The Tso Morari Crystalline complex (TMCC) of eastern Ladakh, India, is part of the north Indian continental margin and is characterized by eclogitic enclaves embedded within ortho- and paragneisses known as the Puga Gneiss. Two fault zones bound the TMCC: the Karzok fault to the southwest and the Zildat fault to the northeast. In the present study, we carried out Electron Backscatter Diffraction study of quartz of 10 samples collected from the Puga Gneiss. The relict and recrystallized quartz grains were treated separately to understand the deformation conditions of the Puga Gneiss during early and late deformation stages related to UHP metamorphism and final stage of exhumation during retrogression, respectively. Microstructural observations suggest dynamic recrystallization in quartz and plagioclase at different temperature ranges. Misorientation analysis of both relict and recrystallized quartz grains reveals presence of Dauphiné Twins. Lattice preferred Orientation (LPO) of <c> axis of relict quartz grains generally shows more than one point maxima indicating that the relict grains preserve LPO developed during different stages of metamorphism/deformation. On the other hand, LPO of <c> axis of recrystallized grains from Karzok and Zildat fault zones shows asymmetric single girdle either normal or at an angle to the foliation plane, which suggests simple shear. We conclude that grain size reduction and recrystallization of the Puga Gneiss was greatly influenced by Dauphiné Twin and the final exhumation of the TMCC took place in a simple shear environment aided by activity along its two binding fault zones.

The microstructure and texture evolution of Ni-5 at%W (Ni5W) alloy substrates were investigated by in situ tensile testing along the rolling direction (RD), transverse direction (TD), and at 45° to the RD (45°-RD), as well as by electron backscatter diffraction characterization. The tensile stress direction had a significant influence on the texture evolution. The cubic texture in the Ni-5 at%W alloy exhibited severe degradation when the tensile angle was 45°-RD. In contrast, the cubic texture was relatively stable under high deformation along the RD or TD. It was found that the slip line system in the 45°-RD specimen was the key to the contrasting behavior. The effect of the tensile testing angle on the cubic texture evolution for Ni–W substrates was investigated, and the corresponding effect on the superconducting properties of coated materials was studied.

During recrystallization, the growth of fresh grains initiated within a deformed microstructure causes dramatic changes in the dislocation structure and density of a heavily deformed matrix. In this paper, the microstructure of a cold rolled and partially recrystallized Al-Mg alloy (AA5052) was studied via electron backscattered diffraction (EBSD) analysis. The structure and density of the geometrically necessary dislocations (GNDs) were predicted using a combination of continuum mechanics and dislocation theory. Accordingly, the Nye dislocation tensor, which determines the GND structure, was estimated by calculation of the lattice curvature. To do so, five components of the Nye dislocation tensor were directly calculated from the local orientation of surface points of the specimen, which was determined by two-dimensional EBSD. The remaining components of GNDs were determined by minimizing a normalized Hamiltonian equation based on dislocation energy. The results show the elimination of low angle boundaries, lattice curvature, and GNDs in recrystallized regions and the formation of low angle boundaries with orientation discontinuities in deformed grains, which may be due to static recovery.

We propose a new methodology for ranking the reflectors used in traditional Hough-based indexing of electron backscatter diffraction (EBSD) patterns. Instead of kinematic X-ray or electron structure factors (Fhkl) currently utilized, we propose the integrated Kikuchi band intensity parameter (βhkl) based on integrated dynamical electron backscatter intensities. The proposed parameter is compared with the traditional kinematical intensity, $I_{hkl}^{{\rm kin}} $, as well as the average Hough transform peak intensity, $I_{hkl}^{{\rm HSP}} $ and used to index EBSD patterns for a number of different material systems of varying unit cell complexities including nickel, silicon, rutile, and forsterite. For elemental structures, βhkl closely follows the kinematical ranking. However, significant ranking differences arise for more complex unit cells, with the βhkl parameter showing a better correlation with the integrated Hough intensities. Finally, Hough-based indexing of a simulated forsterite data set showed an appreciable improvement in the median confidence index (0.15 to 0.35) when βhkl is used instead of $I_{hkl}^{{\rm kin}} $ for ranking the reflectors.

