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Texture stands as a fundamental descriptor in the realms of geology and earth and planetary science. Beyond offering insights into the geological processes underlying mineral formation, its characterization plays a pivotal role in advancing engineering applications, notably in mining, mineral processing, and metal extraction, by providing quantitative data for predictive modeling. Laboratory diffraction contrast tomography (LabDCT), a recently developed 3D characterization technique, offers nondestructive measurement of grain phases including their morphology, distribution, and crystal orientation. It has recently shown its potential to assess 3D textures in complex natural rock samples. This study looks at improving on previous work by examining the artifacts and presents a novel postprocessing workflow designed to correct them. The workflow is developed to rectify inaccurate grain boundaries and interpolate partially reconstructed grains to provide more accurate results and is illustrated using multi-scan examples on chromite sands and natural chromitite from the Upper Group 2 Reef layer in South Africa. The postcorrected LabDCT results were validated through qualitative and quantitative assessment using 2D electron back-scattered diffraction on polished sample surfaces. The successful implementation of this postprocessing workflow underscores its substantial potential in achieving precise textural characterization and will provide valuable insights for both earth science and engineering applications.
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Friction stir spot welding (FSSW) of similar AA5052-H32 joints has numerous benefits in shipbuilding, aerospace, and automotive structural applications. In addition, studying the role of tool rotation speed on the microstructure features, achieved textures, and joint performance of the friction stir spot-welded (FSSWed) joint still needs more systematic research. Different FSSWed AA5052-H32 lap joints of 4 mm thickness were produced at different heat inputs using three tool rotation speeds of 1500, 1000, and 500 rpm at a constant dwell time of 2 s. The applied thermal heat inputs for achieving the FSSW processes were calculated. The produced joints were characterized by their appearance, macrostructures, microstructures, and mechanical properties (hardness contour maps and maximum tensile-shear load) at room temperature. The grain structure and texture developed for all the FSSWed joints were deeply investigated using an advanced electron backscattering diffraction (EBSD) technique and compared with the base material (BM). The main results showed that the average hardness value of the stir zone (SZ) in the welded joints is higher than that in the AA5052-H32 BM for all applied rotation speeds, and it decreases as the rotation speed increases from 500 to 1000 rpm. This SZ enhancement in hardness compared to the BM cold-rolled grain structure is caused by the high grain refining due to the dynamic recrystallization associated with the FSSW. The average grain size values of the stir zones are 11, 9, and 4 µm for the FSSWed joints processed at 1500, 1000, and 500 rpm, respectively, while the BM average grain size is 40 µm. The simple shear texture with B/-B components mainly dominates the texture. Compared to the welded joints, the joint processed at 500 rpm and a 2 s duration time attains the highest tensile-shear load value of 4330 N. This value decreases with increasing rotation speed to reach 2569 N at a rotation speed of 1500. After tensile testing of the FSSWed joints, the fracture surface was also examined and discussed.
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Multiple experimental configurations for performing nanoscale orientation mapping are compared to determine their fidelity to the true microstructure of a sample. Transmission Kikuchi diffraction (TKD) experiments in a scanning electron microscope (SEM) and nanobeam diffraction (NBD) experiments in a transmission electron microscope (TEM) were performed on thin electrodeposited hard Au films with two different microstructures. The Au samples either had a grain size that is >50 or <20 nm. The same regions of the samples were measured with TKD apparatuses at 30 kV in an SEM with detectors in the horizontal and vertical configurations and in the TEM at 300 kV. Under the proper conditions, we demonstrate that all three configurations can produce data of equivalent quality. Each method has strengths and challenges associated with its application and representation of the true microstructure. The conditions needed to obtain high-quality data for each acquisition method and the challenges associated with each are discussed.
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Pre-stretching experiments were carried out on AZ31-0.5Ca magnesium alloy to alter the microstructure and texture for enhancing room-temperature formability. Compared to as-received alloy, the formability of a 5%-stretched sample was improved by 15%. This was attributed to enhanced strain hardening capability related to the weakening of basal texture and less homogeneous microstructure. In addition, in-grain misorientation axis analysis performed on the samples (as-received and stretched) also confirmed the higher activity of the non-basal slip systems in the 5%-stretched sample.
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The effect of equal channel angular pressing (ECAP) through the route Bc and aging treatment on the grain structure and properties of the Cu-1Cr-0.2Si alloy was investigated. Microstructure was detected by scanning electron microscopy (SEM), x-ray diffraction (XRD), and electron backscatter diffraction (EBSD) and the mechanical properties and electrical conductivity were tested. Results shown that after ECAP, accompanying the grains refined to nano-and submicron-structure, the Cr particles were gradually spread along the grain boundaries (GBs), aging treatment promoted Cr particles dispersed in the matrix. ECAP greatly increased the ultimate tensile strength (UTS) while having a small effect on the conductivity, and aging treatment increased electrical conductivity. The stable {111}<110> texture after ECAP and the lower dislocation density after aging treatment maybe the main reasons for the high conductivity of the material.
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Magnesium alloys offer a favored alternative to steels and aluminum alloys due to their low density and relatively high specific strength. Their application potentials are, however, impeded by poor formability at room temperature. In the current work, improved formability for the commercial magnesium AZ80 alloy was attained through the application of the high-rate electro-magnetic forming (EMF) technique. With the EMF system, elongation of 0.2 was achieved while only 0.11 is obtained through quasistatic loading. Systematic microstructural and textural investigations prior, during and post deformation under high strain-rate experiments were carried out using electron back-scattered diffraction (EBSD) and other microscopic techniques. The analysis indicates that enhanced elongation is achieved as a result of the combination of deformation, comprising basal and non-basal slip systems, twinning and dynamic recrystallization. An adopted EMF-forming technique is tested which results in enhanced elongation without failure and a higher degree of dynamically annealed microstructure.
