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A survey is presented on some characteristic features of meteoritic (Fe,Ni)3P which is an abundant and important minor phase of most iron meteorites. This mineral (named schreibersite/rhabdite) plays a decisive role during the formation of the so-called Widmanstätten pattern. Different transmission as well as scanning electron microscopic techniques have been applied to get more precise information about the real structure of the phosphide crystals, their chemical composition and the metal distribution across the phoshide/ kamacite interface. X-ray crystal structure determinations have been performed for selected (Fe,Ni)3P - cystals from various iron meteorites (Toluca, North Chile, Watson, Orange River, Morasko, Agpalilik, Odessa, Canyon Diablo). These experiments revealed a metal ordering, i.e. for the three non-equivalent metal positions a different substitution of Fe by Ni has been found. The perfection of the brittle (Fe,Ni)3P samples differs appreciably and seems to be dependent on the thermal history of each individual meteorite. Moreover, inside Ni-rich rhabdite crystals small monocrystalline inclusions of CrN (carlsbergite) have been detected.
EBSD-Aplikationen in der BAM
(2002)
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.
A Co-Cr-Mo laser cladding applied on railway wheels is characterised by a combination of EBSD and EDX. A complete pass of the cladding is investigated to achieve a better understanding of the microstructure evolution during laser cladding. A microstructure with columnar grains extending over the whole thickness of the cladding is observed. The grains have a <001>-fibre texture with the fibre axis parallel to the normal of the substrate surface, and a substructure consisting of cells/dendrites. During the cladding process, two different kinds of precipitates form in the cell walls, which can be identified as M6C and a non-equilibrium phase. Furthermore, stacking faults are observed to occur in the cladding grains and are discussed with respect to the laser cladding process.
Improved determination of fcc/bcc orientation relationships by use of high indexed-pole figures
(2006)
The use of variants to analyze fcc/bcc orientation relationships is demonstrated by EBSD data. Because of multiply occupied poles in the stereographic projections low indexed pole figures are not always suitable. This is mostly caused by the convolution of all scattered individual orientation data as the single poles cannot resolved in the pole figure. Pole figures of higher indexed lattice planes more reliably reflect the character of the orientation relationship since no overlapping of poles occurs.
Residual stress depth profiles of a cast nickel-base superalloy were measured by regarding the deflections occurring in plate-shaped specimens while successively removing layers from the machined or treated surface by electropolishing. The results are in good agreement with previous findings showing (i) the influence of grinding parameters on the width of so-called white layers, which correspond to steep gradients of residual tensile stress, and (ii) a broad zone of compressive residual stress in the case of shot peening.
The suitability of the electron back-scatter diffraction technique (supported by EDS) in order to study the complex microstructures of iron meteorites is demonstrated on the example of the Watson meteorite. The orientation relationships between the main phases kamacite, taenite and schreibersite/rhabdite as well as effects of the real structure have been investigated. In kamacite bands highly deformed blocks appear which show a contineous change of orientation. Plessitic regions are surrounded by deformed taenite lamellae. Also these lamellae show the typical M-profile of the Ni concentration in cross section. In the center a martensitic microstructure has been proven. The white plessite is characterized by a high number of individual kamacite grains which however are separated mainly by low-angle boundaries. So an orientation clustering occurs. The determination of orientation relationships was only possible for a single plessite region comparing the intensity distribution in pole figures with simulations. Schreibersite is brittle and shows a high number of microcracks. However, the strong deformation of kamacite does not allow us to decide whether an orientation relationship between the phosphides and the surrounding kamacite exists or not.
Interphase Boundary Characterization in Duplex Steel and Iron Meteorites Using EBSD Technique
(2006)
Investigation on laser clads
(2005)
Phase identification by EBSD
(2005)
Phase identification by EBSD
(2005)
FIB Milling and Canneling
(2007)
Investigation of the orientation relationships of carlsbergite in the North Chile iron meteorite
(2005)
The crystallographic orientation of carlsbergite (CrN) in the north Chile meteorite (hexahedrite) was investigated using electron backscatter diffraction and transmission electron microscopy. These studies examined the CrN crystals in the rhabdites (idiomorphic schreibersite) and in kamacite. It was found that the CrN crystals embedded in rhabdite show a number of different orientation relationships with the host crystals. These orientations can be explained based on the lattice dimensions of both coexisting crystalline materials. It was also found that both carlsbergite and kamacite are characterized by a high dislocation density (109 cm2) while rhabdite is free of dislocations. It is supposed that in spite of the deformed metallic matrix, a general connection between the orientation relation of all the phases involved exists.
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 75µm 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.
