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A rapid image segmentation and correlation-based approach to investigating the local microstructural effects on pitting corrosion susceptibility is introduced. The impact of four different microstructural features, consisting of grain orientation, proximity to grain boundaries, proximity to intermetallic particles, and local geometrically necessary dislocation (GND) density, on pitting initiation in the 5083 aluminum alloy was directly investigated using automated pit detection processing in combination with electron microscopy-based characterization. Three different thermomechanical treatments were used to vary the system microstructure and samples were immersed in 3.5 wt% NaCl aqueous solution for 24 h to induce pitting. GND density and proximity to intermetallic particle both showed positive correlations, while grain orientation and proximity to grain boundary showed no correlation with pit initiation sites.

Pure Ti traditionally exhibits the hexagonal closed packed (HCP) crystallographic structure under ambient conditions and the body centered cubic (BCC) structure at elevated temperatures. In addition to these typical structures for Ti alloys, the presence of a face centered cubic (FCC) phase associated with thin films, interfaces, or high levels of plastic deformation has occasionally been reported. Here we show that small FCC precipitates form in freestanding thin foils during in situ transmission electron microscope (TEM) heating and we discuss the potential origins of the FCC phase in light of the in situ observations. This FCC phase was found to be stable upon cooling and under ambient conditions, which allowed us to explore its mechanical properties and stability via nanomechanical in situ TEM testing. It was found that FCC platelets within the HCP matrix phase were stable under mechanical deformation and exhibited similar mechanical deformation behavior as the parent HCP phase.

The mechanical response of modern alloys results from a complex interplay between existing microstructure and its evolution with time under stress. To unravel these processes, in situ approaches intrinsically have a critical advantage to explore the basic mechanisms involving dislocations, grain boundaries (GBs), and their interactions in real time. In this article, we discuss recent findings using in situ nanomechanical testing techniques and refined crystallographic analysis tools. Advancements in in situ nanomechanics not only include multiaxial loading conditions, which bring us closer to real-world applications, but also high strain-rate testing, which is critical to compare experiments and simulations. In particular, unraveling the details of GB-based mechanisms and related microstructural changes will facilitate significant breakthroughs in our understanding of the behavior of materials on macroscopic length scales.

High resolution electron backscatter diffraction (HREBSD), an SEM-based diffraction technique, may be used to measure the lattice distortion of a crystalline material and to infer the geometrically necessary dislocation content. Uncertainty in the image correlation process used to compare diffraction patterns leads to an uneven distribution of measurement noise in terms of the lattice distortion, which results in erroneous identification of dislocation type and density. This work presents a method of reducing noise in HREBSD dislocation measurements by removing the effect of the most problematic components of the measured distortion. The method is then validated by comparing with TEM analysis of dislocation pile-ups near a twin boundary in austenitic stainless steel and with ECCI analysis near a nano-indentation on a tantalum oligocrystal. The HREBSD dislocation microscopy technique is able to resolve individual dislocations visible in TEM and ECCI and correctly identify their Burgers vectors.

Nanocrystalline Al thin films have been strained in situ in a transmission electron microscope using two separate nanomechanical techniques involving a push-to-pull device and a microelectromechanical system (MEMS) device. Deformation-induced grain growth was observed to occur via stress-assisted grain boundary migration with extensive grain growth occurring in the necked region, indicating that the increase in local stress drives the boundary migration. Under applied tensile stresses close to the ultimate tensile strength of 450 MPa for a nanocrystalline Al specimen, measured boundary migration speeds are 0.2 – 0.7 nm s−1 for grains outside necked region and increases to 2.5 nm s−1 for grains within the necked region where the local estimated tensile stresses are elevated to around 630 MPa. By tracking grain boundary motion over time, molecular dynamics simulations showed qualitative agreement in terms of pronounced grain boundary migration with the experimental observations. The combined in situ observation and molecular dynamics simulation results underscore the important role of stress-driven grain growth in plastically deforming nanocrystalline metals, leading to intergranular fracture through predominant grain boundary sliding in regions with large localized deformation.

