Application of Electron Back Scatter Diffraction

Electron Diffraction Subcommittee 22 March 2007 Ray Goehner
Call to Order R. Goehner provided comic relief in the form of a brief Dilbert cartoon. Appointment of Minutes Secretary T. Kahmer Board of Directors Liaison Report Motions presented to the board in March 2006, and their responses. - Not read. Confidential information on record at ICDD. Business R. Goehner gave a presentation of how electron diffraction is used for phase identification. Presentation follows the minutes. Backscattered Electron Kikuchi Patterns BEKP Electron Backscatter Patterns EBSP Backscattered Kikuchi Diffraction BKD Wide Angle Kikuchi Patterns WAKP T. Fawcett will contact the editor of International Materials Reviews and ask for permission to put a copy of the article, Application of electron backscatter diffraction to the study of phase transformations, 2007 vol. 52 no. 2, pp 65-128, on the ICDD web site. Article follows the minutes. There was some discussion on primary and alternate codes, particularly in the case of silicon dioxide because of its many polymorphs. J. Friel volunteered to be our spokesperson for the community. He will try to get a focal group of ~six people together for a conference call to discuss how to get this project started. There is a meeting in aluminum industry in May. J. Friel will most likely get to speak with Scott Sitzman of HKL and Stuart Wright from EDAX. HKL has a lot of information on their website that shows techniques and it explains the phase map, i.e., different colors with different phases. They offer three databases with their product. T. Fawcett and J. Faber talked to Dawn Janney (a new ICDD member from Idaho National Laboratory). She bought a PDF-4+ and was excited about it. She gave input in how to enhance the product for electron diffraction. Adjournment
EBSD in the SEM for the Identification of Unknown Crystalline Phases

DXC 2004 Workshop Principles & Use of Microdiffraction & Microfluorescence
Ray Goehner & Joe Michael Sandia National Laboratories Albuquerque, NM 87185-0886
Sandia is a multiprogram laboratory operated by Sandia Corporation, a Lockheed Martin Company, for the United States Department of Energy under contract DE-AC04-94AL85000.
EBSD Pattern of AlB2

Pattern Features: Parallel lines are Kikuchi line pairs Spacing between pairs is twice the Bragg angle and inversely related to the dspacing Places where lines intersect is called zone axis Angles between zone axes are indicative of crystal structure Angles made by Kikuchi line pairs about a zone axis are the interplanar angles of the crystal
AlB2 (20 kV)
History of EBSP
Backscattered Electron Kikuchi Patterns BEKP Electron Backscatter Patterns EBSP Backscattered Kikuchi Diffraction BKD Wide Angle Kikuchi Patterns WAKP First observed in 1954 - before SEM invented 1970s Venables et al. were first to observe EBSP in SEM 1980s Dingley et al. began using these patterns for orientation studies 1990s Wright and Adams developed automatic system for texture (OIM) Michael & Goehner. develop technique for phase identification
Cameras for EBSD Typical Arrangement
Pole piece
Sample surface
Phosphor screen
Not much room in the sample chamber!
Installation on a Dual Beam FIB
Most SEM sample chambers present challenges to installation of EBSD cameras. But, it can usually be done with a little bit of compromise.
Effect of Sample Tilt on BS Electron Yield
# Backscattered electrons
0
10
20
30
Energy (kV)
Tilted sample has higher BS electron yield Sample tilt results in sharp peak in BS electron energy distribution. Better defined energy of BS electrons results in sharper Kikuchi lines.
Alumina (Al2O3) On Thin Substrate
Ag on MgO Example of EBSD Resolution

Orientation map of Ag particle normal direction
SEM images of Ag particles on MgO substrate
Applications of BEKP to Materials

Two Areas of application for BEKP: Orientation Analysis crystallographic orientation of small areas use patterns to calculate the relationship between the crystallographic axes some external reference frame ( i.e. rolling direction) use patterns to determine the crystallographic relationship between two adjacent areas of the sample (i.e. grain boundary misorientation, precipitate/matrix orientation) Micro-texture imaging of polycrystalline samples with automated pattern indexing (called orientation imaging microscopy OIM) Phase Identification Identify unknown phases from their crystallography Bulk samples (metallographically polished surfaces) Particulate on substrate (no preparation needed) Fracture surfaces (identify phases directly on fracture surfaces)
EBSD Analysis of 11 m Diameter W wire
Microscope conditions: 20 kV, 6 nA beam current Note the very strong <110> fiber texture developed in the wire. This is a tpical texture for BCC wire drawing.
Conventional Approaches to Phase Identification

How do we answer the What is it? question? Chemistry only through EDS may not give correct answer when phases of similar composition are present. Combination of XRD and EDS may work if we have sufficient amounts of material.
EBSD and EDS in the SEM Powerful combinations of techniques with high resolution and the ability to separate compounds of similar composition.
How? Observe symmetry elements in pattern Use angles between planes and composition to search data base Use composition and unit cell volume to search a database
Symmetry elements in EBSD pattern

4mm m m m m
m m m 3m m
Point group m3m 43m 432 <111> 3m 3m 3 <100> 4mm 2mm 4 <110> 2mm m 2 <uu0> m 1 1
2mm
m
<uuw> m m 1 <uvw> 1 1 1
The EBSD pattern show symmetry consistent with m3m (cubic).
Symmetry elements in EBSD pattern
Can identify 27 of the 32 point groups using this approach Distortions of gnomonic projection can add difficulty Generally difficult and time intensive process Becomes more complex for lower symmetry crystal structures Once we have the point group we can begin to infer space group For more information see paper : Baba-Kishi and Dingley, Backscatter Kikuchi diffraction in the SEM for identification of crystallographic point groups, Scanning, vol.11, 1989, p. 305
Phase identification using databases

We really need the qualitative chemistry to achieve phase identification
Use of EBSD pattern and chemistry: Determine chemistry and acquire EBSD pattern Search database based only on composition Phases that match chemistry are then compared to EBSD patterns by simply calculating angles between planes and indexing
Use of EBSD pattern, chemistry and unit cell volume: Determine chemistry and acquire EBSD pattern Analyze EBSD pattern and calculate unit cell volume Search database based on unit cell volume and chemistry Candidate matches are used to index EBSD pattern
Phase Identification - How it is done

Obtain pattern from area of interest. Use EDS to determine chemistry. In this case the EDS showed the presence of Fe, As and S.
Search ICDD PDF for matches based on chemistry and unit cell volume
In this example Arsenopyrite was the only match out of 100,000 compounds in the database

Index pattern based on database information. Index pattern using the angles between the planes selected by the Hough Transform.
Simulate pattern and compare. A good match at this step is an excellent indication that the phase has been identified.
Identification of Phases on Fracture Surfaces with EBSD
Ferrite
30 m The ocurence of hot cracks in stainless steel welds is related to the phases present in the weld. EBSD is the only technique that can directly provide this information.
Austenite
Ni-Gd Phase Diagram

1600
1487C
1400
1313C
(Gd)
1455C
1280C
1270C 1200C 1110C
1285C 87
1275C
1200
1235C
1000
1010C
(Gd)
(Ni) 880C 33
800
735C 635C
Gd 3Ni
Gd 3Ni 2
Gd 2Ni 7
GdNi2
GdNi3
GdNi4
Gd
20
40
60
GdNi5
GdNi
600
Gd 2Ni17
14
80
100
Wt% Nickel
Ni
Phase Identification in an Ni-Cr-Mo-W-Gd alloy

EDS shows presence of Ni and Gd
10 m
EDS shows presence of Ni and Cr
Sample was prepared by standard metallographic techniques. No etch has been applied.
Phase Identification in an Ni-Cr-Mo-W-Gd alloy
Gd-Ni phase is identified as GdNi5 (hexagonal)
Identification of Phases in a Gd modified 304 Stainless Steel Alloy

Sigma (FeCr) 5.84 wt% Gd
Austenite
Ferrite (Ni,Fe)3Gd
Ferrite
Microstructures are complex The secondary rim and the associated gadolinides could not be identified
Fracture of Ta Alloy Weld

Welded component fractures along grain boundaries in the weld region.
Higher magnification shows a wide grain boundary region with precipitates. EDS shows that the grain boundary region contains only Ta and the precipitates contain Hf.
Fracture of Ta Alloy Weld (cont.)
6 possible matches Hf3N2 Trigonal (2.14% error) HfO2 Monoclinic (2.25% error) HfO2 Tetragonal (1.64% error)
HfO2 HfO2 HfO2
Orthorhombic (6.47% error) Monoclinic (1.95% error) Monoclinic (1.95% error)
Fracture of Ta Alloy Weld (cont.)
Precipitate identified as monoclinic HfO2
Particle Identification - Non-volatile Memory Fabrication
Particles formed on Ru barrier layer
EBSP collected from facet on particle . EDS showed that the particle contained Ru and O.
Pattern analyzed and crystallographic database searched. The only match that was identified was RuO2 a tetragonal phase with unit cell dimensions of 0.4499 nm and 0.6906 nm. The indexed pattern is shown at right.
Unknown Mineral Identification
SE
BSE
Patterns obtained at 20 kV from phase containing Pb and O. Database search yielded 7 possible matches. Automated phase identification selected Plattnerite (PbO2), a tetragonal phase, as the correct identification based on chemistry, unit cell volume and pattern simulation.
JRM 971022
HOLZ Rings in EBSD
Mo2C (Hexagonal a = 0.3012 nm c = 0.4735 nm)
Fe3C (Orthorhombic a = 0.5091 nm b = 0.6743 nm c = 0.4526 nm)
Higher Order Laue Zone Analysis of BEKPs

H = spacing of planes in reciprocal space 1/H = spacing of the planes in real space H = k(1-cos 2) = 2k(sin2 ) where k = 1/
1/
Hematite (Fe2O3)
5 kV
10 kV
20 kV
kV 5 10 20 H-1 0.543 0.544 0.544 0.541 0.544 error % 0.05 0.19 0.30 0.38 0.19
25 kV
30 kV
25 30
Actual H-1 for [211] 0.5427 nm
HOLZ Ring Analysis of Chromium Carbide
HOLZ ring around [001] used HOLZ [ 001] Spacing measured normal to [001] is 1.074 nm. The spacing of planes normal to [001] in Cr23C6is 1.067 nm, an error of 0.7%.
HOLZ Ring Measurements for SiC Polytype Identification

H-1 = 1.858 nm
H-1calc= 1.846 nm
H-1
= 1.545 nm
H-1calc= 1.538 nm
HOLZ spacing identifies left pattern as SiC 6H and right pattern as SiC 15R. Consistent with the symmetry observed in the patterns.
Primitive Unit Cell Calculation Any three primary vectors in the EBSP define a arbitrary unit cell representative of the Bravais lattice If these vectors are obtained from Kikuchi lines, the cell determined is a reciprocal cell If these vectors are determined from HOLZ ring measurements, the cell is a direct cell
Use cell reduction algorithm and the arbitrary cell to determine unique primitive reduced unit cell representative of the metric unit cell. References:
A. Santoro et al., Acta Cryst. (1980) A36, p. 796. B. Gruber, Acta Cryst. (1989) A45, p 123. Y. Lepage, Microscopy Research and Tech., (1992) 21,p. 158.
HOLZ Rings for Primitive Cell Calculation

Hmeas= 0.576 nm Hcalc = 0.57704nm 2
Hmeas= 0.645 nm Hcalc = 0.6443 nm
4 Hmeas= 0.822 nm Hcalc = 0.8089 nm 3
Hmeas= 0.837 nm Hcalc = 0.8581 nm
Measured angles between directions: 1-> 2 = 56.1 1->3 = 44.5 2->3 = 66.8
HOLZ Rings for Primitive Cell Calculation

Unit cell from HOLZ Rings: a = 0.82 nm b = 0.65 nm c = 0.65 nm = 56.1 = 44.5 = 66.8 = 89.4 = 112.0 = 89.0
Primitive unit cell from reduction : a = 0.58 nm b = 0.58 nm c = 0.58 nm volume = 179 3
Primitive Unit cell for AsFeS : a = 0.5741 nm b = 0.5668 nm c = 0.57704 nm volume = 174.1 3 = 90 = 111.93 = 90.0
Primitive Unit Cell Determination of Mo 2C (hexagonal)

Zone 2 H-1 = 0.56 nm Angles between zones: 1 -> 2 = 32.0 2 -> 3 = 24.3 3 ->1 = 47.3 Arbitrary Unit Cell: a = 0.71 nm b = 0.56 nm Zone 3 H-1 = 0.71 nm c = 0.48 nm
Zone 1 H-1 = 0.48 nm
= 32.0 = 47.3 = 24.3
Primitive Unit Cell Determination of Mo 2C (hexagonal)

Primitive Unit Cell: a = 0.30 nm b = 0.30 nm c = 0.48 nm Published Unit Cell: a = 0.3012 nm b = 0.3012 nm c = 0.4735 nm
= 88.2 = 89.1 = 118.7
= 90 = 90 = 120
Cell volume = 37.0 3
Cell volume = 37.1 3
Primitive Unit Cell Determination - HOLZ Rings are not required

Primitive Unit Cell from HOLZ Rings a = 0.26 nm = 107 b = 0.27 nm =107 c = 0.27 nm = 111 volume = 15.3 3 Primitive Unit Cell from Kikuchi Lines a = 0.27 nm = 106 b = 0.28 nm = 108 c = 0.29 nm = 111 volume = 15.9 3 Primitive Unit Cell for Mo a = 0.272 nm = 109.47 b = 0.272 nm = 109.47 c = 0.272 nm = 109.47 volume = 15.6 3
Primitive Unit Cell Determination From Kikuchi Line Pairs
Primitive Unit Cell from Kikuchi Lines a = 0.24 nm = 61 b = 0.24 nm = 61 c = 0.24 nm = 61
volume = 10.1 3 Primitive Unit Cell for Ni a = 0.248 nm = 60 b = 0.248 nm = 60 c = 0.248 nm = 60 volume = 10.9 3
Summary
The SEM is now a more complete tool due to the addition of EBSD to the imaging and microanalysis techniques previously available.
EBSD is a robust and reliable technique for the identification of crystalline compounds: Use of diffraction databases allows phase identification HOLZ ring analysis ( with proper attention to details) can be used to determine reciprocal layer spacing Reduced cell algorithm produces recognizable primitive cells using HOLZ rings (better) or Kikuchi lines ( not as good) These cells may be used to search existing structural databases
Application of electron backscatter diffraction to the study of phase transformations

A. F. Gourgues-Lorenzon*
The application of the electron backscatter diffraction technique to the investigation of phase transformations is reviewed. The wide variety of results obtained using this technique is illustrated and discussed, focusing on thermodynamics and kinetics of phase transformations, solidification, solid state phase transformations, environmentally assisted reactions and thin film deposition. Emphasis is also placed on two rapidly growing developments: coupling electron backscatter diffraction with advanced experimental techniques and with more and more complex modelling of phase transformations and of resulting material properties.
Keywords: Electron backscatter diffraction, Scanning electron microscopy, Phase transformations
List of abbreviations and symbols

ACOM bcc BKDP CET EBSD EDX fcc FEG FIB GB GBE HAB HAZ hcp HOLZ KS LAB MR NW ODF OIM OR PTMC SEM SMA TEM TRIP WM XRD 2D 3D automated crystal orientation measurements body centred cubic (crystal structure) backscatter Kikuchi diffraction pattern columnar to equiaxed transition (solidification) electron backscatter diffraction energy dispersive X-ray spectrometry face centred cubic (crystal structure) field emission gun focused ion beam grain boundary grain boundary engineering high angle boundary heat affected zone (welding) hexagonal close packed (crystal structure) higher order Laue zone KurdjumovSachs (see Appendix) low angle boundary misorientation relationship (between product phases) NishiyamaWassermann (see Appendix) orientation distribution function (texture) orientation imaging microscopy orientation relationship (between parent and product phases) phenomenological theory of martensite crystallography scanning electron microscope (or microscopy) shape memory alloy transmission electron microscope (or microscopy) transformation induced plasticity weld metal X-ray diffraction two-dimensional three-dimensional
Introduction
The electron backscatter diffraction (EBSD) technique, also termed automated crystal orientation measurements (ACOM), orientation imaging microscopy (OIM) and the Backscatter Kikuchi diffraction pattern (BKDP) technique, is utilised to determine the local crystal structure and orientation of materials. It makes full use of the versatility and multiscale capability of the scanning electron microscope (SEM). The principles and applications of the technique can be found elsewhere (e.g. Schwartz, 2000; Dingley, 2004) and will be only shortly recalled here. Before leaving the material, backscattered electrons diffract at crystal lattice planes in the probe area. They are then intercepted by a phosphor screen (Fig. 1). Owing to Bragg diffraction conditions and to the sample to screen distance, bands centred on diffracting planes are observed. By measuring the location and spatial orientation of such bands one can either determine the crystal structure or, if the crystal structure is known, crystal orientation. The spatial resolution is about 1050 nm parallel to the tilt axis, depending on the sample and operating conditions (Humphreys, 1999 and 2004; Dingley, 2004). The angular accuracy of measurements is y1 and y0.5u for misorientation between neighbouring areas (Dingley, 2004; Humphreys, 2004) and can be improved down to y0.1u for particular applications if special care is taken (Humphreys, 2004). The technique has been developed since the 1970s (Venables, 1973) and automatic mapping has been readily available for about ten years. The EBSD is used to investigate, e.g. texture and recrystallisation (Jazaeri et al., 2004), deformation mechanisms and local strains (Lehockey et al., 2000; Wilkinson, 2000), interface characterisation (Randle, 2004) and cracking (Gourgues, 2002). Through cooperation between EBSD system providers and users, the technique has strongly developed in the past few years, including a dramatic increase in data acquisition speed thanks to digital cameras, increasing complexity of data processing to extract more information from EBSD
Ecole des Mines de Paris, Centre des Materiaux PM Fourt, UMR CNRS 7633, BP 87, 91003 Evry cedex, France *Corresponding author, email [email protected]
2007 Institute of Materials, Minerals and Mining and ASM International Published by Maney for the Institute and ASM International DOI 10.1179/174328007X160254
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(a)
(b)
a Electron diffraction according to Braggs law (2dhklsinh5nl); b EBSD pattern from a bainitic steel (bcc crystal structure) 1 Principle of EBSD analysis
generally to phase transformations in open literature, while the number of published studies is signicant (to give a gure, more than 700 papers were read to write the present review). The present review aims to survey how EBSD is used to address phase transformations. In this eld, EBSD has mainly been used so far to revisit a number of features concerning phase transformations, the variety of which is illustrated below, and for which crystallographic data were already available. This both validates the EBSD technique and provides a signicant number of data with rather simple sample preparation. The EBSD can now be used as a reference technique, yet with limits that are discussed below, to investigate phase transformations in the future. Original results obtained with EBSD that were not accessible using other techniques are also reviewed, highlighting specic advantages of EBSD in a number of cases. The review is organised according to transformation mechanisms, using tabular form in many cases for clarity. First, information is given on basic phenomena related to phase transformations (phase identication, thermodynamics and kinetics). The next two sections are devoted to solidication and solid state phase transformations respectively. Then, surface phenomena such as environmentally assisted reactions and thin lm deposition, which are of increasing practical interest, are addressed. In the last section, coupling of EBSD with other experimental techniques and with numerical modelling is discussed, illustrating promising ways to obtain better insight into phase transformation phenomena.
data, including new pattern and map processing algorithms (Wright and Nowell, 2006; Brewer et al., 2006), coupling with chemical information or even reconstructing parent grains as will be discussed below. First reviews involving EBSD addressed a variety of topics, often illustrated with a few examples (Dingley and Randle, 1992; Mason and Adams, 1994; Randle, 1994). Up to now, the number of papers mentioning EBSD is growing very rapidly (typically multiplied by two every year), showing that EBSD is now a routinely used technique available in many laboratories. Thus, many reviews focused on one specic topic, such as applicability of EBSD to ceramic materials (Farrer et al., 2000), data collection and processing (e.g. Wright et al., 2000), recent developments of the technique (Dingley, 2004) and studies involving high spatial resolution (Humphreys, 2004). Only few review papers addressed the application of EBSD to phase transformations. This topic is not new but it has developed only gradually. In the rst review by Dingley and Randle (1992) only three examples of studies on multiphase materials were given. Applications of EBSD to solidication (Mason and Adams, 1994) and to phase identication (Randle, 1994) then began to develop. Most detailed reviews on topics close to phase transformations addressed phase identication (Schwartz et al., 2000; Baba-Kishi, 2002). The present author did not nd any review paper addressing applications of EBSD to solidication and more
Phase identification and basic phenomena related to phase transformations

Phase identification
Electron backscatter diffraction can be a powerful tool for phase identication, in particular for new or complex crystal structures or for mineral materials. The EBSD is complementary to longer established techniques based on transmission electron microscopy (TEM), X-ray diffraction (XRD) and even light optical microscopy in the case of minerals.
Crystal structure identification
This topic has been thoroughly addressed in the review by Baba-Kishi (2002). Here, more recent results and results using other techniques together with EBSD are discussed. The main advantage of EBSD versus local XRD (such as Kossel or pseudo-Kossel analysis) is its ability to perform rapid analysis, with high spatial resolution, at the expense of accuracy in crystal orientation and lattice parameter determination (Goehner and Michael, 1995; Dabritz et al., 2001). Lattice parameters can be evaluated either from the band width (which is proportional to the sine of the corresponding Bragg angle) or from the size of higher order Laue zone (HOLZ) rings in EBSD patterns (Baba Kishi, 2002). The accuracy of measurements depends on data acquisition conditions and on the chemical composition of the analysed area. By using HOLZ rings it can be better than 1%, if care is taken to correct for
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distortions due to the gnomonic projection or to atomic number (Baba-Kishi, 1998; Michael, 1999 and 2000; Michael and Eades, 2000). However, for elements such as Mo or W, the error is still about a few per cents (Michael and Eades, 2000). The location of HOLZ rings in EBSD patterns can also be used to distinguish between polytypes, in particular in clay minerals (Kogure et al., 2005). Using the band width gives lower accuracy [typically a few per cents (Michael and Goehner, 1993)] even with increasing the specimen to screen distance or optimising the indexing algorithm (Vatne et al., 1998; Dingley, 2004). Extinction effects (Michael and Eades, 2000) and cell multiplicity (Vaillant et al., 2003) must be taken into account. The feasibility of EBSD assisted phase identication (e.g. Michael and Goehner, 1993) essentially depends on the signal to background noise ratio (Small et al., 2002), on background acquisition (Michael, 2000; Small and Michael, 2001) and on relief effects (Michael, 2000), not much on the yield of backscattered electrons (Small and Michael, 2002). Therefore, good results can be obtained with extraction replicas [e.g. for PbO2 (Michael, 2000) and U3O8 (Small and Michael, 2001)]. Particles over about 0.31 mm in size can be readily analysed with EBSD (Straumal et al., 1999; Small and Michael, 2001). Crystal symmetry has been addressed with EBSD for a long time (Baba-Kishi, 2002). 27 out of the 32 point groups can be identied using EBSD patterns. Identication methods of point and space groups are detailed elsewhere (Baba-Kishi and Dingley, 1989; Michael 2000; Baba-Kishi, 2002). This eld has still been developed since these review papers [(see e.g. Kral et al., 2004) for iron rich phases in an AlSi alloy], in particular for minerals and quasicrystals. Superstructures of ordered intermetallic phases such as the L10 c phase in TiAl alloys are difcult to investigate by rapid, automated analysis, so that they are often ignored if the distinction between them is not of utmost importance for the considered application (Pouchou et al., 2004b). Special attention has been paid to minerals for many years (e.g. Dingley, 1984; Leinum et al., 2004) and in particular to polytype identication. Kogure (2003) developed a method based on band location and intensity, still using kinematic theory of electronmatter interactions, which shows recognisable patterns characteristic of each polytype. This method gives good results for phyllosilicate minerals (Kogure, 2002 and 2003; Kogure and Bunno, 2004; Kogure et al., 2005). Others established robust reection tables (i.e. extinction conditions) as e.g. for omphacite (Mauler et al., 1998). Identication of quasicrystal structures still generally requires manual indexation of patterns [e.g. for Al60Cu26Fe14 (Cheung et al., 2001)]. Special care must be taken to check the symmetry (including from inside the bands) around zone axes, to distinguish true quasicrystals from their crystalline approximants (Ruhnow et al., 2002).
Coupling EBSD with chemical analysis
for off stoichiometry phases and for phases having identical or similar chemical compositions but different crystal structures (Camus, 2000; Kogure, 2002; Boettinger et al., 2003; Kogure and Bunno, 2004; Kral et al., 2004; Leinum et al., 2004). Up to date available systems now combine both crystallographic and chemical analysis for automated phase identication (Michael, 2000; Dingley, 2004; Nowell and Wright, 2004; Zhong et al., 2006). For rapid data acquisition and processing, the location of bands in the EBSD pattern is stored for each data point, together with chemical analysis. The chemical composition is then used to index every pattern in an ofine manner. This is especially useful when the identity of phases is not known in advance, or if data collection must be rapid (e.g. for in situ investigations). The spatial resolution is limited, however, to that of EDX analysis (y1 mm), both for in plane dimensions and along the sample normal.
Distinguishing between known phases
Energy dispersive X-ray spectrometry (EDX) microanalysis is frequently available in the SEM together with the EBSD facility, allowing combination of chemical and crystallographic information (although optimised operating conditions are not the same). Starting from sequential analysis of the same area, EBSD can be used to facilitate EDX-based phase identication, especially
Minerals have been studied with EBSD due to their frequently low crystal symmetry and to the wide collection angle (y90u) provided by this technique. In some instances, a list of reections needs to be rst calculated or corrected and then given to the EBSD system [e.g. omphacite in eclogite minerals (Mauler et al., 1998) and AlSiO triclinic phase in kyanite (Dingley et al., 2004)]. In some cases manual adjustment is still necessary to insure right indexation of the EBSD patterns [e.g. garnets and sulphides (Prior et al., 1999)]. While researchers in the past had to work with lms to improve sensitivity and image contrast (Dingley, 1984), new digital cameras now allow online working in the SEM. The case of polytype minerals involves both numerical calculation of the patterns and visual identication of individual patterns, provided that crystals are suitably oriented (Kogure, 2002 and 2003; Kogure et al., 2002 and 2005; Kogure and Bunno, 2004; Kameda et al., 2005). In many cases, technical improvements of EBSD cameras allow switching from manual to automated EBSD [e.g. for iron ore and sinter (Magalhaes, 2002; Sasaki et al., 2005a)]. Advantages and challenges of using EBSD to investigate ceramic materials have already been reviewed (Farrer et al., 2000) and will not be recalled here. Recent studies addressed an increasing variety of materials such as oxides (Michael and Goehner, 1993; Rogers et al., 1994; Randle, 1994; Korte et al., 2000; Cha et al., 2006), functional materials [YBCO (Koblischka et al., 2003; Koblischka-Veneva et al., 2003)], zeolites (Pennock et al., 2001), PbTiO3 domains (Yang et al., 1994), silicon (Her et al., 2000), eutectic bres (Nakai et al., 2005; Lee et al., 2005), materials for nuclear applications (Medevielle et al., 1999) and applications are still rapidly growing. As an illustration, example studies of quasicrystals and metallic glasses are reported in Table 1. Phase identication is also useful to understand in situ synthesis of composites through interfacial reactions. Good examples are given by AlN/Ti composites leading to several (Ti,Al)Ny nitrides (Paransky et al., 1999, 2000a and 2000b) and by sintered WC/VC/TiC/Co cermets (Arenas et al., 2005). Alignment of strengthening particles during composite processing (Schuh and Dunand, 2001), formation of intermediate phases during transient liquid phase bonding of a Ni base superalloy (Jalilian et al., 2006) and carbide formation in SiC/Ti
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alloy lamentary composites (Duda and Gourgues, 2006) were also investigated with EBSD. As SEM is much easier on electron conducting samples, most EBSD studies have yet been carried out on metals and metal alloys. Besides many others, some specically address phase identication, as for example identication of small precipitates [e.g. NiSn4 (Boettinger et al., 2003), MX particles in Ni base alloys (Ramirez and Lippold, 2004), discontinuous precipitates in ancient components (Wanhill, 2005) and Laves phases in austenitic alloys (Michael and Goehner, 1994; Robino et al., 1997)], of topologically close packed precipitates in tempered weldments (El-Dasher and Torres, 2004), of eutectic aggregates in a Ni base alloy (DuPont et al., 1999) and of complex/multilayered aggregates of phases (Levin et al., 2000; Gomez and Echeberria, 2003; Nolze et al., 2005). First principles calculations have been used to nd crystal structures and lattice parameters for further automatic indexing of EBSD patterns [e.g. in newly discovered Al2(Mg,Ca) ternary Laves phases (Zhong et al., 2006)]. The case of alloys particularly difcult to investigate such as PuGa alloys (Boehlert et al., 2001) and cerium (Boehlert et al., 2003a) should be mentioned. Analysis of EBSD also allows convenient phase separation on fracture surfaces (not readily available with TEM) (Foct and Akdut, 1993; Bache et al., 1997a and 1997b) and for texture determination (not always easy by XRD) (Xu and Russell, 2004; Dunst and Mecking, 1996). The EBSD can also facilitate evidence of phase transformation (Sano et al., 2003b; Neishi et al., 2004; Zhu, 2004). Discrimination by EBSD between phases having close or even identical crystal structures is difcult. In some cases, the lattice parameter is used [e.g. to separate g9T from e in ZnAlCu alloys (Zhu et al., 2001, 2003a and 2003b)]. In other cases, the quality of the patterns is much better in one phase than in the other [e.g. ferrite v. martensite (Wilson et al., 2001; Wilson and Spanos, 2001; Jeong et al., 2002a and 2002c; Petrov et al., 2004; Cabus et al., 2004b; Wu et al., 2005), and ferrite v. bainite (Regle et al., 2004) in steels]. Primary and secondary a phases in a titanium alloy (Germain et al., 2005a) were distinguished using backscattered electron
imaging. An alternative method using light optical microscopy was also developed (Thomas et al., 2005). Discrimination between such phases also allows mapping spatial and size distribution of them (see e.g. Schwarzer et al., 2000).
Equilibrium phase diagram assessment