The high sample tilt angle commonly necessary for an orientation determination by EBSD (electron back-scatter diffraction) is responsible for some simple geometrically caused, but nevertheless essential, image distortions. First of all, the influence of the tilt correction and also the trapezium distortion which appears at low magnifications will be discussed. In the second part, an additional rhomboidal distortion will be introduced which is independent of the magnification used. This distortion appears if the scanned sample surface is out of plane to the tilted stage. Even a small deviation from the parallelity produces an approximately three times bigger error of the Euler angle φ1 when the sample alignment is based on the image captured from the highly tilted sample. This effect especially
concerns small samples (e.g. FIB-lamellae) since they cannot be exactly aligned, but the measurements of bigger samples can also be influenced. As an example a correction procedure is described in detail, based on a repetition of the measurement after a 180° sample rotation.
The role of alpha- to epsilon-Co phase transformation on strain hardening of a Co-Cr-Mo laser clad
(2007)
A laser clad CoCrMo alloy has been analysed by the electron backscatter diffraction (EBSD) technique to examine the microstructural evolution during tensile deformation and to study the role of the evolved microstructure on strain hardening of the clad. The allotropic phase transformation from α- to ε-Co, that did not take place during cooling from the solidification temperature, occurs in the form of a strain-induced transformation during plastic deformation. Combined slip on non-parallel planes in parallel bands of α- and ε-Co prevents the formation of cracks and contributes to the strain hardening of the material. Due to twin formation at intersecting ε-Co bands, {1 1 0 1} planes become almost parallel to {1 1 1} planes of α-Co, and facilitate further glide of dislocations. Owing to the strain-induced transformation of α- to ε-Co, the laser clad CoCrMo investigated in this study can accommodate high deformation before cracks are formed at the wavy slip-lines and the precipitates.
Electron microscopy investigation of the structure of a compact extruded from nanopowder of nickel
(2007)
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.
For the description of (single) crystal orientations, e.g. as measured by electron backscatter diffraction (EBSD) & X-ray diffraction (XRD), Euler angles are still generally used to import and export data. However, because of the lack of standard definitions for the unit cell reference settings and specimen axes, several transformation descriptions exist which produce different sets of Euler angles for the same orientation. There is also no recommended region within the minimal Euler orientation space into which orientations should be placed. This is the reason why different sets of Euler angles for the same orientation are generated by the available software packages for indexing EBSD patterns. These issues are reviewed and addressed.
The influence of crystal symmetry in form of chiral (enantiomorphic) groups is discussed, as well as how multiple, but symmetry-equivalent sets of Euler angles can be reduced in order to deliver a unique orientation description. The Euler coloring algorithms applied to EBSD map data is critically discussed. The specific case of cubic symmetry, especially the effect of the three-fold rotation on the Euler space is investigated in more detail for the highest-symmetric chiral group 432. Recommendations for standard settings of the unit cell to orthogonal coordinate system transformation are given which exploit inherent symmetry.
The visualization of spatially resolved single Orientation data, e.g. collected by electron backscatter diffraction (EBSD) in the scanning electron microscope (SEM), is still a challenge since some Orientation coloring schemes have low color sensitivity, and/or specific color discontinuities. The latter appear even for crystal Orientations which are practically identical and characterized only by a tiny misorientation. Euler angle coloring schemes suffer from their lack of intuitiveness. The inverse pole figure (IPF) coloring that has been widely accepted does not display the real Orientation Information for each measurement point, but only the crystallographic description of a single reference direction. For the representation of the complete Orientation information at least a second IPF Orientation map must be shown which displays the crystallographic description for another reference direction. In this context it must be pointed out that the IPF coloring is also not immune to color discontinuities, which are visible as speckled grains (and usually misinterpreted as erroneous Orientation determinations by EBSD). However, a general analysis of the commonly used color keys shows that color discontinuities are a consequence of the crystal symmetry for 6 of the 11 centrosymmetric Laue groups. This means that the Orientation description is correct, but the representation tool is inappropriate for properly displaying the orientation information.
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 Friedel's 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.
Data about the creep behaviour of metals and their alloys at temperatures close to the melting point are very limited. The reason is that most engineering alloys are used at temperatures below 0.6-0.8 of their melting point, so, Investigation of creep at higher temperatures has no practical relevance. For some special applications however it is important, in our case hot isostatic pressing (HIP) of single-crystal turbine blades cast from nickel-base superalloys. In order to remove porosity the blades are HlPed at temperatures between y'-solvus and solidus where superalloy has no strengthening y'-phase and therefore is very soft. For example, the Company Howmet Castings HIPs the superalloy CMSX-4 at the temperature 1288aC, which corresponds to a homologous temperature of about 0.97=1561 K/1612 K (solidus temperature). Therefore knowledge about the creep behaviour of CMSX-4 at this temperature and understanding of the creep mechanisms are necessary to model the kinetics of pore closure during HIP as well as to plan the Parameters of the HIP process.
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 thermal stability of the microstructure of a heat-resistant cobalt alloy, which consists of a γ solid solution strengthened with γ'-phase precipitates, has been studied. The temperature behavior of the dissolution of the hardening γ' phase and the kinetics of its coarsening at 700 and 800°C have been determined. It is found that, during prolonged annealing at 800°C, the γ' → β phase transformation occurs.
