Crystallographic preferred orientation (CPO) of gypsum measured by electron backscatter diffraction (EBSD)

An investigation by electron backscatter diffraction on gypsum shows that this technique can be used to study the microstructures and crystallographic preferred orientation of gypsum. Presented here are the methods, verification tests and data obtained from a naturally deformed sample of gypsum‐rich rock. The electron backscatter diffraction data show the sample has a strong crystallographic preferred orientation.     

Analysis of traction‐free assumption in high‐resolution EBSD measurements

The effects of using a traction‐free (plane‐stress) assumption to obtain the full distortion tensor from high‐resolution EBSD measurements are analyzed. Equations are derived which bound the traction‐free error arising from angular misorientation of the sample surface; the error in recovered distortion is shown to be quadratic with respect to that misorientation, and the maximum ‘safe’ angular misorientation is shown to be 2.7 degrees. The effects of localized stress fields on the traction‐free assumption are then examined by a numerical case study, which uses the Boussinesq formalism to model stress fields near a free surface. Except in cases where localized stress field sources occur very close to sample points, the traction‐free assumption appears to be admirably robust.     

Comparison of quartz crystallographic preferred orientations identified with optical fabric analysis,electron backscatter and neutron diffraction techniques

Three techniques are used to measure crystallographic preferred orientations (CPO) in a naturally deformed quartz mylonite: transmitted light cross‐polarized microscopy using an automated fabric analyser, electron backscatter diffraction (EBSD) and neutron diffraction. Pole figure densities attributable to crystal‐plastic deformation are variably recognizable across the techniques, particularly between fabric analyser and diffraction instruments. Although fabric analyser techniques offer rapid acquisition with minimal sample preparation, difficulties may exist when gathering orientation data parallel with the incident beam. Overall, we have found that EBSD and fabric analyser techniques are best suited for studying CPO distributions at the grain scale, where individual orientations can be linked to their source grain or nearest neighbours. Neutron diffraction serves as the best qualitative and quantitative means of estimating the bulk CPO, due to its three‐dimensional data acquisition, greater sample area coverage, and larger sample size. However, a number of sampling methods can be applied to FA and EBSD data to make similar approximations.     

Improving the quality of electron backscatter diffraction (EBSD) patterns from nanoparticles

In this study, we investigated the relative contributions of atomic number (Z) and density (ρ) to the degradation of the electron backscatter diffraction (EBSD) pattern quality for nanoparticles < 500 nm in diameter. This was accomplished by minimizing the diffuse scattering from the conventional thick mounting substrate through the design of a sample holder that can accommodate particles mounted on thin‐film TEM substrates. With this design, the contributions of incoherently scattered electrons that result in the diffuse background are minimized. Qualitative and quantitative comparisons were made of the EBSD pattern quality obtained from Al₂O₃ particles approximately 200 nm in diameter mounted on both thick‐ and thin‐film C substrates. For the quantitative comparison we developed a ‘quality’ factor for EBSD patterns that is based on the ratio of two Hough transforms derived from a given EBSD pattern image. The calculated quality factor is directly proportional to the signal‐to‐noise ratio for the EBSD pattern. In addition to the comparison of the thick and thin mounting substrates, we also estimated the effects of Z and ρ by comparing the EBSD pattern quality from the Al₂O₃ particles mounted on thin‐film substrates with the quality of patterns obtained from Fe–Co nanoparticles approximately 120 nm in diameter. The results indicate that the increased background generated in EBSD patterns by the electrons escaping through the bottom of the small particles is the dominant reason for the poor EBSD pattern quality from nanoparticles < 500 nm in size. This was supported by the fact that we were able to obtain usable EBSD patterns from Al₂O₃ particles as small as 130 nm using the thin‐film mounting method.     

Application of electron backscatter diffraction (EBSD) to fracture studies of ferritic steels

The application of electron backscatter diffraction (EBSD) to fracture studies has provided a new method for investigating the crystallography of fracture surfaces. The crystallographic indices of cleavage planes can be measured both directly from the fracture surface and indirectly from metallographic sections perpendicular to the plane of the adjoining fracture surfaces. The results of direct individual cleavage facet plane orientation measurements are presented for carbon–manganese (C–Mn) and low‐alloy Mn–Mo–Ni (similar to ASTM A553 type‐B). Pressure vessel steel weld metals, obtained from fracture surfaces of Charpy impact test specimens fractured at various test temperatures and for an ultra‐low carbon steel (Fe–0.002C–0.058P) fractured at –196 °C by impact. In addition to the direct measurement from the fracture surface, cleavage facet orientation measurements for the ultra‐low carbon steel were complemented by the results obtained from the metallographic sections. Fractographic observations revealed that cleavage fracture is accommodated by a microvoid coalescence fracture micromechanism, which was induced by decohesion of second phase particles (inclusions). The correlation between the direct and indirect methodologies shows that the cleavage facet planes are dominated by the {001} plane orientations, and indicated that even when information concerning the full five degrees of freedom is inaccessible, the cleavage facet plane could still be determined. Finally, the advantages and disadvantages of direct orientation measurements from the fracture surface and indirectly by a destructive sectioning technique are discussed.     

