Dissertations / Theses: 'EBSD - Electron BackScatter Diffraction'

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Hansen, Landon Thomas. "Characterization of Dislocation - Grain Boundary Interactions Through Electron Backscatter Diffraction." BYU ScholarsArchive, 2019. https://scholarsarchive.byu.edu/etd/7536.

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Further understanding of dislocation-GB interactions is critical to increasing the performance of polycrystalline metals. The research contained within this dissertation aims to further dislocation-GB interaction understanding through three research studies. First, the effect of noise in EBSPs on GND calculations was evaluated in order to improve dislocation characterization via HR-EBSD. Second, the evolution of GNDs and their effects on back stress was studied through experimental and computational methods applied to tantalum oligo specimens. Third, statistical analysis was used to evaluate grain parameters and current GB transmission parameters on their correlation with dislocation accumulation.

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Basinger, John A. "Detail Extraction from Electron Backscatter Diffraction Patterns." BYU ScholarsArchive, 2011. https://scholarsarchive.byu.edu/etd/2689.

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Cross-correlation based analysis of electron backscatter diffraction (EBSD) patterns and the use of simulated reference patterns has opened up entirely new avenues of insight into local lattice properties within EBSD scans. The benefits of accessing new levels of orientation resolution and multiple types of previously inaccessible data measures are accompanied with new challenges in characterizing microscope geometry and other error previously ignored in EBSD systems. The foremost of these challenges, when using simulated patterns in high resolution EBSD (HR-EBSD), is the determination of pattern center (the location on the sample from which the EBSD pattern originated) with sufficient accuracy to avoid the introduction of phantom lattice rotations and elastic strain into these highly sensitive measures. This dissertation demonstrates how to greatly improve pattern center determination. It also presents a method for the extraction of grain boundary plane information from single two-dimensional surface scans. These are accomplished through the use of previously un-accessed detail within EBSD images, coupled with physical models of the backscattering phenomena. A software algorithm is detailed and applied for the determination of pattern center with an accuracy of ~0.03% of the phosphor screen width, or ~10µm. This resolution makes it possible to apply a simulated pattern method (developed at BYU) in HR-EBSD, with several important benefits over the original HR-EBSD approach developed by Angus Wilkinson. Experimental work is done on epitaxially-grown silicon and germanium in order to gauge the precision of HR-EBSD with simulated reference patterns using the new pattern center calibration approach. It is found that strain resolution with a calibrated pattern center and simulated reference patterns can be as low as 7x10-4. Finally, Monte Carlo-based models of the electron interaction volume are used in conjunction with pattern-mixing-strength curves of line scans crossing grain boundaries in order to recover 3D grain boundary plane information. Validation of the approach is done using 3D serial scan data and coherent twin boundaries in tantalum and copper. The proposed method for recovery of grain boundary plane orientation exhibits an average error of 3 degrees.

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Wu, Chun-Hsien. "Microstructure of Flash processed Steel Characterized by Electron Backscatter Diffraction." Thesis, Virginia Tech, 2009. http://hdl.handle.net/10919/36377.

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Flash processing is a new heat treatment process being developed to produce steel with relatively high strength and ductility. It involves rapidly heating steel sheet or strip to a temperature in the austenite range and quenching; the entire thermal cycle takes place within 15 seconds. The resulting microstructure is fine and difficult to resolve using standard metallographic techniques. In this investigation, electron backscatter diffraction was used to measure the grain size, grain orientations, and phase fractions in AISI 8620 samples flash processed to a series of different maximum temperatures. The combination of high strength with moderate ductility obtained by flash processing arises from a refined martensitic microstructure. The morphology of the microstructure depends upon the maximum processing temperature; a lower maximum temperature appears to produce a finer prior austenite grain size and an equiaxed martensite structure whereas a higher maximum processing temperature yields a more conventional lath martensite morphology.
Master of Science

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Friedbaum, Samuel Searle. "Studies of Dislocation Density Quantification Via Cross-Correlation EBSD." BYU ScholarsArchive, 2019. https://scholarsarchive.byu.edu/etd/8115.

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One conventional method for studying dislocations uses the Transmission Electron Microscope (TEM), a complex and expensive piece of equipment which requires extensive specimen preparation in order to thin the specimens to electron transparent thickness. Newer High Resolution Electron Backscatter Diffraction (HREBSD) methods of determining geometrically necessary dislocation content via cross-correlation promise to be able to produce estimates of the dislocation density of the sample over a larger area with considerably less preparation time and using a much more accessible instrument. However, the accuracy of the new EBSD technique needs more experimental verification, including consideration of possible changes in the specimen dislocation density due to the different preparation methods. By comparing EBSD and TEM dislocation measurements of Electron Transparent platinum specimens prepared using the Focused Ion Beam (FIB), along with EBSD dislocations measurements of specimens prepared by both FIB and mechanical polishing techniques, this paper seeks to verify the accuracy of the new method and identify any changes in the specimens’ apparent dislocation density caused by the different preparation processes.

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Jiang, Jun. "A high resolution electron backscatter diffraction study of heterogeneous deformation in polycrystal copper." Thesis, University of Oxford, 2013. http://ora.ox.ac.uk/objects/uuid:31926294-d734-42f1-8b26-cbbb56438219.

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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.

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Khosravani, Ali. "Application of High Resolution Electron Backscatter Diffraction(HR-EBSD) Techniques to Twinning Deformation Mechanism in AZ31 Magnesium Alloy." BYU ScholarsArchive, 2012. https://scholarsarchive.byu.edu/etd/3432.

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The application of high resolution electron backscatter diffraction (HR-EBSD) techniques has been used in order to study the evolution of geometrically necessary dislocation (GND). The tested materials were taken from AZ31 magnesium sheet which had strong basal texture. Because of low symmetry of the magnesium crystal lattice, the von Mises criteria cannot be satisfied by the three independent, easily activated, basal slips. The strain along the c-axis of the crystal must be accommodated by either twinning and/or slip systems. HR-EBSD data was taken in order to investigate these phenomena. The HR-EBSD results were post processed in order to resolve total GND density onto the observed possible slip systems. The first chapter of the investigation focused on the correlation between resolved GNDs with tensile twin nucleation, and the subsequent propagation path in the microstructure. For this purpose, 2.5 % strain was applied in a uniaxial compression test along the transverse direction (TD). Several fine scan were done at the boundaries where twin formed. The results show that in order for a twin to nucleate spontaneously at the grain boundaries, two criteria should generally be met: high angle grain boundaries (35-45°) and pile ups of basal slip system in neighboring grain at the other side of the boundary. Furthermore, once nucleation has initiated, twin propagation can occur through low angle grain boundaries (15-25°); if a twin reaches a high angle boundary, it will generally terminate at the boundary at low strain levels. A twin may pass through high angle boundaries with further deformation. In the second chapter, deformation of the AZ31 magnesium alloy was study for different strain paths. For this purpose, compression and tension in-situ tests were done and the texture and GND evolutions were investigated. The results show that the load paths, compression and tension, evolve the microstructure in different ways. Massive twin fractions were formed in compression, and higher GND contents were observed in tension tests. It was observed that at higher strain levels GND contents are roughly independent of the initial texture but the activation of slip systems at low strain strongly depends on initial structure. If the samples were loaded along RD, GND density increased sharply at low strain. In contrast, for the samples loaded along TD, GND increased moderately. A small amount of repetition is apparent in the two parts of the thesis due to them being formatted for individual publication as journal papers.

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Bastos, da Silva Fanta Alice. "Characterization of the microstructure, grain boundaries and texture of nanostructured electrodeposited CoNi by use of electron backscatter diffraction (EBSD)." Göttingen Cuvillier, 2007. http://d-nb.info/991032845/04.

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Bastos, da Silva Fanta Alice. "Characterization of the microstructure, grain boundaries and texture of nanostructured electrodeposited CoNi by use of Electron Backscatter Diffraction (EBSD) /." Göttingen : Cuvillier, 2008. http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&doc_number=017078787&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA.

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Wisniewski, Wolfgang [Verfasser], Christian [Akademischer Betreuer] Rüssel, Thomas [Akademischer Betreuer] Höche, and Joachim [Akademischer Betreuer] Deubener. "Crystal orientations in glass-ceramics determined using electron backscatter diffraction (EBSD) / Wolfgang Wisniewski. Gutachter: Christian Rüssel ; Thomas Höche ; Joachim Deubener." Jena : Thüringer Universitäts- und Landesbibliothek Jena, 2011. http://d-nb.info/1016555318/34.

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Amalaraj, Akash Savio. "5D Grain Boundary Characterization from EBSD Microscopy." BYU ScholarsArchive, 2018. https://scholarsarchive.byu.edu/etd/8816.

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Knowledge of the full 5-degree Grain Boundary Character Distribution (GBCD) is vital to understanding properties, such as gas diffusivity, that are dominated by grain boundary character. Surface characterization techniques, such as Electron Backscattered diffraction (EBSD), can provide only 4 of the 5 GB characteristics (the rotation between the neighboring grains, and the trace of the GB on the surface). The inclination of the GB in the direction normal to the surface is not known. A previous study indicated that the GB inclination could be recovered by correlating the Electron Backscattered patterns (EBSPs) of sample points near the GB with EBSPs taken from the centers of the neighboring grains. The resultant transition curve could be compared with theoretical curves obtained from MonteCarlo simulations of electron yield from the two grains. However, a practical method based upon this study was never implemented. Here, a few microscopy and image filters have been applied to the EBSPs to improve the image quality. Also, several experiments have been conducted to verify and validate the interaction volume of the materials used to produce theoretical transition curves, in order to receive more accurate results. In this work, it is hypothesized that transition curves obtained from considering individual band intensities from the EBSPs will give more informative transition curves. The filtered EBSPs from the band intensities coupled with the accurate interaction volume values, should give us more reliable and repeatable transition curves, and that a more detailed comparison of the experimental and simulated transition curves will give higher fidelity results, in terms of GB inclination determination.