The kinetic energy of keV electrons backscattered from a rutile (TiO2) surface depends measurably on the mass of the scattering atom. This makes it possible to determine separately the angular distribution of electrons backscattered elastically from either Ti or O. Diffraction effects of these backscattered electrons inside the rutile crystal lead to the formation of Kikuchi patterns. The element-resolved Kikuchi patterns of Ti and O differ characteristically, but each can be described fairly well in terms of the dynamical theory of diffraction. Qualitatively, much of the differences can be understood by considering the relative arrangement of the Ti and O atoms with respect to planes defined by the crystal lattice.
Introduction to PowderCell
(2015)
Meteorites are a unique and inspiring material for microstructural studies because if their very specific genesis. Iron meteorites have been formed under unimaginable cooling rates of a few ten Kelvins per million years so that the observable transformation of the formerly huge Fe-Ni single crystals of taenite occurred under nearly-equilibrium conditions. Octahedrites (meteorites having a Ni content between 6...15%) are characterized by ribbons of the low-temperature Fe-Ni phase kamacite separated by rims of residual taenite. This very specific feature is known as Widmanstaetten structure and has been investigated by synchrotron radiation in order to cover a higher volume fraction for a statistically relevant description of orientation relationships. However, plessite – a microstructure mainly consisting of the same phases – reflects the orientation relationship between kamacite and taenite as well. For their characterization, a scanning electron microscope is very suitable in order to investigate crystal orientations or identify phases. Despite the apparently ideal formation circumstances of iron meteorites, Ni concentration profiles prove non-equilibrium conditions. Combined EDS (energy dispersive spectroscopy) and EBSD (electron backscatter diffraction) measurements at a selected plessitic region of the Cape York iron shows that a correlation exists between Ni-concentration and the locally detected orientation relationship.
We have studied the anisotropic milling of Cu with respect to the milling rate and the milling topography, as well. The background is twofold: i) anisotropic milling has to be taken into account during the preparation of TEM specimens and in the manufacturing of micro parts from crystalline materials, and ii) the orientation depending milling behaviour can be used to generate topographies with specific properties with respect to, for example, adsorption, wear, and corrosion.
During focused ion beam microscopy (FIB) of crystalline materials imaging contrast and milling result are effected by orientation of the crystals with respect to the incident ion beam. This is due to the possibility of ion channeling along preferred crystal directions which effects the depth at which interaction between ions and specimen atoms takes place. As a result of channeling emission of ion induced secondary electrons (iiSE) and secondary ions (SI) as well as the sputter rate decreases.
Theoretical channeling orientations and critical angles can be calculated.
These effects have been studied quantitatively for polycrystalline recrystallized Cu as a typical model case.
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 backscattered 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.
Fatigue crack propagation investigations have been performed in austenitic-ferritic duplex stainless steel H22N5M3 in air and during hydrogen charging, using various frequencies of loading. Strong differences of crack propagation velocity depending on the test conditions were noticed. Lower frequency with applied hydrogen charging led to the huge increase of crack propagation velocity compared to the tests performed in air. To understand such a behaviour in each case and characterize crack mode, the samples were observed using electron back-scattered diffraction (EBSD). It was shown that in air, the fatigue crack propagation involved plastic deformation and the resulting cracks had ductile character. The presence of hydrogen led to more brittle mode of cracking. This effect was also connected with frequency of loading: lower frequency, which assured longer time for hydrogen-crack tip interaction, resulted in the highest crack propagation velocity and the brittle cracking mode with lower amount of plastic deformation. The performed observations indicated that the path of the crack went mostly transgranularly through both austenite and ferrite phases. Phase and grain boundaries were not the preferred paths for crack propagation.
Interphase boundary characterization in duplex steel and iron meteorites using EBSD technique
(2006)
The properties of materials are mainly described by the orientation distribution of the crystalline phases in a material. Beside the so considered anisotropy also the grain as well as phase boundaries are of extreme importance for a whole string of properties, e.g. the strength of a material. On the example of the interface between fcc and bcc iron the discovered and derived models are discussed. Although the common models are based on the crystal lattice description, the atomic configuration on the interface is analysed. Since experimentally a wide spread of orientations data appears the consideration of the frequency distribution is proposed to find at least the main orientation relationship between fcc and bcc. High-indexed pole figures as well as the Euler subspace are introduced in order to increase the accuracy and to compare different measurements. For the sake of simplicity EBSD measurements on iron meteorites are used since they commonly consist of large fcc single crystals which transformed to a low and very specific number of bcc grains. In special cases the described procedure could also be used for steels.
