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Characterization of the fcc/bcc orientation relationship by EBSD using pole figures and variants
(2004)
The orientation relationship (OR) between fcc and bcc lattices are described by crystallographic fundamentals using the example of Kurdjumov-Sachs (K-S) and Nishiyama-Wassermann (N-W). Complete pole figures containing all variants will be used to distinguish even between slightly different ORs. EBSD on iron meteorites and duplex steel has been used to analyse a large number of crystal orientations with regard to a high statistical significance and a high probability to capture all variants in a single measurement. It is shown that the use of fixed OR models like K-S, N-W, Bain, Pitsch, or Greninger-Troiano does not satisfacturally reflect the observed experimental pole distributions. It is not convenient to use high-indexed lattice planes and directions to describe the small deviations from the given models. The Euler subspace representation offers a readily comprehensible tool to get an idea about the characteristic of the experimentally detected OR.
Synthesis of Molybdenum and Niobium Mono- and Binary Silicides by the Method of SHS-Metallurgy
(2016)
The process of self-propagating high-temperature synthesis of the Mo–Nb–Si silicides from the powder mixtures has been investigated. Based on performed experiments, the composition of powder mixtures as well as technological parameters are proposed which provide the synthesis of monosilicides MoSi₂, NbSi₂, and binary silicides Mo₁-хNbxSi₂ with different ratios of Nb/Mo by adding different contents of MoO₃ and Nb₂O₅. Microstructure and phase compositions of the obtained silicide ingots are characterized by scanning electron microscopy, electron probe microanalysis, X-ray diffraction, and backscatter electron diffraction.
In the present work, the influence of deuterium on the microstructure of a duplex stainless steel type EN 1.4462 has been characterized by Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) supported by scanning electron microscopy (SEM), focused ion beam (FIB), electron back scattered diffraction(EBSD) and energy dispersive x-ray (EDX) investigations. Characterization has been carried out before and after electrochemical charging with deuterium which has been used as a tracer, due to its similar behavior to hydrogen in the steel microstructure. In a first approach, the distribution of the deuterium occurring at temperatures above 58 °C has been visualized. Further it turned out that sub-surface micro blisters are formed in the ferrite-austenite interface, followed by the formation of needle shaped plates and subsequent cracking at the ferrite surface. In the austenite phase, parallel cracking alongside twins and hexagonal close packed (martensitic) regions has been observed. In both phases and even in the apparent interface, cracking has been associated with high deuterium concentrations, as compared to the surrounding undamaged microstructure. Sub-surface blistering in the ferrite has to be attributed to the accumulation and recombination of deuterium at the ferrite-austenite interface underneath the respective ferrite grains and after fast diffusing through this phase. Generally, the present application of chemometric imaging and structural analyses allows characterization of hydrogen assisted degradation at a sub-micron lateral resolution.
In order to understand the physical and chemical properties of advanced materials, functional molecular adsorbates, and protein structures, a detailed knowledge of the atomic arrangement is essential. Up to now, if subsurface structures are under investigation, only indirect methods revealed reliable results of the atoms’ spatial arrangement. An alternative and direct method is three-dimensional imaging by means of holography. Holography was in fact proposed for electron waves, because of the electrons’ short wavelength at easily accessible energies. Further, electron waves are ideal structure probes on an atomic length scale, because electrons have a high scattering probability even for light elements. However, holographic reconstructions of electron diffraction patterns have in the past contained severe image artifacts and were limited to at most a few tens of atoms. Here, we present a general reconstruction algorithm that leads to high-quality atomic images showing thousands of atoms. Additionally, we show that different elements can be identified by electron holography for the example of FeS₂ .
The inverse pole figure (IPF) coloring for a suitable evaluation of crystal
orientation data is discussed. The major goal is a high correlation between
encoding color and crystal orientation. Revised color distributions of the
fundamental sectors are introduced which have the advantages of (1) being
applicable for all point groups, (2) not causing color discontinuities within grains,
(3) featuring carefully balanced regions for red, cyan, blue, magenta, green and
yellow, and (4) an enlarged gray center in opposition to a tiny white center. A
new set of IPF color keys is proposed which is the result of a thorough analysis
of the colorization problem. The discussion considers several topics: (a) the
majority of presently applied IPF color keys generate color discontinuities for
specifically oriented grains; (b) if a unique correlation between crystal direction
and color is requested, discontinuity-preventing keys are possible for all point
groups, except for 4, 3 and 1; (c) for a specific symmetry group several IPF color
keys are available, visualizing different features of a microstructure; and (d) for
higher symmetries a simultaneous IPF mapping of two or three standard
reference directions is insufficient for an unequivocal orientation assignment.