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Nelson, Benjamin D. "Using Design of Experiments and Electron Backscatter Diffraction to Model Extended Plasticity Mechanisms In Friction Stir Welded AISI 304L Stainless Steel." BYU ScholarsArchive, 2010. https://scholarsarchive.byu.edu/etd/2582.

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Extended plasticity mechanisms (EPM) allow a metal to undergo extended plastic deformation without failure. These mechanisms are responsible for the extended plastic deformation characteristic of hot working processes. In this thesis it is shown that electron backscatter diffraction (EBSD) is capable of detecting EPM artifacts in the final microstructure of AISI 304L stainless steel (304L). Results also indicate that dislocation cells form in hot worked AISI 304L stainless steel. Additionally, in this study EBSD data collection and analysis is used with a design of experiments approach to model the presence of EPM artifacts in the final microstructure of friction stir welded 304L. Texture analysis of the welded material reveals a dominant shear deformation texture and a lack of the rotated cube texture. The shear deformation texture is characteristic of dynamic recovery (DRV) and continuous dynamic recrystallization (CDRX), while the rotated cube texture is characteristic of discontinuous dynamic recrystallization (DDRX). The texture analysis results indicate that dynamic recovery (DRV) and continuous dynamic recrystallization (CDRX) play a role in the final microstructure of the welded material, while DDRX does not. Design of experiments was used to find the relationships between the fraction of cell boundaries and spindle speed, travel speed, location in the stir zone, and tool temperature. The regression analyses reported that predicted fraction of cell boundaries were relatively high (approximately 0.70 or more) and changed by less that 20% in the stir zone and 10% in the TMAZ. The relatively high predictions indicate that in FSW 304L DRV dominates and limited CDRX occurs. The small changes in predictions across the experimental space indicate that the effects, while statistically significant, are not practically significant. Finally, an alternate tool temperature basis was developed, which provides a valid method for selecting welds which should have constant tool temperature.

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Mateescu, Nora-Maria Materials Science &amp Engineering Faculty of Science UNSW. "Development of 3D-EBSD and its application to the study of various deformation and annealing phenomena." Publisher:University of New South Wales. Materials Science & Engineering, 2008. http://handle.unsw.edu.au/1959.4/41541.

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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.

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Mo, Liping. "Microstructural and mechanical characteristics of micro-scale intermetallic compounds interconnections." Thesis, Loughborough University, 2016. https://dspace.lboro.ac.uk/2134/23258.

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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.

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Sperry, Ryan Aaron. "Characterization of Slip Activity in the Presence of Slip Bands Using Surface-Based Microscopy Techniques." BYU ScholarsArchive, 2020. https://scholarsarchive.byu.edu/etd/8680.

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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.

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Gambirasi, Arianna <1970&gt. "La diffrazione degli elettroni retrodiffusi nello studio di materiali micro- e nano-strutturati in matrici eterogenee." Doctoral thesis, Università Ca' Foscari Venezia, 2013. http://hdl.handle.net/10579/3000.

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Nella presente tesi la tecnica di diffrazione degli elettroni retrodiffusi (EBSD) è stata impiegata per lo studio di materiali cristallini di dimensioni sub-micrometriche in campioni complessi sia per il tipo di matrice sia per la morfologia del materiale, per i quali le tecniche analitiche convenzionali risultano inadeguate. Al fine di evidenziare potenzialità e limiti dell’EBSD sono stati scelti due campi di applicazione: lo studio dei materiali nel campo dei Beni Culturali e la caratterizzazione dei materiali nanostrutturati ottenuti con tecniche diverse di sintesi (metal organic chemical vapor deposition, MOCVD; sol-gel; elettrodeposizioni su superfici elettrodiche, ecc.). I risultati ottenuti hanno dimostrato che la tecnica EBSD rappresenta un valido strumento sia per lo studio di fasi cristalline in matrici eterogenee che per la caratterizzazione di materiali innovativi con morfologia complessa. La tecnica EBSD potrà sicuramente contribuire allo sviluppo di nuovi materiali nanostrutturati per i quali è fondamentale disporre di tecniche analitiche adeguate che consentano di caratterizzare con altissima risoluzione materiali sempre più ridotti dimensionalmente e al contempo sempre più complessi.
In this PhD dissertation the electron backscatter diffraction (EBSD) was used to study complex sub-micron sized crystalline materials with peculiar composition and/or morphology, for which the usual analytical techniques result unsuitable. To highlight potential and limitations of EBSD two application fields were explored: the study of Cultural Heritage's materials and the characterization of nanosctructured materials obtained by different synthesis techniques (metal organic chemical vapor deposition, MOCVD; sol-gel, electrodeposition on electrodes' surface; etc.). The results obtained by using EBSD both in the field of Cultural Heritage and Nanomaterials proved that it is a useful tool for the study of crystalline materials in heterogeneous matrices and for the characterization of innovative materials with complex morphology. In the next future the EBSD will contribute to the development and production of nanostructured materials for which it is essential to have suitable analytical techniques with high resolution, thus able to characterize materials with increasingly reduced size and more and more complex morphology.

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Vayrette, Renaud. "Analyse des contraintes mecaniques et de la resistivite des interconnexions de cuivre des circuits integres : role de la microstructure et du confinement geometrique." Thesis, Saint-Etienne, EMSE, 2011. http://www.theses.fr/2011EMSE0599/document.

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L’évolution de la technologie microélectronique conduit à une densité d’intégration toujours plus forte des transistors. Les structures d’interconnexions en cuivre Damascène suivent cette tendance et doivent être maîtrisées en termes de fabrication, de performance et de robustesse, ces différents aspects étant intimement liés aux contraintes résiduelles et à la résistivité. Cette thèse vise à comprendre les mécanismes de génération de contraintes et identifier les différentes contributions à la résistivité de ces objets en fonction des conditions de recuit et des dimensions (de la centaine de nm à plusieurs µm). Pour ce faire, les rôles respectifs de la microstructure et des dimensions de films et de lignes de cuivre électrodéposés ont été découplés sur la base de modèles analytiques intégrants des paramètres microstructuraux et géométriques. La microstructure a été analysée principalement à partir de cartographies d’orientations cristallines réalisées par EBSD. Dans le cas des lignes de cuivre de 0.2 à 1 µm de large, les contraintes résiduelles ont été déduites de l’exploitation de nano-capteurs pivotants spécialement élaborés. Les résultats obtenus montrent qu’indépendamment de la température de recuit, l’augmentation de résistivité et de contraintes résiduelles observée vers les faibles dimensions est le fruit d’une diminution de la taille moyenne de cristallites et d’un confinement géométrique plus prononcé. En outre, l’augmentation de résistivité résulte également d’une élévation de la probabilité de réflexion des électrons aux joints de grains. Cette dernière a été associée à la réduction de la proportion de joints de grains spéciaux de cohérence atomique élevée
The evolution of the microelectronic technology leads to a transistors integration density always stronger. The Damascene copper interconnections structures follow this tendency and must be controlled in terms of manufacturing, performance and robustness, these different aspects being intimately related to the residual stresses and resistivity. This thesis aims to understand the mechanisms of the residual stresses generation and identify the different contributions to the resistivity of these objects as a function of annealing conditions and dimensions (from about a hundred of nm to several µm). In order to do this, the respective effects of the microstructure and dimensions of electroplated copper films and lines were separated on the basis of analytical models integrating microstructural and geometrical parameters. The microstructure was principally analysed from mappings of crystalline orientations achieved by EBSD. For the copper lines of width 0.2 and 1 µm, the residual stresses were deduced from the exploitation of nano-rotating sensors specially elaborated. The results obtained show that independently of the annealing temperature, the resistivity and residual stresses increase observed toward the small dimensions arises from the diminution of the average crystallites size and the geometrical confinement more pronounced. Furthermore, the resistivity increase results also of the electrons reflection probability growth at grains boundaries. This last point was associated to the reduction of the proportion of special grains boundaries having a high atomic coherency

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Shrestha, Sachin. "Characterising the effect of Niobium-rich clusters on the microstructure-property relationships in CASTRIP® steels." Thesis, The University of Sydney, 2013. http://hdl.handle.net/2123/10297.

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Many properties of steels, especially those that are important for engineering purposes, are determined by their microstructures. Therefore the key driver to controlling properties of these materials lies within the characterisation and manipulation of their microstructure down to their atomic-scale structure. For industrial product development, strength and ductility are considered to be the most important properties and are highly ‘microstructure sensitive’. This thesis investigates the effect of niobium microalloying and clustering on the microstructure-property relationship of ultra-thin strip cast steels produced by the CASTRIP® steel manufacturing process using mechanical testing and advanced microanalysis techniques. The CASTRIP® process is a revolutionary new method of steel strip casting that requires significantly less energy, time, equipment, and floor space compared to conventional strip casting methods. New and improved microanalysis characterisation techniques were also developed as a part of this project in order to better characterise these steels. The work presented in this thesis will have industrial and scientific significance that is both of benefit to the CASTRIP® steel making process and its products and more generally for the microstructural characterisation of ferrous alloys, one of the most important classes of engineering materials.