Agates with spectacular micro-structural features were found in volcanic rocks at several occurrences in the Saar-Nahe region (Germany). These agates include spirals of several tens up to several hundreds of μm in size within zones lacking the characteristic structural agate banding. A combined mineralogical study by polarising microscopy, scanning electron microscopy, cathodoluminescence microscopy and spectroscopy, and electron backscatter diffraction provided evidence that the spirals consist of well-ordered trigonal α-quartz, whereas the surrounding matrix is composed of strongly disordered or amorphous SiO2 phases. The quartz micro-crystals show a systematic rotation of the crystal orientation perpendicular to the direction of the spiral loops indicating helical growth.

It is assumed that the spiral growth is initiated by dislocations with a screw component. The lacking symmetry of the strongly disordered or amorphous matrix initiated a curved development by a screw dislocation in a system far from equilibrium. The atoms/molecules are packed into spiral layers, which is energetically favoured in comparison with the incorporation into plane crystal faces. Such self-organisation growth and polymerisation initiated by a screw dislocation can produce variable spiral morphologies sometimes resembling living forms.

We present a deep learning approach to the indexing of electron backscatter diffraction (EBSD) patterns. We design and implement a deep convolutional neural network architecture to predict crystal orientation from the EBSD patterns. We design a differentiable approximation to the disorientation function between the predicted crystal orientation and the ground truth; the deep learning model optimizes for the mean disorientation error between the predicted crystal orientation and the ground truth using stochastic gradient descent. The deep learning model is trained using 374,852 EBSD patterns of polycrystalline nickel from simulation and evaluated using 1,000 experimental EBSD patterns of polycrystalline nickel. The deep learning model results in a mean disorientation error of 0.548° compared to 0.652° using dictionary based indexing.

The hydrogen embrittlement of 12Cr2Mo1R(H) steel at different strain rates were investigated after hydrogen precharging for 4 h in a 0.5 M H2SO4 solution with 2 g/L ammonium thiocyanate. Results showed that the embrittlement index increased and gradually reached a relative stable value of about 20% at the strain rate of 5 × 10−5 s−1 with the decrease of strain rates. SEM images depicted small and deep flakes at high strain rates, while flakes grew larger at slow strain rates. Most hydrogen-induced cracks (HICs) were transgranular fracture through lath grain of bainitic ferrite. High strain field surrounds the crack tips, which makes the crack tips of two close and parallel cracks deflect toward each another and even form crack coalescence. The electron backscatter diffraction technique was used to investigate the effects of grain boundaries, recrystallization fraction, kernel average misorientation map, texture component, and coincidence site lattice boundaries on the HIC propagation. High densities of dislocations and strain concentrations were found around the cracks, where grains are highly sensitive to HIC.

Electron and proton microprobes, along with electron backscatter diffraction (EBSD) analysis were used to study the microstructure of the contemporary Al–Cu–Li alloy AA2099-T8. In electron probe microanalysis, wavelength and energy dispersive X-ray spectrometry were used in parallel with soft X-ray emission spectroscopy (SXES) to characterize the microstructure of AA2099-T8. The electron microprobe was able to identify five unique compositions for constituent intermetallic (IM) particles containing combinations of Al, Cu, Fe, Mn, and Zn. A sixth IM type was found to be rich in Ti and B (suggesting TiB2), and a seventh IM type contained Si. EBSD patterns for the five constituent IM particles containing Al, Cu, Fe, Mn, and Zn indicated that they were isomorphous with four phases in the 2xxx series aluminium alloys including Al6(Fe, Mn), Al13(Fe, Mn)4 (two slightly different compositions), Al37Cu2Fe12 and Al7Cu2Fe. SXES revealed that Li was present in some constituent IM particles. Al SXES mapping revealed an Al-enriched (i.e., Cu, Li-depleted) zone in the grain boundary network. From the EBSD analysis, the kernel average misorientation map showed higher levels of localized misorientation in this region, suggesting greater deformation or stored energy. Proton-induced X-ray emission revealed banding of the TiB2 IM particles and Cu inter-band enrichment.