Rapid phase identication by EBSD, together with assessment of properties of individual constituents by local measurements has recently been reviewed in the framework of diffusion multiples (Zhao, 2006). With this technique, a whole isothermal section of one (or several) ternary diagram can be assessed after only one long term heat treatment. This has been applied to various ternary alloys, assuming local equilibrium at interfaces. However, the effect of local crystallography on diffusion and on phase nucleation was not discussed (Zhao et al., 2001, 2002, 2003, 2004a, 2004b; Zhao, 2004; Zhong et al., 2006). Modication of existing phase diagrams can be suggested by EBSD results [e.g. for 1200 and 1600uC isothermal sections of the quaternary MoTiSiB diagram (Yang et al., 2005)]. Application of EBSD to local adjustment of the liquidus surface of the TiAl(Nb) system is illustrated by identication of the solidication sequence (Takeyama et al., 2004). Except for this latter case, EBSD was mostly used as a complementary technique to discriminate between phases having complex and close chemical compositions but different crystal structures. Rapid mapping facilities that are now available should put EDX plus EBSD as leading experimental techniques for phase diagram investigations in the next future.
Electron backscatter diffraction and kinetic issues of phase transformations

Anisotropy of free surface and interfacial energy
Free surface energy The equilibrium shape of single crystals is a good translation of free surface energy into a measurable property. Provided that crystals are suitably oriented with respect to the SEM, surface planes can be indexed with EBSD, as e.g. ZnO well faceted bres (Huang et al., 2004), clay minerals (Kogure et al., 2005; Kameda et al.,
Table 1 Phase identication assisted by EBSD in quasicrystals and metallic glasses Material Phases of interest Phase identification method Results Ref. Gui et al., 2001 Cheung et al., 2001
Crystal orientations, orientation relationships between phases Structural model of the icosahedral phase consistent with TEM results AA6013 Al alloy Fe rich phase Symmetry in EBSD Not a quasicrystalline patterns, comparison phase but crystalline with XRD results approximant Point analysis Identification of phases, AlCuFeB b-Al(Cu,Fe) (CsCl), Fe2AlB2 (body centred orthorhombic), quasicrystalline orientation relationships matrix between phases Automatic indexing with Identification of this FeCoZrMoWB ZrB2 (hexagonal) various crystal structures residual crystalline metallic glass and lattice parameters phase ZrCuAlNi metallic ZrCuAlNiO [face centred cubic Use of band width Identification of phase glass (fcc)] stemming from oxygen contamination
EBSD z EDX Cast AlCuFe alloys b-Al(Cu,Fe) (CsCl) Cu rich phases, e phases, icosahedral quasicrystalline and R phases, l-Al13Fe4 dendrites Cast Al20Cu15Fe Al60Cu26Fe14 (icosahedral), b-Al(Cu,Fe) Manual indexing and (CsCl), near-l Al44Cu54Fe2 use of Kikuchi atlas (at.-%)
Ruhnow et al., 2002 Brien et al., 2004 Castellero et al., 2004 Vaillant et al., 2003
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2005) and tape cast ceramics (Markondeya Raj et al., 1999). Surface energy of SrTiO3 perovskite has been investigated by trace or 3D plane analysis after both thermal grooving (Sano et al., 2003a) and coarsening with TiO2 rich liquid (Sano et al., 2005). Interface migration assisted by an amorphous phase has been studied in sapphire single crystals bonded to sapphire polycrystals as a function of the local orientation of free surface planes (Farrer et al., 2006). Relative energies of low index planes can be rather easily compared by this way with minimum sample preparation and on a larger data basis compared with TEM techniques. On the other hand, assumptions have to be made to accurately determine the spatial orientation of the free surface planes (see Discussion). Internal interfaces Interfaces are good candidates for heterogeneous phase nucleation, depending on their free energy. Electron backscatter diffraction has been used in many ways in this eld. Interface wetting [e.g. Zn by Ga (Traskine et al., 2005), partially molten olivine aggregates (Faul and Fitz Gerald, 1999)] involve classication of dry and wet interfaces according to e.g. the misorientation angle between neighbouring crystals (this being readily accessible with EBSD). The effect of lattice coincidence in these two cases is not obvious. The same result was obtained with solid state spreading of copper on copper substrate (Missiaen et al., 2005). Thermal grooving coupled with EBSD and near eld microscopy gives access to interface energy anisotropy. Here again, coincidence site lattice criteria fail to qualitatively compare values of various grain boundary energies [e.g. in MgO (Saylor and Rohrer, 1999) and NiAl (Amouyal et al., 2005)]. In the latter case, the boundary energy correlates with none of usual criteria such as coincidence site lattice, misorientation angle, tilt v. twist character or plane boundary matching. Segregation of solute atoms to boundaries has also been investigated with EBSD in hydrogen containing Al5Mg alloy (Horikawa and Yoshida, 2004) and Nb doped rutile (TiO2) (Pang and Wynblatt, 2006). Coincidence site lattice boundaries are often resistant to solute atom segregation and thus to localised corrosion and fracture [e.g. in Ni (Cornen and Le Gall, 2004), in boron containing AISI 304 stainless steel (Kurban et al., 2006) and for intergranular fracture of Fe0.002C0.06P (Williams et al., 2004)]. By readily acquiring a high number of data, EBSD allows study of the grain boundary character distribution, which is in turn inuenced by the interface energy distribution, as a function of parameters such as chemical composition. In SnAgCu lead free solder alloys, Telang et al. (2004) showed that Ag (respectively Cu) tends to reduce (respectively increase) the difference in free energy between various types of boundaries in the material. Diffusion along interfaces Interface diffusion may be characterised with the help of EBSD as a function of the local interface structure. The main difculty is accurate determination of the local crystallographic orientation of the interface plane (Randle, 2004). Discontinuous ordering of Fe 50 at.-%Co highly depends on the grain boundary (GB) misorientation. Special GBs such as low angle boundaries (LABs) and S3 twin boundaries, allowing
only slow diffusion, are not sensitive to discontinuous ordering. Vacancy migration is very difcult if no ,111. direction is close to the GB plane, so that the sensitivity of high angle boundaries (HABs) to discontinuous ordering depends on both GB misorientation and local orientation of the GB plane (Bischoff et al., 1998; Semenov et al., 1998). Surface rearrangement in FeO is also strongly affected by neighbouring GBs, whatever the local free surface orientation (determined by EBSD), due to preferential GB diffusion (Bahgat et al., 2005). Depending on the local crystallographic orientation of free surfaces, a Kirkendall effect due to differences in solute atom diffusion can be observed after phase trans formation [e.g. in Ti9 wt-%Mo (Guo and Enomoto, 2006)]. Anisotropy of bulk diffusion Anisotropy of bulk diffusion strongly depends on the crystal structure. The EBSD was used to investigate diffusion of Cr in tetragonal Mo5Si3, for which the diffusivity along [100] and [010] directions is higher than along the [001] direction (Strom and Zhang, 2005). When single crystals are not readily available, diffusion in coarse grained materials after EBSD identication of each grain orientation is a convenient tool in this eld [see e.g. oxygen tracer diffusion in (La2xSrx)CuO4 (Claus et al., 1994)].
Solidification and semisolid state

Nucleation of solid phase
Nucleation occurs at a very local scale, which cannot be accessed with the SEM. However, one of its consequences (i.e. crystal orientation) can be efciently studied with EBSD, in particular when sample preparation is tedious (e.g. for composite or heterogeneous materials such as welded joints), or if the microstructure is too coarse to be characterised with TEM or XRD. By allowing access to local crystallography over large areas, the EBSD technique facilitates investigation of phenomena that are difcult to access by TEM, such as heterogeneous nucleation at a substrate surface or at scarcely distributed particles. Examples are numerous and will still grow rapidly in number in the next future.
Effect of nucleating agents
A few EBSD studies address nucleation enhancement (or inhibition) by particles or solute elements. Specic orientation relationships (ORs) between nucleating particles and solidifying material have been observed in, e.g. aluminium inoculated with a TiC forming alloy [cubecube OR (Tronche and Greer, 2001)] and in AISI 409 ferritic stainless steel at TiN particles ({001}TiN// {001}ferrite and ,110.TiN//,100.ferrite) (Hunter and Ferry, 2002a) leading to highly textured material. Equiaxed, randomly textured grains nucleate at segregated areas of the heat affected zone (HAZ) of Sc or Zr containing aluminium alloys (Kostrivas and Lippold, 2004). Sb and Pb were shown to strongly inhibit nucleation of the solid phase in zinc based hot dip coatings (Quiroga et al., 2004; Rappaz et al., 2004).
Solidification path
The EBSD has been intensively used for stainless steels, whose solidication path strongly depends on both chemical composition and solidication rate. The austenite (fcc c) phase generally forms rst in rapid
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solidication, whereas ferrite (bcc d) forms rst at lower solidication rates. This has been illustrated in laser (Robino et al., 1998; Katayama et al., 1999; Brooks et al., 2003; Iamboliev et al., 2003) and gas tungsten arc (Robino et al., 1998; Iamboliev et al., 2003) welded alloys. As d and c phases exhibit particular ORs when one forms by solid state transformation from the other, it is rather easy to determine by EBSD, with information on both phase morphology and crystallography, which phase was the rst to form, if any. When a strong texture is observed, but not these particular ORs, one can suppose that both d and c formed simultaneously during solidication. This could be the case in weld metal (WM) deposits (Bouche et al., 2000) (Fig. 2). The EBSD provides information, which in these coarse grained materials cannot by obtained with XRD, and on a much more reliable statistical basis than by TEM. Information about abrupt changes in solidication mode can be given by EBSD. By continuously varying CO2 laser welding speed or base metal composition of Fe18Cr(1014)Ni alloys, Fukumoto and Kurz (1997) showed that the change in solidication mode occurred with no change in crystal orientation and no nucleation of new misoriented crystal, but after some undercooling. Owing to the higher distance between d and the c dendrite tips than between c and the d dendrite tips, the FA (d then c) to AF (c then d) transition occurred more readily than the AF to FA transition. The EBSD proved useful to investigate the solidication path of MCrAlY alloys deposited on a Ni base superalloy by continuous CO2 laser cladding (Bezencon et al., 2003), as soon as the lattice mist could be accommodated by LABs, the fcc c phase rst formed by epitaxial growth. As soon as another primary phase formed (e.g. b-NiAl), nucleation occurred and epitaxy was no longer possible. The solidication structure of small areas in heterogeneous materials was also investigated by EBSD at the right scale in laser deposited Ti 10 at.-%Cr alloys (Banerjee et al., 2002), in eutectic areas of Gd containing NiCrMo alloy ingot (Robino et al., 2003) and in MgLiCa cast alloys (Song and Kral, 2005). A recent example of application of EBSD to a solidication problem of great practical signicance was given by Sengupta et al. (2006), who studied oscillation marks and hooks in continuously cast low carbon steel slabs. As the meniscus line still remained a HAB, it was clearly visible even after several phase transformations occurred during cooling. It was deduced that solid phases did not nucleate at the same time on both sides of the frozen meniscus. Owing to the large grain size and sample geometry, such information could only be accessed using EBSD.
Eutectic solidification
(a)
(b)
2 a light optical micrograph of type 316L stainless steel WM and b {110} pole gure, in c austenite frame, of d ferrite (individual dots) located at c LABs, showing either KS ORs (surrounded by circles and triangles) or near cubecube ORs (surrounded by rectangles) between d and c. After Bouche et al. (2000)
Nucleation of coarse eutectic grains was rst studied with EBSD in white cast irons (Randle and Laird II, 1993). A colony of hexagonal M7C3 carbides was suggested to originate from a single nucleus. Most other studies addressed alloys undergoing dendritic, then eutectic solidication, to check whether the crystal orientation of the eutectic phase was the same as that of its dendritic counterpart, i.e. if there was or not nucleation of that phase from the undercooled liquid. In an arc melted hypereutectic NbSi alloy, Drawin et al. (2005) showed that Nb3Si shared a common crystal
orientation in eutectic colonies and in some dendrite neighbours. The vast majority of published work addressed the solidication of AlSi alloys modied with Sr, Sb, Cr, Na and P and cast as small ingots. The change in morphology of eutectic silicon from lamellar to brous could not be unambiguously related to a change in OR between dendritic and eutectic (Al) phases (Dahle et al., 2001). While in unmodied alloys eutectic (Al) had most often the same crystal orientation as a neighbouring dendrite, this was not the case for
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modied alloys (Wang et al., 1999; Nogita and Dahle, 2001a, 2001b and 2001c; Nogita et al., 2001; Dahle et al., 2005), except for high amounts of added Sr (Dahle et al., 2001; Nogita and Dahle, 2001a). Strontium was thought to increase the efciency of nucleating agents, leading to independent nucleation of eutectic (Al) from the liquid, just as for a columnar to equiaxed transition (CET) (Nogita and Dahle, 2001a). In contrast with these commercial purity alloys, Heiberg and Arnberg (2001) and Heiberg et al. (2002) did not nd any CET in high purity AlSi(Sr) alloys; eutectic and dendritic (Al) phases shared the same crystal orientation and thus no barrier to nucleation of eutectic (Al) from dendritic (Al) was found. Electron backscatter diffraction on both (Al) and (Si) phases (Heiberg and Arnberg, 2001) showed no particular change in internal twinning of eutectic (Si) and no particular OR between both phases, although eutectic (Si) had a ,110. bre texture. Here again, the need to characterise ne scale microstructures within coarse grains obviously suggests EBSD as the most suitable technique to get statistically reliable and metallurgically relevant information.
Peritectic solidification
Rather few studies have been dedicated to peritectic solidication except for stainless steels (see section on solidication path). In cast iron, no OR was found between newly formed M3C and already existing M7C3 carbides at which they very likely nucleated (Randle and Laird II, 1993). The peritectic c2c9 solidication of model and CMSX4 single crystal nickel base superalloys (Warnken et al., 2005) was studied at coarse shrinkage cavities; ball shaped c9 particles had a cube cube OR with the dendritic c substrate.
Orientation relationships between seed (or substrate or mould) and solid
Chill or external zones of ingots or thin strip castings have frequently been shown to exhibit a ne grained, randomly textured microstructure, except for some cases where a strong bre texture was already observed with
EBSD (Summers et al., 2004). At a very local scale, a random texture can be induced by nucleation at a rough substrate followed by locally textured growth [e.g. in stainless steels (Hunter and Ferry, 2002b; Ferry and Hunter, 2002)]. Numerous misoriented equiaxed grains were also observed in molten silicon droplets solidied on a silicon wafer substrate (Nagashio et al., 2004) although liquid spreading did not allow columnar growth perpendicular to the contact plane in that particular case. Single crystal superalloys such as CMSX4 and CM186LC exhibit a randomly textured chill zone. With EBSD one can check that the distribution of misorientation between grains follows the classical curve for textureless cubic materials (Ardakani et al., 2000). Epitaxy between the HAZ and the WM can be readily characterised with EBSD at the local (grain to grain) scale (Table 2). The EBSD was also used to evaluate ORs between seed and solidied material in complex microstructures, as in fully lamellar c-TiAl alloys. Here, various grains appeared at the seed, sharing one ,110. direction with it. In Ti48Al the selected grain had the same crystal orientation as the seed. In Ti48Al8Nb a few variants having one ,110] direction of lamellae parallel to one of the seed were observed (Takeyama et al., 2004). Functionally graded materials may be obtained by laser melt injection. Interfacial reactions and ORs between the injected ceramic powder particles and the hot metal matrix can be characterised with EBSD at a very local scale, allowing better insight into the solidication mechanism. Ocelk et al. (2001) examined one hundred interfaces between Al4C3 and SiC powder in the reaction layer of laser melt injected AlSiC composites. In 25% of observed cases, {0001}SiC was parallel to {0001}Al4C3, according to the angle between the {0001}Al4C3 plane and the temperature gradient. In contrast with extrusion (where Al4C3 is not formed), no OR was observed between SiC particles and (Al) matrix. Specic ORs were observed in reaction zones of
Table 2 Orientation relationships found with EBSD in weld solidication Base metal Be alloy Al alloys Gd containing Ni base alloy CMSX4 Ni base superalloyzMCrAlY AISI 304 and 310S austenitic stainless steels AISI 304 austenitic stainless steel Free machining stainless steel High purity Fe and Monel 7030 filler Weld metal Autogeneous electron beam welding GTAW* with or without filler metal Autogeneous electron beam and GTAW Laser cladding Pulsed YAG laser GTAW Autogeneous pulsed YAG laser GTAW OR between WM and HAZ Epitaxy at HAZ equiaxed grains Equiaxed WM: no OR, no texture; dendritic WM: epitaxy on HAZ Columnar WM in epitaxy with HAZ Cubecube OR if primary solidification into c; no OR otherwise (b or b z c) Cubecube OR for solidification into c, no clear OR for solidification into d KurdjumovSachs (KS) OR between ferritic WM and austenitic HAZ Epitaxy (no fusion boundary) if solidified into c; no clear OR if solidified into d NishiyamaWassermann (NW) and Bain ORs{ Mostly Bain OR{ Bain, sometimes NW OR No OR (chill zone) Ref. Wright and Cotton, 1995 Kostrivas and Lippold, 2004 Robino et al., 2003 Bezencon et al., 2003 Katayama et al., 1999, Iamboliev et al., 2003 Iamboliev et al., 2003 Brooks et al., 2003 Nelson et al., 1999a Nelson et al., 1999a Nelson et al., 1999a Nelson et al., 1999b
2.25Cr1Mo steel and 625 Ni base filler GTAW A508 low alloy steel and AISI 309L GTAW austenitic filler AISI 409 ferritic stainless steel and GTAW Monel 7030 filler
*GTAW: gas tungsten arc welding. { In fact, cubecube OR during solidification into austenite and then solid state transformation into ferrite in HAZ.
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Grain size and morphology
3 Results of EBSD on determination of local dendrite crystallography in splat quenched silicon: after Nagashio and Kuribayashi (2005)
functionally graded Ti6Al4V/SiC or WC composites produced by laser melt injection, depending on the facets of powder particles (Pei et al., 2002; de Hosson and Ocelk, 2003). A functionally graded aluminium alloy containing Al3Ti particles showed no OR between phases in centrifugally casting, leading to a morphological texture of Al3Ti platelets with no crystal texture in the (Al) matrix (Watanabe et al., 2002).
Growth of solid phases

Growth direction
Studies of EBSD on growth direction with respect to the thermal gradient have concentrated on directional solidication, where microstructures are frequently coarse grained (Table 3). In eutectic and peritectic microstructures, morphology and crystallographic ORs are intimately related, as reported below (section on microtextures). As an example of dendritic solidication, Nagashio and Kuribayashi (2005) associated EBSD with light confocal microscopy (Fig. 3) to evidence the transition in growth direction from ,211. to ,110. and then to ,100. for splat quenching of silicon onto silicon wafers. The transition was interpreted with facet planes and liquid/ solid interfacial energy thanks to careful experimental observations.
Table 3 Results of EBSD on solidication growth direction Material Ti26Al27Nb0.03O (at.-%) Pb(Mg1/3Nb2/3)O3 z PbTiO3 Nb33Ti16Si (at.-%) AZ91 Mg alloy Solidification process Solidification mode Induction float zone melting High pressure Bridgman Czochralski Bridgman
The EBSD technique is a good means to evaluate the grain size and shape on a quantitative basis, grains being dened by boundaries of misorientation angle higher than a user xed threshold. This implies that the cleaning procedure used for EBSD data processing should be suitably chosen and clearly reported. Some examples in as solidied microstructures are given in Table 4. The EBSD is particularly useful when the grain size is similar to the size of the part, i.e. for so called multicrystals. This is the case, for example, for lead free, coarse grained single shear lap Sn3.5Ag solder joints (Telang and Bieler, 2002, 2005a and 2005b) and for CoCrMo laser cladding on railway wheels (Farooq et al., 2006). The EBSD may also reveal that individual particles are in fact single crystals [e.g. coarse Bi particles in Bi 24.8In18.0Sn eutectics (Ruggiero and Rutter, 1995)] or polycrystals composed of several grains [e.g. M7C3 carbides in high chromium white cast iron (Powell and Randle, 1997)]. Interrupted solidication tests allow investigating microstructure formation, although the quenched liquid may be difcult to distinguish with EBSD from the growing solid. The EDX may be here of great help to study solid/solid grain boundaries already formed before quenching (Liu et al., 2005). In other cases, EBSD patterns from the quenched liquid cannot be indexed, so that the shape of the solid/liquid interface is easily revealed with this technique [e.g. in Fe4.3Ni (Faryna et al., 2002)]. Phase connectivity is difcult to assess from light optical or electron microscopy imaging only. By identifying areas of the material sharing a common crystal orientation, EBSD provides interesting information even from two-dimensional (2D) sections, i.e. individual crystals of a 2D section may in fact belong to the same three-dimensional (3D) grain. Some examples are given in Table 5. This is particularly useful when individual grains are connected in 3D, but not in 2D (e.g. in EBSD maps or thin foil TEM images). Another side of the problem is grain clustering: misorientation gradients, which may inuence product properties, are readily revealed with EBSD as long as
Crystal direction of solid growth
Ref.
Directional solidification ,100.bcc Cellular Cellulardendritic Columnar
Be alloy Fe3Si AlZnSi Zn Ti6Al4V Ni base Alloy 22
Electron beam welding Columnar Twin roll casting Hot dip galvanising Columnar Dendriticcolumnar (Al) Hot dip galvanising Dendritic (Zn) Vacuum arc remelting Columnar Dendriticcolumnar
Gas tungsten arc welding
Boehlert and Bingert, 2001 [110]rhombohedral, sometimes 1220u Soundararajan et al., from it (trace analysis) 2004 Sutliff and Bewlay, [113]Nb; [001](Nb,Ti)3Si 1996 ,1120. or ,2445. according to Pettersen and Ryum, thermal gradient and growth rate; 1989; Pettersen et al., can be primary and ternary ,1120. 1990 and secondary (,1120. z ,2445.) ,1010. favoured Wright and Cotton, 1995 Takatani et al., 2000 Often close to ,100.bcc Semoroz et al., 2001 Neither ,100.Al nor ,110.Al, close to ,320.Al (trace analysis) Semoroz et al., 2002b Mainly ,1010.hcp Glavicic et al., 2003c ,100.bcc (leading to ,1120.hcp) 0 and , 45u from heat flow El-Dasher et al., 2006 ,100.fcc (followed by partial recrystallisation)
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Table 4 Electron backscatter diffraction characterisation of grain size and morphology of as solidied microstructures Material 2024 Al alloy Solidification process Metal inert gas welding Grain size or morphology More than 80% of the WM 5 equiaxed grains of 50100 mm in size Equiaxed grains nucleate in the chill zone, followed by columnar growth Many equiaxed grains near the centre Grain size 200 mm; cellular (size 3 mm) if the laser beam is focused, non-cellular if irradiation is uniform Globular grains with HABs if cast at liquidus temperature Grain size about 150300 mm depending on magnetic stirring Same grain size found with EBSD and light microscopy (but not in the same observation plane) Same grain size (140 mm) found with EBSD and light microscopy Grain size distribution before solution annealing (not possible in light microscopy) Grain size 6.37.9 mm Average grain size ,300 mm Ref. Lefebvre et al., 2005
Si
Simulated melt spinning
Nagashio and Kuribayashi, 2006 Nagashio et al., 2004 Kell et al., 2005
Si
Splat cooling on Si wafer
AISI 316L stainless steel Autogenous CO2 laser welding 2618 Al alloy Thixoforming
Xia and Tausig, 1998 Kokawa et al., 1999 Slamova et al., 2003
Inconel 82 Ni base alloy Tungsten inert gas welding with low carbon steel 5052 and 5182 Al alloys Direct chill and twin roll casting Al0.15Fe0.07Si AZ91D and AM60B MgAl alloys Fe15 at.-%Ga Al7Si0.3Mg Al7Si0.4Mg Si30Al Direct chill casting High pressure die casting
Samajdar and Doherty, 1994 Bowles et al., 2004 Saito et al., 2004 Buffiere et al., 2001 ` Han et al., 2001 Hogg et al., 2006
Roll casting As cast with artificial shrinkage porosity Low temperature semiliquid Cells clustered into single crystal colonies die casting delimited by HABs Spray forming Grain size (y5 mm for Si and 250 mm for Al) in the divorced eutectic formed after slow cooling; the difference is due to nucleation conditions (Si from droplets, Al within the formed material)
mapping is possible. Grain clustering may be related to the solidication texture, which increases the frequency of LABs (West and Adams, 1997). Here, grain size and grain connectivity strongly depend on the denition of grains given by the EBSD user.
Competitive grain growth
During crystal growth, a strong selection may occur among grains nucleated either in the chill zone or at free
surfaces [e.g. in laser metal forming (Gaumann et al., 1999)] or at the mould/metal interface or even from the undercooled melt. This competition is governed by the growth rate of individual grains, which is in turn related to the local crystal orientation with respect to the local heat ow. During directional solidication, competitive grain growth leading to a columnar zone with an increasing grain size (e.g. Fig. 4) was clearly evidenced thanks to
Table 5 Phase and grain connectivity determined with EBSD in as solidied microstructures Material Al1.25Mn White cast irons Solidification process Directional (cellular) As cast Results obtained with EBSD Highly interpenetrated grains Hypereutectic alloy: M7C3 carbides are single crystalline over large areas (shown by deep etching to be interconnected); hypoeutectic alloy: M7C3 carbides are individual crystallites Connectivity of carbides varies from one material to the other 2D spatial connectivity is not correlated to crystal orientation: 3D percolation is suggested; no coalescence (density of LABs decreases with increasing time): Ostwald ripening a phase: multilayered grains connected in 3D; b phase: connected even in 2D Grain clustering with strong internal orientation gradients Polycrystalline grains with domains of same crystal orientation possibly connected in 3D Ni3Sn (near single crystalline): connected network; Ni: individual textureless particles Ref. Sun and Ryum, 1992 Randle and Powell, 1993
High Cr white cast irons Sn17 wt-%Pb
As cast Quenched from semisolid state
Powell and Randle, 1997 Wolfsdorf-Brenner et al., 1999
Sn1.4 wt-%Cd NiCrCoTiAlMoSi superalloy Zn alloy Ni18.7 at.-%Sn
Directionally solidified oscillating peritectic Directionally solidified ingot Hot dip galvanising
Zeisler-Mashl et al., 1997 West and Adams, 1997 Semoroz et al., 2002a
Containerless anomalous eutectic
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4 Competitive grain growth during solidication, illustrated with EBSD grain boundary map of X750Ni base superalloy: after Gandin et al. (1995)
EBSD in an Al1.25Mn alloy (Sun and Ryum, 1992) and in a beryllium alloy weld (Wright and Cotton, 1995). A more or less strong ,100. texture was found to gradually develop in X750, CMSX4 and CM186LC nickel base superalloys (Gandin et al., 1995; Ardakani et al., 2000; DSouza et al., 2000), in a twin roll cast Fe 3Si alloy (Takatani et al., 2000) and in austenitic stainless steels with simulated strip casting on Cu substrates of controlled roughness (Hunter and Ferry, 2002b and 2002c). In fact, the viscosity of the liquid controls the formation of secondary and tertiary dendrite arms (DSouza et al., 2000). In case of low viscosity, the competition between grains depends on the relative orientations of the primary dendrite arms [e.g. in CMSX4 bicrystals, see (Wagner et al., 2004. Stanford et al., 2004b)]. The origin of new undesirable stray grains cannot be assessed from 2D measurements; in a laboratory nickel base superalloy, serial sectioning coupled with EBSD mapping proved that stray grains nucleated at mould walls and not from dendrite fragmentation or constitutional undercooling (Stanford et al., 2004b). Stray grain formation was also characterised after electron beam and laser welding as a function of alloy composition, welding direction (with respect to crystal orientation), misorientation between welded parts and welding speed (Hirose et al., 2003; Vitek et al., 2003 and 2004). A possibility to avoid small, undesirable grains is to improve the shape of isothermal curves using appropriate modelling coupled with EBSD experimental validation (e.g. (Kermanpur et al., 2000) on IN738 alloy and (Carter et al., 2000) for innovative single crystal casting design) By allowing crystal orientation mapping over large areas, EBSD is particularly well suited to studies of the
Table 6 Studies on CET using EBSD Material Solidification process
5 Competitive grain growth during solidication of duplex stainless steel in FA mode, after Inoue et al. (2000). Unfavourably oriented c austenite grain 1 is eventually replaced by grain 2. Unfavourably oriented d ferrite grains (cases B, D, H) are eventually replaced by d grains keeping (case B) or not keeping (cases D, F, H) KS OR with growing c grain. As a result, lacy d (resulting from KS OR, case A) is less frequently found than vermicular d (no OR, cases C, E, G)
CET during solidication. The CET occurs due to local modication of thermal and/or chemical or mechanical conditions near the tips of growing dendrites. Examples may be found for eutectic solidication (see section on nucleation in eutectic solidication), and also for dendritic and cellular solidication (Table 6). In hot dip galvanising, grains nucleate with no texture and competitive grain growth depends on both dendrite growth directions and grain orientation with respect to the solid/liquid interface (here the grain thickness is much lower than the in plane grain size) (Semoroz et al., 2002a and 2002b; Quiroga et al., 2004). Such EBSD investigations have also been applied to the more complex case of two phase solidication in Fe 19Cr11Ni stainless steels, solidied by autogeneous gas tungsten arc welding interrupted by liquid tin quenching (Inoue et al., 2000). Competitive grain growth in each of the ferrite and austenite phases was eventually governed by the local crystal orientation of the HAZ at the fusion line (Fig. 5).
Dendrite fragmentation and semisolid state
Dendrite fragmentation may appear during recalescence or after partial melting of the seed in single crystal
CET mechanism Constitutional undercooling Constitutional undercooling
Information provided by EBSD Number of nuclei per unit volume Tree rings (solidification defects) consist of equiaxed grains Remaining solid is recognised thanks to twin orientations Grain size and shape; rotation of fragments between nonfragmented dendrites Evidence of equiaxed areas
Ref. Gaumann et al., 2001 Xu et al., 2002a Li et al., 2005a Li et al., 2006 Yasuda et al., 2005
CMSX4 Ni base Laser metal forming superalloy IN718 Ni base superalloy Vacuum arc remelting
Ni1B Ni1B
Cu, Cu1 at.-%Ag, Fe 10 at.-%Ni, low carbon steel
Electrostatic levitation melting Electrostatic and electromagnetic levitation melting Magnetic levitation melting
Cell fragmentation (undercooling ,200 K) Dendrite fragmentation (undercooling: 70200 K) Magnetic stirring: surface oscillation or bulk convection in liquid sphere
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casting. For a high volume fraction of liquid, dendrite fragments may rotate, so that a random texture is found in that area after solidication [e.g. in CMSX4 single crystals (Stanford et al., 2004a) and in Ni1B laser melted under electrostatic levitation (Li et al., 2005a)]. In directionally solidied Ni18.7 at.-%Sn having an anomalous eutectic microstructure, recalescence affected the Ni phase but not the Ni3Sn phase, so that Ni fragments could not rotate easily and only LABs were eventually observed with EBSD (Li et al., 2005b). When the liquid fraction is rather low and no LABs are observed between dendrite fragments, one may conclude to Ostwald ripening instead of coalescence [e.g. in reheated Al7Si0.3Mg alloy (Kliauga and Ferrante, 2005)]. When a 6082 aluminium alloy is cast from the semisolid state, grains tend to cluster into agglomerates having low energy (LAB or twin) boundaries. Thus, EBSD may distinguish former aggregates after solidication completion, showing intensive grain agglomeration if the mix is stirred, but very little in the absence of stirring (Arnberg et al., 1999). Grain fragmentation during agglomeration of silicon particles in thixoformed Al30Si5Cu2Mg (wt-%) alloy has been shown using EBSD to be of {111} type, leading to {111} agglomeration boundaries (Hogg and Atkinson, 2005). One must not forget, however, that EBSD does not distinguish between the former solid phase and the quenched liquid, which may solidify epitaxially on existing crystals, so that great care must be taken while evaluating the grain boundary character distribution (Liu et al., 2005).
primary trunks from tertiary arms [e.g. in directionally solidied Mg9Al1Zn alloy (Pettersen and Ryum, 1989)]. Others focused on internal misorientation within dendritic grains. These may affect both morphology and internal misorientations e.g. in ,112. dendrites of Al 4.3Cu0.3Mg alloy in certain conditions (Henry et al., 1998b). In most cases, however, crystal orientation gradients are found within dendrites, due to uid ow and shrinkage stresses (Doherty, 2003) or to gradient in solute concentration or to substrate induced thermal stresses (Semoroz et al., 2001). Some examples of quantitative measurements using EBSD are given in Table 7.
Practical example: growth of feathery grains
Solidification microtexture and resulting average texture