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Adams, Derrik David. "Characterization of the Factors Influencing Retained Austenite Transformation in Q&P Steels." BYU ScholarsArchive, 2020. https://scholarsarchive.byu.edu/etd/8425.

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Formable Advanced High-Strength Steels (AHSS) have a unique combination of strength and ductility, making them ideal in the effort to lightweight vehicles. The AHSS in this study, Quenched and Partitioned 1180, rely on the Transformation Induced Plasticity (TRIP) effect, in which retained austenite (RA) grains transform to martensite during plastic deformation, providing extra ductility via the transformation event. Understanding the factors involved in RA transformation, such as local strain and grain attributes, is therefore key to optimizing the microstructure of these steels. This research seeks to increase understanding of those attributes and the correlations between microstructure and RA transformation in TRIP steels. To measure local strain, the viability of using forescatter detector (FSD) images as the basis for DIC study is investigated. Standard FSD techniques, along with an integrated EBSD / FSD approach (Pattern Region of Interest Analysis System), are both analyzed. Simultaneous strain and microstructure maps are obtained for tensile deformation up to around 6% strain. The method does not give sub-grain resolution, and surface feature evolution prevents DIC analysis across large strain steps; however, the data is easy to obtain and provides a natural set of complementary information for the EBSD analysis. In-situ tensile tests combined with EBSD allow RA grain and neighboring attributes to be characterized and corresponding transformation data to be obtained. However, pseudo-symmetry of the ferrite (BCC) and martensite (BCT) phases prevents EBSD from accurately identifying all phases. Measuring the relative distortion of the crystal lattice, tetragonality, is one approach to identifying the phases. Unfortunately, small errors in the pattern center can cause significant errors in tetragonality measurement. Therefore, this research utilizes a new approach for accurate pattern center determination using a strain minimization routine and applies it to tetragonality maps for phase identification. Tetragonality maps based on dynamically simulated patterns result in the most accurate maps and can also be used to predict approximate local carbon content. Machine learning is then used on the collected data to isolate key attributes of RA grains and provide a decision tree model to predict transformation based on those attributes. Among the most relevant attributes found, RA grain area, RA grain shape aspect ratio, a “hardness” factor, and major axis orientation are included. Possible correlations between these factors and transformation improve understanding of relevant attributes and show the advantage that machine learning can have in unravelling complex material behavior.

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Svahnberg, Henrik. "Deformation behaviour and chemical signatures of anorthosites: : Examples from southern West Greenland and south-central Sweden." Doctoral thesis, Stockholms universitet, Institutionen för geologiska vetenskaper, 2010. http://urn.kb.se/resolve?urn=urn:nbn:se:su:diva-42854.

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Plagioclase is the most abundant mineral in the lower crust and it is thus important to constrain the behaviour of plagioclase during deformation. Anorthosites, which are plagioclase-rich rocks, are common in Archaean cratons but their origin and rheological importance is still debated. The aims of this thesis are to 1) describe a newly discovered Archaean anorthosite complex (Naajat Kuuat, SW Greenland), investigate its origin and a possible genetic relationship between the anorthosite and associated mafic-ultramafic rocks and 2) to study the rheology and deformation mechanisms in plagioclase-rich rocks. The main focus of this thesis is on the deformation studies. (1) Geochemical whole-rock analyses from the Naajat Kuuat complex are indicative for an origin near a subduction zone setting. A genetic link by crystal fractionation between the anorthosite and associated mafic-ultramafic units is inferred. (2) Deformation behaviour of plagioclase is assessed from analyses of three anorthosite units deformed during different conditions. Samples were analysed using the electron backscatter diffraction technique (EBSD) in combination with optical and chemical analyses. All three case studies show significant strain localisation related to grain size reduction. A wet anorthosite deformed at dry conditions (T ~675-700°C) was dynamically recrystallised. Continuous bands of recrystallised grains developed a texture yet display microstructures and grain relationships indicative for grain size sensitive creep, suggesting that the rheology followed a Newtonian flow law. In the other two studies, samples with initially dry and wet composition, respectively, have experienced deformation during fluid present conditions at T ~550-620°C. These two samples show that fluids effectively caused reactions, replacements and aided strain localisation during deformation at mid crustal conditions.
At the time of the doctoral defence the following papers were unpublished and had a status as follows: Paper 1: Manuscript; Paper 2 Manuscript; Paper 3 Manuscript.

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Parlangeau, Camille. "Quantification des paléocontraintes par l'analyse des macles de la calcite : nouvelle approche d'acquisition et d'inversion des données et mécaniques du maclage." Thesis, Paris 6, 2017. http://www.theses.fr/2017PA066570/document.

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La compréhension et la simulation des mécanismes de déformation dans la croûte supérieure sont des enjeux scientifiques et techniques importants. La calcite étant un minéral commun de la croûte supérieure se déformant essentiellement par maclage sous 200 °C, c'est pour cette raison que l'on s'intéresse plus particulièrement au maclage de la calcite dans le cadre de cette thèse. L'utilisation du maclage de la calcite n'en est pas à son coup d'essai et de nombreuses méthodes d'inversions existent que ce soit pour remonter aux tenseurs des contraintes comme aux tenseurs des déformations. Cette thèse propose une nouvelle méthode d'inversion basée sur l'inversion d'Etchopar permettant de reconstruire 5 sur 6 paramètres du tenseur des contraintes avec une quantification fine des incertitudes. Cette méthode permet de détecter automatiquement l'existence d'un ou de plusieurs évènements tectoniques enregistrés par le maclage de la calcite. Un deuxième volet de la thèse consiste en l'amélioration de la méthode d'acquisition des données de macles en utilisant un EBSD (electron backscatter diffraction). En effet, l'utilisation traditionnelle de la platine universelle a des limitations techniques et amène aussi à un doute visuel sur l'appréciation du statut non-maclé de certains plans, en plus du côté long et fastidieux. Le dernier volet de la thèse consiste à déterminer le seuil de maclage de la calcite pour différentes tailles de grains à l'aide de tests mécaniques sous une presse uniaxiale. Qui plus est, le suivi en continu des déformations sur les monocristaux de calcite a permis de mettre en évidence le comportement macroscopique d'un cristal de calcite et la séquence de maclage
The understanding and modelling of deformation mechanics in the upper crust are important scientific and technical issues. The calcite is a common mineral in the upper crust and mainly deforms by twinning under 200°C. That is why we are interested by calcite twinning as part of this thesis. It is not the first time that calcite twinning is used to reconstruct paleostress or paleostrain tensors. This thesis propose a new inversion method based on the Etchecopar’s one allowing to reconstruct 5 among 6 parameters of the stress tensor with an accurate quantification of the uncertainties. This method allows to automatically detect the realness of one or several tectonic events recorded by calcite twinning. A second part of the thesis consists in the improvement of the data acquisition by using EBSD (electron backscatter diffraction). In fact, the traditional use of the universal stage has technical limitations and brings some optical doubt about the untwinned status of few planes in addition to the long and tedious side. The last part of the thesis consists in the establishing the threshold of calcite twinning for different grain sizes by mechanical tests under a uniaxial press. Moreover, the continuous monitoring of the experiments using single crystals of calcite allowed to highlight the macroscopic behavior of a single crystal and the sequence of twinning

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21

Sibil, Arnaud. "Comportement thermomécanique et endommagement de nouveaux réfractaires verriers à très haute teneur en zircone : investigation des mécanismes de fissuration par EBSD et émission acoustique." Phd thesis, INSA de Lyon, 2011. http://tel.archives-ouvertes.fr/tel-00701526.

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Cette thèse s'inscrit dans une démarche d'investigation des mécanismes d'endommagement de réfractaires électrofondus à très haute teneur en zircone. L'accent est en particulier mis sur la compréhension du phénomène de microfissuration, mécanisme de dégradation le plus dommageable pour ces matériaux. S'opérant au refroidissement, il conduit à la fracture des blocs électrofondus. Réalisés dans le cadre du programme NOREV (NOouveau REfractaires Verriers) soutenu par l'ANR, les travaux présentés sont le fruit d'une collaboration avec Saint Gobain CREE, le Centre des Matériaux P.M. FOURT de l'Ecole des Mines de Paris, le laboratoire GEMH de l'ENSCI de Limoges, ICAR et Euro Physical Acoustics. Ils font suite aux travaux réalisés lors du programme PROMETHEREF (2002-2005). Des expériences préliminaires ont permis de définir et d'affiner les orientations de l'étude. Prenant en considération l'anisotropie de dilatation de la zircone monoclinique et quadratique décrite dans la littérature, l'imagerie des électrons rétrodiffusés a notamment permis de révéler un lien entre l'arrangement de domaines cristallographiques et la fissuration observée. D'autres expérimentations conduites dans le domaine de l'émission acoustique ont mis en lumière son applicabilité et ses apports pour notre problématique ainsi que la nécessité de développer un algorithme de traitement adapté. Ainsi, trois axes de recherche ont été développés. Ils visent, par leur complémentarité, à permettre une analyse à plusieurs échelles de l'endommagement des matériaux de l'étude tout en s'appuyant sur leur comparaison. Ils permettent respectivement d'évaluer l'endommagement de manière indirecte, d'en examiner les origines à l'échelle microscopique et d'en déterminer l'occurrence en température à l'échelle globale de l'échantillon. Le premier volet consiste en une évaluation des propriétés mécaniques en températures soulignant les incidences de la fissuration. La mise en évidence de la fissuration sous-critique, l'évolution des propriétés élastiques ainsi que la détermination des propriétés à la rupture apportent autant d'éléments qui permettent ensuite d'enrichir l'étude fractographique. Le deuxième volet s'attache, après une interrogation quant à la présence simultanée de zircone monoclinique et quadratique, à déterminer les paramètres de maille et les coefficients de dilatation de ces deux structures pour les différents matériaux. La modélisation des mailles correspondantes se révèle alors d'un grand intérêt pour l'analyse de cartographies EBSD. Enfin, la validation et l'application d'un process de traitement novateur des données d'émission acoustique, intégrant un algorithme génétique, permet de quantifier l'endommagement et d'apporter des précisions quant à son action en température. Ces constatations sont confortées par des suivis par acousto-ultrasons.