In this study, we report the characterization of a 304L stainless steel cylindrical projectile produced by additive manufacturing. The projectile was compressively deformed using a Taylor Anvil Gas Gun, leading to a huge strain gradient along the axis of the deformed cylinder. Spatially resolved neutron diffraction measurements on the HIgh Pressure Preferred Orientation time-of-flight diffractometer (HIPPO) and Spectrometer for Materials Research at Temperature and Stress diffractometer (SMARTS) beamlines at the Los Alamos Neutron Science CEnter (LANSCE) with Rietveld and single-peak analysis were used to quantitatively evaluate the volume fractions of the α, γ, and ε phases as well as residual strain and texture. The texture of the γ phase is consistent with uniaxial compression, while the α texture can be explained by the Kurdjumov–Sachs relationship from the γ texture after deformation. This indicates that the material first deformed in the γ phase and subsequently transformed at larger strains. The ε phase was only found in volumes close to the undeformed material with a texture connected to the γ texture by the Shoji–Nishiyama orientation relationship. This allows us to conclude that the ε phase occurs as an intermediate phase at lower strain, and is superseded by the α phase when strain increases further. We found a proportionality between the root-mean-squared microstrain of the γ phase, dominated by the dislocation density, with the α volume fraction, consistent with strain-induced martensite α formation. Knowledge of the sample volume with the ε phase from the neutron diffraction analysis allowed us to identify the ε phase by electron back scatter diffraction analysis, complementing the neutron diffraction analysis with characterization on the grain level.

A detailed microstructural evaluation was executed on the crystallographic texture as well as the mechanisms for nucleation, phase transformation, and grain growth in a Al0.7CoCrFeNi high-entropy alloy. The microstructure and crystallographic orientations were characterized by electron backscatter diffraction, and the chemical composition variations by energy-dispersive X-ray spectroscopy. The cast Al0.7CoCrFeNi alloy started in the BCC phase and partially transformed into the FCC phase. It was found that the Pitsch orientation relationship (OR) dominates the nucleation mechanism of the FCC phase; however, deviations with respect to the Pitsch OR are observed and are attributed to the differently sized atoms forming an ordered B2 phase in the alloy causing lattice distortions. The dual phase BCC–FCC microstructure contains FCC Widmanstätten plates oriented parallel to the {110}BCC planes of the parent grain. It was found that the crystal orientation distribution after the BCC–FCC phase transformation is confined and is explained as a product of the governing mechanisms.

In this work, examination of joint properties of ferritic and dual-phase stainless steel dissimilar welds was carried out by using E2209 duplex and E309LMo austenitic electrodes. The results of E2209 weld showed dual-phase microstructure of ferrite and austenite in the form of grain boundary austenite, Widmanstatten and intragranular austenite, whereas E309LMo weld showed acicular ferrite in the cores of subgrain of austenite. Electron backscatter diffraction was used to study the evolution of the microstructure and micro-texture. The significant variations in the feature of weldments illustrated the presence of a very strong texture. Ferritoscope measurement revealed higher ferrite content in the E2209 weld. Tensile strength, hardness, and absorbed energy of weld metal were dominated by E2209 weld. The modified Strauss test indicated intergranular corrosion attack in the AISI 430 ferritic side heat affected zone. Higher pitting resistance showed by E2209 weld than E309LMo weld. While higher galvanic corrosion observed in the E309LMo weld and AISI 430 ferritic base metal couple.