Nanocrystalline Ni thin films with different as-deposited textures were synthesized by varying the substrate temperature during pulsed-laser deposition. The influence of initial texture variations on the thermal stability and annealing behavior of the thin films was studied via in situ transmission electron microscopy annealing and transmission Kikuchi diffraction analysis. It was found that, as the substrate temperature during deposition was increased, the initial microstructure varied from a random distribution of grains to one almost entirely composed of (001) – oriented grains, with the volume fraction of (001) – oriented grains increasing with increasing substrate temperature. The (001) – oriented grains increased thermal stability and constrained grain growth during annealing, resulting in a bimodal grain size distribution in the annealed films. Despite different surface orientations after annealing, the misorientation distribution functions for the films were similar, suggesting that the boundary state is a primary factor in dictating equilibrium.

In situ straining in the transmission electron microscope and diffraction-contrast electron tomography has been applied to investigate dislocation interactions in α-Ti. Dislocation debris, in the form of small loops, was seen to form from sequential cross-slip events. Electron tomography provided direct three-dimensional visualisation of the dislocation structures, allowing accurate identification of slip planes, dislocation line directions and spatial relations between dislocations.

Domains and domain walls are critical in determining the response of ferroelectrics, and the ability to controllably create, annihilate, or move domains is essential to enable a range of next-generation devices. Whereas electric-field control has been demonstrated for ferroelectric 180° domain walls, similar control of ferroelastic domains has not been achieved. Here, using controlled composition and strain gradients, we demonstrate deterministic control of ferroelastic domains that are rendered highly mobile in a controlled and reversible manner. Through a combination of thin-film growth, transmission-electron-microscopy-based nanobeam diffraction and nanoscale band-excitation switching spectroscopy, we show that strain gradients in compositionally graded PbZr1-xTixO3 heterostructures stabilize needle-like ferroelastic domains that terminate inside the film. These needle-like domains are highly labile in the out-of-plane direction under applied electric fields, producing a locally enhanced piezoresponse. This work demonstrates the efficacy of novel modes of epitaxy in providing new modalities of domain engineering and potential for as-yet-unrealized nanoscale functional devices.

A hexagonal close-packed (HCP) to face-centered cubic (FCC) phase transition has been observed in freestanding alpha-titanium (α-Ti) thin foils under two separate conditions: (1) after focused ion beam (FIB) irradiation, and (2) during in situ heating in a transmission electron microscope (TEM). The FCC phase is not found on the Ti single-component equilibrium phase diagram, however, both FCC structures were found to be stable after formation under these conditions. Here, we combine analytical TEM and Atom Probe Tomography (APT) investigations into the chemical nature of these anomalous FCC Ti-X phases. Both occurrences of the FCC phase were observed in thin films containing (initial) prismatic HCP surface plane texturing and appear to be facilitated by hydrogen and oxygen impurities. Our results suggest that the FIB-induced FCC Ti-X is a form of titanium hydride (δ-TiH2 and/or γ-TiH), while the thermally-induced FCC Ti-X appears to be tied to the incorporation of oxygen.

Automated image recognition and analysis techniques were combined with liquid cell transmission electron microscopy to explore the oxidation kinetics of nanocrystalline Fe thin films in a water vapor environment. From in situ microscopy experiments, localized oxidation was observed to initiate in the film then propagate in an unsteady fashion, alternatingly arresting and progressing. The oxidation front propagation occurred via new oxidation sites initiating 10s of nm ahead of the existing front rather than through a continuous expansion mechanism. The oxidation rate was seen to be highly dependent on electron dose rate, with increasing electron dose rate accelerating the oxidation front propagation and increasing the density of oxidation initiation sites. The in situ experiments were also performed in diffraction space where it was seen that Fe2O3 was formed during oxidation. Coupling in situ microscopy with automated image analysis creates new opportunities for studying the early stages of localized corrosion by providing direct observation of oxidation propagation as well as quantification of the oxidation rates and rapid identification of byproducts.

Multiscale characterization was performed on an Al–Mg alloy, Al 5754 O-temper, including in situ mechanical deformation in both the scanning electron microscope and the transmission electron microscope. Scanning electron microscopy characterization showed corresponding inhomogeneity in the dislocation and Mg distribution, with higher levels of Mg correlating with elevated levels of dislocation density. At the nanoscale, in situ transmission electron microscopy straining experiments showed that dislocation propagation through the Al matrix is characterized by frequent interactions with obstacles smaller than the imaging resolution that resulted in the formation of dislocation debris in the form of dislocation loops. Post-mortem chemical characterization and comparison to dislocation loop behaviour in an Al–Cr alloy suggests that these obstacles are small Mg clusters. Previous theoretical work and indirect experimental evidence have suggested that these Mg nanoclusters are important factors contributing to ...