The hydrogen influence on the microstructure of the austenitic-ferritic Cr22-Ni5-Mo3 stainless steel was investigated. Cathodic hydrogen charging was performed electrochemically from aqueous solution of 0.1M H2SO4 with hydrogen entry promoter addition. The aim of this study was to reveal microstructural changes appearing during the hydrogen charging and particularly to clarify the occurrence of phase transformations induced by hydrogen. The specific changes in both phases of steel were observed. In the ferritic phase, strong increase of dislocation density was noticed. Longer time of hydrogen charging leaded also to the strips and twin plates formation in ferrite phase. In the austenitic phase, the generation of stacking faults, followed by the formation of α' martensite was remarked.
The orientation relationship (OR) between the bcc and fcc phase in the plessite microstructure of the iron meteorites Watson, Agpalilik and Gibeon has been analysed in a scanning electron microscope using electron back-scattered diffraction (EBSD). A very strong OR exists, independently on the analysed plessite type and the observed spreading of single orientation data. The agreement between the experimental orientation distribution and existing models varies for each meteorite. The black plessite in the Agpalilik corresponds to the Nishiyama-Wassermann model whereas the Duplex plessite of the Gibeon meteorite shows an OR close to the Kurdjumov-Sachs model. The Watson meteorite is strongly deformed so that a general OR is difficult to determine due to the blurred experimental orientation distribution.
The main component of this program is a simultaneous representation of the unit cell and the calculated powder pattern. It allows the manipulation of the Crystal structure by moving selected atoms of the asymmetric unit. The resulting powder pattern can be directly compared to experimental data in order to obtain reliable starting values for further computations in refinement programs.
The program PowderCell is a crystallographic tool for visualization of Crystal structures. However, it offers also non-conventional features like the fulautomatical generation of subgroups or the consideration of non-standard settings of space-group types. On the one Hand the program is very useful for non-crystallographers who like to get an impression of the atomic arrangement within the unit cell. But also for crystallographers it is recommendable because it contains a lot of additional information which can be extracted and used like data given in the International Tables for Crystallography, Vol. A. However, the most important advantage of the program is the simultaneous calculation of the X-ray or neutron diffraction powder patterns for a mixture of up to 10 crystalline phases. Between more than 7 different characteristic radiations can be chosen and their influence on the resulting powder pattern can be studied. Furthermore, experimental diffractograms can be analysed using a refinement procedure. The implemented LeBail-algorithm allows the investigation of unknown phases. In combination with the refinement algorithm an interface to Shelx offers the possibility for a step by step ab initio structure analysis. Certainly, the user-friendly shell is one reason that especially users who are not so familar with space-group symmetry, crystal structure data or diffractometry use this powerful tool for the solution of scientific or analytical problems as well as in teaching.
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.
Within the last decade, silicon drift detectors (SDD) systems have become more and more popular in the field of energy-dispersive spectroscopy (EDS). The main characteristic of the SDDs is their extremely high pulse load capacity of up to 750,000 counts per second at good or reasonable energy resolution (<123eV Mn-Kα, <46eV C-Kα at 100.000 cps). These properties in conjunction with electron backscatter diffraction (EBSD) techniques and modern data processing make a range of innovative analysis options possible, not only high speed mapping but also hyperspectral imaging techniques.
The tetragonal crystal- structure type of chalcopyrites (chemical formula AIBIIICVI2) is a superstructure of sphalerite type. The c/a ratio differs generally from the ideal value 2, i.e., the crystal structure is pseudocubically distorted. For CuInSe2 and CuGaSe2 thin films, simulations demonstrate that it is theoretically possible to reveal the tetragonality in electron backscatter-diffraction (EBSD) patterns for CuGaSe2, whereas it may not be possible for CuInSe2. EBSD experiments on CuGaSe2 thin films using the ”Advanced Fit” band-detection method show that it is possible to extract accurate misorientation-angle distributions from the CuGaSe2 thin film. Pole figures revealing the texture of the CuGaSe2 thin film are shown, which agree well with X-ray texture measurements from the same layer.
Irrational orientation relationship derived from rational orientation relationships using EBSD data
(2008)
The determination of the orientation relationship (OR) between α-Fe matrix (bcc) and γ-Fe precipitates (fcc) is discussed using orientation data collected by electron backscatter diffraction (EBSD). The comparatively low accuracy of EBSD is compensated by the high number of measurements what allows a general statement regarding to the mean OR existing in a sample. The representation and discussion is realized on a part of the Bain zone in a {001} pole figure. A discussion of some selected rational OR which are commonly used for the phase boundary characterization between α and γ shows that the pole figures describing a transformation from γ → α are different to those for α → γ. A technique is proposed based on at least three misorientation angles between the experimental OR to the rational OR's as reference. For the misorientation angle distribution a refinement is applied to extract the mean values. They are used to detect the mean OR, what is also possible for only a few or even a single precipitate if the number of measurements describing the phase boundary is sufficiently high.