In this study, we used thermo–mechanical control process (TMCP) technique to investigate the effect of arisen dislocation density and texture components on hydrogen induced cracking susceptibility in as-received API X60 pipeline steel. Dislocations and texture components appeared during cold rolling and annealing treatments. X-ray diffraction and electron backscatter diffraction measurements were used to study these phenomena. We observed that the cold rolling and annealing treatments produced higher dislocation density in deformed and recovered regions. The increase of dislocation density also caused the increased hydrogen trap density. Macro-texture studies by x-ray method indicates that initial weak texture of as-received X60 steel was changed from ζ-fiber to γ-fiber and θ-fiber in 90% cold rolled and annealed specimen. Therefore, the number of grains with 〈100〉||ND orientation which had a harmful effect on hydrogen induced cracking susceptibility increased. The {100} dominant texture and high density of hydrogen traps mitigated against any possible benefits of the other microstructural parameters such as coincidence site lattice boundaries and grain size. As a result, we could not consider this process as a suitable method to increase hydrogen induced cracking resistance in pipeline steel.

Phase identification of multi-phase materials provides essential information relating the material to its mechanical properties. In this study we selected DP980, a type of dual-phase steel, to investigate the content of martensite and ferrite grains. A combination of advanced techniques was used to provide detailed and precise information of the microstructure. Scanning and transmission electron microscopy were used to provide observations of the sample surface at different scales. Martensite and ferrite phases of DP980 were further identified and characterized using electron backscatter diffraction and scanning probe microscopy. Results obtained with nanoindentation tests confirmed that the differences in nanohardness values in single-phase grains are martensite and ferrite with different surface heights shown by scanning probe microscopy. The similarity shown in the image quality map and scanning probe microscopy proves that a large fraction of martensite can be distinguished in this undeformed material using image quality parameters obtained during electron backscatter diffraction imaging.

In this study, the mechanism of ferrite grain refinement during warm compression deformation in the (γ + α) region of Cu–P–Cr–Ni–Mo weathering steel was analyzed by optical microscopy and electron backscatter diffraction. Results showed that fine equiaxed ferrite grains surrounded by high-angle boundaries (HABs) formed along the initial boundaries as the strain is increased. As the deformation temperature decreased, some low-angle boundaries shifted to HABs in intragranular ferrite, and ferrite grain refinement was promoted by continuous dynamic recrystallization. Microstructural observations also indicated that the fine ferrite grains of approximately 1.4–3 μm in size can be obtained by deformation at 750 °C with a strain over 0.69 because of ferrite dynamic recrystallization. Moreover, both strain and deformation temperature influenced the ferrite grain size and volume fraction. Thus, the predominant mechanism for ferrite grain refinement in the (γ + α) region was continuous dynamic recrystallization.

Electron backscatter diffraction (EBSD) is a micro-analytical technique typically attached to a scanning electron microscope (SEM). The vast majority of EBSD measurements is applied to planar and polished surfaces of polycrystalline bulk specimen. In this paper, we present examples of using EBSD and energy-dispersive X-ray spectroscopy (EDX) to analyze specimens that are not flat, not planar, or not bulk – but pillars, needles, and rods. The benefits of low vacuum SEM operation to reduced drift problems are displayed. It is further demonstrated that small and thin specimens enhance the attainable spatial resolution for orientation mapping (by EBSD or transmission Kikuchi diffraction) as well as for element mapping (by EDX).

Samples of Zn-21Al-2Cu alloy (Zinalco) that will be heavily deformed were prepared using five different manual mechanical metallographic methods. Samples were analyzed before tensile testing using the orientation imaging microscopy-electron backscatter diffraction (OIM-EBSD) technique. The effect of type and particle size during the final polishing stages for this material were studied in order to identify a method that produces a flat, damage free surface with a roughness of about 50 nm and clean from oxide layers, thereby producing diffraction patterns with high image quality (IQ) and adequate confidence indexes (CI). Our results show that final polishing with alumina and silica, as was previously suggested by other research groups for alloys that are difficult to prepare or alloys with low melting point, are not suitable for manual metallographic preparation of this alloy. Indexes of IQ and CI can be used to evaluate methods of metallographic preparation of samples studied using the OIM-EBSD technique.

