Combined application of electron backscatter diffraction and stereo-photogrammetry in fractography studies

The main aim of this paper is to report on recent experimental developments that have succeeded in combining electron back-scatter diffraction (EBSD) with stereo-photogrammetry, compared with two other methods for study of fracture surfaces, namely visual fractography analysis in the scanning electron microscope (SEM) and EBSD directly from facets. These approaches will be illustrated with data relating to the cleavage plane orientation analysis in a ferritic and C-Mn steel. It is demonstrated that the combined use of EBSD and stereo-photogrammetry represents a significant advance in the methodology for facet crystallography analysis. The results of point counting from fractograph characterization determined that the proportions of intergranular fracture in C-Mn and ferritic steels were 10.4% and 9.4%, respectively. The crystallographic orientation was determined directly from the fracture surface of a ferritic steel sample and produced an orientation distribution with a clear trend towards the {001} plane. A stereo-photogrammetry technique was validated using the known geometry of a Vickers hardness indent. The technique was then successfully employed to measure the macroscopic orientation of individual cleavage facets in the same reference frame as the EBSD measurements. Correlating the results of these measurements indicated that the actual crystallographic orientation of every cleavage facet identified in the steel specimens is {001}.     

Application of combined EBSD and 3D‐SEM technique on crystallographic facet analysis of steel at low temperature

Electron backscatter diffraction has been increasingly used to identify the crystallographic planes and orientation of cleavage facets with respect to the rolling direction in fracture surfaces. The crystallographic indices of cleavage planes can be determined either directly from the fracture surface or indirectly from metallographic sections perpendicular to the plane of the fracture surface. A combination of electron backscatter diffraction and 3D scanning electron microscopy imaging technique has been modified to determine crystallographic facet orientations. The main purpose of this work has been to identify the macroscopic crystallographic orientations of cleavage facets in the fracture surfaces of weld heat affected zones in a well‐known steel fractured at low temperatures. The material used for the work was an American Petroleum Institute (API) X80 grade steel developed for applications at low temperatures, and typical heat affected zone microstructures were obtained by carrying out weld thermal simulation. The fracture toughness was measured at different temperatures (0°C, ?30°C, ?60°C and ?90°C) by using Crack Tip Opening Displacement testing. Fracture surfaces and changes in microstructure were analyzed by scanning electron microscopy and light microscopy. Crystallographic orientations were identified by electron backscatter diffraction, indirectly from a polished section perpendicular to the major fracture surface of the samples. Computer assisted 3D imaging was used to measure the angles between the cleavage facets and the adjacent polished surface, and then these angles were combined with electron backscatter diffraction measurements to determine the macroscopic crystallographic planes of the facets. The crystallographic indices of the macroscopic cleavage facet planes were identified to be {100}, {110}, {211} and {310} at all temperatures.     

Single-section plane assessment in grain boundary engineered brass

The present paper reports a comparative analysis of Σ3 (in the coincidence site lattice notation) grain boundary types, in two grain boundary engineered brass specimens, by use of electron backscatter diffraction (EBSD) data coupled to the measurement of boundary traces in a single section. Although most of the data were analysed using the new single‐section technique, an analysis of boundary plane orientations in three dimensions was made in a subset of the data in order to validate the single section methodology. The single‐section trace analysis procedure, coupled with EBSD, is a viable and robust tool for analysis of Σ3 grain boundary planes. The procedure provides data which suggest that part of the enhanced strain‐to‐failure in specimen B compared to specimen A is the result of an increased proportion of mobile Σ3 boundaries, i.e. those which are displaced from the {111} symmetrical tilt configuration.     