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 gamma/gamma'-interface causes grooves. This 'fingerprint of the dislocation network' is visualized by deep selective etching, which removes the gamma'-phase down to the gamma/gamma'-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.
X-ray stress analysis on crystalline materials is based on the determination of elastic lattice strains. The strains described by the shift of peak positions are converted to stresses by the means of theory of elasticity. The development of the sin2ψ-method of X-ray stress analysis introduced an enormous progress in X-ray stress analysis during the last decades. This report outlines some important elements of X-ray physics and fundamentals of theory of elasticity. The Standard measuring procedure are described and special experimental differences to the common powder diffractometry are outlined.
PowderCell 2.0 for Windows
(1998)
PowderCell contains a comfortable, user friendly visualization and modification tool for crystal structures. It provides on-line calculation of the corresponding powder diffraction patterns simulating a variety of experimental conditions. The common ICSD and Shelx file formats are supported for importing crystal structure information. It has control of automatic cell transformation and also derivation of subgroups. More than 740 different settings of the 230 space-group types are supported. Up to ten crystal structures can be considered simultaneously. A full pattern refinement enables the direct comparison with experimental diffractograms for quantitative phase analysis, lattice parameter refinement, polynomial background estimation, etc.
PowderCell as teaching tool
(1998)
PowderCell represents a user friendly program which supports the solution of scientific problems as well as teaching and education. Especially for the last one the program offers a lot of information regarding the space-group type as well as crystal structure used. Therefore, on some universities the program is used successfully to make students familiar with x-ray crystallography. The quasi-simultaneous diffraction pattern simulation visualized the changes caused by the respective crystal structure. However, it is also possible to vary different diffraction parameters and investigate the resulting changes in the interference intensity or the reflection position. In principle, the aim of the program is the intuitive generation of structure models. Therefore, special tools have been implemented to move (rotate or shift) or transform the crystal structure.
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.
On April 23rd 2013 at 2:07 a.m., a 1.3 kg meteorite fell in the Braunschweig suburb Melverode (52° 13′ 32.19″ N. 10° 31′ 11.60″ E). Its estimated velocity was 250 km/h and it formed an impact pit in the concrete fall site with a diameter of 7 cm and a depth of 3 cm. Radial dust striae are present around the impact pit. As a result of the impact, the meteorite disintegrated into several hundred fragments with masses up to 214 g. The meteorite is a typical L6 chondrite, moderately shocked (S4) – but with a remarkably high porosity (up to 20 vol%). The meteorite was ejected from its parent body as an object with a radius of about 10–15 cm (15–50 kg). The U,Th-He gas retention age of ∼550 Ma overlaps with the main impact event on the L-chondrite parent body ∼470 Ma ago that is recorded by many shocked L chondrites. The preferred cosmic-ray exposure age derived from production of radionuclides and noble gas isotopes is (6.0 ± 1.3) Ma.
The effect of electrochemical charging of hydrogen on the structure of a lean duplex stainless steel LDX 2101® (EN 1.4162, UNS S32101) was examined by both Time-of-Flight secondary ion mass spectrometry and electron back-scatter diffraction. The goal is to correlate hydrogen concentration and induced structural changes. Chemical and structural characterizations were done for the same region at the sample's surface with sub-micron spatial resolution. Regions of interest were varying in size between 50 × 50 μm and 100 × 100 μm. The results show a phase transformation of austenite to mainly a defect-rich BCC and scarcely a HCP phase. The phase transformation occurred in deuterium rich regions in the austenite.
Advanced structural characterisation techniques which are rapid to use, non-destructive and structurally definitive on the nanoscale are in demand, especially for a detailed understanding of extended-defects and their influence on the properties of materials. We have applied the electron
backscatter diffraction (EBSD) technique in a scanning electron microscope to non-destructively
characterise and quantify antiphase domains (APDs) in GaP thin films grown on different (001)Si substrates with different offcuts. We were able to image and quantify APDs by relating the asymmetrical intensity distributions observed in the EBSD patterns acquired experimentally and comparing the same with the dynamical electron diffraction simulations. Additionally mean angular error maps were also plotted using automated cross-correlation based approaches to image APDs.
Samples grown on substrates with a 4° offcut from the [110] do not show any APDs, whereas samples grown on the exactly oriented substrates contain APDs. The procedures described in our work can be
adopted for characterising a wide range of other material systems possessing non-centrosymmetric point groups.