Electron backscatter diffraction (EBSD) has become a common technique for measuring crystallographic orientations at spatial resolutions on the order of tens of nanometers and at angular resolutions <0.1°. In a recent search of EBSD papers using Google Scholar™, 60% were found to address some aspect of deformation. Generally, deformation manifests itself in EBSD measurements by small local misorientations. An increase in the local misorientation is often observed near grain boundaries in deformed microstructures. This may be indicative of dislocation pile-up at the boundaries but could also be due to a loss of orientation precision in the EBSD measurements. When the electron beam is positioned at or near a grain boundary, the diffraction volume contains the crystal lattices from the two grains separated by the boundary. Thus, the resulting pattern will contain contributions from both lattices. Such mixed patterns can pose some challenge to the EBSD pattern band detection and indexing algorithms. Through analysis of experimental local misorientation data and simulated pattern mixing, this work shows that some of the rise in local misorientation is an artifact due to the mixed patterns at the boundary but that the rise due to physical phenomena is also observed.

Filament condition during hot-wire chemical vapor deposition conditions of multi-walled carbon nanotubes is a major concern for a stable deposition process. We report on the novel application of electron backscatter diffraction to characterize the carburization of tungsten filaments. During the synthesis, the W-filaments transform to W2C and WC. W-carbide growth followed a parabolic behavior corresponding to the diffusion of C as the rate-determining step. The grain size of W, W2C, and WC increases with longer exposure time and increasing filament temperature. The grain size of the recrystallizing W-core and W2C phase grows from the perimeter inwardly and this phenomenon is enhanced at filament temperatures in excess of 1,400°C. Cracks appear at filament temperatures >1,600°C, accompanied by a reduction in the filament operational lifetime. The increase of the W2C and recrystallized W-core grain size from the perimeter inwardly is ascribed to a thermal gradient within the filament, which in turn influences the hardness measurements and crack formation.

A quantitative and automated phase analysis of dual-phase (DP) steel using electron backscatter diffraction (EBSD) was attempted. A ferrite–martensite DP microstructure was produced by intercritical annealing and quenching. An EBSD map of the microstructure was obtained and post-processed for phase discrimination. Band slope (BS), which was a measure of pattern quality, exhibited much stronger phase contrast than another conventional one, band contrast. Owing to high sensitivity to lattice defect and little orientation dependence, BS provided handiness in finding a threshold for phase discrimination. Its grain average gave a superior result on the discrimination and volume fraction measurement of the constituent phases in the DP steel.

Electron backscatter diffraction (EBSD) and electron probe microanalysis (EPMA) measurements are combined to characterize an industrial produced dual-phase steel containing some bainite fraction. High-resolution carbon mappings acquired on a field emission electron microprobe are utilized to validate and improve the identification of the constituents (ferrite, martensite, and bainite) performed by EBSD using the image quality and kernel average misorientation. The combination eliminates the ambiguity between the identification of bainite and transformation-induced dislocation zones, encountered if only the kernel average misorientation is considered. The detection of carbon in high misorientation regions confirms the presence of bainite. These results are corroborated by secondary electron images after nital etching. Limitations of this combined method due to differences between the spatial resolution of EBSD and EPMA are assessed. Moreover, a quantification procedure adapted to carbon analysis is presented and used to measure the carbon concentration in martensite and bainite on a submicrometer scale. From measurements on reference materials, this method gives an accuracy of 0.02 wt% C and a precision better than 0.05 wt% C despite unavoidable effects of hydrocarbon contamination.