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22

Erieau, Philippe. "Étude expérimentale et analyse numérique de l'influence des hétérogénéités induites par la déformation à froid sur la recristallisation primaire d'un acier IF-Ti." Châtenay-Malabry, Ecole centrale de Paris, 2003. http://www.theses.fr/2003ECAP0879.

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Ce travail se situe dans la thématique de l'influence des procédés de mise en forme sur le comportement des matériaux métalliques. La thèse a consisté à étudier le développement d'hétérogénéités induites par la déformation au cours du laminage, ainsi que leur effet sur la germination et la croissance de nouveaux grains. La caractérisation du comportement mécanique et de recuit a permis d'identifier les lois de comportement et de recuit. L'étape suivante a consisté, à l'aide du maillage 3D d'agrégats cristallins et d'une loi de comportement du monocristal intégrée dans la méthode des éléments finis, à étudier l'influence de l'interaction intergranulaire 3D, en compression plane, sur le développement des hétérogénéités. Cet effet est faible, d'où la possibilité d'effectuer des calculs 2D représentatifs. Pour simuler la recristallisation, un intérêt a été porté à l'estimation de l'énergie stockée. Il est montré que le travail plastique ne représente pas cette énergie, au contraire de la densité de dislocations. Différents types d'hétérogénéités ont ensuite été étudiés, à l'aide de calculs éléments finis, et ont été comparés à des résultats de la littérature. Il a été montré qu'une forte déformation locale n'est pas toujours associée à une forte énergie stockée, ou à un fort gradient d'orientation. L'effet résultant en recristallisation est discuté. Ensuite, une comparaison du champ d'orientation a été effectuée entre les déformations expérimentale et numérique d'un agrégat, et un très bon accord est trouvé. Le recuit expérimental de l'agrégat est effectué, et les microstructure et texture résultantes sont comparées aux résultats d'un calcul Monte Carlo prenant les résultats éléments finis comme données initiales. Un accord qualitatif est obtenu, et permet de dégager l'importance du gradient d'énergie, d'orientation et du voisinage sur la germination et la croissance des grains, et sur le développement des texture et microstructure recristallisées.

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23

Medy, Jean Rony. "Évaluation des effets de taille et d'architecture sur les propriétés mécaniques et électriques de fils composites métalliques cuivre/niobium fabriqués par déformation plastique sévère." Thesis, Poitiers, 2016. http://www.theses.fr/2016POIT2312/document.

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Les fils composites Cu/Nb étudiés ici sont d'excellents candidats pour les bobines non destructives générant des champs magnétiques pulsés intenses (B ≥ 100T). Ils sont fabriqués par Accumulative Drawing and Bundling (ADB) et sont constitué de renforts continus de Nb dans une matrice multi-échelles de Cu. Ces travaux rentrent dans le cadre du projet METAFORES (ANR-12-BS09-0002), visant l’évaluation des effets de taille et d’architecture sur les propriétés des conducteurs Cu/Nb. L’objectif principal consiste donc à caractériser leur microstructure et leurs propriétés à chaque étape de la fabrication par différentes techniques de caractérisation. Des essais mécaniques et électriques montrent une augmentation de la limite d’élasticité avec l’affinement de la microstructure tout en conservant une conductivité électrique adéquate. Les études de la texture globale par DRX ont mis en évidence trois composantes de texture de fibre dont deux pour la matrice de Cu (<111> et <100>) et une composante unique <110> pour le Nb. On retrouve ces trois composantes de texture dans les analyses locales (EBSD), cependant les proportions relatives des composantes du Cu varient en fonction du nombre de cycles ADB.Les essais de déformation in-situ sous neutrons ont mis en évidence des comportements élasto-plastique et purement élastique des familles de grains {111} du Cu et {110} du Nb respectivement, quels que soient les échantillons. Pour la famille {200} du Cu, le comportement mécanique varie en fonction du nombre de cycles ADB. Tous ces résultats viendront nourrir les simulations effectuées dans le cadre du projet METAFORES (Thèse de Tang Gu, ENSAM-Paris/Mines ParisTech)
High strength and high conductivity Cu/Nb composites studied here are very good candidates for the design of magnets generating high pulsed magnetic fields (B ≥ 100T). They are fabricated by Accumulative Drawing and Bundling (ADB) and are constituted with a multi-scale Cu matrix embedding continuous Nb filaments that are distributed in a controlled manner. This study is performed within the framework of the METAFORES project (ANR-12-BS09-0002) aiming at assessing size and architecture effects on properties of these Cu/Nb conductors. The main purpose is therefore to characterize the microstructure and properties of these conductors at different stages of the fabrication process. Mechanical and electrical results show an increase in yield strength while maintaining adequate electrical conductivity. Global texture studies confirm three fiber texture components: two for the Cu matrix (<111> and <100>) and a single component <110 > for Nb. These three texture components are also observed at the local scale analysis (EBSD); however the volume fractions of the Cu components locally depend on the number of ADB cycles.In-situ deformation tests under neutrons reveal elasticplastic and purely elastic behaviors of the {111} Cu and {110} Nb grains family respectively, whatever the samples. However, for the {200} Cu grains family, mechanical behavior strongly depends on the number of ADB cycles. These results will feed the simulations conducted in the METAFORES project (Thesis of Tang Gu, ENSAM-Paris / Mines ParisTech)

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Gass, Evan M. "Anisotropy in Drawn and Annealed Copper Tube." Ohio University / OhioLINK, 2018. http://rave.ohiolink.edu/etdc/view?acc_num=ohiou153503217197025.

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25

Azzopardi, Alban. "Evolution microstructurale à haute température de barrières thermiques déposées par évaporation : influence sur la conductivité thermique et le module d'élasticité." Paris 6, 2003. http://www.theses.fr/2003PA066010.

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26

Aydogan, Eda. "Processing And Characterization Of Textured Barium Ferrite Ceramics." Master's thesis, METU, 2012. http://etd.lib.metu.edu.tr/upload/12614465/index.pdf.

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Technological advances results in the fact that quite a large number of electronic equipment interacts with its environment leading to the malfunction of the devices. This brings about the necessity of using proper electromagnetic (EM) wave absorbers/shields to avoid such interactions. In order to absorb EM waves in a large frequency band from several MHz to GHz, barium hexaferrite (BaHF) ceramics which are produced as textured ceramics as well as in multilayered form can be used. Textured ceramics are processed by tape casting using templated grain growth (TGG) phenomenon. In order to obtain textured ceramics, BaHF powders and platelets are required as raw materials in such a way that during sintering small size powders are directioned by large platelet surfaces. In this study, ferrite powders were synthesized by mixed oxide technique while the platelets were produced by both molten salt synthesis (MSS) and reactive templated grain growth (RTGG) methods. In the case of platelet synthesis by MSS, effects of calcination temperature and time as well as type and composition of the flux on the formation and morphology of platelets were investigated based on the XRD and SEM results. Studies have shown that KCl flux led to the formation of sharper platelet morphology, while NaCl resulted in more round shapes. However, extent of BaHF formation in the case of NaCl was higher when compared to KCl flux due to its higher wettability characteristic, and hence faster interaction with the raw materials. Since the aspect ratio of the synthesized platelets was only ca. 2-4, these platelets were not efficient for further TGG studies. Alternatively, BiFeO3 (BiF) particles having ~30-40 &mu
m average size were synthesized as seed crystals for the synthesis of BaHF platelets by RTGG method. After the washing of these platelets with dilute HNO3, pure BaHF powders and platelets were directed by tape casting which was followed by sintering using TGG phenomenon. Degree of achieved texturing in the processed ceramics was studied using Rietveld analysis, pole figure measurement and electron backscattered diffraction (EBSD).

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Favre, Julien. "Recrystallization of L-605 cobalt superalloy during hot-working process." Phd thesis, INSA de Lyon, 2012. http://tel.archives-ouvertes.fr/tel-00876664.