Crystallographic analysis of facets using electron backscatter diffraction

Applications of electron backscatter diffraction (EBSD), also known as backscatter Kikuchi diffraction in the scanning electron microscope (SEM) are first and foremost microtexture and grain boundary misorientation analysis on a single polished section in the specimen. A more subtle and revealing approach to analysis of these data is to use EBSD to probe the orientations of planar surfaces, i.e. facets, which bound crystals. These surfaces include: • grain or phase boundaries • fractures • cracks It is of great interest to know the crystallography of such facets since it provides a key to understanding the physical properties of them.
As far as investigation methodology is concerned, surfaces or facets associated with polycrystals are of two types: exposed or unexposed. Exposed facets, such as a fracture surface, can be viewed directly in the SEM, whereas unexposed facets, such as a grain boundary, are usually revealed as an etched trace on a polished surface. Photogrammetric methods can be used to obtain the positional orientation of an exposed facet, and the crystallographic orientation is obtained either directly from the surface or by indirect sectioning. Calibrated sectioning is required to obtain the equivalent parameters for an internal surface. The present paper compares the methods for obtaining and interpreting the crystallography of facets, with illustrations from several materials.     

Quasi-cleavage fracture planes in spheroidized A533B steel

Electron backscattered diffraction (EBSD) has been used to acquire crystal orientation information around unusual microcracks induced by tensile deformation of notched specimens of spheroidized A533B steel. This unusual fracture mode has been called quasi‐cleavage and occurs at relatively low temperatures with fracture energies below that of the upper shelf. EBSD measurements on sectioned samples showed that the quasi‐cleavage cracks were intragranular. A two‐dimensional analysis technique was used in which EBSD measured crystal orientations were combined with secondary electron imaging to obtain the trace of the crack facet on the section plane. The measurements revealed that the observed crack facets were consistent with crack propagation along the {001} and {011} planes.     

Shear banding in twinned structure of copper deformed at 77 K

The local crystallography and microstructure within shear bands has been examined in single crystals of {112}<111> orientation of pure copper deformed at 77 K by channel‐die compression to true strains of about 1. Setting up a system for making high‐resolution orientation maps using transmission electron microscopy has provided advantageous circumstances for the analysis of orientation changes within shear bands. The present work shows that, despite the plane strain deformation mode, the mechanism of lattice rotation within emerging shear bands may lead to Goss {110}< 001> and Brass{110}<112> texture components.     

Application of electron backscatter diffraction (EBSD) to fracture studies of ferritic steels

The application of electron backscatter diffraction (EBSD) to fracture studies has provided a new method for investigating the crystallography of fracture surfaces. The crystallographic indices of cleavage planes can be measured both directly from the fracture surface and indirectly from metallographic sections perpendicular to the plane of the adjoining fracture surfaces. The results of direct individual cleavage facet plane orientation measurements are presented for carbon–manganese (C–Mn) and low‐alloy Mn–Mo–Ni (similar to ASTM A553 type‐B). Pressure vessel steel weld metals, obtained from fracture surfaces of Charpy impact test specimens fractured at various test temperatures and for an ultra‐low carbon steel (Fe–0.002C–0.058P) fractured at –196 °C by impact. In addition to the direct measurement from the fracture surface, cleavage facet orientation measurements for the ultra‐low carbon steel were complemented by the results obtained from the metallographic sections. Fractographic observations revealed that cleavage fracture is accommodated by a microvoid coalescence fracture micromechanism, which was induced by decohesion of second phase particles (inclusions). The correlation between the direct and indirect methodologies shows that the cleavage facet planes are dominated by the {001} plane orientations, and indicated that even when information concerning the full five degrees of freedom is inaccessible, the cleavage facet plane could still be determined. Finally, the advantages and disadvantages of direct orientation measurements from the fracture surface and indirectly by a destructive sectioning technique are discussed.     

