Gert Nolze

SEM investigation of interfacial dislocations in nickel‐base superalloys

A new technique for investigation of interfacial dislocations in nickel‐base superalloys by scanning electron microscopy is presented. At high temperatures the pressure of interfacial dislocations against the γ/γ′‐interface causes grooves. This ‘fingerprint of the dislocation network’ is visualized by deep selective etching, which removes the γ′‐phase down to the γ/γ′‐interface. Compared with transmission electron microscopy, the proposed method has important advantages: observation of large sample areas, no superposition of dislocations lying in different specimen depths, possibility of three‐dimensional view of dislocation configurations, information about the dislocation mobility, reduced time for preparation and visualization. The method can be applied for multiphase materials where the interface is grooved by interfacial dislocations.

Orientations – perfectly colored

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 {\overline 4}, {\overline 3} and {\overline 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.

Analysis of Kikuchi band contrast reversal in electron backscatter diffraction patterns of silicon

We analyze the contrast reversal of Kikuchi bands that can be seen in electron backscatter diffraction (EBSD) patterns under specific experimental conditions. The observed effect can be reproduced using dynamical electron diffraction calculations. Two crucial contributions are identified to be at work: First, the incident beam creates a depth distribution of incoherently backscattered electrons which depends on the incidence angle of the beam. Second, the localized inelastic scattering in the outgoing path leads to pronounced anomalous absorption effects for electrons at grazing emission angles, as these electrons have to go through the largest amount of material. We use simple model depth distributions to account for the incident beam effect, and we assume an exit angle dependent effective crystal thickness in the dynamical electron diffraction calculations. Very good agreement is obtained with experimental observations for silicon at 20keV primary beam energy.

Point-group sensitive orientation mapping of non-centrosymmetric crystals

We demonstrate polarity-sensitive orientation mapping of non-centrosymmetric phases by Electron Backscatter Diffraction (EBSD). The method overcomes the restrictions of kinematic orientation determination by EBSD, which is limited to the centro-symmetric Laue-groups according to Friedels rule. Using polycrystalline GaP as an example, we apply a quantitative pattern matching approach based on simulations using the dynamical theory of electron diffraction. This procedure results in a distinct assignment of the local orientation according to the non-centrosymmetric point group of the crystal structure under investigation.

Chirality determination of quartz crystals using electron backscatter diffraction.

We demonstrate the determination of crystal chirality using electron backscatter diffraction (EBSD) in the scanning electron microscope. The chirality of α-quartz as a space-group-dependent property is verified via direct comparison of experimental diffraction features to simulations using the dynamical theory of electron diffraction.

Kikuchi pattern analysis of noncentrosymmetric crystals

Different models of Kikuchi pattern formation are compared with respect to their applicability to noncentrosymmetric crystals, and the breakdown of Friedels rule in experimental electron backscatter diffraction (EBSD) patterns is discussed. Different AIIIBV semiconductor materials are used to evaluate the resulting asymmetry of Kikuchi band profiles for polar lattice planes. By comparison with the characteristic etch pit morphology on a single-crystal surface, the polar character of the measured lattice planes can be assigned absolutely. The presented approach enables point-group-resolved orientation mapping, which goes beyond the commonly applied Laue group analysis in EBSD.

Pattern matching approach to pseudosymmetry problems in electron backscatter diffraction

We demonstrate an approach to overcome Kikuchi pattern misindexing problems caused by crystallographic pseudosymmetry in electron backscatter diffraction (EBSD) measurements. Based on the quantitative comparison of experimentally measured Kikuchi patterns with dynamical electron diffraction simulations, the algorithm identifies the best-fit orientation from a set of pseudosymmetric candidates. Using measurements on framboidal pyrite (FeS2) as an example, we also show the improvement of the orientation precision using this approach.

Investigation of the competitive grain growth during solidification of single crystals of nickel-based superalloys

The competitive growth of columnar grains in a single-grain selector, which is used for directional solidification of single-crystal blades from nickel-based superalloys, has been investigated by electron back-scattered diffraction and local X-ray diffraction analysis. It has been found that the competitive grain growth in a starter block is determined by the crystallographic factor: rapidly growing grains with the axial orientation close to the [001] direction dominate in this part of the casting. For the competitive grain growth in a helicoidal separator, the geometric factor (the position of a grain at the input of the separator) is also important. The results obtained suggest that an appropriate geometry of the single-grain selector was chosen. In addition, the distribution of the orientations of columnar grains obtained by electron backscattered diffraction, can be used for approximate estimation of the yield of suitable (i.e., with the deviation of the axial orientation from the [001] direction within a specified tolerance) single-crystal blades.

Mechanism of porosity growth during homogenisation in single crystal nickel-based superalloys

Several mechanisms for porosity growth in single crystal nickel-based superalloys during homogenisation heat treatment have been proposed in the literature. They were carefully checked using different experimental methods, namely quantitative light microscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction and density measurements. It is shown that the main mechanism is the Kirkendall–Frenkel effect, i.e. generation of voids due to uncompensated efflux of Al atoms from dissolving γ/γ′-eutectic areas. The Al diffusion is supported by the afflux of vacancies from surrounding γ-matrix which results in porosity growth. This conclusion is confirmed by the estimation of the vacancy afflux towards the dissolving eutectic.

EBSD and EDX analysis at the cladding–substrate interface of a laser clad railway wheel

Abstract Electron backscatter diffraction and energy-dispersive X-ray spectrometry were used to investigate the intermixed interface produced during laser cladding of a Co–Cr–Mo alloy on a steel substrate. A multi-component system and rapid solidification conditions together lead to a complex microstructure at the interface. The solidification of the cladding starts with the formation of an interface layer, which is about 75lm in thickness and consists of randomly oriented equiaxed grains of Co–Cr–Fe solid solution and martensite. Orientation analysis of the grains in the interface layer revealed that some grains have a special orientation relationship with the former austenite grains in the heat affected zone but the cladding is not formed by epitaxial growth on the substrate. Intermixing of the materials at the interface is providing a strong bond between the substrate and the cladding. For a grain from the interface layer to emerge as columnar grain in the cladding, it was determined that its <001> crystallographic direction is not supposed to deviate more than 25° from the sample normal direction.