We analyse the signal formation process for scanning electron microscopic imaging applications on crystalline specimens. In accordance with previous investigations, we find nontrivial effects of incident beam diffraction on the backscattered electron distribution in energy and momentum. Specifically, incident beam diffraction causes angular changes of the backscattered electron distribution which we identify as the dominant mechanism underlying pseudocolour orientation imaging using multiple, angle-resolving detectors. Consequently, diffraction effects of the incident beam and their impact on the subsequent coherent and incoherent electron transport need to be taken into account for an in-depth theoretical modelling of the energy- and momentum distribution of electrons backscattered from crystalline sample regions. Our findings have implications for the level of theoretical detail that can be necessary for the interpretation of complex imaging modalities such as electron channelling contrast imaging (ECCI) of defects in crystals. If the solid angle of detection is limited to specific regions of the backscattered electron momentum distribution, the image contrast that is observed in ECCI and similar applications can be strongly affected by incident beam diffraction and topographic effects from the sample surface. As an application, we demonstrate characteristic changes in the resulting images if different properties of the backscattered electron distribution are used for the analysis of a GaN thin film sample containing dislocations.
(Bio)geochemical cycling of gold (Au) has been demonstrated in present-day (semi)-arid, (sub)-tropical and temperate environment. Hereby biofilms on Au-bearing mineral- and Au-particle surfaces drive Au dispersion and reconcentration, thereby (trans)forming the particles. However, it is unknown if biogeochemical cycling of Au occurs in polar environments, where air temperatures can reach −40 °C and soils remain frozen for much of the year. Therefore, placer Au-particles, soils and waters were collected at two placer mining districts in arctic Finland, i.e., the Ivalojoki and Lemmenjoki goldfields. Sites were chosen based on contrasting settings ((glacio)-fluvial vs. glacial-till deposits) and depths (surface to 5m below current surface). Gold particles were studied using a combination of tagged 16S rRNA gene next generation sequencing and electron microscopic/microanalytical techniques. Across all sites a range of Au-particle morphologies were observed, including morphotypes indicative of Au dissolution and aggregation. Elevated Au concentrations indicative of Au mobility were detected in placer particle bearing soils at both districts. Typically Au-particles were coated by polymorphic biofilm layers composed of living and dead cells embedded in extracellular polymeric substances. Intermixed were biominerals, clays and iron-sulfides/oxides and abundant secondary Au morphotypes, i.e., nano-particles, microcrystals, sheet-like Au, branched Au networks and overgrowths and secondary rims. Biofilms communities were composed of Acidobacteria (18.3%), Bacteroidetes (15.1%) and Proteobacteria (47.1%), with β-Proteobacteria (19.5%) being the most abundant proteobacterial group. Functionally, biofilms were composed of taxa contributing to biofilm establishment, exopolymer production and nutrient cycling, abundant taxa capable of Au mobilization, detoxification and biomineralization, among them Cupriavidus metallidurans, Acinetobacter spp. and Pseudomonas spp., were detected. In conclusion, these results demonstrate that placer Au-particle transformation and Au dispersion occur in cold, arctic environments. This corroborates the existence of biogeochemical Au cycling in present-day cold environments.
During the energy transformation from fossil fuels to renewable energy sources, the use of hydrogen as fuel and energy storage can play a key role. This presents new challenges to industry and the scientific community alike. The storage and transport of hydrogen, which is nowadays mainly realized by austenitic stainless steels, remains problematic, which is due to the degradation of mechanical properties and the possibility of phase transformation by hydrogen diffusion and accumulation. The development of materials and technologies requires a fundamental understanding of these degradation processes. Therefore, studying the behavior of hydrogen in austenitic steel contributes to an understanding of the damage processes, which is crucial for both life assessment and safe use of components in industry and transportation. As one of the few tools that is capable of depicting the distribution of hydrogen in steels, time-of-flight secondary ion mass spectrometry was conducted after electrochemical charging. To obtain further information about the structural composition and cracking behavior, electron-backscattered diffraction and scanning electron microscopy were performed. Gathered data of chemical composition and topography were treated employing data fusion, thus creating a comprehensive portrait of hydrogen-induced effects in the austenite grade AISI 304L. Specimens were electrochemically charged with deuterium instead of hydrogen. This arises from the difficulties to distinguish between artificially charged hydrogen and traces existing in the material or the rest gas in the analysis chamber. Similar diffusion and permeation behavior, as well as solubility, allow nonetheless to draw conclusions from the experiments.
Interdiffusion in the Face-Centered Cubic Phase of the Co-Al-W-Ta System Between 1090 and 1240 °C
(2018)
Interdiffusion of Al, W, Ta and Co in a Co-base alloy at temperatures between 1090 and 1240 °C has been investigated. The interdiffusion coefficients were found to be close to those reported for these elements in Ni-base alloys. Combining the diffusion simulation software DICTRA with the Ni-base diffusion databases TCNi5 and MobNi3, the interdiffusion profiles of Co, Al W, and Ta were modeled for Co9Al8W2Ta/Co diffusion couples annealed at different temperatures and for different times. The results show that interdiffusion in the Co-Al-W-Ta alloys can be modeled reasonably well using the available commercial databases for thermodynamics and kinetics of Ni-base systems.