Solidification microtexture
Orientation relationships between solid phases in as solidied microstructures have been investigated in modied AlSi alloys (see section on nucleation in eutectics). In as cast Al62.5Cu25Fe12.5 and Al65Cu20 Fe15 alloys (Gui et al., 2001), no OR was found between l-Al13Fe4 single crystal dendrites and respectively the icosahedral quasicrystalline matrix and the polycrystalline R-phase. In as welded austenitic stainless steel, the KurdjumovSachs OR (see Appendix) was found between bcc d ferrite and fcc c austenite in lacy ferrite microstructure (Inoue et al., 2000) whereas only a common ,100. crystal direction, parallel to the growth direction, was found between d and c phases in skeletal ferrite microstructures (Inoue et al., 2000; Bouche et al., 2000). High resolution studies of solidication microtextures are made possible thanks to EBSD. For instance, vacuum cast joints of white irons exhibit M7C3 carbides, surrounded by M3C with the same crystal orientation, which are embedded in a ferritic iron matrix (Wuhrer et al., 2004). Small, highly misoriented grains have been observed in directionally solidied melt textured YBCO alloyed with YBa2CuO5 (KoblischkaVeneva et al., 2003; Koblischka et al., 2003). At (211) phase particles, the orientation of the (123) YBCO matrix was strongly disturbed from its (001) texture, depending on the orientation of the individual (211) phases. The EBSD is particularly useful if dendritic grains are very coarse in size but with a very ne internal microstructure. Few EBSD results addressed identication of
Very coarse, undesirable feathery grains with fan shaped dendrites develop in certain conditions at the expense of columnar grains in aluminium alloys. They mostly appear during direct chill casting of alloys containing no rening elements, with high thermal gradients beyond the solidication front and under convection (Rappaz and Henry, 1999). By EBSD mapping of wide areas at a ne scale compared to the dendrite arm width, Henry et al. showed that feathery grains were composed by parallel lamellae with alternating twin related crystal orientations; {111} boundaries being alternatively (coherent and straight) and (incoherent and wavy) (Henry et al., 1997, 1998a and 1998b). Within one main orientation, some subboundaries were even found (Henry et al., 1997). The corresponding misorientation tended to accumulate leading to the fan shaped morphology (Henry et al., 1998b). The crystal direction parallel to the thermal gradient (,100.Al in columnar grains) was clearly ,110.Al in feathery grains, with both ,110.Al (possibly twinned) and ,100.Al secondary arms. ,110.Al primary arms were twinned, the {111} twinning plane containing the growth direction. Coherent boundaries were found in arms parallel to the thermal gradient. The detailed role of convection on counterow growth of ,110.Al twinned arms is reported elsewhere (Rappaz and Henry, 1999; Henry et al., 2004). Details about the anisotropy of primary dendrite arm spacing and 3D morphology can be found in (Henry et al., 1998a).
Microtexture of eutectic and peritectic alloys
Eutectic and peritectic alloys often exhibit coarse colonies of ne lamellae, so that high spatial resolution is required over wide areas. Sample preparation is made difcult by the difference in electrochemical and hardness properties of the various phases, so that EBSD studies are still scarce. Some results on ORs found in eutectic and peritectic materials are illustrated in Table 8.
Average texture of as solidified products
The average texture is in many cases preferably investigated by XRD. However, when the grain size exceeds a certain value (typically 50100 mm), XRD can no longer provide statistically signicant data. Neutron diffraction can be used for grains up to y1 mm in size. For even coarser grains and for heterogeneous materials such as welded joints, EBSD can still be used thanks to stage motion in the SEM. In EBSD, the orientation distribution function (ODF) is then directly calculated
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Table 7 Electron backscatter diffraction measurements of internal misorientation in dendritic grains Material Al0.15Fe0.07Si CMSX4 Ni base single crystal superalloy CMSX4 Ni base single crystal superalloy Solidification process Direct chill casting CO2 laser metal forming Misorientations measured with EBSD Many misorientations up to 5u within dendrites After 5 passes, arms become trunks with 510u misorientation between dendrites Slight misorientations between dendrite trunks are viewed thanks to specifically developed data processing Steady state growth: internal misorientations of 23u do not cumulate; non-steady state growth: successive branching cumulates misorientation up to y6u Misorientation of 410u over 3 mm along the growth direction; internal LABs of 68u Dendrite arms misoriented by 410u mm21. Misorientations up to 5u within grains, cumulate up to 35u in coarser grains Austenite grains are clusters of subgrains and internal LABs are solute enriched and could originate from dendrite arm bending One nucleus only for dendrites in a given grain; orientation domains related by simple ORs in polycrystalline grains Ref. Samajdar and Doherty, 1994 Gaumann et al., 1999
CO2 laser epitaxial cladding
Cleton et al., 1999
CMSX4 and CMSX10N Ni base single crystal superalloys
Directional casting of turbine blades
DSouza et al., 2005; Newell et al., 2005
99.9% pure Al
Ingot casting (columnar zone)
Bhattacharyya et al., 2001 Semoroz et al., 2001
AlZnSi alloy
Hot dip galvanising
High Cr white cast irons
Electromagnetic stirring and casting
Yang et al., 2003
Zn0.2Al0.15Sb
Hot dip galvanising
Semoroz et al., 2002a
Table 8 Electron backscatter diffraction measurements of orientation relationships in as solidied eutectic and peritectic microstructures* Material NiCr(Si) white cast iron White iron V13 at.-%Si Cr16 at.-%Si Ni45.5Al9Mo (at.-%) Mg33AlSr (wt-%) Nb22 at.-%Si Nb16Si1.5Zr (at.-%) Al7Si(0 150 ppmSr) Solidification mode Microstructure Slow cooling E for 0%Si, P for (0.017 K s1) 2%Si OR between phases Growth direction Strong [0001]M7C3 for 2%Si; no texture in M3C for 0%Si [001]Fe3C // plane of plates [100]V3Si // [111]V Ref. Randle and Laird, II 1993
0%Si: no OR between M3C formed at a given M7C3 Strip casting E Plate like Fe3C: [001]Fe3C // normal direction // [001]a Directional E (broken lamellar) (011)V3Si // (112)V // lamellae boundaries Directional E (lamellar) (011)Cr3Si // (123)Cr // lamellae boundaries, (001)Cr3Si // (011)Cr // lamellae boundaries Directional E (NiAl matrix z {011}Mo // {011}NiAl // interfaces Mo fibres) Directional E (lamellar) (1101)Mg // (101)Mg17Al12 10u from interface Arc melting in E Cu crucible Arc melting in E Cu crucible Ingot casting E {111}Nb3Si // {111}Nb (one area studied) No OR between Nb and Nb3Si No Sr: two twin related Si variants; with Sr: various twin related Si variants with one common ,110. per colony, often parallel to ,100. or ,110.Al; no clear OR between Al and Si ,0001.Al2O3 // ,112.YAG Three intricate single crystals per eutectic grain, ,2110.Al2O3 // ,100.ZrO2, YAG is much less textured No clear OR between fibre textured Al2O3 and ZrO2
Song et al., 2003a Bei et al., 2004 [100]Cr3Si // [111]Cr (close Bei et al., packed directions) 2003 ,100.Mo // ,100.NiAl [1120]Mg // [111]Mg17Al12 215u from growth direction Bei and George, 2005 Guldberg and Ryum, 2000 Drawin et al., 2005 Miura et al., 2005c Heiberg and Arnberg, 2001
Al2O319 mol.-% Directional YAG (fibres) Al2O316%YAG Micropulling 18 mol.-%ZrO2
E E (lamellar)
Nakai et al., 2005 Murayama et al., 2004a
Al2O3 16%YAG Directional 19 mol.-%ZrO2 (rods)
E (geometric or Chinese scripts)
Murayama et al., 2004b
*E: eutectic; P: peritectic; YAG: yttriumaluminium garnet.
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Table 9 Solidication textures determined with EBSD in thin strip castings and hot dip coatings Material Cast iron 0.1%C steel Fe3Si Microstructure Grey, compacted or nodular (dendritic growth) Upper and lower columnar zones versus mid-thickness Average texture Inoculated materials: no texture in austenite and thus no texture in resulting ferrite Strong {100} texture ,100. // local thermal gradient versus randomly textured Strong ,100. texture with many LABs ,001. fibre (ferrite) ,001. fibre (austenite) Ti free (respectively Ti containing) steel: random texture (respectively ,001. fibre) in chill zone, ,001. increases in growth zone in both cases ,001. fibre increases during growth ,110]Sn // heat flow, mainly special GBs Less cube component than in direct chill castings No average texture: the coating does not inherit that of steel substrate 43% of grains have their {0001} planes less than 22.5u from the free surface due to constrained growth Ref. Campos et al., 2005
Umezawa et al., 2003 Takatani et al., 2000
Fe15 at.-%Ga AISI 409 ferritic stainless steel AISI 304 austenitic stainless steel AISI 409 ferritic stainless steel (simulated thin strip casting) Columnar zone Columnar zone Chill zone and growth zone
Saito et al., 2004 Ferry and Hunter, 2002 Ferry and Hunter, 2002 Hunter and Ferry, 2002a
AISI 304 austenitic stainless steel (simulated thin strip casting) Sn3.5Ag and other Pb free solder alloys AlMg 5052 and 5182 alloys Al43.4Zn1.6Si (hot dip coating) Zn0.2Al0.15Sb (hot dip coating)
Chill zone and growth zone Multicrystalline solder joints Elongated and equiaxed grains
Hunter and Ferry, 2002b Telang et al., 2002; Telang and Bieler, 2005a, 2005c Slamova et al., 2003 Semoroz et al., 2001
Semoroz et al., 2002a
from individual orientations by taking one point per grain or by taking all data points and weighting orientation data with the respective area fraction of grains. If the grain size is low enough, EBSD and XRD results can be successfully compared (e.g. Slamova et al., 2003; Saito et al., 2004). One must, however, keep in mind that EBSD is a surface analysis technique. Sectioning effects may be signicant when grains are not equiaxed, which is frequently the case in solidication microstructures.
Spatial information given by EBSD is necessary when the heat ow direction is not uniform within the part, e.g. in thin strip casting (Table 9) and in welded joints (Table 10). In some instances, EBSD is used as a complementary method to evaluate GBs of samples while the average texture is determined by XRD (Park et al., 1999). Some examples obtained in as solidied bulk materials are listed in Table 11. A strong average texture induces particular ORs between grains, as e.g. in a ,100. textured directionally
Table 10 Average solidication textures determined with EBSD after welding or laser metal forming* Material 5182 and 6111 Al alloys Austenitic stainless steel AISI 409 ferritic stainless steel with Monel Ni30Cu Mn Ni alloy 182 Ni alloy 82 Process Laser welding Microstructure Columnar and equiaxed zones Cellular Average texture ,100. for columnar, random for equiaxed ,001. (ferrite) ,100. (austenite) Ref. Hector et al., 2004 Inoue et al., 1995 and 1998 Nelson et al., 1999b Scott et al., 2005 Kokawa et al., 1999
GTA welding then liquid tin quenching Dissimilar GTA welded joints Growth area
Multipass MMA welding Multipass GTA welding with or without magnetic stirring
Columnar Straight solidification front under magnetic stirring, curved front otherwise
,100. ,100. under magnetic field, random otherwise
Mg and AZ31, AZ61 and AZ91 Mg alloys Mg alloys A286 Fe based superalloy CMSX4 Ni base superalloy
Autogeneous EB welding Autogeneous GTA welding CO2 laser welding CO2 laser welding
Weak texture Weak texture Rotated cube ,001. // local thermal gradient
Su et al., 2002 Wu et al., 2004 Wei et al., 2002 Hirose et al., 2003
CMSX4 Ni base superalloy Multipass CO2 laser metal forming
Weld metal centre Welding at 30u from ,001.: many small grains Substrate and deposit
,001. fibre within 5u for Gaumann et al., substrate and within 10u 1999 for deposit
*GTA: gas tungsten arc; MMA: manual metal arc; EB: electron beam.
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solidied nickel base alloy ingot (West and Adams, 1997); many subboundaries developed and grains clustered into coarse entities having internal LABs and strong orientation gradients. The size of such entities grew faster than the grain size itself, due to strongly textured (competitive) grain growth. In directionally solidied CMSX4 and CM186LC nickel base superalloys, misorientation axes got close to the ,100. bre during growth; many LABs were also found, but special GBs such as S5, S13a and S17a (all misorientation around ,100. axes) were not favoured (Ardakani et al., 2000).
Hot cracking and GB resistance

Hot cracking during solidication is of major practical concern. The EBSD was mainly applied to problems associated with welding. In nickel base alloy 718, HAZ liquation was shown to occur at random GBs but not at coincidence site lattice (CSL) boundaries, according to the low sensitivity of CSL boundaries to boron atom segregation (Guo et al., 1998) and to boride and carbide precipitation (Qian and Lippold, 2003). In the [0001] Cu6Sn5 layer of solder interconnects, many HABs apparently provided penetration channels for the solder alloy (Lee et al., 2001). In free machining laser or gas
tungsten arc welded stainless steels, only alloys prone to rst solidify into austenite were prone to hot cracking, according to the higher sensitivity of austenite to boundary segregation and cracking than that of ferrite (Brooks et al., 2003). In gadolinium containing Ni base alloy welded by electron beam or gas tungsten arc processes, epitaxial solidication evidenced with EBSD provided a good resistance to hot cracking according to Varestraint tests (Robino et al., 2003). Welding of nickel base single crystal superalloys may lead to hot cracking if the single crystals to be joined are misaligned from each other or from the welding direction. The EBSD helped to establish adequate welding conditions and to identify, if any, the highly misoriented, newly nucleated grains that can induce hot cracking. Examples are found in laser welded CMSX4 (Hirose et al., 2003), in laser and electron beam welded Rene N5 (Vitek et al., 2003 and 2004) and in laser welded MC2 (Wang et al., 2004) single crystals or bicrystals. Here, EBSD data on base metal orientation and WM microtexture were combined with analytical models involving, e.g. local undercooling at grain boundaries. Hot cracking in Al4Cu alloy was also investigated by EBSD in terms of wetting of GBs by the remaining
Table 11 Solidication textures determined with EBSD in bulk materials (results of Grant et al. (1986) and Hanada et al. (1986) were obtained with pioneering electron channelling pattern technique in SEM) Material Cu AA1100 Al alloy Al1.25Mn AA 5052 and 5182 AlMg alloys Ti6Al4V Ti48Al2Cr2Nb (at.-%) Ni3Al X750 Ni base superalloy Fe18.4 at.-%Ga CMSX4 Ni base superalloy Duplex stainless steel AISI 430 ferritic stainless steel Nb33Ti16Si (at.-%) Process Directional solidification Ingot casting Directional solidification Direct chill and twin roll casting Vacuum arc remelted ingot casting Ingot casting Induction melting Directional solidification Zone melting Directional solidification Statically cast Continuously cast slab Czochralski directional solidification Arc melted ingot casting Microstructure Columnar Almost equiaxed Cellular Equiaxed Average texture ,001. Random ,001. Copper z Brass z cube z other texture components ,100. (b phase) ,0001. of a phase ,001. ,100. increases during growth ,100. (ferrite) ,100. fibre ,100. (ferrite) {001},uv0. (columnar), random (equiaxed) Weak ,113. for (Nb); ,001. (almost single crystalline) for (Nb,Ti)3Si [001] for eutectic Nb3Si; (Nb) randomly textured [001] for dendritic Nb3Si; (Nb) textured due to OR with Nb3Si [0001] Ref. Grant et al., 1986 Wang et al., 1990 Sun and Ryum, 1992 Slamova et al., 2003
Columnar Columnar Columnar Columnar Columnar Columnar Columnar Columnar zone equiaxed zone Cellular
Glavicic et al., 2003c Dupont et al., 1996 Hanada et al., 1986 Gandin et al., 1995 Summers et al., 2004 Carter et al., 2000 Calonne et al., 2000 Hamada et al., 2003 Sutliff and Bewlay, 1996 Drawin et al., 2005
Nb16 at.-%Si
Nb22 at.-%Si
Arc melted ingot casting
Cu6Sn5 ZrB2/ZrC Al/Al3Ti VV3Si Al2O3YAGZrO2 eutectic
Soldering Spark plasma sintering Centrifugal solid particle casting Directional solidification Modified micropulling
(Nb) dendrites z (Nb)/Nb3Si eutectic Nb3Si dendrites z (Nb)/Nb3Si eutectic Cu6Sn5 scallop like grains
Drawin et al., 2005
Lee et al., 2001 Shim et al., 2002 Watanabe et al., 2002 Bei et al., 2004 Murayama et al., 2004b; Lee et al., 2005
ZrB2 weakly textured, ZrC randomly textured Coarse Al grains Both Al and Al3Ti are and Al3Ti platelets randomly textured Eutectic ,111.V//,100.V3Si Chinese scripts ,2110. or ,1010.Al2O3, geometric ,001. or ,220.ZrO2, possibly ,100. or ,111.YAG ,0001. or ,1010.Al2O3, ,001. or ,220.ZrO2, ,100. or ,111.YAG
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liquid as a function of barium content and GB misorientation. By decreasing the liquid/solid interfacial energy (deduced from minimum misorientation angle of wetted GBs and ReadShockley equations) and thus delaying grain coalescence, barium strongly increased hot cracking sensitivity of this alloy (Fallet et al., 2006).
Electron backscatter diffraction and solidification: summary

Electron backscatter diffraction is of particular interest in solidication investigations because of its ability to characterise the microstructures at multiple scales with suitable statistical signicance, from (sometimes very) coarse grains down to submicrometre sized phases such as nucleating agents and eutectic colonies. Its angular and spatial resolution is generally high enough for that purpose. Geometric and statistical effects due to sectioning and sampling effects must be taken into account or, if possible, avoided by carrying out 3D investigations (see Discussion).
Solid state phase transformations