Structure of the (110) antiphase boundary in gallium phosphide

The morphology of antiphase boundaries in GaP films grown by molecular beam epitaxy on Si (001) has been studied by transmission electron microscopy. The inversion of the crystal polarity between antiphase domains was confirmed by convergent‐beam electron diffraction. The APBs were often found to facet parallel to {110} planes. Strong‐beam α‐fringe contrast observed along the (110) facets indicates that adjacent antiphase domains are related by an additional rigid‐body lattice translation. Diffraction‐contrast analysis shows that this R corresponds to a shear parallel to the [001] direction and a small expansion. The magnitude of the translation was inferred, quantitatively, through a comparison between energy‐filtered zero‐loss images of the α‐fringe contrast with numerical calculations. The components of the rigid‐body lattice translation were determined to be 0.023 ± 0.0033 nm in the [001] direction and 0.005 ± 0.002 nm in the 0 direction. Based upon a geometric model of the {110} antiphase boundary, the lengths of the Ga and P antisite bonds were calculated to be 254 ± 2 pm and 227 ± 4 pm, respectively.     

Microstructure evolution and strain localization in Cu and Cu-8Al single crystals subjected to channel-die compression

Single crystals of pure Cu and Cu‐8%Al with two initial orientations, {112}〈111〉 and {112}〈110〉, were subjected to monotonic compression in channel‐die at room temperature (293 K). The dislocation microstructure and local crystallography were investigated by transmission electron microscopy after different amounts of deformation. Various factors, such as initial single crystal orientation, chemical composition and amount of plastic deformation, were analysed in order to determine their influence on the microstructure evolution, local orientation variations and strain localization phenomena.     

Scanning electron microscopy and transmission electron microscopy in situ studies of grain boundary migration in cold-deformed aluminium bicrystals

The crystallography of recrystallization has been investigated in channel‐die deformed pure aluminium bicrystals with {100}<011>/{110}<001> orientations. The microstructural and microtextural changes during the early stages of recrystallization were followed by systematic local orientation measurements using scanning and transmission electron microscopes. In particular, orientation mapping combined with in situ sample heating was used to investigate the formation and growth of new grains at very early stages of recrystallization. Grain boundary migration and ‘consumption’ of the as‐deformed areas was always favoured along directions parallel to the traces of the {111} slip planes that had been most active during deformation.     

Site-specific atomic scale analysis of solute segregation to a coincidence site lattice grain boundary

A site-specific method for measuring solute segregation at grain boundaries in an Aluminum alloy is presented. A Σ7(Σ7=38°〈1 1 1〉) grain boundary (GB) in an aluminum alloy (Zr, Cu as main alloying elements) was evaluated using site-specific Local Electrode Atom Probe (LEAP). A sample containing a Σ7 GB was prepared by combining electron backscatter diffraction (EBSD) and focused ion beam (FIB) milling to locate the GB of interest and extract a specimen. Its composition was determined by LEAP, and compared to a general high angle GB (HAGB). Zr was the only alloying element present in the Σ7 GB, whereas the general HAGB contained both Cu and Zr. This site-specific LEAP method was found to be an accurate method for measuring GB segregation at specific GB misorientations. The method has advantages over other methods of measuring chemistry at GBs, such as spectroscopy, in that GB structure can be assessed in three dimensions.     

Time evolution of sigma 3 annealing twins in secondary recrystallized nickel

Samples of commercially pure nickel have been annealed in air at 0.68T_m (900 °C) for 1, 2 and 3 h in order to study the relationship between the grain growth characteristics and grain boundary misorientation, particularly annealing twins (Σ 3). Orientation mapping by electron backscatter diffraction was used to obtain the experimental data. Anomalous grain growth was observed in commercially pure nickel after each of the anneals. The main findings are as follows. The texture was mainly {100}<001> and {112}<111> and it was more pronounced in coarse-grained areas than in fine-grained areas. The length fraction of Σ 3s (annealing twins) increased with annealing time and therefore with the level of anomalous grain growth. Two to three twins per grain were sited in coarse-grained regions whereas less than one twin per grain was sited in fine-grained regions. It is suggested that the nucleation and growth of twinning is mechanistically linked to anomalous grain growth.     