The creep behavior of single crystals of the nickel-based superalloy CMSX-4 was investigated at 1288 °C, which is the temperature of the hot isostatic pressing treatment applied to this superalloy in the industry. It was found that at this super-solvus temperature, where no gammaPrime-strengthening occurs, the superalloy is very soft and rapidly deforms under stresses between 4 and 16 MPa. The creep resistance was found to be very anisotropic, e.g., the creep rate of [001] crystals was about 11 times higher than that of a [111] crystal. The specimens of different orientations also showed a very different necking behavior. The reduction of the cross-sectional area psi of [001] crystals reached nearly 100 pct, while for a [111] crystal psi = 62 pct. The EBSD analysis of deformed specimens showed that despite such a large local strain the [001] crystals did not recrystallize, while a less deformed [111] crystal totally recrystallized within the necking zone. The recrystallization degree was found to be correlated with deformation behavior as well as with dwell time at high temperature. From the analysis of the obtained results (creep anisotropy, stress dependence of the creep rate, traces of shear deformation, and TEM observations), it was concluded that the main strain contribution resulted from <01-1>{111} octahedral slip.
The alloying system Co-Al-W-Ta is comprehensively investigated in the vicinity of the compositional point Co-9Al-10W-2Ta, at. pct. These investigations provided a large amount of quantitative information, which can be used for alloy development, namely, the compositional dependences of the The alloying system Co-Al-W-Ta is comprehensively investigated in the vicinity of the compositional point Co-9Al-10W-2Ta, at. pct. These investigations provided a large amount of quantitative information, which can be used for alloy development, namely, the compositional dependences of the γ‘-solvus, solidus, and liquidus temperatures; fraction of the extrinsic phases after casting; the compositional dependence of the γ/γ‘-lattice misfit; the element partitioning between γ- and γ‘-phases; and the two Phase compositional area γ/γ‘ in the Co-rich part of the Co-Al-W-Ta phase diagram at 900°C. It is shown that additions of Ta elevate the γ‘-solvus temperature and increase the γ/γ‘-lattice misfit, but adding more than about 3 at. pct Ta results in a large amount of undissolvable extrinsic phases. Additionally, two Co-Al-W-Ta alloys with lower content of W were developed and solidified as [001] single crystals for mechanical testing in a temperature range between 20 and 1200°C. These tests included measurement of the Young modulus, tensile tests with constant strain rate, and stress rupture tests. It was found that at temperatures up to about 750°C the ultimate tensile strength of Co-Al-Ta-W alloys can be at the same level or even higher than of Ni-based superalloys.
We use pattern matching of experimental and dynamically simulated backscattered Kikuchi diffraction (BKD) patterns to increase the orientation precision of electron backscatter diffraction (EBSD) measurements. In order to quantify the improvement in orientation precision, we analyze the experimental distribution of the kernel average misorientation (KAM) angles. We find that for the same raw data, i.e. the same EBSD data acquisition time budget, the pattern matching approach improves the KAM resolution by an order of magnitude compared to orientation data delivered from the conventional Hough-transform based data analysis. This quantitative improvement enables us to interpret small orientation changes in plastically deformed materials which are hidden in noisy orientation data delivered from the reference EBSD system.
As an application example, we analyze a ferritic-martensitic steel (P92) sample before and after low-cycle fatigue (LCF) loading (±0.3% strain) at 620 °C. Whereas the low precision of the EBSD orientation data from the manufacturer software does not allow a reliable discrimination of the gradually changing microstructure, we find very clear systematic differences of the local microstructure after the pattern matching orientation refinement of the initial, raw pattern data. For the investigated P92 sample, the KAM-angle histograms are well described by two log-normal distributions indicating the already tempered and the remaining and mostly untempered martensite.
The Bravais lattices and their lattice parameters are blindly determined using electron backscatter diffraction (EBSD) patterns of materials with cubic or tetragonal crystal structures. Since the geometric relationships in a single EBSD pattern are overdetermined, the relative errors of determining the lattice parameters as well as the axial ratios are confined to about 0.7 ± 0.4% and 0.07 ± 0.03%, respectively, for ideal simulated EBSD patterns. The accuracy of the crystal orientation determination reaches about 0.06 ± 0.03°. With careful manual band detection, the accuracy of determining lattice parameters from experimental patterns can be as good as from simulated patterns, although the results from simulated patterns are often better than expermental patterns, which are lower quality and contain uncertain systematic errors. The reasonably high accuracy is obtained primarily because the detection of the diffracting-plane traces and zone axes is relatively accurate. The results here demonstrate that the developed procedure based on the EBSD technique presents a reliable tool for crystallographic characterization of the Bravais lattices of unknown phases.
Electron backscatter diffraction (EBSD) is a technique to obtain microcrystallographic information from materials by collecting large-angle Kikuchi patterns in the scanning electron microscope (SEM). An important fundamental question concerns the scattering-angle dependent electron energy distribution, which is relevant for the formation of the Kikuchi diffraction patterns. Here we review the existing experimental data and explore the effective energy spectrum that is operative in the generation of backscatter Kikuchi patterns from silicon. We use a full pattern comparison of experimental data with dynamical electron diffraction simulations. Our energy-dependent cross-correlation based pattern matching approach establishes improved constraints on the effective Kikuchi pattern energy spectrum, which is relevant for high-resolution EBSD pattern simulations and their applications.