Orientation relationships between phases
Matrix phase transformations
The EBSD was generally used in this eld to conrm TEM or XRD data or, alternatively, to get statistically reliable results. A huge variety of materials and phase transformations have been addressed with EBSD as illustrated in Table 12 for ceramics, in Table 13 for nonferrous metals and in Table 14 for intermetallic phases and quasicrystals. Details about the most frequently observed ORs are reported in the Appendix. Most ORs were investigated at the scale of individual phases or by comparing the pole gures of product phases (formed from a single grain of the parent phase) to pole gures calculated using known ORs. They successfully compare with TEM data. Only few investigations used the average pole gures (Boehlert and Bingert, 2001). Like eutectic microstructures, products of eutectoid decomposition usually exhibit ne scale features and in many cases only a few colonies may be observed in a single TEM thin foil, whereas large areas may be scanned with EBSD. Four examples of results obtained using EBSD are given here: (i) in Nb(1625)Si1.5Zr (at.-%), the Nb3Si part of the (NbzNb3Si) eutectic further decomposes upon cooling into tetragonal a-Nb5Si3zbcc (Nb). In binary NbSi alloys, eutectoid (Nb) is single crystalline within a given eutectoid colony and may share the same crystal orientation as that of neighbouring eutectic (Nb) (Drawin et al., 2005). No OR was found between (Nb)
and a phases for 16 at.-%Si alloy, while in Nb 22 at.-%Si the authors found (111)Nb//(100)a and (011)Nb//(011)a or (001)a (Drawin et al., 2005). In ternary alloys, occurrence and nature of the OR depend on chemical composition and heat treatment (Miura et al., 2005b and 2005c) (ii) in Al36Mo17Ti (at.-%), the b (A2) phase transforms into Al3Ti (DO22) and Mo3Al (A15) phases. An OR was found between b and DO22, and between b and A15 phases (Miura et al., 2005a). Such OR disappeared after hot deformation (Miura et al., 2005a) probably due to a memory effect on variants due to the ordered structure of both product phases (Miura et al., 2004) (iii) in Fe12Mn0.8C0.3V steels, decomposition of fcc austenite c into bcc ferrite a and tetragonal Fe3C cementite depends on the complex sequence of nucleation events (a formed at VC carbides formed at MnS sulphides) so that the KS OR between c and a is not systematically observed (Guo et al., 2001 and 2002) (iv) in MnSi bearing hypo- and hypereutectoid steels decomposed into pearlite under small undercooling, the OR between a and Fe3C strongly depends on the 3D topology of phases. Given a colony nucleated at a c GB, the Pitsch Petch OR (see Appendix) prevailed if the a phase of the pearlite colony was totally isolated from the c grain where the colony did not develop, while the Bagaryatsky OR (see Appendix) prevailed otherwise (Fig. 6). In both cases, Fe3C crystals at c GBs and in the colony were found to share the same crystal orientation (Mangan and Shiflet, 1999). In the last two examples, only association between careful serial sectioning and EBSD analysis allowed to get the key results. This point will be further addressed in the Discussion section.
Precipitation
Most ORs between matrix and precipitates were investigated with TEM. However, if precipitates are scarcely distributed (e.g. at boundaries of coarse grains) or if no high angular accuracy is required, EBSD may readily provide relevant data (Table 15). The EBSD is also useful to study interactions between precipitation and damage cavitation, as much less sample preparation artefacts are usually induced than by TEM thin foil preparation. Discontinuous precipitation has also been investigated with EBSD. Results illustrated in Table 16 are generally complementary to data obtained with TEM, although the evolution of the OR along the
Table 12 Orientation relationships determined with EBSD in solid state phase transformations of ceramic materials Material (001) MgO coated with In2O3 LaNbO4 Parent phase MgOzIn2O3 Product phase MgIn2O4 Orientation relationships [001]MgO//[111]MgIn2O4 and [110]MgO//[110]MgIn2O4; no OR between In2O3 and MgIn2O4 Misorientation of 94u around [010] between product phase domains ,0001.H//,111.M and ,1010.H//,110.M Ref. Korte et al., 2000
Tetragonal
Monoclinic
Jian and Wayman, 1995
Iron oxides
Hematite Fe2O3 (H)
Magnetite Fe3O4 (M)
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growing colonies might be analysed with EBSD only, especially over large distances (e.g. the last item in Table 16).
Decomposition of ferrite and austenite in ferrous alloys
Austenite (fcc c) and ferrite (bcc a or d) phases have been widely studied with EBSD. Several classical ORs clustered around the 45u,001. Bain OR are recalled in the Appendix. There is still much debate about the relationship between OR and the displacive or diffusive character of phase transformations in steels, in particular concerning acicular ferrite, Widmanstatten ferrite
sideplates and bainite. This debate is well beyond the scope of the present review: to illustrate the variety and interest of EBSD data about these as yet incompletely understood phase transformations. In duplex stainless steels, both d and c phases are still present at room temperature, which facilitates the study of their OR. As solidied microstructures are very coarse, so that TEM based methods are not well suited. Note that c forms at high temperature (.1000uC) and that high thermal stresses are expected to arise from cooling due to the difference in thermal expansion coefcient between c and d. The effect of such stresses on
Table 13 Orientation relationships determined with EBSD in solid state phase transformations of non-ferrous and NiFe metal alloys Material Ti sheet Parent phase a (hcp) Product phase b (bcc) Analysis scale Grains and GBs (in situ) Orientation relationships Ref. Seward et al., 2004 Le Biavant et al., 2002 Banerjee et al., 2004 Bhattacharyya et al., 2003 Karthikeyan et al., 2005
Ti6Al4V Ti8Al(020)V Ti6Al2Sn4Zr6Mo Ti5Ta1.8Nb
b (bcc) b (bcc) b (bcc) b (bcc)
a (hcp) a (hcp) a (hcp) a (hcp)
Burgers; {334}b midrib parallel to the common close packed plane Macrozones Burgers for both primary and secondary a Along one GB with gradient Burgers (with one of chemical composition exception) a colonies near b GBs Burgers Widmanstatten colonies at GBs and primary a
Near-a a IMI834 Ti alloy
b (bcc)
a (hcp)
Colonies of a phase
Co Cu42 wt-%Zn Cu40Zn Cu11 wt-%Ag CuZnAl Pu2 at.-%Ga
b (fcc) b (bcc) b (bcc) b (Cu) b (bcc) e (bcc)
a (hcp) a (fcc) a (fcc) a (Ag) a (fcc) d (fcc)
Individual phases At least b grains Widmanstatten colonies Individual phases Individual variants of bainitic a phase A few d variants
Cu12.55Al4.84Ni P (DO3) (wt-%) shape memory alloy (SMA) Cu7.3Al8.5Mn (wt-%) L21 SMA Fe27.5Ni17.7Co3.8Ti c (fcc) SMA Fe32 at.-%Ni bicrystals c (fcc) Fe32.85 wt-%Ni c (fcc)
2H Microtexture of diamond (orthorhombic) shaped entities 18R1 (monoclinic) a9 (bcc) a9 (bcc) a9 (bcc) Microtexture of lens shaped entities Local scale before and after phase transformation Near the GB Individual variants
More or less close to Burgers, neighbouring Widmanstatten and primary a phases having same crystal orientation Germain Loss of Burgers OR; et al., 2005b common close packed planes preserved after spheroidisation of the a phase Near NW Wright et al., 2005 KS (from unpublished Sakata et al., pole figures) 2000 1.7u from KS; no strict OR Stanford and Bate, 2005 Cubecube, i.e. same Li et al., crystal orientation 1994 Pitsch Marukawa et al., 2000 Boehlert One common ,110.d: possibly KS or NW et al., 2003b {001}2H // {110}P and Chen et al., [010]2H // ,001.P 2000 Twin misorientation relationships (MRs) between product variants 80% of ORs at (5u from NW NW Near GT close to the midrib; near KS close to retained austenite; gradient of OR in between Near NW Probably KS for c/B2 and probably Burgers for a/B2 Habit plane 2u in average from [312] KS Wang et al., 2002 Bruckner et al., 1999 Ueda et al., 2001a Shibata et al., 2005
Fe29.6 wt-%Ni Ni/Ti/Ni multilayers Ti5Al2Sn4Zr4Mo 2Cr1Fe (b-Cez) alloy Ni(3638)Al (at.-%)
c (fcc)
a9 (bcc)
c-Ni (fcc), a-Ti NiTi (B2) (hcp) b (bcc) a0 Individual crystals (two (orthorhombic) perpendicular sections) Individual crystals b (B2) indexed c9 (L12) as bcc indexed as fcc
Former austenite grains, individual variants Average texture
Kitahara et al., 2005 Inoue et al., 2003 Zimmermann and Humbert, 2002 Sakata et al., 2001
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the OR (which is measured at room temperature) is not known yet. The OR was reported to be close to KS in as cast and as welded structures (Inoue et al., 1998; Pinol Juez et al., 2000; Gourgues et al., 2004). In some instances a unique OR, yet different from the well established ones, was identied (Nolze, 2004 and 2006). Widmanstatten austenite tends to grow along the common close packed direction of the KS OR and to share the same orientation as neighbouring allotriomorphic (primary) austenite phase (Inoue et al., 1998), possibly with only one adjacent d grain into which it is growing (Pinol-Juez et al., 2000). Even massive austenite forms in near KS OR with the parent d grain, at least in autogeneous gas tungsten arc welded, then liquid tin quenched 21Cr9.3Ni stainless steel (Inoue et al., 1995). Gas nitrided 22.5Cr5.4Ni1.9Mn3.0Mo0.16N
stainless steel, however, undergoes subsurface growth of needle shaped austenite having close packed planes at y15u from those of d ferrite (however, ferrite and austenite textures were not measured in the same sample) (Tschiptschin et al., 2002). Decomposition of ferrite into austenite has also been studied during heating in ferritic steels. To keep some austenite phase retained after cooling at the end of experiments, the low carbon steel studied (0.06C) was wrapped into either nickel or austenitic stainless steel foils before heating up to y900uC for a few minutes, to stabilise high temperature c by element diffusion (Bruckner et al., 2001; Park et al., 2002). The KS OR was not strictly followed (departing by up to 10 or even 25u). However, artefacts due to surface effects and to the local change in chemical composition still need further
Table 14 Orientation relationships determined with EBSD in solid state phase transformations of intermetallic alloys and quasicrystals Material Al62.5xCu25.3Fe12.2Bx Phase transformation Secondary phases in face centred icosahedral (fci) matrix during sintering Pack cementation Analysis scale Individual phases Orientation relationships No OR between fci and secondary phases {111}L12//{110}B2 and in that plane either ,112.L12//,110.B2 or ,011.L12//,111.B2 (001)[110]L12//either (011),111.B2 or (101),111.B2 or (014),041.B2 (110)bct//(111)L12 and [001]bct//[110]L12 Twin MR between variants consistent with a2 to O phase transformation (0001)a2//{111}c and ,1120.a2//,110.c z identification of order domains Burgers (0001)a2//{111}c and maybe ,1120.a2//,110.c (c indexed as fcc structure) (011)b//(0001)a92 and [111]b//[2110]a92 Burgers OR with one grain, growth into another one ,5u from KS with one b grain, no OR with the other neighbouring b grain Cubecube OR, rafting along ,100. direction Blackburn (see Appendix) Ref. Brien et al., 2004 Wollmer et al., 2003
Ni base superalloy coated with NiAl
Ni3Al coated with NiAl
Pack cementation
Individual phases (L12 phase indexed as fcc structure and B2 phase indexed as bcc structure) Individual phases
Zaefferer and Glatzel, 2002
Ni3Al coated with NiAl Ti25Al24Nb (at.-%)
Precipitation of body centred Individual phases tetragonal (bct) W2Ni A few O variants a2 into O
Zaefferer and Glatzel, 2002 Li et al., 2004
Ti48Al2Cr2Nb (at.-%)
a into massive c (indexed as fcc)
Individual phases
Pouchou et al., 2004a and 2004b Dupont et al., 1996 Buque and Appel 2002 Yang et al., 2003 Wang et al., 2002 Sakata et al., 2001 Stallybrass and Sauthoff, 2004 Dey et al., 2005 Lindsley and Pierron, 2000
Ti48Al2Cr2Nb (at.-%) Ni45 at.-%Al
a (indexed as hcp) into c Individual phases (indexed as fcc) a2 into cz spheroidisation of Individual phases a2 Individual phases Lamellar grains
Ti25Al10Nb2V1Mo (at.-%) b (B2) into a92 (DO19) Ti46.5 at.-%Al hcp a into massive L10 cz DO19 a2 (at GBs) b into c9 (partial, at GBs)
Ni36 at.-%Al
Individual phases
(Fe,Al,Ni)10Cr
a into A2 z B2 (ordering)
Individual phases
Ti46.8Al1.7Cr1.8Nb (at.-%) a into c (L10) z a2 (DO19) Udimet 720LI Ni base superalloy Interactions between recrystallisation of c matrix and c9 precipitates
Individual phases Former c grains
Mo z (210) single crystal MoSi2 Ti26Al27Nb0.03O
Diffusion couple, formation of Mo5Si3 bcc into O
Individual phases
Average texture
Loss of OR between c and c9: c9 keeps the cubecube OR with parent c grain or turns to twin OR with the recrystallised c grain Tortorici and [001] textured Mo5Si3 (cross-sectional observations) Dayananda, 1999 Boehlert and Results consistent with the following OR: (001)O//(110)bcc Bingert, 2001 and [110]O//[111]bcc
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(a)
(b)
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6 Interrelationships between morphology and ferrite cementite OR in pearlite. PitschPetch OR in a hypoeutectoid FeC and b hypereutectoid FeC if pearlitic ferrite is not connected to austenite grain into which it is not growing; c Bagaryatsky OR if pearlitic ferrite appears disconnected from neighbouring austenite grain (top) but is in fact connected as shown by further serial sectioning (bottom). After Mangan and Shiet (1999)
analysis. Synthetic Fe4Cr0.008C heated up to 820uC for 20 h and mapped with EBSD both before and after the heat treatment showed, in view of the interface migration velocity, that starting a phase and newly
formed c phase shared at least one common close packed plane (Watanabe et al., 2005b). The transformation of austenite into proeutectoid Fe3C cementite was investigated with EBSD together with 3D considerations in high-purity Fe1.34C 13.1Mn (Mangan et al., 1999; Kral and Spanos, 2003). Seventy ve per cent of the dendritic Fe3C particles exhibited the Pitsch, FarooqueEdmonds or ThompsonHowell ORs with the neighbouring c matrix. Monolithic Fe3C plates also exhibited the Pitsch OR, while conglomerates of parallel laths exhibited the FarooqueEdmonds OR. Many cementite crystals still exhibited no OR with neighbouring austenite. This was attributed to nucleation outside the investigated volume. Similar results were found with Widmanstatten cemen tite plates grown from austenite in an Fe0.8C12.3Mn steel (Mangan et al., 1997). Decomposition of austenite into ferrite, bainite or martensite is a key point in the processing of most high strength steel grades. Therefore, many results now complete the database acquired with TEM based methods for many years. One major difculty is the absence of retained austenite in many steels of practical interest. Details are given here for three kinds of phase transformations according to their temperature range: (i) martensite (ii) high temperature phase transformations, i.e. formation of idiomorphic, allotriomorphic and Widmanstatten ferrite
Table 15 Determination of OR between matrix and precipitates using EBSD Material Meteoritic minerals Sintered Ti4Fe7.3MozTiB Matrix Precipitate a (bcc) (Fe,Ni)3P b (bcc) Results Ref. Geist et al., 2005 Feng et al., 2005 Une et al., 2004; Une and Ishimoto, 2006
Zr cladded Zircaloy2 in various a (hcp) metallurgical states
SAF2507 superduplex stainless c (fcc) steel Super austenitic stainless steel c (fcc) Austenitic stainless steel c (fcc)
Austenitic stainless steel
c (fcc)
No simple OR (consistently with TEM results) TiB (Widmanstatten) [010] growth of needles (OR: by TEM) d (fcc) hydrides In general (0001)a//{111}d and ,1120.a//,110.d; GB d with such OR with only one neighbouring a grain; little effect of residual stresses s (decomposition 24u from the Nenno OR: here [101]c//[310]s of bcc d) s (111)c//(110)s and [211]c//[110]s (not the Nenno OR) Cubecube OR with one c grain, M23C6 growth with no OR into the neighbouring c grain 50% of particles in cubecube OR, M23C6 ,20% next to creep cavities
Dobransky et al., 2004 Lewis et al., 2006 Hong et al., 2001
Abdul Wahab and Kral, 2005
Table 16 Determination of OR using EBSD for discontinuous precipitation Material Cu11 wt-%Ag Cu4 wt-%Ti Parent phase b(Cu) (fcc) a (fcc) Product phases OR Ref. Li et al., 1994 Mangan and Shiflet, 1997
b(Cu)za(Ag) (all fcc) Cubecube a(Cu)zCu4Ti (orthorhombic) (111)a//(010)O and [011]a//[501]O or (511)a//(010)O and [011]a//[501]O Re and Ru rich nickel czc9 (same czc9ztopologically New c and c9 phases base alloy single crystal crystal orientation) close-packed phases keep cubecube OR Nitrided Fe(13)Cr a (bcc) azCrN a first cubecube with parent a grain but twin boundaries develop during growth because of high volume increase during phase transformation
Lavigne et al., 2001 and 2004 Sennour et al., 2004
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(iii) intermediate temperature phase transformations, i.e. acicular and bainitic ferrite.
Martensite
Martensite results from a displacive phase transformation and develops with a given OR with the parent austenite grain into which it grows. Austenite forming elements may be added to steel composition to retain some austenite, to facilitate investigation of the OR. Otherwise, the MRs between variants formed within a given former austenite grain may be compared to those calculated using known ORs, e.g. KS/KS or NW/NW MRs. The most frequently (tried and) found ORs were KS and NW for a9 (near bcc) martensite and Burgers for hcp e martensite (Table 17). It is then possible to derive the crystal orientation of parent austenite from those of martensite variants formed within that austenite grain. This can be performed by either graphical methods using {100} pole gures (Gourgues et al., 2000; Lambert-Perlade et al., 2004a; Cabus et al., 2004b) (Fig. 7) or by algebraic calculations from MRs between variants (Suh et al., 2002). The former method makes no particular assumption about the OR (except that it is close to the Bain OR), while the latter method assumes that the KS OR is strictly followed, which is never exactly the case.
Allotriomorphic, idiomorphic and Widmanstatten ferrite
7 Retrieving orientation of parent austenite grain (grey squares) from those of variants of product phase formed in it (here, bainitic ferrite in low carbon steel). After Lambert-Perlade et al. (2004a). Labels I, II and III denote three Bain zones derived from orientation of austenite
Orientation relationships between fcc and bcc phases have been investigated with high resolution EBSD in plessite, a mixture of fcc (taenite) and bcc (kamacite) phases found in iron and nickel rich meteorites. The OR varies between KS and NW according to the particular microstructure and chemical composition of phases (Nolze and Geist, 2004). As kamacite may be deformed, such determination may be difcult; close packed planes are not strictly parallel and continuous variations of the local OR may be found (Nolze et al., 2005). In Ni 43 wt-%Cr alloy solution (of course not a ferrous alloy) annealed at 1200uC for 1 h then aged at 1000uC, bcc Cr clusters exhibited close packed planes (respectively close packed directions) 1.27u (respectively 2u) in average from those of the fcc (Ni) matrix, i.e. the OR was up to 6u off KS and NW ORs (Adachi et al., 2005), irrespective of the deformation applied before ageing (Adachi and Tsuzaki, 2005). The OR between primary ferrite and austenite was generally determined by deriving the orientation of austenite from those of several neighbouring martensite variants after interrupted heat treatments (Suh et al., 2002). The assumption of KS OR is, however, a simplication as long as up to 1020% (respectively 50%) of the MRs between martensite variants departed
from the KS/KS one by more that 10u (respectively 5u) (Suh et al., 2002; Cho et al., 2002a; Hernandez et al., 2003). Thus, the method cannot be highly accurate. Even a shift of only a few degrees off the strict KS (or NW) OR leads to an uncertainty double as high for MRs between product phases which can reach at least 8u (Gardiola et al., 2003). In fact, near KS or NW ORs were generally found between primary ferrite grains and (at least) one of the surrounding parent austenite grains (Suh et al., 2002; Gardiola et al., 2003). Application of a loading stress may weaken the OR, as e.g. in 0.15C 1.4Mn0.25SiB and 0.33C1.5Mn2SiB steels transformed at 700uC under uniaxial compression (Suh et al., 2000; Kang et al., 2003). Primary ferrite grains may share a common orientation with neighbouring martensite resulting from quenching (Cabus et al., 2004b) or exhibit MRs far from KS/KS (Dey et al., 2005). Intragranular ferrite generally nucleates at inclusions, so that the austenite to ferrite OR strongly depends on the nature of inclusions. V(C,N) precipitates may break the austeniteferrite OR by introducing incoherent interfaces with one of the ferrite (or more probably austenite) phases, leading to ORs (if any) far from the Bain zone, e.g. Cho et al. (2002a and 2002b), Miyamoto
Table 17 Determination of ORs using EBSD between austenite and martensite in steels Steel composition 9Cr1MoNbV 0.2C12Cr1MoV 0.6C1.5Si1.5Mn 0.6C1.5Si1.5Mn Interstitial free and plain carbon steels (0.2 to 0.6C) AISI 301 0.13C austenitic stainless steel 19.6Mn3.1Si2.9Al Martensite phase a9 a9 a9 a9 a9 (ybcc) (ybcc) (ybcc) (ybcc) (ybcc) Investigation method MR between a9 variants MR between a9 variants OR between retained c and a9 OR between retained c and a9 MRs between a9 variants OR between a9 and c OR between e and c OR Near KS KS Near KS Close to NW and KS Near KS Near KS Burgers Ref. Nakashima et al., 2001 Dronhofer et al., 2003 Regle et al., 2004 Cabus et al., 2004a Morito et al., 2003 Lee et al., 2005 Godet et al., 2005
a9 (ybcc) e (hcp)
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(a)
(b)
(c)
8 Electron backscatter diffraction maps of primary and acicular ferrite from two adjacent austenite grains; ferrite grains in OR with a lower and b upper austenite grain; c corresponding {001} pole gures (no unique OR is found between ferrite and austenite in either case)
et al. (2003), Hernandez et al. (2003), Furuhara et al. (2003). Intragranular ferrite nucleated at deformation bands of strained austenite is also strongly textured according to the local orientation of austenite crystals (Hurley et al., 1999 and 2000; Hurley and Hodgson, 2000). Owing to high local misorientation in austenite, no classical OR was evidenced between austenite and ferrite (Hurley et al., 1999; Kang and Lee, 2004). Widmanstatten ferrite also exhibits ORs close to the Bain zone with the parent austenite grain, e.g. in iron meteorites (He et al., 2005), although the OR may continuously vary along the interphase interfaces (He et al., 2006).
Acicular and bainitic ferrite
Mechanisms of austenite to bainite phase transformations are still highly controversial (Hillert et al., 2002). Just as similar ORs prevail for both diffusive (e.g. primary ferrite) and displacive (e.g. martensite) decomposition of austenite, they also prevail for acicular ferrite (Fig. 8) and bainitic ferrite. Plate and lath bainite are a multiple scaled microstructure. Constitutive units are readily studied by TEM; they cluster into packets (or sheaves) whose size is close to the former austenite grain size, so that the size and morphology of packets is best studied using either SEM or light optical microscopy, and their crystallography using EBSD. Bainite packets often contain a high density of LABs (e.g. Tsunekage and Tsubakino, 2002; Lambert-Perlade et al., 2004a). In low carbon steels, the austenite phase is generally no longer present at room temperature, so that ORs are generally studied by reconstructing the average crystal orientation of individual austenite grains (Lambert-Perlade et al., 2004a) (Fig. 7) or by comparing MRs between packets to those calculated using, e.g. KS and NW ORs (Gourgues et al., 2000). Results obtained with EBSD (Table 18) generally well agree with those obtained with TEM at the same scale. By considering the {001} pole gures, e.g. those from Gourgues et al. (2000) and Verlinden et al. (2001) and the high
frequency of LABs in upper bainite packets, one nds that no unique OR is generally followed: there are preferred ORs and continuous (although minor in number) data points between these preferred ORs. The same applies for acicular ferrite (Fig. 8c). Such data can only be obtained by automated analysis over large areas, which are now made possible by EBSD. Thanks to eld emission gun (FEG)-SEMs, local ORs along bainite laths can also be checked. In a 0.6C1.5Si1.5Mn steel, the orientation gradient along bainitic laths maintained the KS OR with neighbouring lm like austenite (Regle et al., 2004). Owing to its limited angular accuracy, EBSD is not the best tool to precisely determine an OR, for which TEM based techniques appear best suited. However, FEG-SEMs now provide high spatial resolution, allowing local analysis over wide areas and thus good statistics. There is hardly a unique OR at room temperature, in particular in metals, because local residual stresses or plastic rotation develop either during the phase transformation or during cooling. The induced crystal rotation or distortion may modify a genuine OR obeyed at the very beginning of the phase transformation. Therefore, for most applications, the angular accuracy of EBSD is generally high enough for OR determination. As with other diffraction techniques, ORs may be represented with pole gures, including higher index poles for which known ORs yield easily recognisable patterns, which can be compared with experimental data collected from a single parent grain (Nolze, 2004 and 2006). Convoluted pole gures may be calculated by the EBSD software to improve accuracy and sharpness and facilitate such comparisons (Nolze, 2004). The RodriguesFrank space is also increasingly used for ORs between fcc and bcc phases (He et al., 2005). Euler angles may also be useful in certain cases, provided that an uncertainty interval is suitably given (Nolze et al., 2004).
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Ferry and Xu, 2004 Marrow and Cetinel, 2000 Marrow et al., 2001 Regle et al., 2004; Cabus et al., 2004a; Cabus, 2005 Godet et al., 2001
Heterogeneous nucleation
Gourgues et al., 2000 Gourgues et al., 2000 Gourgues et al., 2000 Lambert-Perlade et al., 2004a
Close to KS Close to KS ,5u from KS Locally rather close to KS (1u from neighbouring pixels) Hot rolling z step quenching (400uC) Bainitezretained austenite Not exactly KS (bainite is deformed) Step quenching (400uC) Bainitez1520% retained Not exactly KS austenite Bainitezretained austenite Close to KS or NW Step quenching (400uC) Cold rolling z intercritical tempering Very close to KS (both with z step quenching TEM and EBSD) Thermally simulated coarse grained HAZ Upper bainite Closer to NW than to KS Weld metal deposit Acicular ferrite Closer to NW than to KS Controlled hot rolling Upper bainite Closer to NW than to KS Thermally simulated coarse grained HAZ Upper bainite Not necessarily KS or NW, also close to other less classical ORs Weld metal deposit Acicular ferrite Near KS (point analysis) Step quenching Bainite No MR between 20 and 47u, consistent with KS or NW Step quenching Acicular ferrite MRs ,5u from KS/KS variants Sand casting Austempering Austempering Step quenching Ausferrite (azc) Ausferrite (azc) Ausferrite (azc) Bainitezretained austenite 3.2C1Cu2Si0.55Mn 3.6C0.3Cu2.5Si0.6Mn0.15Mo 3.6C0.3Cu2.5Si0.6Mn0.15Mo 0.6C1.5Si1.5Mn 0.07C0.3Si1.5MnCrMoNiNb 0.07C0.2Si1.6MnCrNiNbTiVB 0.2C0.2Si1.4MnCrMoNi (A533) 0.07C0.3Si1.5MnCrMoNiNb Low carbon steel 0.09C0.5Si1.9MnBO Low carbon steels 0.06 to 0.1CMnSiCuNiCr Low alloy, Sibearing steel 0.39C1.37Si1.45Mn 0.2C0.5Si1.4Mn0.7Al 0.4C1.5Si1.5Mn TRIP steel TRIP steel Cast iron Cast iron Cast iron TRIP steel TRIP steel TRIP steel HSLA steel Low carbon steel Low alloy steel HSLA steel Low carbon steel 0.2C2Mn0.3VNS
Investigation of homogeneous nucleation requires a high density of nuclei and high resolution EBSD to get good observation conditions. The EBSD analysis of Fe nanodendrites during crystallisation of Fe74Si11B14Ni1 amorphous powders during isothermal annealing has been reported (Godec et al., 2006). On the other hand, nucleation in solid state phase transformations is most often heterogeneous and relies on crystal structure and orientation of both parent and product phases, so that heterogeneous nucleation has been extensively studied with EBSD. This section focuses on nucleation of both precipitates and matrix phases.
Heterogeneous nucleation of precipitates
Kluken et al., 1991 Daz-Fuentes et al., 2003
Verlinden et al., 2001 Zaefferer et al., 2004
Ref.
Godet et al., 2004
Miyamoto et al., 2003
Austenitic and duplex stainless steels suffer from boundary precipitation of chromium rich phases after particular heat treatments or during high temperature service. By analysing a number of GBs with EBSD it was shown in both duplex (Sato et al., 1999; Sato and Kokawa, 1999; Dobransky et al., 2004) and austenitic AISI 304 (Zhou et al., 2001; Hong et al., 2001) stainless steels that secondary Cr23C6 and s phases hardly nucleated, or at least nucleated much more slowly at coincident GBs (or near KS interphase interfaces). Comparing EBSD maps and corrosion tests at the same scale yielded statistically reliable data upon sensitised grain or phase boundaries. Other criteria, such as plane matching boundaries or near coincident axial direction did not seem to be selective enough. Even the well known Brandon criterion for coincident site lattice boundaries was not always selective enough, especially for LABs (Zhou et al., 2001). Precipitate nucleation has been studied with EBSD in a variety of materials for nuclear power generation. In Ni16Cr9FexC alloys, random GBs are favourite paths for intergranular stress corrosion cracking and also for precipitation of M23C6 (M,Cr) carbides (Alexandreanu et al., 2001). Here again, the GB structure seems to inuence the precipitation kinetics, morphology and size distribution of carbides (Liu et al., 1995). Hydridation of uranium and zirconium alloys is also affected by the local GB structure; in as cast uranium, hydrides form at twin boundaries and at LABs, which are readily imaged with EBSD but not with light optical microscopy (Bingert et al., 2004). The spheroidisation of pearlite in 0.36C0.53Mn 0.22Si steel was further investigated with EBSD, by monitoring LABs after thermomechanical treatments and imaging dissolution and reprecipitation of cementite coupled with continuous recrystallisation of ferrite grains (Storojeva et al., 2004). Discontinuous reactions have also been investigated with EBSD. In Fe50 at.-%Co, discontinuous ordering starts from GBs, but LABs and some coincident site lattice boundaries seem much less sensitive (Bischoff et al., 1998; Semenov et al., 1998). The local extent of the reaction depends on both crystal misorientation and orientation of the GB plane (Bischoff et al., 1998). Such information can be gathered with EBSD (associated with determination of the local 3D boundary geometry) over a statistically signicant number of grains or GBs (more than 200 in this particular example). This would not be possible by using other diffraction methods.
Table 18 Determination of orientation relationships using EBSD between austenite and acicular or bainitic ferrite in steels
Material
Chemical composition (main elements) Heat treatment
Microstructure
OR
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Similar studies have been carried out for discontinuous (cellular) precipitation in Mg10 wt-%Al (Mg z Mg17Al12) (Bradai et al., 2002) and nickel base single crystal superalloy (c z c9 z topologically close packed phases) (Lavigne et al., 2004). Here, LABs (Lavigne et al., 2004) or GBs with low index misorientation axes (Bradai et al., 2002) were less sensitive to the involved reaction. In Cu4 wt-%Ti, Mangan and Shiet (1997) combined EBSD with careful serial sectioning to show complex interactions between the moving boundary of (fcc azorthorhombic Cu4Ti) colonies and the twin boundaries of the starting microstructure.
Heterogeneous nucleation in matrix phase transformations
(a)
Nucleation of major phases is of course also strongly inuenced by local crystallography. In white cast irons, phase transformation from eutectic cementite (Fe3C) into graphite involved nucleation of graphite at curved ferrite/Fe3C interfaces; however, no nucleation occurred at straight interfaces parallel to the [001] direction of Fe3C and to the normal direction of the product (Song et al., 2002). Most reported EBSD studies on this topic focused on steels. In situ light optical microscopy observations of ferrite to austenite phase transformation of a coarse grained Fe4.8 at.-%Cr0.008C alloy coated with SiO2 showed preferential nucleation of austenite at triple junctions involving three random ferrite HABs; the higher the number of special boundaries connected to the triple junction, the lower the probability for austenite to be found there (Watanabe et al., 2005b). However, the use of coarse grained material (to get only one grain in thickness) does not prevent from free surface effects and from rather low statistics of results. In a low carbon steel wrapped into an austenitic stainless steel foil and heat treated in molten salt baths, no preferential nucleation of austenite was found near special grain boundaries (Bruckner et al., 2001). Nucleation of primary ferrite at ferrite/austenite phase boundaries of a 0.15C1.4Mn0.25Si0.006B steel at 700uC was strongly favoured by an applied stress, due to a less strictly observed OR and thus to an increase in the phase boundary energy; this effect seemed stronger than at austenite GBs (Suh et al., 2000). Nucleation of intragranular ferrite at secondary phases or inclusion particles has been widely studied by TEM (although the probability to nd a nucleation site in a TEM thin foil is low) and by EBSD over a large variety of inclusions (van der Eijk et al., 1999). The effect of deformation of the austenite phase on nucleation of ferrite has also been studied with EBSD, especially in ultrane grained ferrite formed at deformation bands and cell boundaries of hot rolled austenite (Hurley et al., 2000, Hurley and Hodgson 2001). In contrast, austenite LABs did not inuence markedly its transformation into martensite after accumulated roll bonding (Kitahara et al., 2004). Nucleation of acicular ferrite at TiN particles may occur with an OR between every individual ferrite phase and the TiN particle (Jin et al., 2003). In low carbon steels, the competition between acicular ferrite and bainite at the austenite/ ferrite phase boundaries depends on both the chemical composition and the austenite grain size (Daz-Fuentes et al., 2003). The formation of Widmanstatten ferrite sideplates at primary ferrite crystals already formed at former
(b)
(c)
a no variant selection; b local, but no average variant selection; c local and average variant selection 9 Two-dimensional view of variant selection (one variant per shape)
austenite GBs was shown thanks to EBSD and serial sectioning to occur not by interfacial instability but by nucleation and growth of individual plates. A distinct GB (and a 510u low angle MR) was found with EBSD between Widmanstatten sideplates and primary ferrite from which they were growing (Spanos and Hall, 1996; Phelan and Dippenaar, 2004; Phelan et al., 2005). As nucleation events are distributed everywhere within the material, 3D observations are often necessary; TEM seems best suited to ne scale and nely dispersed nucleation events; for scarcely distributed nucleation sites, 3D investigations involving EBSD can be better suited due to both statistical relevance of data and the possibility to perform serial sectioning.
Evidence of variant selection