'Five-parameter' analysis of grain boundary networks by electron backscatter diffraction

This paper describes state‐of‐the‐art analysis of grain boundary populations by EBSD, with particular emphasis on advanced, nonstandard analysis. Data processing based both on misorientation alone and customised additions which include the boundary planes are reviewed. Although commercial EBSD packages offer comprehensive data processing options for interfaces, it is clear that there is a wealth of more in‐depth data that can be gleaned from further analysis. In particular, determination of all five degrees of freedom of the boundary population provides an exciting opportunity to study grain boundaries by EBSD in a depth that was hitherto impossible. In this presentation we show ‘five‐parameter’ data from 50 000 boundary segments in grain boundary engineered brass. This is the first time that the distribution of boundary planes has been revealed in a grain boundary engineered material.     

Microstructure, toughness and flexural strength of self-reinforced silicon nitride ceramics doped with yttrium oxide and ytterbium oxide

Self-reinforced silicon nitride ceramics with additions of either yttrium oxide or ytterbium oxide have been investigated at room temperature after various processing heat treatments. Devitrification of the intergranular phase in these materials is very sensitive to the heat treatment used during processing and does not necessarily improve their strength and toughness. Hot-pressed ceramics without a subsequent devitrification heat treatment were the strongest. The ytterbium oxide-doped silicon nitride ceramics were consistently tougher, but less strong, than the yttrium oxide-doped silicon nitride ceramics. In all the ceramics examined, the fracture toughness showed evidence for R -curve behaviour. This was most significant in pressureless sintered ytterbium oxide-doped silicon nitride ceramics. A number of toughening mechanisms, including crack deflection, bridging, and fibre-like grain pull-out, were observed during microstructural analysis of the ceramics. In common with other silicon nitride-based ceramics, thin amorphous films were found at the grain boundaries in each of the ceramics examined. Arrays of dislocations left in the elongated silicon nitride grains after processing were found to belong to the {101¯0}<0001> primary slip system.     

Texture heterogeneities in αp/αs titanium forging analysed by EBSD-Relation to fatigue crack propagation

The microstructure and the local texture of a large IMI 834 forging were characterized using the Electron Back Scattered Diffraction (EBSD) technique. Crystallographic domains called macrozones and formed by a majority of primary α_p grains with their     axes in nearly the same direction were found. They had a band-like structure, parallel to the axial direction of the forging. The influence of these macrozones on the cold dwell-fatigue properties was studied. Several samples were tested under cold dwell-fatigue conditions. The crack initiation and the short-distance propagation region optically matched a bright region that contained numerous quasi-cleavage facets. The analysis of the EBSD measurements showed that this bright region was enclosed within a sharp textured region with     axes at less than 30° from the loading axis. The crystallographic features of the crack nucleation site and the crack propagation path were also analysed.     

Deformation and Fracture of Single-Crystal and Sintered Polycrystalline Silicon Carbide Produced by Cavitation

An investigation was conducted to examine the deformation and fracture behavior of single-crystal and sintered polycrystalline SiC surfaces exposed to cavitation. Cavitation erosion experiments were conducted in distilled water at 25°C using a magnetostrictive oscillator in close proximity (1 mm) to the surface of SiC. The horn frequency was 20 kHz, and the double amplitude of the vibrating disk was 50 μm. The results of the investigation indicate that the SiC {0001} surface could be deformed, in a plastic manner during cavitation. Dislocation etch pits ware formed when the surface was chemically etched. The number of defects, including dislocations in the SiC {0001} surface, increased with increasing exposure time to cavitation. The presence of intrinsic defects such as voids in the surficial layers of the sintered polycrystalline SiC determined the zones at which fractured grains and fracture pits (pores) were generated during cavitation. Single-crystal SiC had superior erosion resistance to that of sintered polycrystalline SiC.     