Progress toward combining time-resolved experiments with periodic three-dimensional analysis of the evolved microstructural state has been made recently. In situ electron microscopy is used to observe in real time the development of irradiation defects and the influence of these defects on dislocation behavior. Three-dimensional characterization provides information on the true spatial distribution of defects and clarifies effects of the free surfaces in thin films. This quasi-four dimensional analysis approach has been applied to understand the formation of channels in irradiated alloys, the depth distribution of ion damage in an electron transparent foil, and the dislocation channel interactions with grain boundaries. The new insight obtained from these experiments is highlighted and contrasted with findings from simulations.

We develop new efficient online algorithms for detecting transient sparse signals in TEM video sequences, by adopting the recently developed framework for sequential detection jointly with online convex optimization [1]. We cast the problem as detecting an unknown sparse mean shift of Gaussian observations, and develop adaptive CUSUM and adaptive SSRS procedures, which are based on likelihood ratio statistics with post-change mean vector being online maximum likelihood estimators with $\ell_{1}$ . We demonstrate the meritorious performance of our algorithms for TEM imaging using real data.

The mechanical behavior of pure rhenium was investigated using uniaxial compression tests, transmission electron microscopy and electron backscatter diffraction characterization. The plasticity was characterized by a large amount of twin formation and propagation, including twin transmission across grain boundaries. In-depth analysis of the interactions of { 1 1 2 ¯ 1 } 〈 1 ¯ 1 ¯ 2 6 〉 twins with grain boundaries found that grain boundaries with misorientation angles below ∼25° allowed twin transmission, while grain boundaries with higher angles did not. Similar to dislocation interactions with grain boundaries, twin transmission was largely dictated by the minimization of the angle between the shear vectors of the incoming and outgoing twins.

Characterizing plasticity mechanisms below the ductile-to-brittle transition temperature is traditionally difficult to accomplish in a systematic fashion. Here, we use a new experimental setup to perform in situ cryogenic mechanical testing of pure Sn micropillars at room temperature and at −142 °C. Subsequent electron microscopy characterization of the micropillars shows a clear difference in the deformation mechanisms at room temperature and at cryogenic temperatures. At room temperature, the Sn micropillars deformed through dislocation plasticity, while at −142 °C they exhibited both higher strength and deformation twinning. Two different orientations were tested, a symmetric (1 0 0) orientation and a non-symmetric (4 5 ¯ 1) orientation. The deformation mechanisms were found to be the same for both orientations.

Recent progress in understanding dislocation interactions with grain boundaries and interfaces in metallic systems via static and in situ dynamic experimental approaches is reviewed.

The interaction of lattice dislocations with grain boundaries in proton- and ion-irradiated austenitic stainless steels is investigated. At the macroscale, interactions of dislocation channels with grain boundaries result in slip blockage, slip transmission and slip along the grain boundary with an associated in-plane displacement. At the dislocation level, slip transmission prediction is governed by the strain energy density minimization. However, the importance of the local resolved shear stress increases, in the sense that it must be of sufficient magnitude to propagate the dislocations through the damaged matrix. If this condition is not satisfied, the grain boundary will activate an alternative mechanism to relieve the strain accumulated from accommodation of lattice dislocations and the stress concentration associated with the formation of a dislocation pile-up. One observed relief mechanism involves the nucleation and propagation of a crack along the grain boundary, which is accompanied by an out-of-plane displacement of the boundary.

In situ straining in the transmission electron microscope and diffraction-contrast electron tomography have been applied to the investigation of dislocation/grain boundary and dislocation/twin boundary interactions in α-Ti. It was found that, similar to FCC materials, the transfer of dislocations across grain boundaries is governed primarily by the minimization of the magnitude of the Burgers vector of the residual grain boundary dislocation. That is, grain boundary strain energy density minimization determines the selection of the emitted slip system.

