ) around a silicon particle embedded in a softer aluminum matrix. Results show that the proposed experimental methodology has the unique capability of providing a complete description of the micro and mesoscale mechanics of crystal plasticity. HDIC therefore emerges as a key technique in the development of accurate physical-based multiscale crystal plasticity models.

Thesis advisor: Seth C. Kruckenberg / Quantitatively describing the deformational behavior (i.e. the rheology) of lower crustal materials has proven challenging due to the highly variable nature of structural and compositional fabrics in the lower crust. Further, many flow laws describing the rheology of monophase aggregates are experimentally derived and do not necessarily apply to polyphase materials, such as gabbro, that dominate the lower crust. Here, we present the results of integrated microstructural analysis and electron backscatter diffraction (EBSD) textural analysis from exhumed lower crustal granulites in the Mount Hay block of central Australia. The preservation of heterogeneous mafic and felsic granulites containing monophase and/or polyphase mixtures of anorthite, pyroxene, and quartz (interlayered on the mm- to m-scale) make this region uniquely suited for advancing our knowledge of the processes that affect deformation and the rheology of the lower crust. Forty-two samples from distinct structural and compositional domains were chosen to compare the microstructural record of deformation, the development of crystallographic textures, and to provide estimates of lower crustal rheology and deformation conditions. Full thin-section maps of crystallographic texture were produced using EBSD methods. The resultant orientation maps were processed to characterize crystallographic textures in all constituent phases, and all other quantifiable aspects of the rock microstructure (e.g., grain size, grain shape, misorientation axes). The EBSD analysis reveals the presence of strong crystallographic preferred orientations (CPO) in nearly all constituent phases, suggesting deformation dominated by dislocation creep. Differential stresses during deformation are calculated using grain size piezometry for all major phases, and range between 34-54 MPa in quartz within monophase layers. Two-pyroxene geothermometry was used to constrain deformation temperatures to ca. 780-810 C. Based on the estimated CPO patterns, stress, and temperature, we quantify strain rates and effective viscosities of all major phases through application of monophase flow laws. Monophase strain rates range from 2.10 x 10-12 s-1 to 1.56 x 10-11 s-1 for quartz, 4.68 x 10-15 s-1 to 2.48 x 10-13 s-1 for plagioclase feldspar, 1.56 x 10-18 s-1 to 1.64 x 10-16 s-1 for enstatite, and 5.66 x 10-16 s-1 to 1.00 x 10-14 s-1 for diopside. The determined flow law variables used for monophase calculations were subsequently applied to two different models – the Minimized Power Geometric model of Huet et al. (2014) and the Asymptotic Expansion Homogenization (AEH) method of Cook (2006) – in order to calculate a bulk aggregate viscosity of the polyphase material. At a strain rate of 10-14 s-1, polyphase effective viscosities for our samples range from 3.07 x 1020 to 2.74 x 1021 Pa·s. We find that the bulk viscosity of heterogeneous, gabbroic lower crust in the Mount Hay region lies between that of monophase plagioclase and monophase quartz, and varies as a function of composition. These results are consistent with past modeling studies and geophysical estimates. / Thesis (MS) — Boston College, 2019. / Submitted to: Boston College. Graduate School of Arts and Sciences. / Discipline: Earth and Environmental Sciences.

Further understanding of mesoscale slip mechanics is crucial to future development of polycrystalline metals with improved performance. The research contained within this thesis aims to characterize localized mesoscale slip on slip bands further through two studies. First, a comprehensive comparison of slip system identification techniques was carried out to further validate each method as well as compare advantages and disadvantages of each. Second, slip bands in the presence of grain boundaries were studied to better characterize the dislocation content and behavior. In the first study, the use of SEM-DIC, AFM, ECCI, and HR-EBSD to characterize slip-system activity was assessed on the same material volume of Ti-7Al. This study presents a robust comparison of the various methods for the first time, including an assessment of their advantages and disadvantages, and how they can be used effectively in a complementary manner. The analysis of the different approaches was carried out in a blind manner independently at three different universities. A Ti-7Al specimen was deformed in uniaxial tension to approximately 3% axial strain, and the active slip systems were independently identified using (i) trace analysis; (ii) in-SEM digital image correlation, (iii) observations of residual dislocations from ECCI, and (iv) long-range rotation gradients through HR-EBSD, with consistent trace identification in all cases. Displacement data from AFM was used to augment the SEM-DIC displacement data by providing complementary out of plane displacement information. Furthermore, short-range dislocation gradients (measured by DIC) provided insight into the residual geometrically necessary dislocation (GND) content, and was consistent with the GND content extracted from EBSD data and ECCI images, confirming the presence of residual GNDs on the dominant slip systems resulting in visible slip bands. These approaches can be used in tandem to provide multi-modal information on slip band identification, strain and orientation gradients, out-of-plane displacements, and the presence of GNDs and SSDs, all of which can be used to inform and validate the development of dislocation-based crystal plasticity and strain gradient models. In the second study, shear strain profiles along slip bands in a modified Rolls-Royce nickel superalloy (RR1000) were analyzed for a tensile sample deformed by 2%. The strain increased with distance away from a grain boundary (GB), with maximum shear strain towards the center of the grain, indicating that dislocation nucleation generally occurred in the grain interior. The strain gradients in the neighborhood of the GBs were quantified and generally correlated with rotation about the active slip system line direction. This leads to an ability to determine the active slip system in these regions. The dislocation spacing and pileup stresses were inferred. The dislocation spacing closely follows an Eshelby analytical solution for a single ended pileup of dislocations under an applied stress. The distribution of pileup stress values for GBs of a given misorientation angle follows a log-normal distribution, with no correlation between the pileup stress and the GB misorientation angle. Furthermore, there is no observed correlation between various transmissivity factors and slip band pileup stress. Hence it appears that the obstacle strength of any of the observed GBs is adequate to facilitate the dislocation pileups present in the slip bands. However, slip band transmission does correlate with transmissivity factors, with the current study focusing on the Luster and Morris m'-factor. Observation of strain profiles of transmitted bands indicate dislocation nucleation locations.

Residual stress measurement methods have commonly been used to characterize states of stress in various elastic isotropic materials. In order to investigate the effects of elastic anisotropy on residual stress measurements, commercially pure grade 2 titanium (CP Ti Gr 2) was selected to study a strong texture, or preferred grain orientation. Warm rolled and air-cooled CP titanium is well known to have a texture from the factory. This texture and resulting elastic anisotropy were confirmed using two material characterization methods, resonant ultrasound spectroscopy (RUS) and electron backscatter diffraction (EBSD). The texture was further developed using a rolling mill to cold roll the titanium. A vacuum furnace set to a temperature of 550 C for one hour was used to stress relieve the titanium without reducing the texture. RUS and EBSD methods were used again to confirm the texture achieved by cold rolling. Well-characterized residual stresses were introduced with a shrink-fit ring and plug. The residual stress hole drilling method was used to characterize stresses in the rolling and transverse directions of the ring and plug assemblies. Stress profiles from hole drilling indicated some possible elastic anisotropic effects in two assemblies and are presented. However, more assemblies are needed to confirm the results. A stress determination technique with higher sensitivity may be necessary to substantiate assembly stress profile results.