Creep behavior of a γ΄-strengthened Co-base alloy with zero γ/γ΄-lattice misfit at 800 °C, 196 MPa
(2017)
Deformation and structural behavior of an experimental γ΄-strengthened Co-base alloy during creep at 800 °C and 196 MPa have been investigated. The characteristic features of this alloy are zero γ/γ΄-lattice misfit and a fine γ/γ΄-microstructure. In the initial condition, the γ΄-precipitates in this alloy are small (size of about 100 nm), have polyhedral morphology, and are separated by the very narrow c-channels (width of about 10 nm). The tests performed up to about 1% creep strain (about 500 h creep time) gave creep curves with a slow constant strain rate and without an apparent transient creep, typical for superalloys with nonzero misfit. In this initial stage of creep, entering of the narrow γ-channels by dislocations is blocked by a strong Orowan force. The micromechanism of creep was identified as an octahedral glide of h011i superdislocations simultaneously in two phases, γ and γ΄. The γ/γ΄-microstructure with zero misfit shows no rafting but rapidly coarsens isotropically. It is concluded that zero misfit is beneficial at the initial stages of the creep but is unfavourable for longterm creep because of the continuous microstructural coarsening.
Due to the increasing global demand for pure silver, native wire silver aggregates in very high purities are gaining more industrial attention. Up to the present, no substantial metallurgical Investigation of natural wire silver exists in the accessible literature. To convey urgently needed cross-disciplinary fundamental knowledge for geoscientists and metallurgical engineers, twenty natural wire silver specimens from eight different ore deposits have been investigated in detail for the first time by EBSD (Electron Back Scattering Diffraction), supported by light microscopy and micro-probe analyses. The improved understanding of the natural silver wire microstructure provides additional Information regarding the growth of natural silver aggregates in comparison to undesired artificial growth on electronic devices. Clear evidence is provided that natural silver curls and hairs exhibit a polycrystalline face-centered cubic microstructure associated with significant twinning. Although the investigated natural wire silver samples have relatively high purity (Ag > 99.7 wt.-%), they contain a variety of trace elements such as, S, Cu, Mn, Ni, Zn, Co and Bi, As and Sb. Additionally, Vickers micro-hardness measurements are provided for the first time which revealed that natural silver wires and curls are softer than it might be expected from conversion of the general Mohs hardness of 2.7.
The work focuses on the potential of structural and chemical examinations by scanning electron microscopy based methods for archaeometric studies on ceramics. Achieved by a single preparation technique (polished block sections), the feasibility and benefits of electron backscatter diffraction are demonstrated as case studies using polychrome examples of pre-Columbian pottery (Wari, Moche and Cajamarca). Elemental and phase maps allow for separate consideration of clay and temper. Identification of mineral phases and intergrowths of temper particles provide information for clarifying clay procurement and firing techniques with respect to local versus non-local pottery to enlighten trade relations, technological transfer and shared heritage of pre-Columbian cultures.
We demonstrate the determination of crystal chirality using electron backscatter diffraction (EBSD) in the scanning electron microscope. The chirality of a-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.
We discuss the application of EBSD for the analysis of structural features of magnetite and hematite relevant in the topotactic growth of both phases. The orientation relationships of both phases are investigated using characteristically related sets of Kikuchi patterns, which were collected from topotactically intergrown hematite variants and their parent magnetite crystal grain. We address the hexagonal description of trigonal and cubic phases with respect to crystallographic relationships. The combination of locally resolved EBSD measurements and microstructural investigations thus offers a promising opportunity to evaluate orientation relationships and intergrowth between magnetite and hematite.
An experimental Co-base superalloy was designed from the Ni-base system by exchange of Ni and Co concentrations. The alloy consist of a Co-matrix (γ phase) strengthened by cuboidal precipitates Co3(Al,X) (γ' phase). The γ'-solvus temperature is 1?005?°C. [001] single crystals of this alloy were solidified and tested for tension at different temperatures up to 1?000?°C. It was found that the Co-base alloy has a much lower yield stress than a corresponding Ni-base alloy, but a much higher ductility. The partitioning behaviour of the alloying elements in the Co-base alloy and the deformation mechanisms were investigated by scanning and transmission electron microscopy.
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.
Methodenkopplung mit EBSD
(2012)
Analysis of Kikuchi band contrast reversal in electron backscatter diffraction patterns of silicon
(2010)
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 art exit angle dependent effective crystal thickness in the dynamical electron diffraction calculations. Very good agreement is obtained with experimental observations for silicon at 20 key primary beam energy.