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Co-20Cr-15W-10Ni alloy (L-605) is a cobalt-based superalloy combining high strength with keeping high ductility, biocompatible and corrosion resistant. It has been used successfully for heart valves for its chemical inertia, and this alloy is a good candidate for stent elaboration. Control of grain size distribution can lead to significant improvement of mechanical properties: in one hand grain refinement enhance the material strength, and on the other hand large grains provide the ductility necessary to avoid the rupture in use. Therefore, tailoring the grain size distribution is a promising way to adapt the mechanical properties to the targeted applications. The grain size can be properly controlled by dynamic recrystallization during the forging process. Therefore, the comprehension of the recrystallization mechanism and its dependence on forging parameters is a key point of microstructure design approach. The optimal conditions for the occurrence of dynamic recrystallization are determined, and correlation between microstructure evolution and mechanical behavior is investigated. Compression tests are carried out at high-temperature on Thermec-master Z and Gleeble forging devices, followed by gas or water quench. Mechanical behavior of the material at high temperature is analyzed in detail, and innovative methods are proposed to determine the metallurgical mechanisms at stake during the deformation process. Mechanical properties of the material after hot-working and annealing treatments are investigated. The grain growth kinetics of L-605 alloy is determined, and experimental results are compared with the static recrystallization process. Microstructures after hot deformation are evaluated using SEM-EBSD and TEM. Significant grain refinement occurs by dynamic recrystallization for high temperature and low strain rate (T≥1100 ◦ C, strain rate < 0.1s−1), and at high strain rate (strain rate > 10s−1). Dynamic recrystallization is discontinuous and takes place from the grain boundaries, leading to a necklace structure. The nucleation mechanism is most likely to be bulging from grain boundaries and twin boundaries. A new insight of the modeling of dynamic recrystallization taking as a starting point the experimental data is proposed. By combining the results from the mechanical behavior study and microstructure observation, the recrystallization at steady-state is thoroughly analyzed and provides the mobility of grain boundaries. The nucleation criterion for the bulging from grain boundaries is reformulated to a more general expression suitable for any initial grain size. Nucleation frequency can be deduced from experimental data at steady-state through modeling, and is extrapolated to any deformation condition. From this point, a complete analytical model of the dynamic recrystallization is established, and provides a fair prediction on the mechanical behavior and the microstructure evolution during the hot-working process.

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Danielsson, Olivia. "Effect of carbon activity on microstructure evolution in WC-Ni cemented carbides." Thesis, KTH, Materialvetenskap, 2018. http://urn.kb.se/resolve?urn=urn:nbn:se:kth:diva-226566.

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The aim of this work was to systematically study how the microstructure evolution is affected by the carbon activity in WC-Ni cemented carbides. Seven WC-9.59at%Ni alloys with different carbon activity were sintered at 1500 °C. From investigating these alloys, the carbon window has been experimentally evaluated using light optical microscopy and compared to theoretical carbon window calculated using Thermo-Calc. The overall microstructure of cross sections and raw surfaces have been investigated using scanning electron microscopy. Finally, the WC grain size and distribution have been evaluated using electron backscatter diffraction. It was found that the experimental carbon window was slightly wider than the theoretical carbon window. The WC grain size increased and the grain size distribution got wider with increasing carbon activity. In addition, the largest WC grains showed the largest grain growth by increasing carbon activity. By comparing the present results of grain size and distribution of WC-Ni to previous results of WC-Co, it was found that the WC grain growth was more pronounced and more influenced by the carbon activity.

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29

Mackenzie, R. A. D. "Computer analysis of electron backscatter diffraction patterns." Thesis, University of Bristol, 1986. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.373724.

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30

Man, Ondřej. "Aplikace metody difrakce zpětně odražených elektronů v materiálovém inženýrství." Doctoral thesis, Vysoké učení technické v Brně. Fakulta strojního inženýrství, 2010. http://www.nusl.cz/ntk/nusl-233915.

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The thesis deals with principles and common applications of the electron backscatter diffraction (EBSD) method. Some practical experience in application of the method to a study of highly deformed structure of copper and its thermal stability is described on one hand, and, on the other hand, to a study of phase composition of TRIP steel on various levels of imposed strain. The limitations of EBSD method are discussed along with its resolution in comparison with other complimentary techniques.

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Watt, Lauren Elizabeth. "Characterising the matrix of primitive meteorites using electron backscatter diffraction." Thesis, Imperial College London, 2006. http://hdl.handle.net/10044/1/11953.

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Britton, Thomas Benjamin. "A high resolution electron backscatter diffraction study of titanium and its alloys." Thesis, University of Oxford, 2009. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.547449.

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L'Hôte, Gabriel. "Etude de la dynamique des dislocations de monocristaux de cuivre sous chargement cyclique : Emission acoustique et caractérisations microstructurales." Thesis, Lyon, 2019. http://www.theses.fr/2019LYSEI125.

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Pendant la déformation plastique des matériaux cristallins, une plasticité douce, faite de nombreux mouvements de dislocations non corrélés peut coexister avec une plasticité plus sauvage, sous la forme de mouvements collaboratifs : les avalanches de dislocations. La coexistence des deux plasticités dépend de la mise en place d’une structure de dislocations, celle-ci étant supposée entraver la propagation des avalanches. On se propose d’étudier la corrélation entre les évolutions microstructurales et les arrangements de dislocations sous chargement cyclique, d'une part, et la nature de la dynamique collective des dislocations, d'autre part, pour le cas de monocristaux de cuivre purs. Différents essais de fatigue à amplitude de contrainte imposée sont effectués pour étudier l’influence (i) du chemin de chargement, (ii) le rapport de chargement et (iii) l’orientation cristallographique sur les phénomènes de plasticité. La technique d’émission acoustique (EA) est utilisée pour étudier les deux types de plasticité. L’EA continue peut-être associée à la plasticité douce, tandis que l'EA discrète, présentant des signaux plus énergétiques que ceux émis en continu sont associés à la plasticité sauvage. Les microstructures de dislocations sont étudiées à l’aide des techniques EBSD (Electron Backscattered Diffraction, pour mesurer la désorientation cristalline) et ECCI (Electron Channeling Contrast Imaging, pour imager les dislocations au MEB) à la fin de chaque palier de fatigue. Le couplage EA-ECCI donne de précieuses informations quant à la dynamique des dislocations. Le suivi par ECCI, lors d’un essai de fatigue à Rσ=0,1 montre qu’une structure de dislocation n’est stable que pour le niveau de contrainte qui la vue naître. L’émergence d'une structure de dislocations constituent un obstacle aux mouvements des avalanches. Toutefois, l’application d’une amplitude de contrainte plus importante permet un réarrangement de la structure, celui-ci se faisant en grande partie sous la forme d’avalanches de dislocations pouvant se déplacer sur de plus longues distances que le libre parcours moyen. Les petits mouvements de dislocations non corrélés sont confinés à l'intérieur des structures de dislocations, entre les arrangements denses de dislocations (cellules, murs, etc.). La plasticité douce est en conséquence de plus en plus restreinte à mesure que le libre parcours moyen diminue. Le rapport de chargement (Rσ=-1) a une grande influence sur la formation des structures de dislocations, avec l’émergence de structures veines, matrices, bandes de glissement persistant et cellules denses, mais aussi sur la dynamique des dislocations, avec une évolution progressive de la plasticité douce au cours des cycles et une réduction du nombre d’avalanches pendant le durcissement du matériau. Concernant l’influence de l’orientation cristallographique, un nombre plus important de systèmes de glissement activés permet de limiter la contribution des avalanches à la plasticité
During the plastic deformation of crystalline materials, a soft plasticity, made up of many uncorrelated dislocation movements, can coexist with a wilder plasticity, in the form of collaborative movements: dislocation avalanches. The coexistence of the two plasticities depends on the establishment of a dislocation structure, which is supposed to hinder the spread of avalanches. It is proposed to study the correlation between microstructural evolutions and dislocation arrangements under cyclic loading on the one hand, and the nature of the collective dynamics of dislocations on the other hand, in the case of pure copper single crystals. Various stress imposed fatigue tests are performed to study the influence of (i) the loading path, (ii) the loading ratio and (iii) the crystallographic orientation on the plasticity phenomena. The acoustic emission (EA) technique is used to study both types of plasticity. Continuous EA, which can be considered as background noise resulting from the cumulative effect of many sources, is associated with mild plasticity. Discrete EA, with more energetic signals than those emitted continuously, is associated with wild plasticity. Dislocation microstructures are studied using EBSD (Electron Backscattered Diffraction) and ECCI (Electron Channeling Contrast Imaging) techniques at the end of each fatigue level. The EA-ECCI coupling provides valuable information on the dynamics of dislocations. The monitoring by ECCI, during a fatigue test at Rσ=0.1 shows that a given dislocation structure is stable only for given level of stress. The emergence of a dislocation structure act as an obstacle to avalanche movement. However, the application of a larger stress amplitude allows the rearrangement of the structure, which is largely in the form of dislocation avalanches that can travel longer distances than the dislocation mean free path. Small uncorrelated dislocation movements are confined within the dislocation structures, between dense dislocation arrangements (cells, walls, etc.). Mild plasticity is therefore increasingly restricted as the mean free path decreases. The various tests carried out show that the loading path (at Rσ=0.1) has no influence on the dislocation structure formed, but that the dynamics of the dislocations adapt to the way the material is loaded. The loading ratio (Rσ=-1) has a major influence on the formation of dislocation structures, with the emergence of veins, matrices, persistent slip bands and dense cells, but also on the dynamics of dislocations, with a gradual evolution of mild plasticity during cycles and a reduction in the number of avalanches during the hardening of the material. Concerning the influence of crystallographic orientation, a larger number of activated slip systems limit the contribution of avalanches to plasticity

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Yuan, Hui. "3D morphological and crystallographic analysis of materials with a Focused Ion Beam (FIB)." Thesis, Lyon, INSA, 2014. http://www.theses.fr/2014ISAL0134/document.