Given an OR between parent and product phases, there are a xed number of crystal orientations of the product phase that can form from a given crystal of the parent phase. These are called variants. Not all possible variants are generally observed in metallographic sections of former individual grains of the parent phase. This can be due to either sampling effects or to a true variant selection, or both. Variant selection is illustrated in Fig. 9. Variant selection is readily studied at the scale of the former parent grains by TEM or EBSD and, from a statistical point of view, using the average texture of the material (obtained by, e.g. neutron diffraction, XRD or EBSD). Both approaches have successfully used EBSD in a number of materials. At the scale of individual parent grains, the microtexture may readily
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10 Variant selection evidenced with EBSD in Fe 32 at.-%Ni bicrystal containing 90u ,211. tilt boundary and transformed under tension at 45u from tilt axis. Only variants V29 and V3 are found in each austenite grain near GB. After Ueda et al. (2001b)
be investigated; at the global scale, such as with XRD, the experimental ODF is compared to that calculated from the orientation of the parent phase by assuming an OR to be strictly obeyed (with or without variant selection criteria).
Martensitic transformations in shape memory and FeNi alloys
and misorientation between GB and tensile axis, variant selection favoured martensite crystals having a habit plane parallel to the GB plane and enhancing accommodation of the transformation strain across the GB (Ueda et al., 2001b). This stands generally for other tilt angles under no applied stress (Ueda et al., 2003a) and in prestrained 90u,211. bicrystals (Ueda et al., 2001a). For 90u {211} bicrystals, no strain accommodation was possible through variant selection across the GB, so that the martensite start temperature was lower. However, variant selection was also found (Ueda et al., 2001b) together with local plastic deformation on the other side of the GB (Ueda et al., 2001a). As residual stresses (resulting from only partial accommodation of transformation strains) were higher in the twist than in the tilt bicrystal, a better memory of the starting austenite crystal orientation was observed after reverse transformation of the twist bicrystal while many LABs appeared in the new austenite phase of the tilt bicrystal (Ueda et al., 2003b and 2004). Owing to the large size of bicrystals together with the small size of individual martensite variants, multiscale EBSD study was a key tool to investigate phase transformations in such materials.
Non-ferrous metal alloys
In NiTi shape memory alloys (SMAs) fabricated by accumulative roll bonding of Ni and Ti foils, NiTi does not directly form from Ni and Ti phases and intermediate compounds such as Ni3Ti and Ti2Ni are involved. However, a KS OR is observed between Ni and NiTi and a Burgers OR is observed between Ti and NiTi, suggesting that intermediate phase transformations involve variant selection (Inoue et al., 2003). Local variant selection was shown in Fe27.5Ni17.7Co3.8Ti quenched at 196uC (Bruckner et al., 1999). Variant selection was also suggested by average texture calculations in undeformed (but not in deformed) Fe28Ni 0.02C (wt-%) (Kestens et al., 2003) (with the Bain OR, however, which is not exactly relevant in that case). The detailed microtexture of fork and spear like martensite in Cu7.3Al8.5Mn (wt-%) (among 24 possible variants of 18R1 martensite) showed two groups of two variants of common spatial but different crystal orientations (Wang et al., 2002). Self-accommodating variants, twin related by {121}2H and {101}2H planes respectively were found in spear like and fork like martensite of Cu12.55Al4.84Ni (wt-%) after transformation of DO3 austenite (Chen et al., 2000). At the scale of parent grains, not all possible variants are generally found by EBSD in e.g. Fe29.6 wt-%Ni (Kitahara et al., 2005) and Co thin lms (Hesemann et al., 2001), where variants such that {0001}hcp//{111}fcc at 20u from the surface of the lm are favoured. The formation of lenticular martensite in Fe(31 32) at.-%Ni bicrystals was extensively investigated using EBSD, in particular for symmetric ,211. tilt (Fig. 10) and 90u {211} twist boundaries. In single crystals of similar chemical composition, all 12 possible variants were observed, even when transformation occurred under applied stress (Ueda et al., 2001b). For bicrystals having a tilt boundary and whatever the applied stress
Some examples of variant selection evidenced (or not evidenced) by EBSD in titanium and zirconium alloys are given in Table 19 at various scales. In hot rolled b (bcc) heat treated Cu40Zn alloys, which then partially transformed into fcc a during cooling, coarse a grains with strong internal misorientations were found. The a phase formed from cold rolled and annealed (but not recrystallised) b showed only one Bain zone (i.e. near KS or NW ORs clustered around the same 45u,100.b Bain OR). This suggests strong variant selection that, surprisingly, decreased with the transformation temperature (Yasuda et al., 1999). Such variant selection was also found for (azb) heat treated Cu42 wt-%Zn, at least for a grains that were clustered into bands (Sakata et al., 2000). In Al36Mo17Ti (at.-%), thermal cycling across the b (A2) into Al3Ti (DO22)zMo3Al (A15) eutectoid phase transformation temperature tended to maintain the initial orientation of the b phase, showing a memory effect on texture and thus involving variant selection in both eutectoid and reverse phase transformations (Miura et al., 2004 and 2005a). In near-c Ti 46.8Al1.7Cr1.8Nb (at.-%), orientation of both Widmanstatten and lamellar c crystals strongly depends on twinning in the parent a phase, leading to particular MRs between neighbouring Widmanstatten and lamel lar c phases (Dey et al., 2005).
Steels and ferrous alloys
Variant selection in ferrite (a) to austenite (c) phase transformation has only been scarcely studied in low carbon steels, as the c phase cannot be retained at room temperature. In a cold rolled 0.065C1Mn steel, Park et al. (2002) found variant selection from average texture measurements. By measuring average textures of interstitial free steels before and after complete a to c then back to a phase transformations, Ryde et al. (1999) showed no variant selection in the absence of titanium, but a strong memory of initial texture in Ti bearing steels, possibly due to some retained ferrite in the vicinity of TiN particles. However, such studies are very
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Table 19 Evidence of variant selection aided by EBSD in hcp metals and metal alloys (items in italics more specically address variant selection at parent grain boundaries) Scale of EBSD investigation Average and local texture Results Ref. Gey and Humbert, 2002
2007
Material
Parent phase Product phase
Cold rolled Ti
VOL
52
b a b
NO
Ti Ti Cold rolledzb heat treated IMI 834 Ti alloy Ti6Al4V
Wang et al., 2003 Seward et al., 2004 Germain et al., 2005a and 2005b Humbert et al., 1994 Gey et al., 1996 Stanford and Bate, 2004
Up to 30% hot rolled Ti6Al4V Hot rolledzheattreated Ti6Al4V
Ti6Al2Sn4Zr6Mo
Bhattacharyya et al., 2003
Ti8AlxV (laser deposited) b
Banerjee et al., 2004
Zircaloy4
In addition to strengthening of texture of the b phase, variants almost common to adjacent b grains are selected a9 (lath martensite) One parent b grain From MRs between variants, there is variant selection b (plates z allotriomorphs) Parent a grains Variant selection probably mainly during growth of the b phase Primary and secondary a Macrozones (large clusters of b No particular variant selection for primary a; strong variant selection grains of similar crystal orientation) (only one texture component) for secondary a a plates (diffusional Average texture and individual No variant selection in average; at least three families of a plates mechanism) parent grains per b grain a (diffusional) Average texture and individual No variant selection in average; all 12 variants found in each parent grains parent b grain a (diffusional) Average texture and along Evidence of variant selection at GBs individual GBs two alternating variants of primary a; LAB between Widmanstatten and primary a if no special OR between b grains; ,0001.a//common ,110.b if existing Widmanstatten and GB a Parent b grains Widmanstatten variants as close as possible to primary a while obeying the Burgers OR with the parent b grains into which they are growing. If not possible, parallel close packed directions as close as possible to the parent GB GB a Along one huge GB over the whole Two alternating variants with {0001}a// to the same {110}b, misoriented 10u from another; OR strictly obeyed on one side, as closely as composition range possible with the other parent grain a (diffusional) Average texture There is variant selection, especially when no stress is applied
Gey et al., 2002
Gourgues-Lorenzon
difcult and the majority of results concern transformations from austenite to ferrite (or martensite) in steels.
Diffusional formation of primary ferrite
Globular ferrite growing from residual d ferrite of strip cast 0.1C0.17Si0.6MnP steels obviously shows a strong texture (with only internal LABs) within alignments (Umezawa et al., 2003). If no d ferrite is retained (i.e. for the majority of ferritic steels), variant selection depends on the deformation state of parent austenite. In weakly prestrained austenite of a 0.3Si1.5Mn steel, coarse primary ferrite formed from coalescence of a grains of close crystal orientations (i.e. from the same variant). For strains higher than y40%, neighbouring a grains formed as misoriented variants (Torizuka et al., 2000). In a 0.002C1.66MnSiMoNiAl steel vacuum cast into 2 mm thick sheets and then hot rolled, a strong texture was found in individual former c grains, strongly depending on the c crystal orientation, but well predicted by using all 24 KS variants, so that no variant selection could be evidenced (Hurley et al., 1999). The diffusional formation of primary ferrite may also be signicantly driven by free surface energy, such as in coarse grained ferritic steels obtained by intercritical annealing (i.e. in the azc temperature range) in a decarburising atmosphere. Carbon depletion starting from free surfaces induced transformation of the two phase alloy into a fully ferritic microstructure. Abnormal grain growth then occurred due to the lower free surface energy of {100} grains and to some memory of the initial texture and grain size effect, so that a coarse grained microstructure with a desirable {100} texture was nally obtained (Tomida, 2003; Tomida et al., 2003; Dzubinsky et al., 2004).
Transformation of austenite into Widmanstatten ferrite, bainite and martensite
packets, although it could possibly exist according to near KS ORs (Fig. 12). Thus, as evidenced by local histograms of misorientation angles, there are forbidden pairs of neighbours and thus local variant selection, even if it may have no consequence on the average texture (Gourgues et al., 2000; Gourgues, 2003). In hcp e martensite (Godet et al., 2005) showed only two over the four possible {111}c parallel to {0001}e in a 19.6Mn3.1Si2.9Al steel, suggesting that there could also be variant selection in this case. In AISI 304 austenitic stainless steel tensile deformed at 60uC, e martensite appeared in parent grains as families of parallel bands (one variant per family). Within these bands, e martensite then probably partially transformed into bcc a9 martensite having one {110} plane parallel to the (0001)e plane. Six variants out of 24 were thus selected for each band family. Moreover, there was further local variant selection among these six variants (Gey et al., 2005).
Variant selection at parent grain boundaries
Whatever the transformation mechanism, variant selection in bainite and Widmanstatten ferrite has already been widely investigated with EBSD (Table 20). Owing to the coarse size of bainite packets with respect to the parent c grain size, a relatively low number of packets are generally observed within a given c grain by 2D sectioning. This leads to signicant sampling effects. The complex, non-convex and non-equiaxed shape of bainite packets may also lead, even in the absence of variant selection, to an inhomogeneity in variant distribution due to the morphological orientation of packets with respect to the sample surface plane (Fig. 11). This purely geometric phenomenon has recently been called pseudo variant selection (Cabus, 2005). By assuming a given shape and habit plane of bainite packets, one can attempt to process microtexture data to take pseudo variant selection into account in each parent austenite grain (Cabus, 2005). Nevertheless, the vast majority of literature data does not take either these considerations or even the (sometimes low) number of analysed c grains into account. Variant selection is generally investigated at the scale of the former c grain (i.e. from the resulting local texture or number of bainite variants). In some instances, however, such as in fatigue and cleavage crack propagation, the relevant parameter is the misorientation between neighbouring packets only. Whatever the bainitic or lath martensite microstructure, no misorientation angle of y20u was found between neighbour
Intergranular nucleation of a new matrix phase involves at least three contributions to the change in free energy: (i) GB interfacial energy (ii) chemical variation in free energy due to phase transformation (iii) interface and strain energy of coupled new phase and individual matrix grains. (i) and (iii) are variant dependent, so that new variants may tend to obey a given OR with both parent grains. This is best studied with EBSD, especially if the parent grain size is coarse. Examples from hexagonal metals and metal alloys are given in italics in Table 19. In Cu40Zn with {001},110. textured bcc b, fcc a variants either of close crystal orientations or in twin MR formed on either side of the b GBs. Coarse a colonies nucleated on either side of the same GB generally shared at least a common low index direction, with ,111.a directions close to the common ,110.b. In contrast to Ti alloys, this has only little effect on the average texture (Stanford and Bate, 2005). In Ni43Cr heat treated in the fcc c phase range and then cooled down slightly below the solvus of the bcc a phase, when existing, the only variant selected was that having a KS OR with both c grains; otherwise, selected variants obeyed the KS OR with one c grain, and had their close packed plane of the OR as close as possible to the c GB plane (Adachi and Tsuzaki, 2005; Adachi et al., 2005). In cold rolled low alloy (0.065C0.05Si0.99Mn) steel annealed in the c temperature range, EBSD results suggested that a memory of the initial a crystal orientation still existed, with selection of a variants in KS OR with the neighbouring c grains (frequently in KS OR themselves with the same initial a crystal) (Bruckner and Gottstein, 2001). Such variant selection was also observed in a 0.15C0.3Si1.42Mn steel after hot torsion (Novillo et al., 2004). In austenitic 0.0015C22Cr(8 9)Ni stainless steels, gas tungsten arc welding followed by liquid tin quenching showed that at least at the beginning of bcc d to fcc c phase transformation, c variants at d GBs were more frequently in KS OR with both neighbouring d grains than with one d grain only (Inoue et al., 1998). The same result was found in annealed and quenched duplex stainless steels (Gourgues et al., 2004; Monlevade et al., 2006) (Fig. 13).
2007
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89
90
Table 20 Evidence of variant selection aided by EBSD in formation of bainitic or Widmanstatten ferrite* Analysis technique Number of variants per c grain One huge c grain analysed Individual orientation of variants Several variants per c grain Results Variant selection Ref.
Gourgues-Lorenzon
Alloy composition
Final microstructure
3.2C1Cu0.55Mn2Si
NiFe-rich meteoritic mineral Low alloy, Si bearing (TRIP)
As cast grey iron: bainitezretained c Widmanstatten a Bainitezretained c
Not enough data Ferry and Xu, 2004 to conclude No He et al., 2006 Yes Godet et al., 2001 Verlinden et al., 2001
Possibly yes
De Meyer et al., 2001
2007
Possibly yes
VOL
Regle et al., 2004; Cabus et al., 2004a
52
Yes
Hase et al., 2004
NO
Yes Yes
Cabus, 2005 Godet et al., 2004
Possibly yes
Jonas et al., 2005
Possibly yes
Matsuoka et al., 1999 Locally yes
All 12 near NW variants were found Variants selected according to active slip systems 0.39C1.37Si1.45Mn (TRIP) Lath bainitezretained c Number of morphological variants; Lower number of morphological variants average texture within parent c grain for step quenching from deformed c; maximum intensity of texture varies from one c grain to another 0.19C1.46Si1.57Mn and Bainitezretained c Average texture of c calculated from {001},100.c weaker (respectively stronger) than predicted for AlSi (respectively Al free) 0.31C0.34Si1.57Mn1.23Al (TRIP) that of bainite steel 0.6C1.5Si1.5Mn (TRIP) Bainite z .20% Number of variants per c grain (over Less than the 24 possible KS variants; close czmartensite a few c grains) packed planes of KS OR are parallel to only one or two {111}c planes; possible sampling effects? 0.79C1.56Si1.98Mn1.01Al Carbide free bainite Trace of bainite packets, morphology Traces are parallel to maximal shear planes; 0.24Mo1.01Cr1.51Co (TRIP) of crystallographic packets packets are better aligned if transformed under compression 0.6C1.5Si1.5Mn (TRIP) Bainitez .20% cz Average a and c textures taking pseudo Close packed planes of near KS OR are martensite variant selection into account parallel to one or two dominating {111}c planes. 0.4C1.5Si1.5Mn (TRIP) Bainitez1520% c from Number of KS variants per parent c All 24 variants are found for e50.2, not all for c deformed grain e50.8; internal misorientation increases with by 0.2 or 0.8 increasing deformation of austenite 0.22C1.6Si1.5Mn0.045Nb (TRIP) Bainitezretained c NW variants v. active partial dislocation In a given c grain, both variants associated slip systems to active slip system and opposite system are found 0.04C0.2Si1.5MnNiNb (HSLA) Elongated bainite along MRs between bainite colonies Low (,15u) misorientations: one colony per c the hot rolling direction grain. Possibly one colony 5 1 to 2 closely oriented KS variants 0.07C0.32Si1.5MnCrMoNbV Lath bainite from coarse MRs between packets compared to KS Close packed planes of OR parallel to different (HSLA) grained c or NW related MRs {111}c planes in neighbouring packets; there are locally forbidden MRs Locally yes
0.2C0.25Si1.38MnCrMoNi AlNbTiV (A533)
Tempered bainite
Gourgues et al., 2000; Lambert-Perlade et al., 2004a Gourgues et al., 2000
0.05C0.5Si1.6MnV (HSLA)
Yes Locally yes
Humbert et al., 2002b Gourgues, 2003
0.15C2.25Cr1Mo, 0.05C9Ni, 0.07C0.4Si1.4MnV
0.2C0.5Si1.4Mn0.7Al (TRIP)
MRs between packets compared to KS Upper bainite: close packed planes of OR parallel or NW related MRs to different {111}c planes in neighbouring packets; lower bainite: close to martensite microtexture (see section on microtextures) Bainitezretained c Average texture, NW ORs Experimental texture not the same as calculated one Upper bainite (simulated MRs between packets, size of cleavage Upper bainite: many internal LABs; lower bainite: coarse grained HAZs) facets many HABs; there are locally forbidden MRs. Cleavage facets of same size as c grains Ferritezbainite shellz Local MRs LABs between ferrite and bainite: bainite orientation retained c dictated by that of ferrite
Yes
Zaefferer et al., 2004
*TRIP: transformation induced plasticity aided steels; HSLA: high strength low alloy.
Gourgues-Lorenzon
11 Sectioning effects inducing pseudo variant selection, here in case of rod shaped phases: area intercepted by sectioning plane (in white) is schematically represented in dark grey; variants having their long axis closest to sectioning plane have high apparent fraction
In summary, EBSD investigations of various metal alloy systems showed that at GBs of the parent phase, variant selection may occur, favouring those variants either obeying as strictly as possible the OR with both parent grains, or having a special OR with the GB plane.
12 Histogram of misorientation angles in low carbon steels, showing apparently forbidden pairs of neighbouring ferrite variants. Arrows denote theoretically possible angles between pairs of variants in KS or NW ORs with parent austenite grain into which they grow. After Gourgues et al. (2000)
Examples of practical applications of variant selection

Grain boundary engineering (GBE) through phase transformations
Grain boundary engineering is a method by which, through well controlled metallurgical and thermomechanical processing, special GBs are strongly favoured leading to improved product properties (see e.g. Watanabe, 1984). This has been made possible by extensive EBSD characterisation (Gourgues, 2002). The GBE is generally achieved through series of hot working and annealing treatments, making use of grain boundary motion, recrystallisation and annealing twinning. However, variant selection in phase transformations could be another way to produce special GBs
between grains of product phases through controlled phase transformations. The feasibility of GBE was shown in orthorhombic TiAlNb alloys by various metallurgical routes (Li et al., 2004; Boehlert et al., 2004; Li and Boehlert, 2005a). According to the DO19 a2 or ordered B2 parent phases, special MRs were found between orthorhombic O grains. Some MRs between variants were favoured (e.g. 65u,001. or 90u misorientations). Other MRs seemed to be locally forbidden (e.g. 30u,001. starting from the a2 phase). Local texture could thus possibly be tailored through variant selection, even for random average textures. The GBE might also be achieved by phase transformation under particular conditions, such as in paramagnetic fcc austenite into ferromagnetic (pearlitic) bcc ferrite in a medium carbon steel (Zhang et al., 2005) and in a 1.0CSiMnCr steel (Zhang et al., 2006). A high applied magnetic induction (12 to 14 T) both increases
a light optical micrograph; b EBSD map of same area (ferrite in black, austenite in various grey levels) 13 Growth of austenite colonies across parent ferrite grain boundaries in cast duplex stainless steel. Austenite colonies keep near KS OR with both ferrite grains. Ferrite GB is delineated with broken white line. After Gourgues et al. (2004)
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the transformation temperature and strongly decreases the amount of LABs between ferrite crystals. Grain boundary engineering on one phase (or more) at a time might also be achieved in two phase alloys such as in azb9 Cu40 wt-%Zn alloys (Lee et al., 2003). Conversely, variant selection could possibly be used to avoid certain low strength GBs in product phase, such as 90u MRs between hcp a grains in Ti6Al4V (Bieler et al., 2005a); this would be very useful to avoid extensive cavitation of such GBs during upset forging.
Preventing growth and coarsening of ferritic steels
Among the practical issues of phase transformations, structure renement is achieved by monitoring not only the number of nucleated grains, but also the evolution of microtexture during or after phase transformation. As an example, it is still very difcult to achieve a grain size lower than y5 mm in ferritic steels, although the high number of nucleated grains should lead to a ner ferrite grain size. This is attributed to coarsening, a phenomenon which is intimately related to the microtexture of the initially formed ferrite. Thus, coarsening could be limited by better control of the phase transformation stage, where EBSD is of great help as illustrated in Table 21. The EBSD was used here to investigate, over a signicant number of grains, the deviation from strict OR (and thus decreasing probability that ferrite grains of the same crystal orientation nucleate close to each other and eventually coalesce) and to quantitatively dene the grain size by a threshold criterion involving the misorientation angle.
Microtexture: relationships between morphology and local crystallography

Owing to anisotropic interfacial energy or to transformation strains, there can be strong correlation between crystal orientation and morphology resulting from solid state phase transformations (see e.g. habit planes of martensite or of certain precipitates). The morphology of phases may be observed using conventional light microscopy or SEM imaging techniques. However, if product phases come in intricate or complex shaped entities, or if only 2D trace analysis is possible, such techniques may give a confusing appearance of product phases. One must then distinguish between what appears by imaging (here denoted as morphological entities) and true crystals surrounded by user dened boundaries (here denoted as crystallographic entities). The right scale is generally that of the SEM/EBSD technique. Several cases have been encountered using EBSD, namely: (i) several morphological units may belong to the same crystallographic unit, as in e.g. pearlite colonies of pearlitic steels (Aernoudt et al., 2005), in misoriented intragranular ferrite nucleated at a given inclusion, in acicular ferrite in certain low carbon steels (Daz-Fuentes et al., 2003), in hcp a phase colonies from bcc b phases in Ti6Al2Sn4Zr6Mo (azb) titanium alloy [close Burgers variants in that case (see Bhattacharyya et al., 2003)] and in plates or conglomerates of laths in proeutectoid Fe3C of a Fe1.34C13.1Mn steel (Mangan et al., 1999) (ii) several crystallographic units may be morphologically parallel and become undistinguishable from each other in 2D metallographic sections.
This is the case of groups of variants in martensitic Cu15.4Al8.9Mn (at.-%) SMA (Wang et al., 2002). This is also the case for blocks of lath martensite or even bainite in steels (see below) (iii) crystallographic units may correspond to a few, very intricate morphological entities, which appear as knitted or woven (Fig. 14a). This is clearly the case in upper bainite steel microstructures (Gourgues et al., 2000; Nohava et al., 2003; Lambert-Perlade et al., 2004a) and also possibly (by closely looking at micrographs) in hcp a colonies in Ti5Ta 1.8Nb (Karthikeyan et al., 2005). This microtexture appears when variants of close crystal orientations, but highly misoriented in morphology are selected. Although there are in fact many crystals in such a crystallographic entity, these are separated by LABs only, which do not strongly affect properties such as resistance to cleavage or fatigue crack propagation. This leads to coarser unit crack path and lower toughness properties (Gourgues et al., 2000; Kim et al., 2000; Daz-Fuentes et al., 2003; Nohava et al., 2003; Lambert-Perlade et al., 2004a). As a result, no obvious correlation between morphology and crystal orientation can be found in this case (Gourgues et al., 2000; Nohava et al., 2003) (iv) intricate, both crystallographically and morphologically misoriented units may be found. This is the case of, e.g. Widmanstatten cemen tite in Fe0.8C12.3Mn steel (Mangan et al., 1997) and in acicular ferrite of steel weld deposits (Gourgues et al., 2000) (Fig. 8) (v) irregular entities, where no particular correlation between morphology and crystal orientation can be evidenced, such as primary hcp a formed from bcc b in Ti8Al6V (Banerjee et al., 2004) and individual pearlite colonies in fully pearlitic steels (Aernoudt et al., 2005). In some instances, coupled information on crystal and morphological orientations may give information about the phase transformation scheme during metal processing, e.g. plate hcp a plates in extruded Zr2.5Nb pressure tubes; in this example, some pro-monotectoid a phase already formed before extrusion, whereas discrete clusters of a particles having their ,0001. axes parallel to the tube axis appeared during extrusion only (Grifths et al., 1998, Holt and Zhao, 2006). The microtexture of lath martensite in steels may readily be determined with EBSD, at least from 2D maps, even for coarse parent austenite grains (Fig. 14b) (Nakashima et al., 2001; Morito et al., 2003 and 2006; Dronhofer et al., 2003). The following description of martensite microtexture, which was built from EBSD results only, is based on the KS OR, even though this OR is not strictly followed in lath martensite. It has recently been extended, with some modications, to bainite in Fe9Ni steels transformed between 450 and 350uC (Furuhara et al., 2006). Laths sharing almost the same crystal and morphological orientation are gathered together into so called subblocks. Subblocks having the same morphological orientation but slightly different crystal orientations (same parallel close packed planes
92
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52
NO
Table 21 Electron backscatter diffraction investigation of growth and coarsening of ferritic steels related to austenite to ferrite phase transformation Starting c microstructure OR Results on coarsening Ref. Suh et al., 2000
Steel composition
Thermomechanical treatment
0.15C0.25Si1.4Mn0.006B
0.17C0.3Si1.5Mn
1150uC for 3 min then 10% uniaxial Transformation stress free compression strain at 700uC, 50 s and under stress dwell before cooling 1200uC, 1 min then, compressed Plastically deformed at 750uCzcooling (2050%) Heavily deformed
Torizuka et al., 2000
0.0022C0.22Si1.66MnMoNi 47% plastic strain at 850uCzair cooling 0.1C plain carbon steel Hot rolled to strain of 1.5 dwell for 10 s then water quenching 0.17C0.45Si1.5MnAlV Hot torsion Austenite grain size of 14 or 84 mm Deformed or recrystallised KS Not specified
KS, weaker for Affects mainly ferrite nucleation under stress than for stress free Not specified Ferrite grains more equiaxed, HAB more numerous with increasing plastic strain of c (but less than 30 grains studied in certain samples) KS Most ferrite grains are surrounded by HABs (but KS/KS MRs not clearly visible on pole figures) Not specified Extensive coalescence of ferrite grains (LABs disappear)
Hurley et al., 1999 Kelly et al., 2002
Gourgues-Lorenzon
0.15C0.3Si1.42MnNbV
Hot torsion (simulating roughing and finishing rolling) KS
0.15C0.25Si1.4MnB and 0.33C2.1Si1.5MnB Heavily deformed Not specified
0.082C0.36Si1.5MnNbV
1200uC down to 700uC, 10% compression z cooling down to 400uC with or without stress Multipass hot torsion
0.032C0.15Si0.74MnNb Deformed
0.19C1.5Si1.5MnAl(0.003 or 0.01)N (TRIP) Deformed
1150uC for 5 min then 0.8 compressive strain at 845uC at various strain rates then water quenching Simulated continuous annealing Recrystallised with more or Not specified less numerous AlN particles Not specified
0.15C1.5Si1.5Mn (TRIP)
950 or 1200uC then hot torsion at various temperatures
Coalescence of ferrite during cooling, controlled by 2D Beladi et al., 2004 (rafts) or 3D meeting of a grains; EBSD gives the a grain size distribution Deformed c: few LABs (,15u) due to variant selection or Novillo et al., 2004 plastic rotation; recrystallised c: many LABs, a grain size controlled by coalescence favoured by such variant selection Shift off KS OR increases if the load is sustained, less Kang et al., 2003 coalescence of neighbouring a grains (but many ORs .15u from KS in the paper) Ferrite grains meet first at c GBs; there is coalescence behind Cotrina et al., 2004 the transformation front; EBSD gives ferrite fraction and size distribution and migrating interface area per unit volume Eghbali and Strained at 0.001 s1: dynamic softening via strain induced transformation, randomly oriented a grains, little coalescence; Abdallah-Zadeh, 2006 0.1 s1: most a GBs are HABs, finer final a grain size Finer ferrite grain size and higher volume fraction of retained Baik et al., 2006 c (both measured with EBSD) with increasing the density of AlN (measured with TEM) The ferrite grain size (EBSD measurements) depends on the Godet et al., 2006 thermal mechanical treatment; best results if deformed at Ar3 temperature
2007
VOL
52
NO
93
Gourgues-Lorenzon
(Nakashima et al., 2001). No particular neighbour selection was found among the six possible blocks in a given packet (Morito et al., 2003). In martensite formed from ne grained austenite, one packet may dominate (at least in 2D sections) (Morito et al., 2005), or less than six variants may be found in every packet (Kitahara et al., 2006). Such results conrm those previously obtained with TEM, yet with much higher statistical signicance. The determination of crystallographic units needs careful selection of the threshold angle used in EBSD to dene their boundaries. In fatigue and cleavage sensitive materials, this is related to crack arrest, e.g. in austempered ductile cast iron, whose packet boundaries dened with EBSD may in fact stop fatigue crack propagation (Marrow et al., 2001). The size of these units can be used to compare steel microstructures such as bainite and martensite (Tsunekage and Tsubakino, 2002). Note, however, that cracks only arrest at continuous boundaries, while 2D sections also take into account small packets locally embedded in larger ones. Consequently, the true unit crack path may be much larger than that measured from 2D EBSD maps [e.g. in lath martensite steel microstructures (Gourgues, 2003)]. Local orientation gradients also disturb the denition of relevant boundaries. They are common along bainite laths [e.g. in high carbon steels (Regle et al., 2004) and along the LAB network within crystallographic units of pearlitic steels (Aernoudt et al., 2005)].
a
Resulting average textures

