Electron backscattering diffraction analysis of an ancient wootz steel blade from central India

The electron backscattering diffraction technique was used to analyse the nature of carbides present in an ancient wootz steel blade. Bulky carbides, pro-eutectoid carbide along the prior austenite grain boundaries and fine spheroidized carbides were detected. Electron backscattering diffraction was employed to understand the texture of these carbides. The orientations of the cementite frequently occur in clusters, which points to a common origin of the members of the cluster. For the bands of coarse cementite, the origin is probably large coarse particles formed during the original cooling of the wootz cake. Pearlite formed earlier in the forging process has led to groups of similarly oriented fine cementite particles. The crystallographic texture of the cementite is sharp whereas that of the ferrite is weak. The sharp cementite textures point to the longevity of the coarse cementite throughout the repeated forging steps and to the influence of existing textured cementite on the nucleation of new cementite during cooling.

Electron backscattering diffraction analysis of a reconstructed wootz damascus steel blade

The historical impact and subsequent fame of wootz weaponry in the ancient world has created interest in what has come to be seen as an advanced material even by modern standards. Ancient wootz artifacts are classed as high carbon (hypereutectoid) crucible steels and are characterised by high strength, hardness and wear resistance, but especially by their attractive surface pattern.

The 3-D Structure of Polycrystalline Diamond Film by Electron Backscattering Diffraction (EBSD)

A lithographic method was used to produce polycrystalline diamond films having highly defined surface geometry, showing an array of diamond tips for possible application as a field emitter device. The films grown in this study used microwave plasma assisted chemical vapour deposition (MACVD) on a silicon substrate; the substrate was then dissolved away to reveal the surface features on the diamond film. It is possible to align the crystallite direction and affect the electron emission properties using a voltage bias to enhance the nucleation process and influence the nuclei to a preferred orientation. This study focuses on the identification of the distribution of crystal directions in the film, using electron backscattering diffraction (EBSD) to identify the crystallographic character of the film surface. EBSD allows direct examination of the individual diamond grains, grains boundaries and the crystal orientation of each individual crystallite. The EBSD maps of the bottom (nucleation side) of the films, following which a layer of film is ion-milled away and the mapping process repeated. The method demonstrates experimentally that oriented nucleation occurs and the thin sections allow the crystal texture to be reconstructed in 3-D. (C) 2003 Elsevier B.V. All rights reserved.

Wootz steel project by electron backscatter diffraction

The data is from an electron backscatter diffraction (EBSD) study of the microstructure of high carbon ‘Wootz’ steel. The objective of the study is to infer an unknown thermomechanical history from observation and analysis of the final microstructure in various ancient artefacts (swords and tools), and then compare the findings with heat treatments of the ancient artefacts and modern attempts at duplication of the structure. Electron backscatter data reveals the orientation relationships between various phases in the material, particularly cementite and ferrite. The dataset is randomly structured and organised. The data is automatically generated by an electron backscattered diffraction system attached to a field emission scanning electron microscope. The dataset uses proprietary software (cannot be copied or distributed without complying with licensing agreements): Oxford HKL Channel 5. As the native formats are binary they cannot be read with standard software.

Characterization of nano-composite M-2411/Y-123 thin films by electron backscatter diffraction and in-field critical current measurements

Thin films of nano-composite Y-Ba-Cu-O (YBCO) superconductors containing nano-sized, non-superconducting particles of Y2Ba 4CuMOx (M-2411 with M = Ag and Nb) have been prepared by the PLD technique. Electron backscatter diffraction (EBSD) has been used to analyze the crystallographic orientation of nano-particles embedded in the film microstructure. The superconducting YBa2Cu3O7 (Y-123) phase matrix is textured with a dominant (001) orientation for all samples, whereas the M-2411 phase exhibits a random orientation. Angular critical current measurements at various temperature (T) and applied magnetic field (B) have been performed on thin films containing different concentration of the M-2411 second phase. An increase in critical current density J c at T < 77 K and B < 6 T is observed for samples with low concentration of the second phase (2 mol % M-2411). Films containing 5 mol % Ag-2411 exhibit lower Jc than pure Y-123 thin films at all fields and temperatures. Samples with 5 mol % Nb-2411 show higher Jc(B) than phase pure Y-123 thin films for T < 77 K. © 2010 IOP Publishing Ltd.