Recent developments in the application of electron tomography for characterizing microstructures in crystalline solids are described. The underlying principles for electron tomography are presented in the context of typical challenges in adapting the technique to crystalline systems and in using diffraction contrast imaging conditions. Methods for overcoming the limitations associated with the angular range, the number of acquired images, and uniformity of image contrast are introduced. In addition, a method for incorporating the real space coordinate system into the tomogram is presented. As the approach emphasizes development of experimental solutions to the challenges, the solutions developed and implemented are presented in the form of examples.

The dislocation microstructure beneath surface slip traces produced by fatigue loading of Haynes 230 was revealed to be a function of distance from a crack tip. The microstructure beneath these traces evolves from planar slip bands with increasing dislocation density and decreasing interband spacing as the crack tip approaches one of refined subgrains and lamellar bands at and in the vicinity of the crack tip. Similarly, beneath fatigue striations the microstructure evolves from nanosized subgrains to a banded structure with increasing distance from the fracture surface. These structures are significantly different to those predicted to develop under fatigue loading of a planar slip material. The evolved structures are considered in terms of the microstructure generated by severe plastic deformation.

The effects of NiO multilayer additions to pulsed-laser deposited nanocrystalline Ni on the grain growth and texture evolution during annealing have been studied using a combination of in situ annealing in the transmission electron microscope and the recently developed transmission electron backscatter diffraction technique. Grain growth in pure Ni proceeds in an abnormal manner with a small number of grains growing rapidly at the expense of the surrounding nanocrystalline matrix. The addition of NiO layers in the Ni suppressed grain growth and twin formation upon annealing, with increasing oxide content resulting in decreasing extent of grain growth. In pure Ni, the post-annealing texture was found to be composed of a strong {001} texture coupled with the four {122} twin variants from the {001}. With the addition of NiO, annealing twinning, and hence the {122} orientation, was suppressed and instead the final texture was composed of the {001} and {111} orientations.

Nanostructured metal thin films have been shown to have unique thermal, mechanical, and electrical properties when the internal structure can be maintained. However, this far-from-equilibrium structure has been shown in many cases to be unstable at elevated temperatures. This work investigates the role of surface ledges, large nickel inclusions, electron beam exposure and film thickness on the evolution of high purity, pulsed-laser deposited, free-standing, nickel films via in situ transmission electron microscopy annealing. Grain growth appeared enhanced in a limited temperature range near surface ledges present in the film, but was not affected by large nickel inclusions. In addition, extended exposure to the electron beam resulted in abnormal grain growth. This was hypothesized to be a result of enhanced nickel oxide growth on the surfaces. Finally, increasing film thickness was observed to accelerate the onset of abnormal grain growth and increased the size and number of larger grains. These observations should provide warning that the initial and dynamic surface present in thin films should be taken under consideration during any annealing study, as it may significantly impact the final crystalline structure.

The effects of heavy-ion irradiation on dislocation processes in stainless steels were investigated using in situ irradiation and deformation in the transmission electron microscope as well as post mortem electron tomography to retrieve information on the three-dimensional dislocation state. Irradiation-induced defects were found to pose a strong collective barrier to dislocation motion, leading to dislocation pileups forming in grain interiors and at grain boundaries. The passage of multiple dislocations along the same slip plane removes the irradiation defects and leads to the eventual formation of a defect-free channel. These channels are composed of densely tangled dislocation networks which line the channel-matrix walls as well as residual dislocation debris in the channel interiors. The structures of the dislocation tangles were found to be similar to those encountered in later stages of deformation in unirradiated materials, with the exception that they developed earlier in the deformation process and were confined to the defect free channels. Also, defect free channels were found to widen through both source widening as well as complex cross-slip mechanisms.

A combination of electron tomography, electron backscatter diffraction and traditional |g.b| analysis is used to characterize a dislocation transmission event across a Σ3 grain boundary in 304 stainless steel. The parallel {1 1 1} planes across a Σ3 boundary allow simultaneous imaging of dislocations in both grains. The interaction is explained in terms of residual strain energy density in the grain boundary due to the accommodation and emission of dislocations and the magnitude of the local shear stress.