Thanks to the development of high speed systems, EBSD is now increasingly used for average texture measurements, avoiding the problem of calculating the ODF from pole gures (as for XRD or neutron diffraction). The EBSD is also used to infer the texture of the parent phase from that of low temperature product phase. Here, spatial information provided by EBSD is very useful. Such texture history is of outstanding value to understand and improve processing routes to get optimal texture of nal product at low costs.
Retrieving texture of parent phase
b
a partially transformed upper bainite with highly misoriented sets of parallel units sharing close crystal orientation as shown in {001} pole gure: after Lambert-Perlade et al. (2004); b fully transformed lath martensite, where each block B delineated by white lines always contains same pair of low misoriented variants V: after Morito et al. (2003) 14 Microtexture evidenced using EBSD in product phase
but different ,111. directions parallel to the ,110. close packed directions of parent austenite) are in turn clustered into blocks, so that particular MRs between variants (e.g. 60u,111. twin MR) are found between blocks. These blocks are parts of packets. Within one packet, all laths are morphologically parallel; however, a packet consists in a variety (up to six) of intricate, highly misoriented crystals. Martensite blocks are highly intricate over the whole martensite packets (Gourgues et al., 2000; Nakashima et al., 2001; Dronhofer et al., 2003) although they may look equiaxed in 2D sections
To infer the ODF of the parent phase from that of the product phase, one can work directly with individual grains (i.e. by calculating individual orientations of parent phase grains from resulting variants of the product phase). This is here referred to as a local approach. Another possibility is to work with average ODFs only. Here, EBSD is of particular use if the parent phase is coarse grained (e.g. b grains hundreds of microns in size in heat treated titanium alloys). This will be referred to as a global approach. The local approach was rst used in materials where the parent grains were still easily reconstructed with imaging techniques. One can then select appropriate variants of the product phase, determine their crystal orientation by EBSD point or map analysis and then calculate the orientation of the parent grain by assuming an OR between parent and product phases. This works well in titanium and zirconium alloys, where the Burgers OR is rather strictly obeyed. Two or three variants are generally needed to calculate every grain orientation of the parent b phase (Humbert et al., 1995). This method was successfully used for Ti6Al4V, a number of
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triplets of a plates giving about 100 orientations of former b grains (Humbert et al., 1994; Stanford and Bate, 2004) and by using both primary and colony a phase in equiaxed b grains (Humbert et al., 1996; Moustahd et al., 1997a) and coarse a colonies of pure Ti (Gey and Humbert, 2002). The method requires, however, that GBs of the parent phase be readily recognised. It works well even if there is variant selection, but also requires that the OR be strictly obeyed. This is not the case in steels, where no unique OR is generally found; the uncertainty in the OR strongly decreases the accuracy of results concerning the parent phase: a departure of .5u from the OR prevents from nding the right orientation of the parent grain (Decocker et al., 2003). In steels, provided that there are enough ferrite crystals formed within a former austenite grain, it is possible to determine the orientation of that former c grain by an iterative graphical method using {001} pole gures (Gourgues et al., 2000; Cabus et al., 2004b). Such methods are rather tedious, however. To get statistically reliable data, automated analysis was also developed, with criteria to determine whether the chosen set of variants in fact stems from the same parent grain. Several ways exist, e.g. one calculation of departure of MRs from well known (e.g. Burgers/ Burgers) MRs [e.g. in a colonies of T40 titanium alloy (Gey and Humbert, 2003)], and iterative combination of neighbouring product variants [e.g. in Ti6Al4V alloys (Glavicic et al., 2003b and 2004b)], improved by use of weighting coefcients representing the reliability of individual parent grain orientation data (Glavicic et al., 2003a). With such improvements, EBSD maps of the former parent phase may even be automatically generated in a robust manner and used to investigate, e.g. the solidication or forging texture of the parent phase, even after it completely disappeared during subsequent processing steps (e.g. in near-a IMI834 (Germain et al., 2004) and in Ti6Al4V (Glavicic et al., 2004a) titanium alloys). A method to simply reconstruct parent grains from EBSD data, based on a rigorous algebraic analysis, that also works for fcc to bcc transformations (e.g. in steel martensite with high internal plastic strain) has been recently developed (Cayron et al., 2006), although not yet able to calculate the crystal orientation of the reconstructed parent grains. The global approach requires little (if no) variant selection to avoid local negative values of the ODF (Humbert and Gey, 1999). In addition, the parent phase should not exhibit lower crystal symmetry than the product phase (Gey et al., 1999). In these conditions, EBSD data may be used to calculate the ODF of product phase, and then (by numerical computations) that of the parent phase. Classical tools used in XRD may readily be used. More than 2700 data points were acquired with EBSD in Ti6Al4V alloy for this purpose (Humbert and Gey, 1999). A positivity criterion may also be introduced to allow calculations even with weak variant selection [e.g. in metastable b Ti alloys (Gey et al., 1999; Humbert et al., 2001), tentatively in Zircaloy4 alloy (Gey et al., 2002) and in 99.85%Ti (Gey and Humbert, 2002)]. The quality of the results strongly depends on the accuracy of the ODF of the product phase and of possible variant selection. This method is much less tedious than non-automated local
approach and much less complicated than automated local approach. The calculated ODF of the parent phase may be used in turn to calculate the ODF of the product phase by assuming no variant selection and a given OR (Humbert et al., 1994; Moustahd et al., 1997a; Gey et al., 2002; Stanford and Bate, 2004; Glavicic et al., 2004b). To conclude about variant selection from comparison between experimental and calculated ODFs of the product phase, one must however bare in mind that: (i) not all product variants were generally measured by point analysis (ii) analysis of 2D sections may bias the results due to sampling effects or pseudo variant selection (iii) local variant selection may have no effect on the resulting average texture (Stanford and Bate, 2005). Methods using only some well known texture components of the parent phase should be avoided unless results are experimentally conrmed by, e.g. especially designed heat treatments retaining a signicant part of the parent phase down to room temperature (Yasuda et al., 1999).
Correlation between average texture and phase transformations
Little literature is available on average textures determined by EBSD related to solid state phase transformations, except for hexagonal metals and alloys (often due to the coarse grain size of parent grains, which excludes use of XRD) and for steels. There is a study on NiTi SMA sheets, where the nal {223},110. texture results from both rolling and variant selection (Inoue et al., 2003). The effect of processing parameters on the nal texture of product phase have also been investigated in Cu39Zn2.6Pb (azb) brass, where appropriate extrusion in the b phase range leads to an optimised balance of a texture components controlling ductility and machinability respectively (Mapelli and Venturini, 2006). A strong ,110. texture inuencing magnetic properties appears when Fe9Si13B bulk metallic glass crystallises under a high magnetic induction (Watanabe et al., 2005a). Cyclic nitriding of 22.5Cr5.4Ni duplex stainless steels leads to a fully austenitic case with desirable corrosion resistant {100},001.z{110},112. texture, while avoiding detrimental columnar grain structure (Garzon and Tschiptschin, 2004). In diffusion bonded Ti45Al, Ti depletion near the bond interface lead to partial transformation of lamellar DO19 a2 phase into L10 c lamellae and to spheroidisation of a2 grains. While the c phase was randomly textured, new a2 particles tended to have {1010} or {0002} planes parallel to the bonding direction (Buque and Appel, 2002). In commercially pure titanium with initial {2205},1120. texture, the transformation from hcp a into bcc b was eventually dominated by the growth of huge allotriomorphic b grains leading to a nal {001},110. texture, even if other texture components also initially appeared (Seward et al., 2004). In acicular ferrite of steel WM deposits, the strong ,100. solidication texture of bcc d ferrite was shown by Kluken et al. (1991) in their pioneering EBSD point analysis study to lead to three main texture components for fcc c. As near KS ORs prevail for both dc and ca phase transformations, a part of the nal acicular ferrite (a) microstructure recovered the initial solidication texture. In a hot
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rolled low carbon microalloyed steel, the nal texture of ferrite was found to be random for a low number of passes or a low strain per pass; it turned to typical texture of recrystallised ferrite with increasing strain, suggesting strain induced transformation from austenite to ferrite, followed by deformation and recrystallisation of ferrite (Seo et al., 2000). The average texture of phases is readily determined by EBSD in multiphase materials, without any need for deconvolution of average pole gures, e.g. in steels containing some retained austenite (Field et al., 1996; Hutchinson et al., 1998; de Meyer et al., 2001; Wasilkowka et al., 2006) and in duplex stainless steels (Jura et al., 1999 and 2002). Care must be taken to assess whether the texture of retained austenite accurately represents that of all starting austenite grains present before phase transformation, and that EBSD patterns of all phases are correctly indexed (Field et al., 1996). The stability of retained austenite during plastic deformation can also be studied for each texture component separately (Wasilkowka et al., 2006). Microtexture data obtained with EBSD could here also be used in advanced micromechanical models, to get local stresses more accurately than by classical Taylor and Sachs approximations. Texture components and/or pattern quality of the parent phase provide information about its metallurgical state before phase transformation. By separating recrystallised from deformed austenite based on their well known texture components and by distinguishing between various bcc products such as primary ferrite, bainite and martensite, it was made possible to assess which product phase formed from a given state of austenite in a low carbon steel (Mesplont and De Cooman, 2003), in hot rolled dual phase steels (Waterschoot et al., 2002) and in low alloy TRIP aided steels (Hutchinson et al., 1998; De Meyer et al., 2001). Primary ferrite tended to form from deformed austenite whereas bainite formed from deformed and also possibly from recrystallised austenite. Local inhomogeneity in the parent phase may strongly inuence the local texture of the product phase. For instance, locally severely sheared ,110. austenite of a 0.16C0.61Mn steel transforms into a ,111. bre of ferrite (Ping et al., 2005). When comparing experimentally measured textures with calculated ones (with assumptions about OR and variant selection), one can nd that there is no signicant variant selection at that scale [as e.g. in spontaneous reverse transformation of warm deformed steel (Yokota et al., 2005)]. One may even nd little or no resulting texture at all [e.g. in 0.2C0.2Si1.3Mn 0.1Ti steel hot rolled and transformed under high magnetic induction (Maruta and Shimotomai 2002)]. Several criteria such as active slip systems or elastic strain energy (see section on modelling for further details) have been used to include variant selection into average texture calculations (Bruckner and Gottstein, 2001; Humbert et al., 2002b; Moustahd et al., 1997b; Humbert and Gey, 2003). Agreement between experiment and modelling has still to be improved even when taking pseudo variant selection into account.
solid state phase transformations is now extensively used from very early growth of small, scarcely distributed nuclei up to growth and coalescence of phases. At the scale of parent grains, quantitative description of microtexture as crystallographic entities, now also available for coarse grained structures, is of great practical signicance as far as e.g. plasticity or fracture properties are concerned. The EBSD may even replace XRD determination of textures, especially for very coarse grains and when several phases of close crystal structures coexist in the investigated microstructure. Data of EBSD may be gathered and processed with routine procedures, so that results little depend on the users interpretation (except for the data cleaning procedure, which should be clearly reported). The number of EBSD studies of solid state phase transformations in metallic materials is exponentially increasing. With the help of EDS to facilitate phase identication, similar use of EBSD is expected for non-metallic materials such as ceramics and natural minerals in the future.
Environmentally assisted and surface reactions

Surfaces play an increasing role in the properties of materials, and in particular of functional materials. Although surface reactions are usually not referred to as phase transformations, they are also considered here for their strong similarities with phase transformations in closed systems, for their practical implications and because to the authors knowledge, there is no recent review of the wide use of EBSD in this eld in open literature.
Environmentally assisted surface reactions

Microstructure and microtexture of oxide layers
Solid state phase transformations: summary

With increasing development of EBSD systems, in particular for FEG-SEMs, crystallographic investigation of
Application of EBSD to the structural investigation of oxide layers requires good spatial resolution. Oxide scales usually have a complex structure and exhibit strong backscattered electron contrast with the underlying metal substrate, so that cross-section examinations require careful sample preparation and high performance EBSD systems with, e.g. automated background acquisition during mapping. A signicant practical application of EBSD in this eld is the investigation of oxide scales on steel products, whose structure and mechanical properties are of prime importance for hot rolling, cold rolling and wire drawing. Both FeO1x (wustite), Fe3O4 (magnetite) and Fe2O3 (hematite) may be distinguished with EBSD, although there is usually little Fe2O3 (Kim and Szpunar, 2001) or the Fe2O3 layer is too thin to be detected with EBSD (Burke and Higginson, 2000; Birosca and Higginson, 2003). Interstitial free and low carbon steels are of primary concern. According to oxidation conditions (temperature, atmosphere and cycling conditions) and steel composition, the internal wustite layer may be either columnar (Burke and Higginson, 2000; Kim and Szpunar, 2001 and 2002; West et al., 2005) or equiaxed (Birosca and Higginson, 2003; Birosca et al., 2004). A strong ,100. texture may be encountered in wustite whatever that of the steel substrate (Kim and Szpunar, 2001 and 2002; Higginson et al., 2002). A cubecube OR between wustite and magnetite may also prevail, possibly due to the defect structure of wustite (West
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(a)
(b)
(c)
a prior EBSD mapping of surface to be oxidised; b exposure to oxidising environment; c characterisation of oxidised surface (e.g. with near eld or interferometry techniques) 15 Principle of EBSD investigation of oxidation
et al., 2005), but is not always found (Birosca and Higginson, 2003). Silicon signicantly affects the structure and texture of the oxide layers (Kim and Szpunar, 2002; Higginson et al., 2002). The oxide texture may be correlated with porosity and thus mechanical properties of oxide layers (Higginson et al., 2002). Scales produced in industrial conditions have also been characterised with EBSD (Burke and Higginson, 2000). The limits of such analysis are spatial resolution (for very thin scales to be observed in cross-sections) and statistical reliability of data. However, sample preparation is much less tedious than for TEM cross-sections and usually does not need to use advanced techniques such as focused ion beam (FIB) milling. Oxide scales have also been studied in cross-sections of T40 and Ti3Al2.6V titanium alloys, where rutile TiO2 grows faster in Ar rich atmospheres than in N2 rich atmospheres and a tendency to (0002)Ti//(100)TiO2 was observed (Lenarduzzi et al., 2002). Thermal barrier coatings on nickel base superalloys have also been studied with EBSD, for various coating processes. The alumina scale may, or may not be strongly ,0001. textured. This controls internal stresses and nal properties of the thermal barrier coatings (Karadge et al., 2006). The development of internal stress and strain elds was investigated with EBSD after oxidation of buried AlGaAs layers; residual stresses and plastic zone geometry were calculated by a nite element
Table 22 Some EBSD studies of intergranular corrosion Material Ni3940Fe (at.-%) Corrosion conditions 1000uC for 5 h in O2 atmosphere EBSD results
method and compared to the distribution of pattern quality (Keller et al., 2004). Another way to investigate the microtexture of layers is to carry out EBSD analysis of oxidised surfaces directly (Fig. 15). This provides data over a wide area, although only at the external surface. Oxidation of recrystallised {100},001. (cube) textured nickel lead to two types of areas: (i) rough areas with coarse cube or {111} textured grains and smaller, possibly faceted intergranular grains (ii) smooth regions having the desired epitaxial cube or rotated cube texture (Woodcock et al., 2002a, 2002b and 2004).
Role of interfaces and free surfaces
As environmentally assisted mechanisms are closely related to diffusion, interfaces and free surfaces strongly inuence morphology and growth kinetics of products. As there is already review literature on EBSD studies of intergranular cracking (Gourgues, 2002), only corrosion is addressed here (Table 22). Most results were obtained by analysis of the corroded surface and of parallel planes prepared by serial sectioning, sometimes conrmed by cross-section analysis. The crystal orientation of free surface planes, which is readily determined with EBSD, also inuences the layer growth kinetics. The relevant parameter is generally the
Ref. Yamaura et al., 1999 and 2000
Ni39 at.-%Fe Low carbon ship steels AA6061 aluminium alloy Sensitised AISI 316LN stainless steel Nickel base alloy 718
800927uC for 1824 h in air Seawater environment Intergranular attack in seawater environment Intergranular attack in oxalic acid 900uC for 30 h in air
Random GBs are sensitive and LABs are not sensitive to corrosion; the sensitivity of coincident site lattice GBs increases with oxygen pressure and with departure from S3, S11, S19 and S27 coincidence Sensitivity increases with applied stress; 65% of random GBs in the sample is enough to oxide over the full width Not all GBs are corroded, some can only be imaged by EBSD LABs are immune; intergranular attack stops when there is a loss in connectivity of sensitive HABs LABs and twin boundaries are not sensitive; misorientation angle of sensitive GBs spreads between 30 and 55u; such boundaries form a continuous network Twin boundaries are immune; random GBs are oxidised
Yamaura et al., 2003 Katrakova and Mucklich, 2000 Minoda and Yoshida, 2002 Kunkova et al., 2004 Yang et al., 2005
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angle between the local free surface and low-index crystal planes such as {0001} planes in oxidised Grade 1 titanium (Konig and Davepon, 2001) and {100} planes in nickel base alloy 690 subjected to plasma assisted nitriding (He et al., 2003; Czerwiec et al., 2003). Transmission electron microscopy results are difcult to obtain, whereas EBSD may be conducted before the environmentally assisted reaction, without affecting the sample geometry. This has been done for Co51.6Ga48.3 oxidised into Ga2O3, for which the oxide growth kinetics on {211} substrate planes was about ve times higher than that on {100} planes (Koops et al., 2002). In nickel base alloys, atomic force microscopy of corroded surfaces (characterised by EBSD before corrosion) allowed quantitative assessment of the dissolution rate as a function of the local surface orientation (Gray et al., 2006; Schuh et al., 2003) and crystallographic investigation of ne scaled surface features of individual corroded grains (Schuh et al., 2003). Strong interactions between substrate GBs and free surfaces have been evidenced thanks to EBSD for wustite reduction into iron in CO/CO2 atmospheres by the following reactions : COad z2 hzVFe zOX ?CO2 ad (1) O : FeX ?Fe0 z2 hzVFe Fe (2)
silicon by metal assisted nucleation in amorphous Si:H layer (Chang et al., 2004) and silicide mediated versus laser assisted crystallisation of silicon on glass (Kim et al., 2004). Quantitative determination of the amount of given phases or polytypes may also be given by EBSD analysis of deposited lms, such as SiC deposition onto 4H and 6H SiC substrates (Chaussende et al., 2004; Latu-Romain et al., 2005). Once the right phase is obtained, the next point is to control its crystal quality and orientation. Crystal quality may be assessed by inspection of GBs or by looking at EBSD pattern quality (Kim et al., 2004). Controlling the lm texture (e.g. through epitaxial growth combined with variant selection) can be more difcult than controlling the nature of polytype (Chaussende et al., 2004). Except when deposited lms were thick enough [e.g. TiN in nickel base superalloys (Jeong et al., 2002b)], only free surfaces of lms were generally investigated, making full use of the sensitivity of EBSD to extreme surface layers only. Some results given by EBSD analysis about the feasibility of obtaining suitably oriented lms on various substrates are illustrated in Table 24. Extensive mapping was not always necessary, simple eye observation of changes in EBSD patterns by rastering the electron beam over the entire sample surface being preferred in many cases.
Orientation relationships between layers and substrate
Reaction (1) leads to local depletion in oxygen and then to nucleation of metallic iron by reaction (2). It also leads to surface rearrangement, in particular near GBs (Bahgat et al., 2004a). Surface rearrangement leads to local roughness depending on the individual wustite grain orientation (Bahgat et al., 2004b and 2005). Even when still not visible in the SEM, iron nuclei can be clearly identied by EBSD, since EBSD is sensitive to the very surface of the specimens (Sasaki et al., 2005b). Iron particles nucleate at surface ledges and their size and number strongly depend on the local wustite grain orientation (Bahgat et al., 2004a and 2004b). The growth of iron particles also depends on the local rearranged surface (Sasaki et al., 2005b). Such studies make full use of the non-destructive, highly resolved in thickness EBSD technique.
Other results on environmentally assisted reactions
The OR between substrate and deposited layers has been investigated with EBSD in a variety of cases, mainly by surface analysis of lms (Table 25). In some cases, however, sampling or phase size effects may cause missing of variants that were indeed found by XRD (Cain and Lange, 1994).
Layer structure and resulting texture
A variety of reactions have been explored with EBSD for either phase identication or determination of OR and microtexture (Table 23). Another interesting example is given by in situ reaction synthesis of alumina from reaction between molten aluminium and surrounding SiO2 quartz tube (Murthy et al., 2005). Al2O3 and Al were found as fully interconnected colonies with only twin boundaries between Al2O3 grains, which should be benecial to mechanical properties of the nal product if complete synthesis could be obtained.
Spatial information provided by EBSD has been used to determine the grain size, variant morphology and clustering and even grain morphology on polished crosssections. Data are now available for various materials and deposition processes (Table 26). The resulting texture is usually analysed with XRD but has also been investigated with EBSD (Table 27). Information on local roughness has been used to link thin lm morphology to EBSD determined crystal structure and orientation of substrate and lm. One may cite, e.g. copper electrodeposits (Cho and Szpunar, 2002), dendritic silicon splats (Nagashio and Kuribayashi, 2005), CeO2 buffer layers (Van Driessche et al., 2003), NiO grown on Ni substrate (Woodcock et al., 2004), SiC (3C) grown on SiC (6H) (Latu-Romain et al., 2005), and sputter deposited Nb, Cu, Co and Permalloy epitaxial layers (Loloee et al., 2001).
Surface reactions: a summary

Essential features of the EBSD technique in the eld of surface reactions are as follows: (i) its sensitivity to extreme surface layers allows surface characterisation of as deposited extremely thin films (down to y20 nm in thickness) (ii) its non-destructive character is essential to determine ORs between substrate and layers for polycrystalline substrates (iii) the possibility is given to scan over large areas at a fine scale.
Thin film deposition

EBSD has been used at all stages of process development for thin lm deposition, from feasibility demonstration to quality control of the nal product.
Process feasibility
Electron backscatter diffraction has been used to nd out processing conditions yielding the desired phase, such as amorphous versus crystalline silicon on single crystal silicon substrate (Gao et al., 2000), crystalline
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Table 23 Electron backscatter diffraction studies of environmentally assisted surface reactions Surface reaction
4
Material Filamentary corrosion
Environment
EBSD results
Ref. Schmutz et al., 2003
Pure Mg
0.01M NaClz10 M Na2Cr2O7 aqueous solution Internal TiN (hcp a) nitriding Internal TiN1x (d, fcc) nitriding Internal formation of tetragonal FeB2 particles Surface dissolution of bcc d phase
Ti8 at.-%Mo
Nitriding environment
Guillou et al., 2004 Guillou et al., 2004 Kulka et al., 2006
Ti16 at.-%Mo
Nitriding environment
Gourgues-Lorenzon
Pure iron and two low carbon low alloy steels
Boriding with or without carburising
Duplex stainless steels
Nitriding at 1200uC
Padilha et al., 1999 Chezan et al., 2004
Fe4 at.-%Ni(2%Ti or 3%Cr)
Nitriding environment (thin sheet)
Corrosion initiates only on {0001} oriented grains. Surface propagation along ,1120. and ,1010. directions Burgers OR with matrix, 13 variants per bcc b grain of the substrate Near-KS OR, MRs between particles are often 60u,111. Single crystalline Fe2B particles in borided Fe; polycrystalline Fe2B particles in boridedzcarburised steels Identification of the c phase and of disappearance of d phase Phase identification (EBSD), grain size and morphology (TEM) Crystallographic continuity between substrate grains and grains of the nitrided layer Phase identification of a
Fe18 wt-%Cr
Plasma nitriding
Miyamoto et al., 2006 Fukai et al., 2005 Gray et al., 2006
Fe28Mn6Si5 wt-%Cr
900uC for 1 h in a vacuum of 102 Pa
Ni base alloy 22
NaClzHCl aqueous solutions
Partially reversible bulk transformation into nitrides and resulting grain refinement Nitride precipitation and cellular precipitation Evaporation of Mn causing external fcc c to bcc a transformation Competition between passivation and metal dissolution
Ni base alloy 600
0.1 N HCl droplet Dissolution and oxidation
3M HCl: dissolution according to the local normal to free surfaces: increasing rates for {111},{100},{110} 1M HCl: residual oxidation competes with dissolution; resulting rate {111},{110},{100} (quantitative description in inverse pole figures) ,100. bands on corroded {110} surfaces. Dissolution rate: {111},{110},{100} (quantitative description in inverse pole figures)
Schuh et al., 2003
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Table 24 Some EBSD results on quality of thin lm deposits for feasibility demonstration Deposition process Same EBSD pattern over the entire sample surface Epitaxy (cubecube OR) Miller et al., 1993 Alper et al., 1993 Van Driessche et al., 2003 Davydov et al., 2004 Results Ref.
Gourgues-Lorenzon
Substrate
Film
(100) ZrO29.5%Y2O3 (cubic) Aqueous precursorzcertain annealing conditions Potentiostatic electrodeposition Solgel dip coating Metallisation
ZrO2
(100) Cu (fcc)
Rolled and polished NiW alloy (0001) GaN,
Cu and CoNi multilayers (0.15 nm per layer) CeO2 Ni then Au
2007
(1120) Al2O3 (sapphire) Tl2Ba2Ca2Cu3Ox (001) and (111) MgO* (100) SrTiO3 Si of various orientations DC magnetron sputtering at 750uC DC magnetron sputtering Pulsed laser depositionzanneal Pulsed laser deposition Electron cyclotron resonance chemical vapour deposition Solid state conversion of Al Electrodeposition
Nb LaAlO3 In2O3 (Pb0.52Zr0.48)TiO3 Si
Loloee et al., 2001 Bramley et al., 1998 Johnson et al., 1999a Hamedi et al., 1998 Rau et al., 2004 Park et al., 2005 Devilliers et al., 2004
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(0001) Al2O3 (sapphire)
Al2O3
Anodised polycrystalline Ti
PbO2
Cubecube orientation with polycrystalline substrate Crystal quality of both layers in various conditions; suitable epitaxy if Ni, then Au are deposited Closer than ,1u to epitaxy Cubecube epitaxy Epitaxy, OR being 1.70.5u ,111.* Cubecube epitaxy{ (100) Si: epitaxy; (210) Si: epitaxy with defects; (311), (111), (221): no epitaxy All converted Al2O3 particles are of same crystal orientation as substrate (nanoheteroepitaxy) Feasibilility only on {0001} Ti grains, too difficult otherwise
NO
*Investigation in cross-section. { Surface investigation by electron channelling pattern analysis (close to the EBSD technique).
Table 25 Electron backscatter diffraction investigation of orientation relationships between thin deposited layers and substrate Deposition process Results Ref. Loloee et al., 2001 Loloee et al., 2001 Trager-Cowan et al., 2001 Cain and Lange, 1994; Cain et al., 1995 Missiaen et al., 2005 Davydov et al., 2004 Cosandey, 1997
Substrate
Film
(1120) Al2O3 (sapphire) Nb (of preceding row) (bcc)
Nb Cu (fcc)
GaN (30 nm) (0001) Al2O3 (sapphire) rotated by 10u toward (1010) ZrO210 mol.-%Y2O3 Aqueous precursor (0001) and (1120) Al2O3 (sapphire)
DC magnetron sputtering at 750uC (110)Nb // (1120)Al2O3 and [111]Nb // [0001] Al2O3 by ,1u DC magnetron sputtering at 350uC NW OR, with two variants or (150uCzanneal at 350uC) Chemical vapour deposition (1010)GaN // (1210)Al2O3 i.e. 90u around ,0001.
Polycrystalline Cu
Cu droplets
GaN (110) TiO2
Ni 15 nm sized Au particles In situ metallisation at 20uC (zanneal) or 502uC
Anneal at 1050uC in H2/He atmosphere Electron beam deposition In situ metallisation and anneal at 527uC
(110) TiO2
12 nm sized Au particles
(0001): three variants (001)ZrO2 // (0001)Al2O3 and ,100.ZrO2 // ,1210.Al2O3 with one dominating variant; (1120): four variants with various ORs, some others detected by XRD only There are preferred initial ORs but with limited effect on spreading. Epitaxy at the end of spreading (GB migration). [110]Ni // [1120]GaN or [1210]GaN 80% of 101 analysed particles have (111) ,10u from (110)TiO2; two variants are found with (111)Au // (110)TiO2 and (I) [110]Au // [001]TiO2 and (II) [110]Au // [001]TiO2 20uC: (111)Au // (110)TiO2by 3u; two variants are found (I) [110]Au // [001]TiO2 and (II) [110]Au // [001]TiO2 502uC: (112)Au // (110) TiO2 by 2u and [110]Au // [001]TiO2 or [110]Au // [001]TiO2 or twin related with these
Cosandey et al., 2001
Table 26 Using EBSD to determine the structure of deposited layers* Deposition processzobservation conditions Results Pulsed laser depositionz(IP) Stack electroplatingz(CS) DC sputtering at 780uCz(IP) Electrodepositionz(CS) Electrodeposition z (IP) Physical vapour depositionz(CS) Chemical vapour deposition in recycled gas at 830uCz(IP, CS) DC magnetron sputteringz(IP) Ref.
Substrate
Film
(001) MgO
Fe2O3
Four self-accommodating variants grouped into rectangular domains Johnson et al., 1999b (with detailed microtexture)zpossible internal twinning (220) texture, average grain size y21 mmzevolution during annealing Ezawa et al., 2004 Fairhurst et al., 2000 Cho and Szpunar, 2002 Read et al., 2004 Jeong et al., 2002b Mao et al., 2005 Loloee et al., 2001
(100) Si coated with Ti, then Ni, then (111) Pd (?)
Sn3.5%Ag (b-Sn phase) YBa2Cu3O7d
Gourgues-Lorenzon
Pure polycrystalline Cu of various textures ,111. Si coated with 60 nm Cu Nickel base superalloy Mo
Cu (50 mm)
Grain size distribution (y1 mm2), desirable [001] texture obtained at 98.5% Coarse epitaxial columnar grains, competitive growthztwinning Grain size y1.5 mm much higher than size of individual spheres Small (0.151.5 mm) columnar grains, grain size distribution Competitive growth and twinning and associated texture evolution in thickness Cu and Permalloy: two variants with 180u,111. MR, 45 mm in size
Cu (2.5 mm) TiN (6 mm) Diamond
(1120)Al2O3 (sapphire) coated with (110) Nb
Polycrystalline Ni3Al
Permalloy (Ni16Fe), then Cu Diamond
Nucleation density depends on substrate grain orientation
Chen and Chang, 2005 Schreck et al., 2003 Chen and Rudolph, 2003
(001) SrTiO3 coated with Ir
Diamond
,111. Sin
Diamond
Nucleation structures: same EBSD pattern as Ir but are in fact future diamond domains; the reaction is autocatalytic Columnar, mostly epitaxial grains
No substrate
SiC (3C)
Plasma assisted chemical vapour deposition with positive bias enhanced nucleationz(IP) Plasma assisted chemical vapour deposition with bias enhanced nucleationz(IP) Plasma assisted chemical vapour deposition with bias enhanced nucleationz(serial sections parallel to IP) Fluidised bed deposition from CH3SiCl3 (CS)
Helary et al., 2006 Bastos et al., 2006 Bera et al., 2004
Ti
AISI 316 stainless steel
Nanostructured Electrodeposition (CS, IP) Co20 at.-%Ni Pd Electrodepositionz(CS)
Columnar grains from the equiaxed chill zone; internal twinning; almost no average texture 5% fcc (Co) phase with OR to hcp matrix; grain size, GB characterisation; crystal orientation gradient in columnar grains Grain size distribution (140 nm in average), growth from substrate grains far from GBs
*IP: in plane observations; CS: observation of cross-sections.
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Arnould et al., 2003 Bastos et al., 2006 Bramley et al., 1998 Choi et al., 2004 and 2005
Son et al., 2001
Cosandey et al., 1999 Markondeya Raj et al., 1999
Buchheit et al., 2002
For in plane analysis, a balance must be found between spatial resolution and sampling effects and the roughness of the analysed surface must be low. Cross-section analysis may require specic sample preparation (e.g. by FIB milling techniques) to avoid edge effects.
Ito et al., 2003
Discussion: coupling EBSD with other investigation methods