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L’objectif principal de ce travail est d’optimise la tomographie par coupe sériée dans un microscope ‘FIB’, en utilisant soit l’imagerie électronique du microscope à balayage (tomographie FIB-MEB), soit la diffraction des électrons rétrodiffusés (tomographie dite EBSD 3D). Dans les 2 cas, des couches successives de l’objet d’étude sont abrasées à l’aide du faisceau ionique, et les images MEB ou EBSD ainsi acquises séquentiellement sont utilisées pour reconstruire le volume du matériau. A cause de différentes sources de perturbation incontrôlées, des dérives sont généralement présentes durant l'acquisition en tomographie FIB-MEB. Nous avons ainsi développé une procédure in situ de correction des dérives afin de garder automatiquement la zone d'intérêt (ROI) dans le champ de vue. Afin de reconstruction le volume exploré, un alignement post-mortem aussi précis que possible est requis. Les méthodes actuelles utilisant la corrélation-croisée, pour robuste que soit cette technique numérique, présente de sévères limitations car il est difficile, sinon parfois impossible de se fier à une référence absolue. Ceci a été démontré par des expériences spécifiques ; nous proposons ainsi 2 méthodes alternatives qui permettent un bon alignement. Concernant la tomographie EBSD 3D, les difficultés techniques liées au pilotage de la sonde ionique pour l'abrasion précise et au repositionnement géométrique correct de l’échantillon entre les positions d'abrasion et d’EBSD conduisent à une limitation importante de la résolution spatiale avec les systèmes commerciaux (environ 50 nm)3. L’EBSD 3D souffre par ailleurs de limites théoriques (grand volume d'interaction électrons-solide et effets d'abrasion. Une nouvelle approche, qui couple l'imagerie MEB de bonne résolution en basse tension, et la cartographie d'orientation cristalline en EBSD avec des tensions élevées de MEB est proposée. Elle a nécessité le développement de scripts informatiques permettant de piloter à la fois les opérations d’abrasion par FIB et l’acquisition des images MEB et des cartes EBSD. L’intérêt et la faisabilité de notre approche est démontrée sur un cas concret (superalliage de nickel). En dernier lieu, s’agissant de cartographie d’orientation cristalline, une méthode alternative à l’EBSD a été testée, qui repose sur l’influence des effets de canalisation (ions ou électrons) sur les contrastes en imagerie d’électrons secondaires. Cette méthode corrèle à des simulations la variation d’intensité de chaque grain dans une série d’images expérimentales obtenues en inclinant et/ou tournant l’échantillon sous le faisceau primaire. Là encore, la méthode est testée sur un cas réel (polycritsal de TiN) et montre, par comparaison avec une cartographie EBSD, une désorientation maximale d'environ 4° pour les angles d’Euler. Les perspectives d’application de cette approche, potentiellement beaucoup plus rapide que l’EBSD, sont évoquées
The aim of current work is to optimize the serial-sectioning based tomography in a dual-beam focused ion beam (FIB) microscope, either by imaging in scanning electron microscopy (so-called FIB-SEM tomography), or by electron backscatter diffraction (so-called 3D-EBSD tomography). In both two cases, successive layers of studying object are eroded with the help of ion beam, and sequentially acquired SEM or EBSD images are utilized to reconstruct material volume. Because of different uncontrolled disruptions, drifts are generally presented during the acquisition of FIB-SEM tomography. We have developed thus a live drift correction procedure to keep automatically the region of interest (ROI) in the field of view. For the reconstruction of investigated volume, a highly precise post-mortem alignment is desired. Current methods using the cross-correlation, expected to be robust as this digital technique, show severe limitations as it is difficult, even impossible sometimes to trust an absolute reference. This has been demonstrated by specially-prepared experiments; we suggest therefore two alternative methods, which allow good-quality alignment and lie respectively on obtaining the surface topography by a stereoscopic approach, independent of the acquisition of FIB-SEM tomography, and realisation of a crossed ‘hole’ thanks to the ion beam. As for 3D-EBSD tomography, technical problems, linked to the driving the ion beam for accurate machining and correct geometrical repositioning of the sample between milling and EBSD position, lead to an important limitation of spatial resolution in commercial softwares (~ 50 nm)3. Moreover, 3D EBSD suffers from theoretical limits (large electron-solid interaction volume for EBSD and FIB milling effects), and seems so fastidious because of very long time to implement. A new approach, coupling SEM imaging of good resolution (a few nanometres for X and Y directions) at low SEM voltage and crystal orientation mapping with EBSD at high SEM voltage, is proposed. This method requested the development of computer scripts, which allow to drive the milling of FIB, the acquisition of SEM images and EBSD maps. The interest and feasibility of our approaches are demonstrated by a concrete case (nickel super-alloy). Finally, as regards crystal orientation mapping, an alternative way to EBSD has been tested; which works on the influence of channelling effects (ions or electrons) on the imaging contrast of secondary electrons. This new method correlates the simulations with the intensity variation of each grain within an experimental image series obtained by tilting and/or rotating the sample under the primary beam. This routine is applied again on a real case (polycrystal TiN), and shows a max misorientation of about 4° for Euler angles, compared to an EBSD map. The application perspectives of this approach, potentially faster than EBSD, are also evoked

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35

Serrano, Munoz Itziar. "Influence of casting defects on the fatigue behaviour of an A357-T6 aerospace alloy." Thesis, Lyon, INSA, 2014. http://www.theses.fr/2014ISAL0117/document.

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L’excellente coulabilité, les coûts de production relativement bas, et ratio poids/résistance mécanique élevé des alliages de fonderie Al-Si-Mg en font une des solutions les plus intéressantes dans le secteur automobile ainsi que dans le domaine aérospatial. Toutefois, il est bien connu que la durée de vie de ces composants moulés à grand nombre de cycles (105 < Nf < 107 cycles) est sévèrement réduite lorsque des défauts de fonderie (notamment pores et oxydes) sont débouchants et/ou subsurfaciques sont présents. Ces défauts concentrent les contraintes et peuvent considérablement réduire la période d’amorçage des fissures de fatigue en fonction de leur taille, forme et des caractéristiques microstructurales du matériau. Les défauts internes (à partir desquels les fissures peuvent amorcer et propager sans interaction avec l’air ambiant) ainsi que les défauts de surface (ceux qui sont placés à la surface et en contact direct avec l’air ambiant) vont également nuire la durée de vie des composants moulés. Toutefois, dans le cas des défauts internes, les coefficients de sécurité préconisés par les règles de conception ne font pas intervenir la distance de défaut par rapport à la surface. Le suivi de fissures de fatigue effectué à la surface d’éprouvettes macroscopiques de traction indique que la présence d’un défaut avec une taille supérieure à celle des fissures microstructuralement courtes (√A ≈ 500 μm, taille contrôlée par la SDAS) produit une remarquable réduction de la durée vie. En revanche, la durée de vie n’est pas affectée lorsqu’un défaut plus petit (√A ≈ 300 μm) est présent à la surface car l’amorçage et les premiers stades de propagation sont encore influencés par la SDAS. Les essais de fatigue en torsion pure montrent que la morphologie des surfaces de rupture est fortement influencée par le niveau de contrainte. De plus, le nombre de cycles à l’amorçage est réduit par rapport à la traction. Cet amorçage est multi-site et plusieurs fissures peuvent croitre simultanément au cours de la durée de vie d’une éprouvette, la rupture finale se produisant lors de la jonction de certaines de ces fissures. La propagation des fissures en torsion est largement influencée par la cristallographie locale et les retassures ne semblent pas être des sites de nucléation préférentiels. Les durées de vie odes échantillons macroscopiques contenant défauts artificiel internes (Øeq ≈ 2 mm) sont pratiquement similaires à celles obtenues avec un matériau de référence. L’amorçage et la propagation de fissures internes a été rarement observé lors des expériences de tomographie synchrotron. Dans les rares cas où de telles fissures ont pu être observées, le chemin de fissuration semble fortement influencé par la cristallographie alors que les fissures amorcées depuis la surface se propagent globalement en mode I. La vitesse de propagation des fissures internes est très inférieure à celle des fissures se propageant à partir de la surface
The excellent castability, relatively low production costs, and high strength to weight ratios make Al-Si-Mg cast alloys an attractive choice for use in cheaper and lighter engineering components, in both automotive and aerospace industries. However, it is well known that High Cycle Fatigue (HCF) lives (105 < Nf < 107 cycles) of cast components are severely reduced when casting defects (notably pores and oxides) are present at the free surface or subsurface. They act as stress raisers which can considerably reduce the crack incubation period depending on their size, shape and the microstructural features of the surrounding material. Internal casting defects are of special interest to this work. The application of safety coefficients considers that all casting defects present in a component have the same deleterious effect and no attention is paid, for example, to their distance to the free surface. In other words, internal defects (corresponding to the case where the depth of the defect allows crack nucleation and propagation to essentially occur without interaction with the air environment) are considered as damaging to fatigue life as surface defects (those placed at the free surface and in contact with the air environment). Surface crack monitoring performed on uniaxial fatigue specimens indicates that the presence of a surface microshrinkage exceeding the size of microstructurally small cracks (√A ≈ 500 μm, controlled by the SDAS) readily nucleates a fatigue cracks producing steady crack propagation and remarkable reduction in the expected fatigue life. A smaller surface defect (√A ≈ 300 μm) nucleated a crack that did not reduced the expected fatigue life as in this case early stages of propagation are still nfluenced by the SDAS. Pure torsional cycling reveals that the morphology of fracture surfaces is highly influenced by the stress level. In general, torsional fatigue behaviour is described by having reduced (with respect to uniaxial testing) and multisite crack nucleation periods. Several dominant cracks can evolve simultaneously and the final failure occurs by the linkage of some of those cracks. Crack propagation is controlled by the crystallography and pores do not appear to be preferential nucleation sites. S-N curves show that macroscopic specimens containing Øeq ≈ 2 mm internal artificial defect produce similar fatigue lives to those obtained with a defect-free material. Internal crack nucleation was rarely observed during synchrotron tomography experiments; instead the fatal cracks initiated from much smaller surface defects. Tomographic images show that, in the case of internal propagation, crystallographic paths are formed while surface cracks propagate in mode I. The crack growth rate of internal cracks is much smaller than that of cracks propagating from the free surface