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Misorientation angle distribution gives information about the type and fraction of grain boundaries present in a material. Since grain boundaries affect various mechanical and functional properties of the material, the distribution of grain boundary misorientation is important in order to evaluate these properties. This becomes particularly important when we want to study the microstructure in finer detail, such as understanding the average misorientation within a grain. One of the techniques increasingly used in past two decades for characterization of grain boundary misorientation is electron back scatter diffraction (EBSD). Reliable detection of very small misorientation angles using conventional EBSD system is quite challenging due to the presence of measurement error. This makes the comprehensive characterization of microstructures difficult and prone to error. In order to prevent such problems, it is important to understand the nature of measurement error and find ways to minimize it. The present work aims to elucidate the effect of measurement error on the observed misorientation angle and its statistical distribution in low misorientation angle regime. A true strain of 0.3 was imposed during cold-rolling of Cu-5%Zn alloy sample. The rolled sample was then subjected to in-situ heating from room temperature to 500⯰C (â¼0.58â¯Tm). It was found that the overall measurement error in misorientation distribution consists of random error caused by limited angular precision and systematic error which manifests primarily in the statistical distribution of low angle misorientation. In this work, we show a way to deconvolute this overall error based on the measurement technique. We further show that this systematic error is not limited to any particular measurement technique, rather related to the presence of a lower bound in the measurement.
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Here we examine the potential of serial Broad Ion Beam (BIB) Ar+ ion polishing as an advanced serial section tomography (SST) technique for destructive 3D material characterisation for collecting data from volumes with lateral dimensions significantly greater than 100µm and potentially over millimetre sized areas. Further, the associated low level of damage introduced makes BIB milling very well suited to 3D EBSD acquisition with very high indexing rates. Block face serial sectioning data registration schemes usually assume that the data comprises a series of parallel, planar slices. We quantify the variations in slice thickness and parallelity which can arise when using BIB systems comparing Gatan PECS and Ilion BIB systems for large volume serial sectioning and 3D-EBSD data acquisition. As a test case we obtain 3D morphologies and grain orientations for both phases of a WC-11%wt. Co hardmetal. In our case we have carried out the data acquisition through the manual transfer of the sample between SEM and BIB which is a very slow process (1-2 slice per day), however forthcoming automated procedures will markedly speed up the process. We show that irrespective of the sectioning method raw large area 2D-EBSD maps are affected by distortions and artefacts which affect 3D-EBSD such that quantitative analyses and visualisation can give misleading and erroneous results. Addressing and correcting these issues will offer real benefits when large area (millimetre sized) automated serial section BIBS is developed.
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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 (â¼0.58 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.
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In this study, new microscopy techniques were developed for understanding the mechanism for the bainitic transformation in a Cu-17Al-11Mn (at%) alloy. An orthogonally arranged focused ion beam and a scanning electron microscope were employed to observe three-dimensional (3D) morphology of the bainite phase, in addition to compositional analysis by using a scanning transmission electron microscope equipped with a double-detector energy-dispersive X-ray spectrometer system. The 3D morphology of these samples was observed at different aging times and aging temperatures; the results obtained indicated that with increasing aging time and/or aging temperature, the bainite phase at the initial stage of formation exhibits a plate-like shape, which changes to a lenticular form. A habit plane was uniquely determined as â¼{9 3 2} by the combination of 3D image reconstruction and an electron back-scattered diffraction technique. The compositional analysis revealed the spatial distribution of the compositional variation between the bainite and matrix phases in the initial stages of the transformation. In the bainite phase, the Cu concentration was higher, while the concentrations of Al and Mn were lower than those in the surrounding matrix, indicative of the diffusion of the constituent elements with the growth of the bainite phase.
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Iron hollow sphere filled aluminum matrix syntactic foams (AMSFs) were produced by low pressure, inert gas assisted infiltration. The microstructure of the produced AMSFs was investigated by light and electron microscopy, extended by energy dispersive X-ray spectroscopy and electron back-scattered diffraction. The investigations revealed almost perfect infiltration and a slight gradient in the grain size of the matrix. A very thin interface layer that ensures good bonding between the hollow spheres and the matrix was also observed. Compression tests were performed on cylindrical specimens to explore the characteristic mechanical properties of the AMSFs. Compared to other (conventional) metallic foams, the investigated AMSFs proved to have outstanding mechanical properties (yield strength, plateau strength, etc.) and energy absorbing capability.
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We introduce a new experimental approach for the identification of the atomistic position of interstitial carbon in a high-Mn binary alloy consisting of austenite and ε-martensite. Using combined nano-beam secondary ion mass spectroscopy, atomic force microscopy and electron backscatter diffraction analyses, we clearly observe carbon partitioning to austenite. Nano-beam secondary ion mass spectroscopy and atom probe tomography studies also reveal carbon trapping at crystal imperfections as identified by transmission electron microscopy. Three main trapping sites can be distinguished: phase boundaries between austenite and ε-martensite, stacking faults in austenite, and prior austenite grain boundaries. Our findings suggest that segregation and/or partitioning of carbon can contribute to the austenite-to-martensite transformation of the investigated alloy.