As EBSD mapping has become in most cases a routine technique, it has widely been used together with other experimental characterisation techniques for multiscale investigation of materials. The case of EBSD/EDX coupling for phase identication has already been addressed in the present paper. On the other hand, information on coupled crystal orientation and morphology is used in advanced models, which are now even able to take into account individual or clustered crystals to optimise process conditions or product properties.
Ref.
(S): ,100. columnar zone; (W): fine, poorly indexed microstructure, weaker ,110. ,110. columnar, many low misorientations within columns Strong {1120}a and {220}b texture (001) fibre and many HABs: poor film properties Strong (100) texture, no texture in plane
MoSi2: [001] at external surface; Mo5Si3: [001] columnar
Cellular growth with preferential (110) texture
TiO2: (001) texture, [001] growth direction (0001) parallel to both film and plane of plates
Coupling EBSD with other experimental techniques

Validation of experimental results
Table 27 Using EBSD to determine average texture of deposited layers
Al coated with Zn then with Cu Ti MgO Si coated with SiO2 then with Ti then with Pt then with La(NO3)3zpossible buffer layers Mo9Si18 at.-%B
Oxidised (100) Si coated with 100 nm Cu then with 282 nm Al No substrate No substrate
Poly(methylmethacrylate) coated with Cu
In mineralogy samples, the orientation of individual crystals is generally investigated with the light microscope. Advantages and drawbacks of EBSD and light microscopy respectively, as well as coupled use of both have already been reviewed (Trimby and Prior, 1999). The main advantages of EBSD are its ability to analyse small grains, optically isotropic crystals and transparent materials. Grain boundaries are more quantitatively characterised than by light microscopy (which is not sensitive to LABs) or backscattered electron imaging (Trimby and Prior, 1999). However, a robust reection table must be constructed for each analysed mineral (Mauler et al., 1998). The EBSD technique has also been used together with FIB imaging. In Al0.5Cu, the ion channelling contrast was shown with EBSD to rely on the angular misorientation between the local normal to the sample surface and the nearest ,111. crystal direction (Barr et al., 1992). Coupled analysis with EBSD and near eld microscopy has been performed for less than a decade for phase identication [e.g. to distinguish ferrite from austenite in multiphase steels (Wendrock et al., 2001; Ros-Yanez et al., 2001 and 2002)], and to investigate GB grooving [e.g. shallow thermal grooves at LABs or coincident site lattice boundaries of polycrystalline MgO (Farrer et al., 2000)]. The high spatial resolution of atomic force microscopy has been used to check accuracy of EBSD determination of GB traces in TiO2 polycrystals (Pang and Wynblatt, 2006), and to check that sapphire crystals obtained by solid state conversion were of sufcient height (here y100 nm) for their orientation to be determined with EBSD independently of that of the sapphire substrate (Park et al., 2005).
Multiscale analysis
Results
Electrodeposition in sulfamate (S) or Watts bath (W) Electrodeposition Electrodeposition DC magnetron sputtering Solgel coating
Pack cementationzannealing
Electron beam evaporation
Ni Co20 at.-%Ni Tl2Ba2Ca2Cu3Ox (Pb,Zr)TiO3
MoSi2ztransformation into Mo5Si3 during annealing Al2Cu
Ni
TiO2 (rutile) Al2O3
Film
Tape castingzsintering Tape castingzsintering
Deposition process
Although EBSD makes full use of the large magnication range of the SEM, there is still a need for ner scale analysis and for analysis of higher amounts of material to reduce sampling effects. The coupled use of various techniques for that purpose is discussed in this section.
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Substrate
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Additional information provided by coupling EBSD with near field microscopy Near eld microscopy gives access to local 3D surface morphology and material properties at a very ne scale. Shreck et al. (2003) were able to detect diamond nuclei on iridium substrate by Kelvin probe microscopy, although the local crystal structure was still determined by EBSD to be that of iridium. Magnetic force microscopy readily detected magnetisation domains at GBs of AISI 304 austenitic stainless steel, which were conrmed by ne scale EBSD mapping to be martensite particles (Takaya et al., 2004). Local surface modication after thermal grooving [e.g. in SrTiO3 (Sano et al., 2003a)] gives information about free surface and GB energy. Local surface relief produced on polished surfaces by phase transformation (e.g. from bcc b to orthorhombic a in Ti9 wt-%Mo (Guo and Enomoto, 2006), from austenite into Widmanstatten ferrite (here characterised with a specic procedure by light microscopy) (Hall and Aaronson, 1994) or into bainite (Ohmori, 2002) in steel) suggests surface reconstruction or previous twinning of the parent phase near single crystal, tent shaped plates (i.e. a diffusional mechanism) and no diffusion near plates showing an invariant plane strain morphology. More generally, the macroscopic strain induced by displacive solid state phase transformations at polished surfaces can be determined in 3D using near eld microscopy, whereas local crystallography in the same area is determined with EBSD. Such precious data are essential for validation of phenomenological theories of martensite crystallography (PTMCs) (see Modelling section). The measurement of local properties coupled with EBSD determination of the local crystal structure and orientation has been recently reviewed in the framework of phase diagram determination (Zhao, 2006). Nanoindentation on individual phases identied with EBSD was performed in PdRhPt diffusion multiples (Zhao et al., 2002), on Ag3Sn and Cu6Sn5 intermetallic phases in SnAgCu solder interconnects (Li et al., 2005b) and in various layers formed on a nickel base superalloy coated with NiAl by pack cementation (Wollmer et al., 2003). The anisotropy of properties may be quantied thanks to information about local crystal orientation [e.g. in the NiAl phase of NiAlMo eutectic (Bei and George, 2005)]. There are cases for which a simple rule of mixtures between the various phases worked well for the investigated microstructure [e.g. hardness and elastic modulus of a VV3Si eutectic (Bei et al., 2004)]. In other instances, no agreement could be found, e.g. for elastic modulus and for hardness (Zhao et al., 2002). Correlation between nanohardness and local loss of EBSD pattern quality is still in progress (Wu et al., 2005). EBSD versus TEM investigations A huge amount of studies use both TEM and SEMEBSD investigations of the same phenomena; automated indexing of Kikuchi bands is now possible in the TEM, allowing orientation imaging at very ne scales. This section focuses on complementary use of SEMEBSD and TEM techniques. Transmission electron microscopy investigations are needed for ne scale characterisation of deformation structures, such as
dislocation clustering into LABs that are observed with EBSD but do not affect the martensitic transformation [e.g. in CuAlNi SMA (Rodriguez, 2004)], and if there are local deformation bands in the parent phase, in which particular variant selection may then occur [e.g. in Cu42 wt-%Zn (Sakata et al., 2000)]. Interactions between the local texture and very ne scale precipitation also require TEM observations [e.g. precipitation in Zircaloy4 (Loge et al., 2000)]. The effect of GB misorientation on discontinuous precipitation in Al 2.8Mg1 at.-%Ga was determined with EBSD, whereas the ORs between phases had to be determined with TEM (Hirth and Gottstein, 1998). In precipitation aided matrix phase transformations, the OR between matrix phases may be determined with EBSD while the ORs with ne nucleating agents are still studied in the TEM [e.g. ferritic steels (Furuhara et al., 2003)]. Fine scale microstructural features (such as those differentiating ferrite from bainite in low alloy TRIP steels) were rst studied by TEM, giving qualitative or quantitative criteria for further (and easier) investigation by SEM-EBSD. In this particular case (Fig. 16), orientation gradient and internal LABs were observed in bainite, but not in ferrite (Zaefferer et al., 2004). The internal structure of c phases in c-TiAl gave complementary information to EBSD determined ORs between lamellar and Widmanstatten c phases in this alloy (Dey et al., 2005). The gradual misorientation determined by EBSD within lenticular a martensite of Fe 32.85 wt-%Ni (Fig. 17) was shown by TEM to be linked to a change in the internal structure of martensite (and local accommodation of transformation induced lattice strains) from dislocation network to microtwinning (Shibata et al., 2005). Internal microtwinning in selfaccommodating martensite of Cu12.55Al4.84 wt-%Ni (Chen et al., 2000) and in Cu7.3Al8.5 wt-%Mn (Wang et al., 2002) was detected in the TEM but not by SEMEBSD, so that only a part of the self-accommodating variants could be identied in each martensite unit by EBSD. TEM based techniques remain necessary if very ne scale features or dislocation structures have to be investigated. Other diffraction techniques X-ray diffraction is a reference technique for texture determination, so that the comparison of results obtained by XRD and EBSD respectively, since pioneering studies of e.g. Schwarzer and Weiland on dual phase steels (Schwarzer and Weiland, 1988), has already been reviewed (Dingley and Randle, 1992). In addition to providing spatial information, EBSD is well suited for coarse grained materials. Lattice parameters are better determined with XRD, and a large area can be analysed at a time. The probability to miss particular variants or phases is much lower with XRD than with EBSD [e.g. in cubic ZrO2 deposited onto sapphire (Cain and Lange, 1994)]. For moderately coarse microstructures or for very low amounts of phases, neutron diffraction coupled with EBSD is a well suited tool. The pioneering study of Grant et al. (1986) focused on directionally solidied copper, where optical microscopy revealed a columnar grain structure, neutron diffraction showed a ,100. bre texture that was conrmed by local electron channelling pattern analysis. In an austenitic stainless steel WM deposit, Bouche et al. (2000) showed by both neutron diffraction (providing
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b
a information obtained with TEM reported on a micrograph; b EBSD map of misorientation with respect to point X 17 Coupled EBSD and TEM investigation of the internal structure of plate martensite in Fe32.85 at.-%Ni: a misorientation prole is superimposed, showing misorientation up to 3u, following the change in OR between austenite (A) and martensite (M). After Shibata et al. (2005)
b
a TEM thin foil observation of heavily dislocated, slightly misoriented bainite b next to a ferrite grain f together with retained austenite particles a; b EBSD map of a ferrite grain: angular deviation from the crystal orientation of the grain centre (from 0 in white up to 4u in black), showing bainite areas in dark 16 Coupled use of EBSD and TEM to characterise bainite in a low alloy TRIP aided steel: hatched particles are retained austenite, other ferrite grains are in white. After Zaefferer et al. (2004)
statistics over y1 cm3 of material), point EBSD analysis of submicron sized bcc ferrite and local TEM observations that the OR between austenite and ferrite was not only the classical near KS OR, but could be much closer to a cubecube OR, at least for ferrite particles located at austenite LABs. Cold rolled duplex stainless steel Uranus 45N was shown by neutron diffraction to have ferrite and austenite phase textures identical to those of their single phase steel counterparts. In fact, a loss of the OR between ferrite and austenite was found with EBSD, due to complex deformation structures imaged in the TEM (Baudin et al., 2002). Electron backscatter diffraction may also suggest ORs that are useful for global
texture calculations to be coupled to hot stage XRD texture characterisation of the product phase [e.g. in a low carbon steel (Bruckner and Gottstein, 2001)]. In (Ni,Co)O single crystals, neutron diffraction gave average results on crystal quality (here, mosaicity), XRD gave details on lattice parameters and EBSD provided spatial information on crystal orientation (Brewer et al., 2002). The ORs between Ni and NiO were obtained by carrying out EBSD (sensitive to NiO only) and XRD (sensitive to the Ni substrate) in the same area (Woodcock et al., 2004). As XRD and TEM are well known techniques they can easily be combined to get quantitative data on crystal structure and orientation. Neutron diffraction is much less commonly used but provides useful bulk characterisation. Transmission electron microscopy is still necessary for ne scale imaging and crystal characterisation, although sample preparation is destructive and more tedious and analysed areas are small.
In situ investigations
Very few EBSD analyses associated with in situ investigations have been published yet. Hot stage microscopy associated with crystallographic EBSD characterisation of initial and/or nal state has already provided new interesting data (Table 28). With the development of high speed, highly sensitive EBSD systems this is a
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Table 28 Investigation of phase transformations by EBSD associated with in situ microscopy
Monitoring reverse transformation from martensite into austenite Nucleation sites of austenite during heating Internal stresses (one selected grain)
Spreading of contact zone
Time resolved monitoring nucleation and growth of individual phases
Information provided by hot stage device
promising way to get information about phase transformation mechanisms, at least at the sample surface. Environmental SEMs may be equipped with EBSD analysis. Nothing seems to have been published yet about in situ EBSD investigation of surface reactions but the feasibility of EBSD analysis in various environmental and thermal conditions has already been demonstrated in water and nitrogen environments for both conducting and non-conducting materials (Garmestani and Harris, 1999; Habesch, 2000). In situ phase transformation of low alloy TRIP aided steels conrmed that retained austenite gradually transformed upon straining, coarse equiaxed particles being less stable that elongated ones in the area monitored by EBSD (Oh et al., 2002; Park et al., 2002). Electron backscatter diffraction in hot stage SEM has been made possible by a low effect of temperature on pattern quality for various materials up to 650 or even 700uC (Garmestani and Harris, 1999; Seward et al., 2002) and by the recent development of fast EBSD systems (Wright et al., 2005). Published studies mainly concentrated on recrystallisation and grain growth, e.g. in aluminium (Ferry, 1998; Huang et al., 2002) and nickel and deformed NaCl (Piazolo et al., 2004a). Some studies have already been published on phase transformations, e.g. in hcp a into bcc b and then back into hcp a transformations of titanium (Seward et al., 2002). By heating titanium, bcc b phase transformed from hcp a may appear as plates with a Burgers OR and a tent shaped surface relief (Fig. 18) (Seward et al., 2004). Orientation relationships close to NW were identied in hcp a into fcc b and then back into hcp a transformations of cobalt (Wright et al., 2005). Phase transformations in iron oxides such as that from hematite into magnetite have also been investigated using hot stage EBSD (Piazolo et al., 2004b). The main difculties in hot stage EBSD mapping are temperature measurements (Seward et al., 2002) and the high kinetics of phase development, which may restrict in situ monitoring to only a small area, possibly leading to sampling effects if no repeated experiments are to be made.
Three-dimensional considerations
Nagashio et al., 2004; Nagashio and Kuribayashi, 2006 Phelan and Dippenaar, 2004; Phelan et al., 2005
Watanabe et al., 2004 and 2005b
Misorientation between primary and Widmanstatten ferrite
The contact zone consists of fine, equiaxed grains
Final microtexture: back to original austenite crystal orientations together with formation of LABs Effect of parent GB misorientation, subsequent abnormal growth and twinning of austenite Crystal orientation of neighbouring grains
Information provided by EBSD
Kaouache et al., 2004
Ref.
Ueda et al., 2004
Splat cooling and melt spinning of molten Si Formation of primary and Widmanstatten ferrite in low carbon steel Fe32 at.-%Ni bicrystals
Electron diffraction cannot give information about crystal orientation in the bulk of the material; 3DXRD techniques are being developed for this purpose but still require a high ux synchrotron X-ray facility to get the 3D shape of individual crystals and of orientation gradients (Fu et al., 2003; Barabash et al., 2006). The spatial resolution is coarser (about a few mm) than that of EBSD but the angular resolution is high (y0.05u) (Juul Jensen, 2000). Being non-destructive, 3D-XRD may be used for in situ investigation of e.g. recrystallisation (Juul Jensen, 2000) and possibly phase transformations. However, it is far from being readily available, so that other methods are generally used to get 3D information about crystal morphology.
*Tensile stage device.
Light optical microscopy
Light optical microscopy
Hot stage device
Infrared microscopy
X-ray diffraction*
Laser confocal microscopy
Three-dimensional investigations The reconstruction of the 3D morphology is difcult (Fig. 19) and involves both careful experimental sectioning and complex 3D image processing. For coarse grained materials, it may be useful to analyse both parallel sides of the sample and to assume that no other crystal is embedded in the bulk [e.g. in single shear lap
Fe4.18 at.-%Cr
CuAlBe SMA
Material
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(a) (a)
(b)
(c)
(d)
(e) (b)
19 3D morphological investigations to assess the hidden volume a of the iceberg by b deep etching, c nonparallel plane sectioning, d serial sectioning and e one plane trace analysis: a practical example is given in Fig. 6
(c)
a backscattered electron image (A1, A2, A3: b allotriomorphs; P1: intragranular b); b pole gures of {111}b and {11.0}a; c pole gures of {110}b and {00.1}a for grains A3 and a2 18 In situ EBSD investigation of ORs between growing allotriomophic b phase and starting a phase at 882uC: after Seward et al. (2004)
Sn3.5Ag solder joints (Telang and Bieler, 2005a)]. Habit planes of plates may be determined by analysis of two perpendicular sections (Fig. 19c) such as in the b to a phase transformation of titanium based b-Cez alloy (Zimmermann and Humbert, 2002). Electron backscatter diffraction analysis of interfaces and facets
has been recently reviewed (Randle, 2004) and will not be detailed here. Another way to get 3D information on phase morphology and connectivity is deep etching performed after EBSD analysis (Fig. 19b). The morphology of eutectic silicon was studied as a function of alloying elements and local crystallography of phases in AlSi hypoeutectic alloys (Nogita and Dahle, 2001a and 2001b). Proeutectoid cementite in Fe1.34C13.1Mn was shown to appear as both monolithic single crystals and polycrystalline conglomerates of parallel laths, the OR with the austenite matrix being different from one case to the other (Mangan et al., 1999). The morphology of intergranular cementite in Fe1.3C13Mn was studied by TEM observation of deep etched material and by EBSD investigation of OR with the austenite matrix (Kral and Spanos, 2003). Deep etching is also useful to investigate 3D connectivity of phases, e.g. in eutectic M7C3 carbides of white cast irons. These appear as interconnected colonies of parallel rods. Colonies are single crystalline in hypereutectic alloys and polycrystalline in hypoeutectic alloys (Randle and Powell, 1993). 3D analysis also gives access to nucleation sites, for example in successive nucleation of MnS particles at oxides, of VC carbides at MnS sulphides, and of pearlite at VC carbides in intragranular pearlite of hypereutectic 0.8C12MnV steel (Guo et al., 2002). The surface geometry may be determined by use of stereo pairs as is already done on fracture surfaces (Hebesberger et al., 2000). Provided that the surface
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relief does not impede EBSD analysis by shadowing effects, phase identication on fracture surface of multiphase materials [e.g. in c za2 TiAl alloys (Hebesberger et al., 2000)] is possible. Grain boundary geometry (Randle, 2004) provides additional data for the understanding of segregation phenomena [e.g. in Niz7 at. ppm S (Cornen and Le Gall, 2004)] and precipitation. The most widely used technique to get 3D information from EBSD is serial sectioning (Fig. 19d) either to get the 3D morphology alone (uncoupled use in Table 29) or even to get an EBSD map of all or part of the slices (coupled use in Table 29). Manual or automatic metallographic polishing is the most conventional method. Ion milling is now in development (Chen and Rudolph, 2003). Dual beam SEMs now allow more or less automated sequences of FIB milling followed by EBSD analysis in the same apparatus (Groeber et al., 2006; Zaafarani et al., 2006; Konrad et al., 2006). As the specimen has to be moved between successive milling and EBSD mapping sequences, absolute spatial location and orientation of the sample must be adjusted for each slice (King et al., 2000) and distortion due to, e.g. electron beam drift during EBSD mapping is to be strictly avoided. Data processing is now much easier, thanks to the increase in computer power and the development of dedicated software. Three-dimensional analysis from 2D results Just as for exposed versus non-exposed facets (Randle, 2004), many EBSD investigations rely on analysis of traces (Fig. 19e) to determine facet orientation in crystal growth, interphase interfaces, habit planes and interactions between cracks and microstructure of product phases (Table 30) for both metallic and non-metallic materials. Most studies determine probable crystal plane families to which the observed traces could belong. Several methods exist to assess the reliability of these results. If crystal planes are considered, one can normalise the results (e.g. fraction of interfaces whose traces are closer to experimental ones than a user dened threshold) by the frequency that would be obtained if these planes were randomly oriented with respect to the crystal. This is particularly useful if the plane multiplicity is high due to crystal symmetry. For example, in a simulated HAZ of a low carbon steel, {223} and {557} austenite planes are of high multiplicity (12) but habit traces of bainite lath groups were still two times more frequently close to the trace of these planes than a randomly oriented plane would have been (Gourgues, 2003). The same kind of calculations was carried out for the growth direction of bainite in a 0.6C1.5Si1Mn steel (Cabus, 2005). Such normalising takes the actual crystallographic orientation of phases into account and thus reduces the bias induced by the crystallographic texture. Habit planes are generally expressed in the frame of the parent phase, so that normalising has to be carried out for each grain orientation of the parent phase separately, which can be tedious when this phase is totally absent from the resulting microstructure. Stereological methods based on extensive data analysis over a number of non-parallel sections are now available to up to date computer systems and provide statistically based information on interfaces [e.g. in GB segregation of Nb in TiO2 (Pang and Wynblatt, 2006)]. Other methods assuming tetrakaidecahedron shaped
grains help getting from 2D sections to 3D investigations of effective grain size after phase transformation in hot rolled steel (Bhattacharjee and Davis, 2002). Another way to investigate the 3D connectivity of low misoriented phases is to break the sample by brittle crystallographic fracture (e.g. by cleavage in bcc steels) and to look at fracture surfaces. Although lower bainite and martensite in steel HAZs come with a high density of HABs in 2D sections, areas of close crystal orientations within a given parent grain are actually connected to each other in 3D, so that the size of cleavage facets is much coarser (in this case, close to the huge austenite grain size) and the toughness is much lower than predicted from the crystallographic grain size calculated from individual 2D EBSD sections, although embedded misoriented crystals induce some roughness in cleavage fracture surfaces (Gourgues, 2003). In summary, although the vast majority of EBSD results focus on 2D considerations only, one must not forget how to get to a 3D view, which is relevant to material properties and reduces sampling effects such as pseudo variant selection. This is particularly true for complex shaped microstructures such as bainite and martensite, and for all studies involving nucleation or variant selection. The fast development of new 3D analysis techniques should make it possible to increasingly include 3D considerations into the crystallography of many phase transformations.
Coupling EBSD results with quantitative modelling