Grain boundary migration associated with abnormal grain growth in pulsed-laser deposited Ni was studied in real time by annealing electron transparent films in situ in the transmission electron microscope. The resulting texture evolution and grain boundary types produced were evaluated by ex situ electron backscatter diffraction of interrupted anneals. The combination of these two techniques allowed for the investigation of grain growth rates, grain morphologies, and the evolution of the orientation and grain boundary distributions. Grain boundaries were found to progress in a sporadic, start/stop fashion with no evidence of a characteristic grain growth rate. The orientations of the abnormally growing grains were found to be predominately 〈1 1 1〉//ND throughout the annealing process. A high fraction of twin boundaries developed during the annealing process. The intermittent growth from different locations of the grain boundary is discussed in terms of a vacancy diffusion model for grain growth.

Electron Backscatter Diffraction (EBSD) based Orientation Imaging Microscopy (OIM) is used routinely at ~500 materials laboratories worldwide for the characterization and development of diverse crystalline materials. Statistically significant data sets (~107 individual EBSD measurements) can be collected and analyzed within time periods of acceptable beam stability (~105s). However, limitations in angular and spatial resolution have motivated a continued search for more robust EBSD-based methods. Herein is a gathered presentation of advanced techniques in use, intended as a guide to researchers in selecting the most appropriate method for their work. Wilkinson’s method has been shown to increase angular resolution nearly two orders of magnitude to ±0.006°, facilitating measurement of elastic strain, lattice curvature, and dislocation density. A simulated pattern adaptation of Wilkinson’s method extends these measurement capabilities to polycrystalline materials, by avoiding the need for an experimental strain free reference pattern. The angular resolution limit obtained is ~0.04°. Accurate pattern center calibration, essential to the high resolution methods, is accomplished by parallelization of band edges projected onto a sphere centered at the interaction volume. FFT powered cross-correlation functions improve the spatial resolution near grain boundaries and correct for measurement inaccuracies induced by overlapping patterns. To corroborate these claims, exemplary results taken from a wedge-indented nickel single crystal, cold-worked copper polycrystal, and rolled nickel polycrystal are shown.

This work explores the deposition of Pt monolayers on 3D graphene and 2D MoS2 as catalyst architectures for electrocatalysis. Ni foam was utilized as a starting substrate for the 3D graphene growth before Pt was deposited layer-by-layer in a surface-limited electrochemical scheme to achieve highly wetted and atomically thin growth. A similar surface-limited technique was utilized for the deposition of Pt on both vertically and horizontally aligned MoS2. High resolution TEM, XPS, SEM/EDX, and electroanalytical techniques were used to characterize these samples and reveal the evolution of the atomic/electronic structure as a function of the number of Pt monolayers. Specifically, the ORR and the HER reactions were used to characterize the catalytic activities of the graphene- and the MoS2-templated catalysts, respectively. It is demonstrated that the synthesis scheme outlined here allows for the design of dimensionally-controlled and ligand-flexible catalyst architectures that can have a wide range of chemical applications.

This work explores the novel concept of electrochemically deposited wetted monolayer to few multilayers of Pt on a graphenated 3D Ni foam (Pt-ML/GR/Ni). Commercially available, highly porous, Ni foam capped with graphene was utilized as a substrate for layer-by-layer Pt growth by surface-limited electrochemical deposition. A survey of literature reveals that our resulting Pt-ML/GR/Ni architecture is the first instance of 3D rendered graphene being used as a template for 2D Pt growth via room-temperature synthesis. XPS, CV, SEM/EDS and high-resolution TEM characterization reveals that graphene covers much of the Ni foam and that the Pt grows epitaxially on the graphene. This scheme allows us to approach theoretical limits of Pt utilization for electrocatalytic applications, such as the canonical oxygen reduction reaction (ORR). Analysis of the ORR overpotential in Pt-ML/GR/Ni in comparison to that of the Ni-free Pt-ML/GR shows that the Dirac cone of the Pt/GR is intact, making the graphene essentially ‘electron transparent’ to the Ni-to-Pt charge transfer. Such Pt-ML/GR architectures can thus allow the surface Pt atoms to be electronically tuned by an underlying ligand of choice. This synthesis approach may prove extremely valuable for high-utilization, low-loading, electronically tunable catalysts. We present here a thorough investigation of the atomic/electronic structure and of the related evolution of electrocatalytic properties as a function of the number of graphene-templated 2D Pt layers.