Microstructure evolution of 6061 O Al alloy during ultrasonic consolidation:An insight from electron backscatter diffraction

6061 O Al alloy foils were welded to form monolithic and SiC fibre-embedded samples using the ultrasonic consolidation (UC) process. Contact pressures of 135, 155 and 175 MPa were investigated at 20 kHz frequency, 50% of the oscillation amplitude, 34.5 mm s sonotrode velocity and 20 °C. Deformed microstructures were analysed using electron backscatter diffraction (EBSD). At all contact pressures deformation occurs by non-steady state dislocation glide. Dynamic recovery is active in the upper and lower foils. Friction at the welding interface, instantaneous internal temperatures (0.5-0.8 of the melting temperature, T), contact pressure and fast strain rates result in transient microstructures and grain size reduction by continuous dynamic recrystallization (CDRX) within the bonding zone. Bonding occurs by local grain boundary migration, which allows diffusion and atom interlocking across the contact between two clean surfaces. Textures weaken with increasing contact pressure due to increased strain hardening and different grain rotation rates. High contact pressures enhance dynamic recovery and CDRX. Deformation around the fibre is intense within 50 μm and extends to 450 μm from it. © 2009 Acta Materialia Inc.

Wootz steel project by electron backscatter diffraction

The data is from an electron backscatter diffraction (EBSD) study of the microstructure of high carbon ‘Wootz’ steel. The objective of the study is to infer an unknown thermomechanical history from observation and analysis of the final microstructure in various ancient artefacts (swords and tools), and then compare the findings with heat treatments of the ancient artefacts and modern attempts at duplication of the structure. Electron backscatter data reveals the orientation relationships between various phases in the material, particularly cementite and ferrite.

Electron backscatter diffraction (EBSD) map of AZ31 compressed to 1% strain at room temperature in a direction parallel to the extrusion direction

The collection contains an EBSD map of AZ31 compressed to 1% strain at room temperature in a direction parallel to the extrusion direction. The map was collected as part of an investigation into the role of twinning in the occurrence of a yield point elongation during deformation.

Grain boundary segregation in Fe-Mn-C twinning-induced plasticity steels studied by correlative electron backscatter diffraction and atom probe tomography

We report on the characterization of grain boundary (GB) segregation in an Fe-28Mn-0.3C (wt.%) twinning-induced plasticity (TWIP) steel. After recrystallization of this steel for 24 h at 700 °C, ∼50% general grain boundaries (GBs) and ∼35% Σ3 annealing twin boundaries were observed (others were high-order Σ and low-angle GBs). The segregation of B, C and P and traces of Si and Cu were detected at the general GB by atom probe tomography (APT) and quantified using ladder diagrams. In the case of the Σ3 coherent annealing twin, it was necessary to first locate the position of the boundary by density analysis of the atom probe data, then small amounts of B, Si and P segregation and, surprisingly, depletion of C were detected. The concentration of Mn was constant across the interface for both boundary types. The depletion of C at the annealing twin is explained by a local change in the stacking sequence at the boundary, creating a local hexagonal close-packed structure with low C solubility. This finding raises the question of whether segregation/depletion also occurs at Σ3 deformation twin boundaries in high-Mn TWIP steels. Consequently, a previously published APT dataset of the Fe-22Mn-0.6C alloy system, containing a high density of deformation twins due to 30% tensile deformation at room temperature, was reinvestigated using the same analysis routine as for the annealing twin. Although crystallographically identical to the annealing twin, no evidence of segregation or depletion was found at the deformation twins, owing to the lack of mobility of solutes during twin formation at room temperature.