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36

Essex, Stephen. "Ultrasonic characterisation of rolled aluminium and steel sheet correlated with electron backscatter diffraction measurements." Thesis, University of Warwick, 2009. http://wrap.warwick.ac.uk/3147/.

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This thesis is based on the characterization of material properties of interest in rolled aluminium and steel sheet, both popular materials used across a wide-range of applications. The forming processes involved in producing rolled sheet metal depend on plastic deformation, inducing elastic anisotropy as a consequence. These changes result in a variation from the simple isotropic and cubic symmetry systems possessed by steel and aluminium prior to cold-working. The most significant changes include the introduction of crystallographic texture and the morphology of the crystallographic grains in size and shape to accommodate the plastic deformation. It is desirable in industries that use rolled product for manufacturing components to quantify such changes. The literature has postulated links between plastic and elastic properties, and hence any quantification of the elasticity, crystallographic texture and grain morphology can aid in the prediction of future formability behaviour. This thesis presents non-destructive, rapid ultrasonic measurements to characterize some of the changes that are evident in rolled aluminium and steel sheet. These ultrasonic results have then been correlated to crystallographic orientation measurements generated from using a microscopic technique called electron backscatter diffraction (EBSD). The level of agreement between the two contrasting methods has been analysed and is presented here. The non-destructive ultrasonic measurements include quantifying crystallographic texture utilising theory linking the S0 Lamb wave velocity and the direction of propagation in a rolled sheet with respect to the rolling direction. This leads to the determination of texture coefficients known as orientation distribution coefficients (ODC). Through-thickness linearly polarized SH waves have then been used to analyse grain morphology using attenuation data, and elasticity measurements from velocity data. EBSD datasets have been manipulated to produce predictions of the effective elastic stiffness constants, which in turn can be used to generate comparable S0 Lamb wave velocity predictions to be directly compared to the ultrasonic measurements. This process has required a novel method to generate such ultrasonic velocity predictions as a function of angle, together with predictions for the nine effective elastic stiffness constants inherent to rolled orthorhombic sheet. The facility to measure grain size and shape accurately from EBSD data has been utilized. The thesis starts with a general introduction in non-destructive testing and microscopy, with focussed discussion on ultrasound, electromagnetic acoustic transducers (EMATs), EBSD and metallurgy in the subsequent chapters. Chapter 6 introduces the development of correlation methods between the ultrasound and EBSD results, with chapters 7 and 8 displaying the empirical ultrasound and EBSD data respectively. Chapter 9 compares the data from the two methods, with the final conclusions given in chapter 10.

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Lim, Ching Ee. "An Electron Backscatter Diffraction Study of Archean Impact Spherules from the Pilbara Craton, Western Australia." Thesis, Curtin University, 2022. http://hdl.handle.net/20.500.11937/89772.

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This thesis describes a systematic morphological study of minerals in feldspathic impact spherules from both Dales Gorge and Bee Gorge spherule layers in the Hamersley Basin of Pilbara Craton in Western Australia. The overarching goals are to advance interpretations on spherule formation processes. The research involves the characterisation of feldspathic spherules of the two impact horizons to propose a vapor plume model to identify where various spherule types may have formed. This includes the comparison of representative optical photomicrographs with their respective electron backscatter diffraction (EBSD) analytical results.

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Oliphant, Clive Justin. "Hot-wire chemical vapour deposition of nanocrystalline silicon and silicon nitride : growth mechanisms and filament stability." Thesis, University of the Western Cape, 2012. http://hdl.handle.net/11394/5203.

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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.

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39

Singh, Saransh. "Application of Forward Modeling to Materials Characterization." Research Showcase @ CMU, 2017. http://repository.cmu.edu/dissertations/1009.

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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.

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40

Seward, Gareth Gordon Edward. "The development of high temperature scanning electron microscopy and electron backscatter diffraction with application to the study of phase transformations." Thesis, University of Liverpool, 2004. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.417249.

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Barrie, Craig David. "An electron backscatter diffraction approach to understanding pyrite evolution from it's genesis to it's near destruction." Thesis, University of Liverpool, 2008. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.494152.

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Pyrite (FeSz) is the most abundant sulphide mineral in the crust and a common constituent of ore deposits. The refractory nature of pyrite means it has the potential to preserve information about initial formation, deformation and/or metamorphism of ore deposits. An understanding of primary formation controls and deformation mechanisms in pyrite may therefore assist In determination of the evolutionary history of ore deposits and so aid in their successful exploitation.

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42

Goudy, Secana Portia. "Assessment of Cluster Chondrite Accretion Temperature Using Electron Backscatter Diffraction and Implications for Chondrule Formation Models." PDXScholar, 2019. https://pdxscholar.library.pdx.edu/open_access_etds/5268.

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This thesis studies ordinary chondrites with cluster chondrite lithologies using electron backscatter diffraction so as to measure the temperatures of their olivine grains during deformation, for the purpose of constraining the accretion temperatures of cluster chondrites and creating new constraints on chondrule formation models. Samples analyzed with the technique are shock classified in this thesis as S1 and are type 3, so the deformation analyzed is interpreted to represent the temperatures of the chondrules during accretional deformation. It is found that the studied samples are primarily composed of chondrules at hot temperatures (>850°C) during deformation, mixed with a questionable minority at cold ((

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43

Terhune, Shannon Derek. "An electron backscatter diffraction analysis of the microstructure of pure aluminum processed by equal-channel angular pressing." Thesis, Monterey, California. Naval Postgraduate School, 1998. http://hdl.handle.net/10945/8304.

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Equal-channel angular (ECA) pressing is a promising method to achieve refinement of grain size to 1.0 micrometer or less for aluminum and its alloys. Computer-aided electron backscatter diffraction (EBSD) analysis of high purity aluminum (99.99%) which had been subjected to one pass, four passes, and twelve passes through an ECA die was performed. Grain and subgrain size and boundary misorientation distributions during such large-strain deformation processing were of particular interest. A texture was present after one pressing and the boundary misorientation distribution had a peak at 5 deg - 10 deg although boundaries were present in all misorientation ranges. Fine equaixed grains were achieved after twelve passes through the ECA die, accompanied by random orientation and misorientation distributions

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44

Ondračka, Václav. "Užití elektronové difrakce k mapování elastického napětí." Master's thesis, Vysoké učení technické v Brně. Fakulta strojního inženýrství, 2021. http://www.nusl.cz/ntk/nusl-449747.

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Electron backscatter diffraction is a method that is well described and commonly used for orientation image mapping, including grain size estimation. The use of this method for measuring elastic deformation and rotations caused by plastic deformations is not so well decribed. This diploma thesis first describes the typical EBSD system. The information regarding the standard coordinate systems, grain orientation notation and system calibration is then used to create an open-source software for mapping elastic deformations and rotations inside a single grain or a monocrystal. This software uses data acquired during standard EBSD mapping on a commercial system.

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45

Ornek, Cem. "Performance characterisation of duplex stainless steel in nuclear waste storage environment." Thesis, University of Manchester, 2016. https://www.research.manchester.ac.uk/portal/en/theses/performance-characterisation-of-duplex-stainless-steel-in-nuclear-waste-storage-environment(4db73e9b-c87c-40a6-9778-0b823b1c499f).html.