Detailed defect structure of dendrite formation was studied in order to connect the mesoscopic with the atomistic structure. It was demonstrated that twinning and stacking fault formation play a central role in the growth of electrodeposited Ag dendrites. The broad faces of Ag dendrites and the main trunk growth direction were found to be ((1) over bar 11) and [(1) over bar1 (2) over bar], respectively. Dendrite branches also formed and grew from the main trunk parallel to the [12 (1) over bar] and [(211) over bar] crystallographic directions. Twins and stacking faults were found to reside on the {111} crystallographic planes, as expected for a face centered cubic (FCC) Ag crystal. Using electron back scattered diffraction (EBSD) we found two variants of in-plane 60 degrees rotational twin domains in the ((1) over bar 11) broad dendrite surface plane. The intersections of twins and stacking faults with dendrite arm surfaces are perpendicular to the (112) arm growth directions. However, occasionally twins on the {111} planes parallel to the (112) arm growth directions were also observed. Although defect assisted dendrite growth is facilitated by twinning and stacking fault formation on {111} planes, the growth directions of the trunk and branches are not of the (111) type, but rather close to (112). The (112) growth directions are maintained by breaking dendrite facets into thermodynamically stable 111 and 200 steps and structural ledges of different length.

Correlating the mechanical behavior of metals with the underlying defect mechanisms remains an outstanding challenge for the development of new material systems. In situ Transmission Electron Microscopy (TEM) nanomechanical testing provides an experimental technique whereby the behavior of defects such as dislocations and twins can be observed in real time while quantitatively correlating their behavior with an applied stress. This paper highlights recent experiments utilizing in situ TEM testing to investigate the behavior of twins and dislocations in FCC, BCC, and HCP materials. Examples of recently developed experimental approaches and future directions of in situ TEM nanomechanical testing are presented.

Density-functional-theory calculations of twin-boundary energies in hexagonal close packed metals reveal anomalously low values for elemental Tc and Re, which can be lowered further by alloying with solutes that reduce the electron per atom ratio. The anomalous behavior is linked to atomic geometries in the interface similar to those observed in bulk tetrahedrally close packed phases. The results establish a link between twin-boundary energetics and the theory of bulk structural stability in transition metals that may prove useful in controlling mechanical behavior in alloy design.

A reply to Maurice et al.'s comment on "Bragg's Law Diffraction Simulations for Electron Backscatter Diffraction" is presented. A new method for microscope geometry calibration is briefly presented. Also, evidence that simple diffraction simulations can be profitable tools for absolute elastic strain measurements in crystalline materials is reiterated.

Decorating 1D nanostructures (e.g., wires and tubes) with metal nanoparticles serves as a hierarchical approach to integrate the functionalities of metal oxides, semiconductors, and metals. This paper examines a simple and low-temperature approach to self-assembling gold nanoparticles (Au-np)—a common catalytic material—onto silicon nanowires (SiNWs). A conformal ultra-thin film (i.e.

The mobility of defects such as dislocations controls the mechanical properties of metals. This mobility is determined both by the characteristics of the defect and the material, as well as the local stress and strain applied to the defect. Therefore, the knowledge of the stress and strain during deformation at the scale of defects is important for understanding fundamental deformation mechanisms. Here, we demonstrate a method of measuring local stresses and strains during continuous in situ deformation with a resolution of a few nanometers using nanodiffraction strain mapping. Our results demonstrate how large multidimensional data sets captured with high speed electron detectors can be analyzed in multiple ways after an in situ TEM experiment, opening the door for true multimodal analysis from a single electron scattering experiment.

Transmission electron microscopes play a critical role in building our knowledge base of the atomic structure and composition as well as the electronic and magnetic state of materials. This information is a two-dimensional snapshot of the material state and requires a posteriori analysis to reveal the reaction or processing pathway, or to correlate with a macroscopic property. However, using electron tomography it is feasible to recover the information lost in the electron beam direction and obtain a three-dimensional view of the internal structure in an electron transparent foil. In this paper, example applications of diffraction-contrast electron tomography to understand various dislocation-obstacle interactions are presented and discussed.