Crystallography of zirconium hydrides in recrystallized Zircaloy-2 fuel cladding lay electron backscatter diffraction

Precipitation morphology and habit planes of the delta-phase Zr hydrides, which were precipitated within the a-phase matrix grains and along the grain boundaries of recrystallized Zircaloy-2 cladding tube, have been examined by electron backscatter diffraction (EBSD). Radially-oriented hydrides, induced by residual tensile stress, precipitated in the outside region of the cladding, and circumferentially-oriented hydrides in the stress-free middle region of the cladding. The most common crystallographic relationship for both types of the hydrides precipitated at the inter- and intra-granular sites was identical at (0001)(alpha) // {111}(delta), with {1017}(alpha) // {111}(delta) being the occasional exception only for the inter-granular radial hydrides. When tensile stress was loaded, the intra-granular hydrides tended to preferentially precipitate in the grains with circumferential basal pole textures. The inter-granular hydrides tended to preferentially precipitate on the grain faces opposite to tensile axis. The change of prioritization in the precipitation sites for the hydrides due to tensile stress could be explained in terms of the relaxation effect of constrained elastic energy on the terminal solid solubility of hydrogen at hydride precipitation.

Beyond simple imaging with energetic beams – nanopatterning, correlative microscopy and statistical analysis of inclusions

Electron microscopy (EM) has advanced in an exponential way since the first transmission electron microscope (TEM) was built in the 1930’s. The urge to ‘see’ things is an essential part of human nature (talk of ‘seeing is believing’) and apart from scanning tunnel microscopes which give information about the surface, EM is the only imaging technology capable of really visualising atomic structures in depth down to single atoms. With the development of nanotechnology the demand to image and analyse small things has become even greater and electron microscopes have found their way from highly delicate and sophisticated research grade instruments to key-turn and even bench-top instruments for everyday use in every materials research lab on the planet. The semiconductor industry is as dependent on the use of EM as life sciences and pharmaceutical industry. With this generalisation of use for imaging, the need to deploy advanced uses of EM has become more and more apparent. The combination of several coinciding beams (electron, ion and even light) to create DualBeam or TripleBeam instruments for instance enhances the usefulness from pure imaging to manipulating on the nanoscale. And when it comes to the analytic power of EM with the many ways the highly energetic electrons and ions interact with the matter in the specimen there is a plethora of niches which evolved during the last two decades, specialising in every kind of analysis that can be thought of and combined with EM. In the course of this study the emphasis was placed on the application of these advanced analytical EM techniques in the context of multiscale and multimodal microscopy – multiscale meaning across length scales from micrometres or larger to nanometres, multimodal meaning numerous techniques applied to the same sample volume in a correlative manner. In order to demonstrate the breadth and potential of the multiscale and multimodal concept an integration of it was attempted in two areas: I) Biocompatible materials using polycrystalline stainless steel and II) Semiconductors using thin multiferroic films. I) The motivation to use stainless steel (316L medical grade) comes from the potential modulation of endothelial cell growth which can have a big impact on the improvement of cardio-vascular stents – which are mainly made of 316L – through nano-texturing of the stent surface by focused ion beam (FIB) lithography. Patterning with FIB has never been reported before in connection with stents and cell growth and in order to gain a better understanding of the beam-substrate interaction during patterning a correlative microscopy approach was used to illuminate the patterning process from many possible angles. Electron backscattering diffraction (EBSD) was used to analyse the crystallographic structure, FIB was used for the patterning and simultaneously visualising the crystal structure as part of the monitoring process, scanning electron microscopy (SEM) and atomic force microscopy (AFM) were employed to analyse the topography and the final step being 3D visualisation through serial FIB/SEM sectioning. II) The motivation for the use of thin multiferroic films stems from the ever-growing demand for increased data storage at lesser and lesser energy consumption. The Aurivillius phase material used in this study has a high potential in this area. Yet it is necessary to show clearly that the film is really multiferroic and no second phase inclusions are present even at very low concentrations – ~0.1vol% could already be problematic. Thus, in this study a technique was developed to analyse ultra-low density inclusions in thin multiferroic films down to concentrations of 0.01%. The goal achieved was a complete structural and compositional analysis of the films which required identification of second phase inclusions (through elemental analysis EDX(Energy Dispersive X-ray)), localise them (employing 72 hour EDX mapping in the SEM), isolate them for the TEM (using FIB) and give an upper confidence limit of 99.5% to the influence of the inclusions on the magnetic behaviour of the main phase (statistical analysis).