Many modelling approaches now use EBSD data as an experimental basis. Some examples are given in this section to illustrate the specic use of EBSD for that purpose.
Modelling phase transformations
Geometry considerations have been used for a decade to interpret EBSD results of interphase interface properties, phase connectivity and stereology (Table 31). Such models should now benet from 3D investigations as mentioned in the previous section. Another eld of modelling is coupling EBSD data with heat and/or uid ow calculations, especially for solidication (Table 32). In many instances, heat and uid ow models are simplied either to speed up calculations or to avoid introduction of parameters that are difcult to calibrate (e.g. thermal exchange coefcients). Little literature is available concerning coupling EBSD data and modelling of phase transformation kinetics, except for CET (see section on solidication). A simple model for diffusion anisotropy was used to discuss results of oxygen tracer diffusion in La2xSrxCuO4d (Claus et al., 1996). Grain boundary migration coupled with diffusion anisotropy allowed to explain EBSD data on heterogeneous kinetics of discontinuous ordering in Fe50 at.-%Co (Bischoff et al., 1998). Simple analytic kinetic models were used and their results compared with crystal connectivity determined with EBSD to investigate fragmentation of the nickel skeleton in containerless eutectic solidication of Ni18.7 at.-%Sn (Li et al., 2005b), oscillation of peritectic solidication in Sn1.4 wt-%Cd (ZeislerMashl and Lograsso, 1997) and dendrite tip undercooling in laser treated FeCrNi alloys (Fukumoto and
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Table 29 3D microstructural investigations using EBSD Coupled or uncoupled EBSD analysis Results (new information) Ref. Dahle et al., 2005 Henry et al., 1998 Xia and Tausig, 1998 Lewis et al., 2006 Abdul Wahab and Kral, 2005 Uncoupled Coupled Uncoupled Coupled (EBSD every tenth slice) Coupled
Material
Phase transformation
Al10Si Al1Si0.17Ti 2618 aluminium alloy
Eutectic solidification Solidification (feathery grains) Solidification (thixoforming)
Intergranular precipitation of s phase
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AL6XN superaustenitic stainless steel Austenitic stainless steel for hydrogen reforming Coupled Coupled Uncoupled Coupled
Precipitation of M23C6
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Cu4 wt-%Ti
Discontinuous precipitation from a into azCu4Ti
FeC plain carbon steels
Eutectoid pearlite formation
NO
Fe0.8C12Mn0.3V
Eutectoid pearlite formation
Mangan and Shiflet, 1997 Mangan and Shiflet, 1999 Guo et al., 2002 Mangan et al., 1997
Fe0.8C12.3Mn
Formation of Widmanstatten cementite plates
Low carbon steel
Transformation of austenite into intergranular ferrite Coupled
Yokomizo et al., 2003
High purity Fe0.12C3.28Ni Coupled
Transformation of austenite into intergranular primary and Widmanstatten ferrite Uncoupled
Spanos et al., 2005; Kral and Spanos, 2005 Spanos and Hall, 1996
High-purity Fe0.12C3.28Ni
Transformation of austenite into ferrite sideplates
Austempered ductile cast iron
Transformation of austenite into ausferrite
Coupled
Marrow et al., 2002 Rowenhorst et al., 2006 Amouyal et al., 2005 Chen and Rudolph, 2003
0.07C0.8Mn3.5Ni1.6Cu0.6Mo Transformation of austenite into coarse martensite Coupled (HSLA100) Ni45.6 at.-%Al Intergranular segregation Uncoupled Coupled, parallel to the film plane
Diamond on silicon
Crystal growth
Radial growth of eutectic Si from Si polyhedra Dendrite growth direction, twinning planes Globular morphology as already suggested by 2D analysis, HABs Morphology, crystallography, GB plane, OR between s and matrix All creep cavities are connected to M23C6; these M23C6 are less frequently in cubecube OR with the matrix than if not connected to creep cavities Extensive information about morphology and crystallography of colonies 3D crystallography of pearlite colonies, OR between ferrite and cementite linked to nucleation sites 3D imaging: nucleation conditions; EBSD: no OR between austenite and pearlitic ferrite Interlocked plates are in fact different crystals and not bifurcations of the same crystal; information about nucleation, growth and ORs Polycrystalline ferrite (including LABs); all crystals are in contact with a MnS nucleating particle; the number of ferrite crystals per MnS increases with the size of the MnS particle Peak morphology: pyramidal single crystals; laths and secondary plates: polycrystals with internal LABs (repeated nucleation); one crystal orientation far from austenite GBs Primary ferrite film and sideplates separated by a LAB: there is indeed nucleation of Widmanstatten ferrite, not only unstable growth of the ferrite film Fatigue cracks arrest at packet boundaries; stage I cracks are contained in {111} planes of austenite Tapered 3D morphology and crystal indices of interface planes The GB energy depends on the GB plane even for random GBs Columnar {111} growth
Table 30 Trace analysis from EBSD results (except those concerning the growth direction in solidication, see corresponding section) Facet Crystal free surfaces Trace analysis (no detail provided) Crystal free surfaces Trace analysis {100} facets Orientation of lateral facets Analysis conditions Results Ref.
Material
Pb(Mg0.33Nb0.67)O3zPbTiO3 Reactive sintering Kaolinite and dickite minerals Crystal growth
SrTiO3 in TiO2 rich liquid
Coarsening of crystals
Li et al., 1998 Kogure et al., 2005; Kameda et al., 2005 Sano et al., 2005 Bouyne et al., 1998 Daz-Fuentes et al., 2003 Gourgues et al., 2004 Cotrina et al., 2003 Marrow et al., 2002 Strom and Zhang, 2005 Lambert-Perlade et al., 2004a Mangan and Shiflet, 1998 Mangan and Shiflet, 1998 Seward et al., 2004
Gourgues-Lorenzon
Crystal free surfaces Trace analysiszstereological model Shape change into {100} facets and ,100. zone axes during coarsening 2.25Cr1Mo steel Austenite into bainite Cleavage cracks Traces plotted onto stereographic Compatible with {100} planes of bainite projection Three low carbon steels Austenite into acicular Cleavage cracks Trace analysis, crack arrest {100} traces, crack deviation for misorientation ferrite and bainite conditions angle .15u Duplex stainless steel Ferrite into austenite Fatigue cracks Trace analysis Strong effect of the two phase microstructure on crystal orientation of traces 0.78C microalloyed steel Austenite into pearlite Cleavage cracks Orientation units (5single crystal The size of orientation units is the same as that of ferrite in pearlite colonies) cleavage facets corrected from 2D/3D stereology Austempered ductile cast iron Austenite into ausferrite Fatigue cracks 2D and 3D (serial sectioning) {111} planes of parent (and retained) austenite propagation planes Solidification (segregated Cleavage near Trace analysis (001) crystal planes Mo5Si3(Cr,Ti) zones) indentation marks High strength low alloy steel Austenite into upper bainite Straight interfaces Trace analysis {557} and {223} austenite planes more probable of lath groups than {111} austenite planes 0.8C12.3Mn steel Austenite into pearlite Habit planes Work on EBSD patterns (001)c//{125}c with PitschPetch OR, (101)c//{211}c with Isaichev OR; (001)c//{121}c with Bagaryatsky OR depending on the individual colony Cu3 wt-%Ti Cellular precipitation Habit planes Work on EBSD patterns (111)a//(010)b Habit plane of b Straight interface of lath groups GB planes GB plane Near to {334}b, contains the [0001]a//[110]b {557} or {223} but not {111} planes of austenite
Ti
hcp a into bcc b
High strength low alloy steel
Austenite into bainite
In situ trace analysiszshape considerations Trace analysis
Gourgues, 2003 Li et al., 2004 Pang and Wynblatt, 2006 Cabus, 2005
Ti25Al24 at.-%Nb
a2 into O
TiO2 doped with Nb
GB segregation
2007
0.6C1.5Si1.5Mn steel Straight interfaces of lath groups
Austenite into bainite
Automated trace analysis of MR (110) for 39% of twin related crystals and interphase interfaces Trace analysiszstereological model The amount of segregated Nb is inversely proportional to the frequency of GBs; Nb seems to flatten the GB energy distribution Trace analysisznormalising 66% of traces at ,10u from ,110. projection onto sample surface (50% for randomly oriented planes)
VOL
52
NO
109
110
Gourgues-Lorenzon
Table 31 Modelling phase geometry using EBSD data Model Coincidence site lattice boundaries Coincidence site lattice boundaries Interpretation of results of atomic force microscopy Embedded atom model Embedded atom model More ORs predicted than those observed by EBSD Use of or comparison with EBSD data Ref.
Physical phenomenon of interest
Material
Heteroepitaxy
ZrO2/Y2O3 onto Al2O3
Directional solidification
Cain and Lange, 1994; Cain et al., 1995 Ardakani et al., 2000 Sano et al., 2003a Read et al., 2004 Amouyal et al., 2005 King et al., 2000 Traskine et al., 2005 Cabus, 2005 West and Adams, 1997
Free surface energy
CMSX4 and CM186LC Ni base superalloys SrTiO3
Solid state spreading
Copper onto copper
2007
Relative HAB energy
Ni rich NiAl
VOL
GB network GB wetting and finite size scaling Variant selection
No particular material Ga in Zn
52
Bainite in steels
NO
Directional solidification
NiCrCoTiAlMoSi superalloy
Geometry of GB network Lattice model for sampling effects similar to those of EBSD measurements Cross-section effects on texture determination (i.e. pseudo variant selection) Effect of texture strengthening on grain clustering
With the observed ,001. fibre texture, not all predicted coincidence site lattice boundaries are observed Results were coupled to EBSD crystal orientation data to determine anisotropic free surface energy For times up to 30 ps, the model works well for morphology of phases, but not with crystal alignment observed by EBSD EBSDzscanning probe microscopy give values of 0.2 up to 1.1; the model gives 0.3 up to 0.9 How to extract the random GB network from EBSD data Effect of sample width on the depth of intergranular invasion of Zn by Ga Even while taking pseudo variant selection into account, average textures still show variant selection EBSD measured grain clustering agrees with geometric effects induced by texture strengthening
Table 32 Coupling EBSD data with heat/uid ow calculations Model Use of EBSD data Ref. Sengupta et al., 2006 Takatani et al., 2000
Physical phenomenon of interest
Materials and processes
Meniscus shape
Slab casting of ultralow carbon steels Bickerman (analytical) fluid flow equations
Direction of dendrite growth
Twin roll casting of Fe3Si
Formation of feathery grains during solidification Competitive grain growth during solidification
Direct chill casting of AA 1050 aluminium alloy ingots Directional solidification of IN738LC, IN718 and single crystal nickel base superalloys, solidification of Zn (hot dip galvanising)
The actual shape of frozen meniscus determined with EBSD agrees with model output 3D dendritic growth with simplified geometry, EBSD determined density of nuclei in chill zone taking fluid flow into account is a model input; the dendrite growth direction (model output) compares well with that measured with EBSD Fluid flow in mould: effect of fluid convection Local microtexture predicted by the model is compared to EBSD data Heat transfer, dendrite or grain growth (cellular Predicted local texture, grain size and shape automatonzfinite element analysis), coupled are compared with EBSD data for process or not with temperature calculations optimisation
Henry et al., 2004
Columnar to equiaxed transition and Welding and laser metal forming of stray grain formation in solidification nickel based superalloys; hot dip galvanisation with Zn alloy
Simplified thermal model (e.g. Rosenthal equations for welding) gives cooling rate and temperature gradient; a kinetic model is used in post-processing calculations
Density of nuclei (input for the model); the predicted volume fraction of equiaxed grains is compared to EBSD observations
Kermanpur et al., 2000; Carter et al., 2000; Semoroz et al., 2002b; Newell et al., 2005; Xu et al., 2002a and 2002b Gaumann et al., 2001; Vitek et al., 2004; Quiroga et al., 2004
Gourgues-Lorenzon
Moustahfid et al., 1997b Kaouache et al., 2004 Ueda et al., 2001a
Cabus et al., 2004a
Godet et al., 2001
Modelling local crystallography and variant selection
Crystallographic models of ORs have been only scarcely used together with EBSD data, except for counting the number of possible variants or calculating the MRs between variants (for instance, the present author found at least 11 EBSD related papers with detailed description of MRs between variants for KS or NW ORs). Phenomenological theories of martensite crystallography are widely used to describe crystallographic features such as ORs, habit planes and macroscopic transformation eigenstrains. The traditional way to compare predictions with experiment is TEM investigation of thin foils, but EBSD may provide statistically signicant datasets for both ORs and (if coupled with surface analysis techniques such as near eld microscopy) transformation eigenstrains. EBSD is much less suited to habit plane determination unless habit planes are dened by straight interphase interfaces (and may not be true habit planes). Predictions of PTMCs have been compared with EBSD measurements for habit planes of a phase in titanium based b-Cez alloy (in fact EBSD results suggest that the highest value of lattice invariant shear should be taken) (Zimmermann and Humbert, 2002). Habit planes close to {223} or {557} austenite planes were found for groups of upper bainite laths in a simulated HAZ of low carbon steel (Lambert-Perlade et al., 2004a). Both a Pitsch type OR and a macroscopic shear eigenstrain of 0.20 were determined in Cu 39.3 at.-%Zn (from bcc b to fcc a bainite, treated as 9R martensite in the PTMC) (Marukawa et al., 2000), as were habit plane and transformation eigenstrain determined in Ti9 wt-%Mo alloy (from bcc b into orthorhombic a phase) (Guo et al., 2000). The OR versus lattice invariant shear mechanism was discussed in lenticular a martensite of Fe32.85 wt-%Ni (Shibata et al., 2005). Coupled use of EBSD results and modelling generally aims at accounting for variant selection in solid state phase transformations. Various criteria have been developed to model how a limited number of variants appear under certain conditions due to local stress or strain elds. In the active slip model, common plane and direction between parent and product phases should describe the slip system (of perfect or even partial dislocations) of highest Schmid factor. This local Schmid factor is generally calculated using the applied loading with either a Sachs assumption (homogeneous stress in the material) or a more or less constrained Taylor assumption (homogeneous strain in the material) (Table 33). Active slip models give general trends and often show limited agreement with experiments, as local stress and strain elds in polycrystalline materials strongly vary from one grain to another, especially at grain boundaries where nucleation often occurs. Another criterion is the total eigenstrain calculated for the simultaneous formation of at least two variants. This criterion is used to describe self-accommodation by local variant selection within the parent grain. Very good agreement was found between groups of variants
Qualitative agreement with experimental average texture Small values of criterion lead to no phase transformation Agreement with experiment on identity of selected variants Feasibility demonstrated, promising results
Only partial agreement with experiment
Table 33 Predictions of active slip models for variant selection compared with EBSD experimental results
{110},111.b and {112},111.bzSachs
Common close-packed planes parallel to planes of activated slip systems {111},110.czcorresponding Shockley partial Maximum resolved dislocations; Taylor model shear stress
Local stresses from elastic strains measured by XRD; slip systems not specified Macroscopic shear direction and habit plane normal
{111},110.c, fully constrained Taylor model
Minimum constrained macroscopic strain at GB Schmid factor
{111},110.c, fully constrained Taylor and Sachs models
Slip systemszlocalisation assumption
b1 austenite into martensite (tension) 24 variants (OR not specified) fcc austenite into lenticular bcc NW (24 couples martensite (tension) of variantzhabit plane) fcc austenite (c) into bcc bainitic Near KS ferrite; hot rolling reduction of 0.2 at 750uC fcc austenite (c) into bcc bainitic Unique, close to ferrite; channel die compressionz KS and NW step quenching fcc austenite (c) into bcc bainitic NW, KS ferrite; 2550% reduction by hot rolling at 750uC Steel with bainitez retained austenite CuAlBe alloy Low alloy TRIP aided bainitic steel 0.6C bainitic steel Fe32 at.-%Ni bicrystals
bcc b into hcp a after compression Burgers
Low alloy and high fcc austenite (c) into body centred Mn TRIP aided steels tetragonal or hcp martensite under tension
52
NO
Transformation conditions
Ti6Al4V
Material
KS and Burgers {111},110.c, Sachs Assumption respectively
OR
Positive and negative slip variants are accounted for by spreading about certain NW variants Common close packed Good agreement with planes parallel to planes experiment on identity of activated slip systems of selected variants
VOL
Results
Maximum resolved shear stress Schmid factor
Criterion
Godet et al., 2005
Jonas et al., 2005
Kurz, 1997). Agglomeration of silicon particles in semisolid AlSi alloy evidenced by EBSD investigations was also suggested by the failure of a liquid lm migration model to t experimental data (Hogg and Atkinson, 2005).
Ref.
2007
111
Gourgues-Lorenzon
minimising the total eigenstrain (calculated with a PTMC) and groups actually found with EBSD in spear like martensite of Cu7.3Al8.5 wt-%Mn (Wang et al., 2002), in plate martensite at a symmetrical 180u,211. tilt boundary of a Fe32 at.-%Ni bicrystal (Ueda et al., 2003a), in groups of three variants of hcp a phase in titanium (Wang et al., 2003). By contrast, lath martensite subblocks evidenced with EBSD in FeC alloys were not efcient self-accommodating structures according to this criterion (Morito et al., 2003). Accommodation of large strains imposed by hot rolling was found to take place by variant selection in a low carbon bainitic steel (Matsuoka et al., 1999); however, in that study the lattice Bain strain was surprisingly chosen as the transformation eigenstrain. More complex criteria for strain accommodation within a given parent grain involve elastic interaction energy calculated with the transformation eigenstrain (or more surprisingly lattice Bain strains in some cases) associated with candidate variants. Consistent results between observed variants and negative interaction energy were found in austenitic AISI 301 austenitic stainless steel in tension and in compression, under the Sachs assumption (Lee et al., 2005). By using a threshold value for the interaction energy criterion, good average texture predictions were obtained for compact strip processed high strength low alloy steel by using anisotropic elasticity of phases and either the lattice Bain strain (Humbert et al., 2002b) or the macroscopic transformation eigenstrain (Humbert et al., 2002a). In Fe32 at.-%Ni bicrystals, the interaction energy term can be overwhelmed by the necessity for strain compatibility at the GB according to the particular GB misorientation (Ueda et al., 2001b and 2003a). Coupled effects of transformation eigenstrain and phase geometry have been taken into account by modelling local stress and strain elds based on the Eshelby inclusion problem. The matrix is generally taken to be the parent phase with isotropic or anisotropic elasticplastic properties. Variants are modelled as oblate ellipsoids extending along their macroscopic habit plane. Mechanical coupling between phases is achieved under self-consistency assumptions. The model outputs are the interaction strain energy, and sometimes also the plastic strain in the parent phase as a function of candidate variants. Such calculations were compared to variant selection experimentally evidenced with EBSD to account for the identity of variants in stress free materials and as a function of applied stress for, e.g. martensite formation in carburised steels (Karaman et al., 1998), for microtexture of upper bainite packets in low carbon steel HAZ (Gourgues, 2003; Lambert-Perlade et al., 2004a) and for average texture affected by variant selection in Zircaloy4 alloy (Humbert and Gey, 2003). There is still much to do in this eld, in particular to get accurate data on the constitutive behaviour of phases under such extreme conditions (e.g. elevated temperature, possibly high local strain rates and high strains). 3D EBSD coupled with local measurements of phase property (Zhao, 2006) could be a promising way to further improve these models.
Modelling average transformation textures
processing conditions. A lot of work has been carried out in this eld using EBSD data either alone or together with XRD data (Table 34). Most studies in this eld concentrate either on variant selection effects on average texture or on accuracy of quantitative texture prediction. However, the texture of the parent phase is generally difcult to assess, even if some phase is retained, unless specic calculation methods are used to retrieve it (see section on average textures in solid state phase transformations).
Modelling resulting properties
The prediction of average transformation textures is of utmost importance to infer product properties from
In service properties of transformed microstructures may be tentatively predicted using EBSD data about microtexture, macrotexture and morphology of individual phases together with homogenisation models to calculate average or macroscopic properties. The simplest homogenisation model used is the rule of mixtures, which successfully predicted, e.g. the compression peak stress of eutectic Al2O3YAGZrO2 rods as a function of the texture of individual phases (Murayama et al., 2004b). More complex microtextures may induce failure of this model to account for experimental measurements, e.g. in wrought duplex stainless steels, where areas maintaining the KS OR between both phases behave as hard particles in a much softer matrix (Iza-Mendia et al., 1998). More advanced micromechanical models have also been used to predict yield properties of heterogeneous materials such as columnar and equiaxed zones of Ti 6Al4V ingots under Taylor assumption and with crystal plasticity models (Glavicic et al., 2003c and 2004a). Local stresses arising from upset forging of Ti 6Al4V were also calculated with a nite element method, allowing local Taylor factors to be calculated thanks to a simple micromechanical model (Bieler et al., 2005b) and cavity initiation sites to be related to local crystal orientation and spheroidisation mechanisms (Bieler and Semiatin 2002, Bieler et al., 2005a and 2005b). Micromechanical models of crystal plasticity have been used to assess strain localisation in bainitic and martensitic microstructures of A508Cl.3 low alloy steel under tension (Sekfali et al., 2002) and yield and fracture properties of cast and aged duplex stainless steels (Bugat et al., 2001). In the two latter cases, local measurements of surface strains together with EBSD mapping of initial state were used to mesh the actual surface microstructure and to compare experimental measurements of strains with model predictions. The OR between parent and product phases, and MR between product variants play a key role in both slip localisation and cleavage cracking properties. More simply, the crystallographic packet size, which is the unit crack path for cleavage microcracking could also be used with a HallPetch type equation to predict the fracture toughness of low carbon acicular ferrite steels as a function of the packet size (Daz-Fuentes et al., 2003). It was also quantitatively used to predict fracture toughness of a bainitic steel HAZ microstructure (Lambert-Perlade et al., 2004b). A local micromechanical model was used together with a transformation induced superplasticity model to predict the evolution of Ti6Al4V/TiBw composite tensile loaded during thermal cycling around the matrix transformation temperatures (Schuh and Dunand, 2001).
112
2007
VOL
52
NO
Table 34 Modelling average transformation textures using data generated with EBSD Experimental data Average texture (both EBSD and XRD) Average texture of a and c after heat treatment Average texture Starting from a texture, 24 KS variants, no variant selection Starting from c texture, 24 KS variants, no variant selection Model Results Ref. Abiko et al., 2000
Material
High purity iron
fcc c into bcc a
Low carbon steel
bcc a into fcc c
Park et al., 2002
Low carbon steel
fcc c into bcc a
There are missing variants in experimental versus predicted ODF, attributed to grain growth but not to variant selection One texture component experimentally missing, another too strong versus predictions, thus there is variant selection The a phase nucleates from deformed (not recrystallised) c
Hurley and Hodgson, 2001
Low carbon steels
bcc a into fcc c back into a EBSD: OR; XRD and neutron diffraction: average texture
EBSD: grain structure; XRD: average texture
Starting from typical texture components of deformed c, 24 KS variants, no variant selection Starting from a texture, 12 NW variants
Ryde et al., 1999
Gourgues-Lorenzon
Low carbon steel
bcc a into fcc c
Predictions consistent with experiment for one steel, insufficient texture memory predicted for two other steels Model predictions consistent with experiment only if both criteria are combined
Bruckner and Gottstein, 2001
HSLA* steel (compact fcc c into bcc a strip production)
EBSD: OR; XRD: average texture of a and retained c
Possible variant selection: predicted textures are sharper than experimental ones
Humbert et al., 2002a and 2002b
Low alloy TRIP steel
fcc c into bainitic bcc a
Starting from c texture, 24 KS variants; variant selection: assuming rolling strain and Taylor hypothesis, both active slip and transformation work criteria were tested Starting from c texture, 12 NW variants; variant selection: elastic strain energy (Bain strain or macroscopic transformation eigenstrain) Three Bain, 12 NW or 24 KS variants, no variant selection
Predicted texture with right components but too weak versus experiment Primary a forms from deformed c; bainite and martensite preferably form from recrystallised c Primary and bainitic a form from deformed c; retained c is partially recrystallised Model predictions are consistent with experiment: no variant selection
De Meyer et al., 2001
Dual phase steel
Low carbon microalloyed steel
fcc c into bcc a, here both primary a, bainitic a and martensite fcc c into primary and bainitic bcc a
EBSD: ODFs for a and retained c; XRD: volume fraction of c EBSD: individual ODF of product phases; XRD: texture of retained c EBSD: individual ODFs of product phases; XRD:
Hutchinson et al., 1998; Waterschoot et al., 2002 Mesplont and De Cooman, 2003 Yokota et al., 2005
0.3C9Ni steel
bcc a into fcc c into near-bcc a martensite
2007
AISI 304 stainless steel
fcc c into hcp e and near bcc a martensite
Petit et al., 2006
VOL
Starting from various c textures, three Bain variants, no variant selection Starting from various c textures; 24 KS variants; no variant selection EBSD: ODF, microstructure Starting from various c texture and microtexture; XRD: components; 24 KS variants, no average texture variant selection Starting from experimental c texture; EBSD: local deformation mechanisms (including phase 24 variants deduced from a PTMC, transformation); XRD: volume coupled variant selection and crystal fraction of phases and average plasticity of austenite, localisation texture of austenite rule by a self-consistent scheme for the austenite polycrystal
Model predictions are partially consistent with experiment concerning the orientation of austenite grains that transform first; despite that the model is not yet able to take e martensite into account
52
NO
113
Gourgues-Lorenzon
Germain et al., 2005b; Humbert et al., 2006
Humbert et al., 1994; Gey et al., 1996; Moustahfid et al., 1997a; Stanford and Bate, 2004 Seward et al., 2004
Yasuda et al., 1999
Sakata et al., 2001
Coupling EBSD with other advanced techniques: a summary

The following key issues should be considered in the next future.
Think in 3D
One component underestimated in the model, due to growth of b allotriomorphs {0001}a and {110}b pole figures are significantly different: there is variant selection; accounted for by the elastic energy criterion
Agreement with experiment depends on b or (azb) initial state and b deformation state before phase transformation
The right Bain zone is predicted by the model
,111.b fibre gives the right fibres for the texture of c
Not only should experimental techniques be further developed, but models should be improved, inasmuch as they are frequently based on 2D assumptions about, for example, the morphology of newly formed phases and the determination of nucleation sites from 2D observations. Crystal connectivity should be necessarily considered from a 3D point of view. Phenomena such as variant selection should include 3D considerations, to differentiate true variant selection from stereology artefacts. In situ investigations are still in progress, to be combined with 3D considerations as detailed above.
Model improvements
Ref.
Model
Starting from a texture; Burgers variants Starting from b texture; Burgers variants with or without elastic energy criterion based on the Bain strain Contribution of Bain strain to reduction in residual stresses from rolling Starting from b texture, 24 KS variants
Starting from b texture; Burgers variants
Micromechanical modelling of phase transformations is a favourite frame to use EBSD data combining crystallographic and spatial information. However, the most advanced micromechanical models are not often used together with EBSD. As an example, PTMCs are often used with approximations on mechanical properties (e.g. stiffness, strength, strain rate and temperature effects) of parent and product phases. They are often used as if they were descriptive, although they are phenomenological in nature. On the other hand, localisation and homogenisation rules used in multiscale modelling of resulting properties could also be improved.
Results
Concluding remarks
An exponential increase continues in the number of published papers on application of EBSD to phase transformations, a topic that is still developing rapidly. From revisiting a number of features of phase transformations, EBSD has progressed and now provides original results in a number of specic areas. As for other topics related to EBSD, a careful literature review is required before starting a new study. The vast majority of the literature is devoted to metallic materials; promising results already exist for ceramics despite experimental difculties. It would be interesting to cross-reference what is commonly found with metallic and ceramic materials. Electron backscatter diffraction is now a mature technique. It is easy to use (except for minerals or for 3D investigations), although handling the amount of data produced by 2D or 3D EBSD mapping is increasingly difcult. Coupling EBSD with in situ investigations, local property measurement and advanced modelling is now required to get deeper insight into phase transformation mechanisms. The development of high speed systems and computer aided volume reconstruction techniques strongly suggests that many results on phase transformation crystallography and mechanisms should be revisited using 3D characterisation of partially or fully transformed microstructures, which provide input data for process optimisation and prediction of product properties.
EBSD: microtexture; XRD: average texture bcc b into colonies of fcc a
EBSD and XRD: average texture
EBSD: average textures
EBSD: average textures
B2 b (indexed as bcc) into EBSD: average texture L12 c after hot compression
52
Experimental data
bcc b into hcp a
hcp a into bcc b
bcc b into hcp a
114
2007
VOL
NO
*HSLA: high strength low alloy.

2
Table 34 Continued
Ni(3638) at.-%Al
Ti6Al4V
IMI834 Ti alloy
Cu40Zn
Material
Ti
Gourgues-Lorenzon
Table 35 Commonly encountered ORs in EBSD studies Name and acronym Crystal structure Crystal structure of of one phase the other phase Parallel planes hcp fcc fcc fcc fcc {011}bcc//{0001}hcp {011}bcc//{111}fcc {011}bcc//{111}fcc {011}bcc//{001}fcc {011}bcc ,1u from {111}fcc Parallel directions ,111.bcc//,1120.hcp ,111.bcc//,110.fcc ,011.bcc//,211.fcc ,111.bcc//,110.fcc Midway between KS and closest NW ,112.fcc//,1100.hcp ,110.c//,1120.a2 ,100.c 2.6u from ,311.a and ,010.c 2.6u from ,131.a ,100.c//,110.a and ,010.c//,111.a ,100.c//,554.c and ,010.c//,010.c and ,001.c//,225.c
Burgers bcc KurdjumovSachs (KS) bcc NishiyamaWassermann (NW) bcc Pitsch bcc GreningerTroiano (GT) bcc NishiyamaWassermann (NW) fcc Blackburn c (L10) PitschPetch a (bcc)
hcp {111}fcc//{0001}hcp a2 (DO19) {111}c//{0001}a2 c (Tetragonal Fe3C) {001}c//{215}a c (Tetragonal Fe3C) {001}c//{112}a c (Tetragonal Fe3C)
Bagaryatsky Pitsch
a (bcc) c (fcc)
Appendix Orientation relationships

The most commonly encountered ORs between phases in solid state transformations are reported in Table 35.
Acknowledgements
Technical assistance from Mrs Odile Adam for paper tracking is gratefully acknowledged. Many thanks are due to Professor Pineau for his kind and continuous support to achieve the present work. The present paper is dedicated to the memory of late Professor Flower, who kindly gave me my first opportunity to make extensive EBSD measurements in his research group at Imperial College.
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Application of Electron Back Scatter Diffraction

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Electron Diffraction Subcommittee 22 March 2007 Ray Goehner

EBSD in the SEM for the Identification of Unknown Crystalline Phases

EBSD Pattern of AlB2

AlB2 (20 kV)

Cameras for EBSD Typical Arrangement

Not much room in the sample chamber!

Installation on a Dual Beam FIB

Effect of Sample Tilt on BS Electron Yield

Alumina (Al2O3) On Thin Substrate

Ag on MgO Example of EBSD Resolution

SEM images of Ag particles on MgO substrate

Applications of BEKP to Materials

EBSD Analysis of 11 m Diameter W wire

Conventional Approaches to Phase Identification

Symmetry elements in EBSD pattern

The EBSD pattern show symmetry consistent with m3m (cubic).

Symmetry elements in EBSD pattern

Phase identification using databases

Phase Identification - How it is done

Phase Identification - How it is done

Phase Identification - How it is done

Phase Identification - How it is done

Identification of Phases on Fracture Surfaces with EBSD

Ni-Gd Phase Diagram

1270C 1200C 1110C

Phase Identification in an Ni-Cr-Mo-W-Gd alloy

EDS shows presence of Ni and Cr

Phase Identification in an Ni-Cr-Mo-W-Gd alloy

Gd-Ni phase is identified as GdNi5 (hexagonal)

Identification of Phases in a Gd modified 304 Stainless Steel Alloy

Fracture of Ta Alloy Weld

Fracture of Ta Alloy Weld (cont.)

HfO2 HfO2 HfO2

Orthorhombic (6.47% error) Monoclinic (1.95% error) Monoclinic (1.95% error)

Fracture of Ta Alloy Weld (cont.)

Precipitate identified as monoclinic HfO2

Particle Identification - Non-volatile Memory Fabrication

Particles formed on Ru barrier layer

Particle Identification - Non-volatile Memory Fabrication

Particle Identification - Non-volatile Memory Fabrication

Unknown Mineral Identification

HOLZ Rings in EBSD

Mo2C (Hexagonal a = 0.3012 nm c = 0.4735 nm)

Fe3C (Orthorhombic a = 0.5091 nm b = 0.6743 nm c = 0.4526 nm)

Higher Order Laue Zone Analysis of BEKPs

Actual H-1 for [211] 0.5427 nm

HOLZ Ring Analysis of Chromium Carbide

HOLZ Ring Measurements for SiC Polytype Identification

HOLZ Rings for Primitive Cell Calculation

Hmeas= 0.645 nm Hcalc = 0.6443 nm

4 Hmeas= 0.822 nm Hcalc = 0.8089 nm 3

Hmeas= 0.837 nm Hcalc = 0.8581 nm

HOLZ Rings for Primitive Cell Calculation

Primitive Unit Cell Determination of Mo 2C (hexagonal)

Zone 1 H-1 = 0.48 nm

= 32.0 = 47.3 = 24.3

Primitive Unit Cell Determination of Mo 2C (hexagonal)

= 88.2 = 89.1 = 118.7

Cell volume = 37.0 3

Cell volume = 37.1 3