All color keys are available in MTEX, a freely available MATLAB toolbox.
Using channeling-enhanced energy-dispersive X-ray spectroscopy (EDX), we demonstrate polarity sensitive orientation determination of a non-centrosymmetric crystal in the scanning electron microscope. The authors observe a characteristic asymmetry in the channeling-enhanced, angle-dependent EDX data of a GaAs sample, which is in good agreement to simulations using the dynamical theory of diffraction for the incident electron beam. This allows us to assign the orientation of the GaAs crystal according to the non-centrosymmetric point group. The method shown here overcomes the limitation of a reduced point-group sensitivity of electron backscatter diffraction Patterns and electron channeling patterns for crystalline phases that contain atoms of approximately equal electron scattering cross sections.
Electron backscatter diffraction (EBSD) and scanning electron microscopy were combined to study the effect of residual defect density on corrosion initiation in aluminium alloy AA2024-T3. EBSD was used to determine the level of misorientation (MO), from pixel to pixel, within individual grains. The MO can be determined with respect to either the average orientation angle of the grain or with respect to the average orientation angle of the surrounding pixels (in this instance, a matrix of 7×7 surrounding pixels has been applied). Herein, the MO, determined using the surrounding pixels, was used as the means for the assessing the level of defect density within a grain. It was found that there was a noteworthy, but not definitive, correlation of MO with corrosion initiation after 1 min exposure to 0.1 M NaCl solution. Additionally, the S and θ-phase particles were also identified using EBSD, displaying a range of MO and therefore defect density.
We present special applications of electron backscatter diffraction (EBSD) which aim to overcome some of the limitations of this technique as it is currently applied in the scanning electron microscope. We stress that the raw EBSD signal carries additional information which is useful beyond the conventional orientation determination. The background signal underlying the backscattered Kikuchi diffraction (BKD) patterns reflects the chemical composition and surface topography but also contains channeling-in information which is used for qualitative real-time orientation imaging using various backscattered electron signals. A significantly improved orientation precision can be achieved when dynamically simulated pattern are matched to the experimental BKD patterns. The breaking of Friedel’s rule makes it possible to obtain orientation mappings with respect to the point-group symmetries. Finally, we discuss the
determination of lattice parameters from individual BKD
patterns. Subgrain structure in a single quartz grain. The increased noise level in the left map reflects the lower precision of a standard orientation determination using band detection by the Hough transform. The right map results from the same experimental raw data after orientation refinement using a pattern matching approach. The colors correspond an adapted inverse pole figure color key with a maximum angular deviation of about 2° from the mean orientation.
During the processing of superconducting Nb3Sn wire, several intermediate intermetallic phases including a previously encountered Cu-Nb-Sn phase show up. The yet unknown crystal structure of this phase is now identified by a combination of different experimental techniques and database search to be of the hexagonal NiMg2 type with a proposed composition of about (Nb0.75Cu0.25)Sn2. The structure determination started from an evaluation of the lattice parameters from EBSD Kikuchi patterns from quenched material suggesting hexagonal or orthorhombic symmetry. A database search then led to the hexagonal NiMg2 type structure, the presence of which was confirmed by a Rietveld analysis on the basis of high energy synchrotron X-ray powder diffraction data. Assuming a partial substitution of Nb in orthorhombic NbSn2 by Cu, the change of the valence electron concentration provokes a structural transformation from the CuMg2 type for NbSn2 to the NiMg2 type for (Nb0.75Cu0.25)Sn2. In the previous literature the (Nb0.75Cu0.25)Sn2 phase described here has occasionally been referred to as Nausite.
Kikuchi diffraction patterns can provide fundamental information about the lattice metric of a crystalline phase. In order to improve the possible precision and accuracy of lattice parameter determination from the features observed in Kikuchi patterns, some useful fundamental relationships of geometric crystal-lography are reviewed, which hold true independently of the actual crystal symmetry. The Kikuchi band positions and intersections and the Kikuchi band widths are highly interrelated, which is illustrated by the fact that all lattice plane trace positions of the crystal are predetermined by the definition of only four traces. If, additionally, the projection centre of the gnomonic projection is known, the lattice parameter ratios and the angles between the basis vectors are fixed. A further definition of one specific Kikuchi band width is sufficient to set the absolute sizes of all lattice parameters and to predict the widths of all Kikuchi bands. The mathematical properties of the gnomonic projection turn out to be central to an improved interpretation of Kikuchi pattern data, emphasizing the importance of the exact knowledge of the projection centre.