Use of EBSD to identify phases in interdendrite region of a cast Zn–Al-based alloy (ZA27)

Electron backscattered Kikuchi diffraction methodology was used to identify phases in the interdendrite region of an alloy ZA27. Two Zn‐rich hexagonal close‐packed structure phases η and ɛ phases were distinguished using predetermined lattice parameters of the phases. In relation to studies of scanning electron microscopy and X‐ray diffraction, electron backscattered diffraction results revealed that the Al‐rich precipitates of the α phase were from decomposition of the η′_T, and the four‐phase transformation: α+ɛ→ T′+η, had occurred in the ɛ phase after ageing at 150°C for 8 h.     

User‐independent EBSD parameters to study the progress of recovery and recrystallization in Cu–Zn alloy during in situ heating

Microstructural evolution of cold‐rolled Cu–5%Zn alloy during in situ heating inside field‐emission scanning electron microscope was utilized to obtain user‐independent parameters in order to trace the progress of static recovery and recrystallization. Electron back‐scattered diffraction (EBSD)‐based orientation imaging microscopy was used to obtain micrographs at various stages of in situ heating. It is shown that unlike the pre‐existing methods, additional EBSD‐based parameter can be used to trace the progress of recovery and recrystallization, which is not dependent on user input and hence less prone to error. True strain of 0.3 was imposed during cold rolling of alloy sample. Rolled sample was subjected to in situ heating from room temperature to 500°C (～0.58 Tm) with soaking time of 10 min, at each of the intermediate temperatures viz. 100, 200, 300, 400 and 450°C. After reaching 500°C, the sample was kept at this temperature for a maximum duration of around 15 h. The sample showed clear signs of recovery for temperature up to 450°C, and at 500°C, recrystallization started to take place. Recrystallization kinetics was moderate, and full recrystallization was achieved in approximately 120 min. We found that EBSD parameter, namely, band contrast intensity can be used as an extra handle to map out the progress of recrystallization occurring in the sample. By contrast, mean angular deviation can be used to understand the evolution of recovery in samples. The parameters mentioned in the current study, unlike other pre‐existing methods, can also be used for mapping local microstructural transformations due to recovery and recrystallization. We discuss the benefits and limitations in using these additional handles in understanding the changes taking place in the material during in situ heating.     

Is fast mapping good mapping? A review of the benefits of high‐speed orientation mapping using electron backscatter diffraction

Orientation mapping using automated electron backscatter diffraction (EBSD) is now a common technique for characterizing microstructures. Improvements in software and hardware have resulted in high‐speed mapping capabilities above 80 000 points h^?1. For ‘routine’ microstructural analyses of materials such as steel and aluminium (e.g. texture and grain size measurements and high angle boundary characterization), high‐speed orientation mapping is an ideal approach with minimal penalty on the final statistics. However, for the accurate analysis of very low angle boundaries and for routine analyses of more difficult materials (e.g. most rock samples), we advocate a more patient approach to orientation mapping with an emphasis on data accuracy and reliability. It is important that the objectives of any EBSD analysis are carefully considered before starting – in this way the maximum potential of an EBSD system can be achieved.     

Scanning Electron Microscopy (SEM) and Light Microscopy (LM)‐based Palyno‐morphological views of Solanaceae in Western Himalaya

In this study, plants belonging to family Solanaceae growing in Western Himalaya region have been observed palynologically under Light Microscope and Scanning electron microscope. Present investigation comprises of 10 genera and 23 species, namely, Atropa acuminata, Capsicum decoraticus, Capsicum frutescens, Cestrum aurantiacum, Cestrum diurnum, Cestrum nocturnum, Datura alba, Datura innoxia, Datura stramonium, Hyoscymus niger, Lycopersicon esculentum, Nicotiana rustica, Nicotiana tabacum, Petunia alba, Petunia hybrida, Solanum erianthum, Solanum melongena, Solanum miniatum, Solanum pseudocapsicum, Solanum surratense, Solanum tuberosum, Withania coagulans, Withania somnifera. Solanaceae is a eurypalynous family. Grains are usually Tricolporate and Tetracolporate, radially symmetrical, isopolar, prolate‐spheroidal to oblate‐spheroidal to oblate‐spheroidal to subprolate to per prolate or suboblate to oblate, size range: 8.55–72 μm, amb circular, semi‐angular or subangular, aperture drop‐type, labrum common‐type, exine usually 2 μm thick, nexine 1–1.5 μm thick. Tectum usually psilate, sexine reticulate, granulate or striato‐reticulate, with obscure pattern, sexine 1–2 μm thick, nexine 1–1.5 μm thick, and intine 0.5–1 μm thick. Most striking variation has been found in the shape class, aperture‐type, and tectal surface. Based on these characters, taxonomic keys have been made for correct identification of members in Solanaceae. However, the grains of this family are usually tricolporate and have direct relationship with certain members of the family Scrophulariaceae. Palyno‐morphological characters of family Solanaceae have been studied for the first time in Western Himalayan region of Pakistan. These palyno‐morphological characters are significant for identification of the members of family Solanaceae.     

The application of convergent beam electron diffraction (CBED) analysis on transformation‐induced plasticity (TRIP) steels

Convergent beam electron diffraction (CBED) in transmission electron microscopy (TEM) was applied to determine local carbon concentrations in low‐carbon transformation‐induced plasticity (TRIP) steels. High‐order Laue‐zone (HOLZ) lines were experimentally obtained for comparison with simulation results. A new procedure for calculating carbon content is thus proposed. Retained austenite (RA) is classified into three types by morphology; the relationship between the carbon content and the corresponding RA morphology is discussed based on CBED results. Furthermore, results of X‐Ray diffractometry measurements are also used for comparison.