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The majority of UK’s intermediate level radioactive waste is currently stored in 316L and 304L austenitic stainless steel containers in interim storage facilities for permanent disposal until a geological disposal facility has become available. The structural integrity of stainless steel canisters is required to persevere against environmental degradation for up to 500 years to assure a safe storage and disposal scheme. Hitherto existing severe localised corrosion observances on real waste storage containers after 10 years of exposure to an ambient atmosphere in an in-land warehouse in Culham at Oxfordshire, however, questioned the likelihood occurrence of stress corrosion cracking that may harm the canister’s functionality during long-term storage. The more corrosion resistant duplex stainless steel grade 2205, therefore, has been started to be manufactured as a replacement for the austenitic grades. Over decades, the threshold stress corrosion cracking temperature of austenitic stainless steels has been believed to be 50-60°C, but lab- and field-based research has shown that 304L and 316L may suffer from atmospheric stress corrosion cracking at ambient temperatures. Such an issue has not been reported to occur for the 2205 duplex steel, and its atmospheric stress corrosion cracking behaviour at low temperatures (40-50°C) has been sparsely studied which requires detailed investigations in this respect. Low temperature atmospheric stress corrosion cracking investigations on 2205 duplex stainless steel formed the framework of this PhD thesis with respect to the waste storage context. Long-term surface magnesium chloride deposition exposures at 50°C and 30% relative humidity for up to 15 months exhibited the occurrence of stress corrosion cracks, showing stress corrosion susceptibility of 2205 duplex stainless steel at 50°C.The amount of cold work increased the cracking susceptibility, with bending deformation being the most critical type of deformation mode among tensile and rolling type of cold work. The orientation of the microstructure deformation direction, i.e. whether the deformation occurred in transverse or rolling direction, played vital role in corrosion and cracking behaviour, as such that bending in transverse direction showed almost 3-times larger corrosion and stress corrosion cracking propensity. Welding simulation treatments by ageing processes at 750°C and 475°C exhibited substantial influences on the corrosion properties. It was shown that sensitisation ageing at 750°C can render the material enhanced susceptible to stress corrosion cracking at even low chloride deposition densities of ≤145 µm/cm². However, it could be shown that short-term heat treatments at 475°C can decrease corrosion and stress corrosion cracking susceptibility which may be used to improve the materials performance. Mechanistic understanding of stress corrosion cracking phenomena in light of a comprehensive microstructure characterisation was the main focus of this thesis.

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Petráš, Roman. "Únavová odolnost a mechanizmy únavového poškození v materiálech pro vysoké teploty." Doctoral thesis, Vysoké učení technické v Brně. CEITEC VUT, 2021. http://www.nusl.cz/ntk/nusl-433631.

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Superaustenitická korozivzdorná ocel typu 22Cr25NiWCoCu určená pro vysokoteplotní aplikace v energetickém průmyslu byla studována za podmínek nízkocyklové únavy při pokojové a zvýšené teplotě. Jednotlivé vzorky byly podrobeny různým zátěžným procedurám, což umožnilo studium materiálové odezvy spolu s mechanismem poškození. Křivky cyklického zpevnění/změkčení, cyklického napětí a Coffin-Mansonovy křivky byly vyhodnoceny. Únavová životnost materiálu byla diskutována s ohledem na uplatňované mechanismy poškození, které se vyvinuly za specifických zátěžných podmínek. Standardní izotermální únavové experimenty byly provedeny při pokojové a zvýšené teplotě. Hysterezní smyčky zaznamenané během cyklického zatěžování byly analyzovány pomocí zobecněné statistické teorie hysterezní smyčky. Pro různé amplitudy napětí byla určena jak distribuce hustoty pravděpodobnosti interních kritických napětí (dále PDF), tak rovněž zjištěn její vývoj během cyklického namáhání. Zjištěné průběhy PDF byly korelovány s vývojem povrchového reliéfu a vnitřního dislokačního uspořádání zdokumentované pro obě teploty pomocí rastrovací elektronové mikroskopie (SEM) vybavené technikou fokusovaného iontového svazku (FIB), která umožnila rovněž efektivní studium nukleace povrchových únavových trhlin. Při cyklickém zatížení při pokojové teplotě byla pozorována lokalizace cyklické plastické deformace do perzistentních skluzových pásů (PSP). V místech, kde tyto PSP vystupují na povrch materiálu byly pozorovány perzistentní skluzové stopy (PSS) tvořené extruzemi a intruzemi. Postupné prohlubování intruzí, zejména na čele nejhlubší intruze, vede k iniciaci únavové trhliny. Odlišný mechanismus tvorby trhlin byl zjištěn při únavové zkoušce při zvýšené teplotě, kde zásadní roli hrál vliv prostředí. Rychlá oxidace hranic zrn a jejich následné popraskání představuje dominantní mechanismus v I. stádiu nukleace trhlin. Aplikace desetiminutové prodlevy v tahové části zátěžného cyklu vedlo k vývoji vnitřního (kavitačního) poškozování. Mechanismy vnitřního poškozování byly studovány na podélných řezech rovnoběžných s napěťovou osou zkušebních vzorků. Trhliny a jejich vztah k hranicím zrn a dvojčat byly studovány pomocí difrakce zpětně odražených elektronů (EBSD). Vliv prodlevy na únavovou životnost byl korelován s vývojem povrchového reliéfu a vnitřního poškození. Vzorky z uvedené oceli byly rovněž podrobeny zkouškám termomechanické únavy (TMF), při nichž se v čase mění jak zátěžná síla tak i teplota. Termomechanické únavové zkoušky v režimu soufázném (in-phase) a protifázném (out-of-phase) byly provedeny jak s prodlevou, tak i bez ní. Ve všech případech bylo pozorováno rychlé cyklické zpevnění bez ohledu na použitou amplitudu deformace, u vzorků testovaných v out-of-phase režimu byla zjištěna tendence k saturaci. Zkoumáním povrchového reliéfu za pomocí technik SEM a FIB byla odhalena přednostní oxidace hranic zrn a následné praskání těchto hranic kolmo k ose zatížení. Prodlevy v cyklech při maximálním napětí vedly ke zvýšení amplitudy plastické deformace a následně ke creepovému poškození ve formě vnitřních kavit a trhlin. Interkrystalické šíření trhlin bylo pozorováno na vzorcích testovaných v režimu in-phase. Vývoj poškození v režimu out-of-phase nebyl principiálně ovlivněn zařazením prodlevy do zátěžného cyklu. Charakteristickým znakem namáhání v režimu out-of-phase je nukleace několika trhlin v homogenní oxidické vrstvě jdoucích napříč zrny kolmo k ose zatěžování.

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47

Kayser, Tobias [Verfasser], Bob [Akademischer Betreuer] Svendsen, and Alexander [Gutachter] Brosius. "Characterization of microstructure in aluminum alloys based on electron backscatter diffraction / Tobias Kayser. Betreuer: Bob Svendsen. Gutachter: Alexander Brosius." Dortmund : Universitätsbibliothek Dortmund, 2011. http://d-nb.info/1103029142/34.

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48

Shea, Lauren. "Microstructural and textural analysis of naturally deformed granulites in the Mount Hay block of central Australia: Implications for the rheology of polyphase lower crustal materials." Thesis, Boston College, 2019. http://hdl.handle.net/2345/bc-ir:108578.

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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

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Cocle, Jennifer. "Development of the EBSD Intensity Response for Quantitative Strain Analyses of Materials." Thesis, McGill University, 2008. http://digitool.Library.McGill.CA:80/R/?func=dbin-jump-full&object_id=93017.

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Abstract:

Electron BackScattered Diffraction (EBSD) systems can be considered as a tool providing three kinds of responses: EBSD patterns (EBSPs) themselves, an indexing response (orientation data), and an intensity response (also called Band Contrast "BC", Image Quality "IQ", or Pattern Quality "PQ or P"). This work focused on the characterization and development of the intensity response. For now, the intensity response cannot be used for quantitative microstructural analyses, including strain analyses of materials. Indeed, this response is affected by several material and experimental conditions. Moreover, properties of the intensity response (strain sensitivity, reproducibility, exact relation with EBSP quality or diffraction band intensities) are not well-known and understood. This project constitutes an exploratory study on the development of the intensity response for quantitative strain analyses of materials. A new modelling and statistical approach is presented and assessed for transforming the raw (current) intensity response (values and grey-tones of intensity images) of commercial EBSD systems into an accurate and reproducible parameter allowing objective visualization and measurements of strain.
Les systèmes de diffraction des électrons rétro-diffusés (EBSD) peuvent être considérés comme un outil offrant trois types de réponses: les patrons EBSD (EBSPs), la réponse d'indexation (données d'orientation) et la réponse d'intensité (aussi appelée Contraste de Bande «BC », Qualité d'Image « IQ », ou Qualité de Patron « PQ ou P »). Le présent projet s'est concentré sur la caractérisation et le développement de la réponse d'intensité. En effet, pour l'instant, la réponse d'intensité ne peut être utilisée pour réaliser des analyses microstructurales quantitatives des matériaux. En effet, cette réponse est influencée par de nombreux facteurs relatifs au matériau analysé et aux conditions expérimentales utilisées. De plus, les propriétés de la réponse d'intensité (sensibilité à la déformation, reproductibilité, relation exacte avec la qualité des EBSPs ou les intensités des bandes de diffraction) ne sont pour l'instant pas bien connues ni même compnses. Le présent projet représente donc une étude exploratoire visant le développement de la réponse d'intensité des systèmes EBSD commerciaux pour l'analyse quantitative de la déformation des matériaux. Dans ce projet, une approche de modélisation statistique est présentée et évaluée afin de transformer la réponse d'intensité actuelle (valeurs et tons de gris des images d'intensité) des systèmes EBSD commerciaux en une réponse précise et reproductible permettant de visualiser et de mesurer objectivement la déformation.

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Di, Gioacchino Fabio. "Characterization of mesoscopic crystal plasticity from high-resolution surface displacement and lattice orientation mappings." Thesis, University of Manchester, 2013. https://www.research.manchester.ac.uk/portal/en/theses/characterization-of-mesoscopic-crystal-plasticity-from-highresolution-surface-displacement-and-lattice-orientation-mappings(77c47c76-e2ee-44ff-bdef-c53e25bb6bc1).html.

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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.

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