First combined electron backscatter diffraction and transmission electron microscopy study of grain boundary structure of deformed quartzite

The structures of boundaries in a deformed and dynamically recovered and recrystallized quartz polycrystal (mylonite) were characterized by transmission electron microscopy, after the misorientation angles across the same grain boundaries had been analysed using electron backscatter diffraction in a scanning electron microscope. In this new approach, a specific sample area is mapped with electron backscatter diffraction, and the mapped area is then attached to a foil, and by the ion beam thinned for transmission electron microscopy analysis. Dislocations in grain boundaries were recognized as periodic and parallel fringes. The fringes associated with dislocations are observed in boundaries with misorientations less than 9°, whereas such fringes cannot be seen in the boundaries with misorientations larger than 17°. Some boundaries with misorientations between 9° and 17° generally have no structures associated with dislocation. One segment of a boundary with a misorientation of 13.5° has structures associated with dislocations. It is likely that the transition from low‐angle to high‐angle boundaries occurs at misorientations ranging from approximately 9° to 14°. Change in the grain boundary structure presumably influences the mobility of the boundaries. In the studied deformed quartz vein, a relative dearth of boundaries between misorientation angles of θ = 2° and θ = 15° has previously been reported, and high‐angle boundaries form cusps where they intersect low‐angle boundaries, suggesting substantial mobility of high‐angle boundaries.     

某船用2.25Cr1Mo钢中P-Mo的晶界共偏聚研究

P元素在晶界的偏聚被认为是导致钢回火脆性的一个重要的原因.Mo作为合金元素会减轻钢的回火脆性.然而,通过对晶界处元素的俄歇测定发现,2.25Cr1Mo钢中P与Mo在晶界处存在共偏聚现象.     

Energy dispersive spectroscopy analysis of aluminium segregation in silicon carbide grain boundaries

The aluminium distribution in polycrystalline SiC hot‐pressed with aluminium, boron and carbon additives was studied using X‐ray energy‐dispersive spectroscopy (EDS) and transmission electron microscopy (TEM). The Al excess in homophase SiC grain boundary films was determined, taking into account dissolved Al in the SiC lattice. In the spot‐EDS analysis, an electron beam probe with a calibrated diameter was formed, and the total beam–specimen interaction volume was defined, taking the beam spreading through crystalline TEM foil into consideration. EDS spectra were collected from regions containing intergranular films and adjacent matrix grains, respectively. A theoretical treatment was presented and experimental errors were estimated, with a further discussion about the effects of foil thickness. Experimental examples are given, followed by statistical EDS analyses for grain boundary films in SiC samples hot‐pressed with increased amounts of Al additions. The results demonstrated a substantial Al segregation in the nanometer‐wide intergranular films in all samples. Al additions higher than 3 wt% saturated the Al concentrations in SiC grains and in grain boundary films. The effect of foil thickness, and the parameters for determining the optimum incident beam diameter in the EDS analysis are discussed.     

Three-dimensional EBSD study on the relationship between triple junctions and columnar grains in electrodeposited Co–Ni films

Electrodeposited nanocrystalline materials are expected to have a homogeneous grain size and a narrow grain size distribution. In Co–Ni electrodeposited films, however, under certain conditions an undesired columnar grain structure is formed. Fully automated three‐dimensional (3D) orientation microscopy, consisting of a combination of precise material removal by focussed ion beam and subsequent electron backscatter diffraction (EBSD) analysis, was applied to fully characterize the grain boundaries of these columnar grains in order to gain further understanding on their formation mechanisms. Two‐dimensional orientation microscopy on these films indicated that the development of columnar grains could be related to the formation of low‐energy triple junctions. 3D EBSD allowed us to verify this suggestion and to determine the boundary planes of these triples. The triplets are formed by grain boundaries of different quality, a coherent twin on the {} plane, an incoherent twin and a large‐angle grain boundary. These three boundaries are related to each other by a rotation about the 〈〉 direction. A second particularity of the columnar grains is the occurrence of characteristic orientation gradients created by regular defects in the grain. Transmission electron microscopy was applied to investigate the character of the defects. For this purpose, a sample was prepared with the focussed ion beam from the last slice of the 3D EBSD investigation. From the TEM and 3D EBSD observations, a growth mechanism of the columnar grains is proposed.