The pattern center of an electron backscatter diffraction (EBSD) image indicates the relative position of the image with reference to the interaction volume of the sample. As interest grows in high-resolution EBSD techniques, accurate knowledge of this position is essential for precise interpretation of the EBSD features. In a typical EBSD framework, Kikuchi bands are recorded on a phosphor screen. If the flat phosphor were instead shaped as a sphere, with its center at the specimen's electron interaction volume, then the incident backscattered electrons would form Kikuchi bands on that sphere with parallel band edges centered on great circles. In this article, the authors present a method of pattern center (PC) refinement that maps bands from the planar phosphor onto a virtual spherical screen and measures the deviation of bands from a great circle and from possessing parallel edges. Potential sources of noise and error, as well as methods for reducing these, are discussed. Finally, results are presented on the application of the PC algorithm to two types of simulated EBSD patterns and two experimental setups, and the resolution of the method is discussed.

The effects of ion irradiation damage on dislocation generation and propagation in austenitic stainless steels were studied by means of in situ transmission electron microscopy and electron tomography. Tensile samples were irradiated in situ to a dose on the order of 1017 ions/m2 with 1MeV Kr+ and strained at 300 K as well as 673 K. Dislocation motion through the irradiation-obstacle field was jerky and discontinuous, dislocation pile-ups formed in grain interiors and at boundaries, long straight dislocations were generated decorating the channel-matrix walls, and dislocation cross-slip within the channel created debris along the channel leading to channel widening. Electron tomography was applied for the first time to reveal new detail about the dislocation reactions in the channel wall.

In 2006, Angus Wilkinson introduced a cross-correlation-based electron backscatter diffraction (EBSD) texture analysis system capable of measuring lattice rotations and elastic strains to high resolution. A variation of the cross-correlation method is introduced using Bragg's Law-based simulated EBSD patterns as strain free reference patterns that facilitates the use of the cross-correlation method with polycrystalline materials. The lattice state is found by comparing simulated patterns to collected patterns at a number of regions on the pattern using the cross-correlation function and calculating the deformation from the measured shifts of each region. A new pattern can be simulated at the deformed state, and the process can be iterated a number of times to converge on the absolute lattice state. By analyzing an iteratively rotated single crystal silicon sample and recovering the rotation, this method is shown to have an angular resolution of approximately 0.04 degrees and an elastic strain resolution of approximately 7e-4. As an example of applications, elastic strain and curvature measurements are used to estimate the dislocation density in a single grain of a compressed polycrystalline Mg-based AZ91 alloy.

It has become apparent through experimentation at the micro- and nanolevels that the crystalline defects known as dislocations have significant effects on a material’s properties. Accordingly, a complete material state description must include the characterization of the dislocated state. However, this characterization presents a twofold problem: resolution and representation. In general, high-resolution microscopy techniques are only useful for considering a few dislocations at a time, but automated high-speed methods are only capable of resolving dislocation densities well above the average density in a typical annealed metal. The second challenge is developing a method of representation for the dislocated state. Unlike most state quantities, dislocation lengths are not conserved and complete representation would require tracking of position, momentum, and interactions, as well as the creation and annihilation of dislocations. Such a scheme becomes unwieldy when considering the large numbers of dislocations involved in common crystal plasticity. In 1970, Kröner (“Initial Studies of a Plasticity Theory Based Upon Statistical Mechanics,” Inelastic Behaviors of Solids (Materials Sciences and Engineering), M. F. Kanninen et al., eds., McGraw-Hill, New York, pp. 137–147), a pioneer in the continuum representation of dislocations, proposed a statistical method using n-point correlations to classify the dislocated state in a compact form. In addition to providing a convenient form, the correlations naturally identify dipoles, multipoles, and other higher order structures, such as cells, networks, and braids. As formulated, Kröner’s method would require high-resolution microscopy techniques, which limits its utility for experimental measurements. The current work presents a modification to Kröner’s method that would allow it to be used within the currently available resolution limits of bulk microscopy. Furthermore, in this work, newly developed microscopy techniques are employed to refine those resolution limits to more significant levels. The high-resolution bulk dislocation characterization is applied to a well-annealed nickel specimen and the results including visualizations of mesoscale structures are presented.

Extended abstract of a paper presented at Microscopy and Microanalysis 2011 in Nashville, Tennessee, USA, August 7–August 11, 2011.