Application of Electron Back Scatter Diffraction

$: Application of Electron Back Scatter Diffraction$
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 WorkshopDXC 2004 WorkshopPrinciples & Use of Principles & Use of Microdiffraction &Microdiffraction &MicrofluorescenceMicrofluorescence

Ray Goehner & Joe MichaelSandia National LaboratoriesAlbuquerque, 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 d-spacing

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

1970’s Venables et al. were first to observe EBSP in SEM

1980’s Dingley et al. began using these patterns for orientation studies

1990’s Wright and Adams developed automatic system for texture (OIM)

Michael & Goehner. develop technique for phase identification

Cameras for EBSD – Typical Arrangement

Sample surface Phosphor screen

Pole piece

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

# B

acks

catte

red

elec

tron

s

0 10 20 30Energy (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 µm 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 similarcomposition.

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

m m

m

m

4mm

m

m

m3m

m

m

2mm

Point group <111> <100> <110> <uu0> <uuw> <uvw>

m3m 3m 4mm 2mm m m 1

43m 3m 2mm m 1 m 1

432 3 4 2 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

.

30 µm

Austenite

Ferrite

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.

Ni-Gd Phase Diagram

600

800

1000

1200

1400

1600

0 20 40 60 80 100

Wt% Nickel

1455°C

1275°C1285°C1270°C

1200°C

1110°C

1010°C

880°C

1280°C

14635°C

735°C

1313°C

1235°C

33

87

1487°C

Gd

3Ni 2

Gd

3Ni

GdN

i

GdN

i 2

GdN

i 3

Gd

2Ni 7

GdN

i 4

GdN

i 5

Gd

2Ni 17

(Ni)(αGd)

(βGd)

L

Gd Ni

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

10 µm

EDS shows presence of Ni and Gd

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

5.84 wt% Gd

Microstructures are complexThe secondary rim and the associated

gadolinides could not be identified

Sigma (FeCr)

Ferrite

Austenite

(Ni,Fe)3Gd

Ferrite

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 matchesHf3N2 Trigonal (2.14% error) HfO2 Orthorhombic (6.47% error)HfO2 Monoclinic (2.25% error) HfO2 Monoclinic (1.95% error)HfO2 Tetragonal (1.64% error) HfO2 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 IdentificationUnknown Mineral Identification

SEPatterns obtained at 20 kV Patterns obtained at 20 kV from phase containing from phase containing PbPband O. Database search and O. Database search yielded 7 possible matches. yielded 7 possible matches. Automated phase Automated phase identification selected identification selected PlattneritePlattnerite (PbO(PbO22), a ), a tetragonal phase, as the tetragonal phase, as the correct identification based correct identification based on chemistry, unit cell on chemistry, unit cell volume and pattern volume and pattern simulation. simulation.

BSE

JRM 971022

HOLZ Rings in EBSD

Mo2C (Hexagonala = 0.3012 nm c = 0.4735 nm)

Fe3C (Orthorhombica = 0.5091 nm b = 0.6743 nmc = 0.4526 nm)

Higher Order Laue Zone Analysis of BEKPs

1/λ

HG

θ

H = spacing of planes in reciprocal space

1/H = spacing of the planes in real space

H = k(1-cos 2θ) = 2k(sin2 θ)

where k = 1/λ

Hematite (Fe2O3)

5 kV 10 kV 20 kV

30 kV

kV H-1 error %

5 0.543 0.05

10 0.544 0.19

20 0.544 0.30

25 0.541 0.38

30 0.544 0.19

Actual H-1 for [211] 0.5427 nm

25 kV

HOLZ Ring Analysis of Chromium Carbide

[ 001]HOLZ

HOLZ ring around [001] used

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 determineunique 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 nmHcalc = 0.57704nm

Hmeas= 0.822 nmHcalc = 0.8089 nm



1

3

2

4

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 α = 56.1°

b = 0.65 nm β = 44.5°

c = 0.65 nm γ = 66.8°

Primitive unit cell from reduction :

a = 0.58 nm α = 89.4°

b = 0.58 nm β = 112.0°

c = 0.58 nm γ = 89.0°

volume = 179 Å3

Primitive Unit cell for AsFeS :

a = 0.5741 nm α = 90°

b = 0.5668 nm β = 111.93°

c = 0.57704 nm γ = 90.0°

volume = 174.1 Å3

Primitive Unit Cell Determination of Mo 2C (hexagonal)

Zone 1H-1 = 0.48 nm

Zone 2H-1 = 0.56 nm

Zone 3H-1 = 0.71 nm

Angles between zones:

1 -> 2 = 32.0°

2 -> 3 = 24.3°

3 ->1 = 47.3°

Arbitrary Unit Cell:

a = 0.71 nm α = 32.0°

b = 0.56 nm β = 47.3°

c = 0.48 nm γ = 24.3°

Primitive Unit Cell Determination of Mo 2C (hexagonal)

Primitive Unit Cell:

a = 0.30 nm α = 88.2°

b = 0.30 nm β = 89.1°

c = 0.48 nm γ = 118.7°

Cell volume = 37.0 Å3

Published Unit Cell:

a = 0.3012 nm α = 90°

b = 0.3012 nm β = 90°

c = 0.4735 nm γ = 120°

Cell volume = 37.1 Å3

Primitive Unit Cell Determination - HOLZ Rings are not required

Primitive Unit Cell from HOLZ Rings

a = 0.27 nm α = 106°

b = 0.28 nm β = 108°

c = 0.29 nm γ = 111°

volume = 15.9 Å3

Primitive Unit Cell from Kikuchi Lines

a = 0.26 nm α = 107°

b = 0.27 nm β =107°

c = 0.27 nm γ = 111°

volume = 15.3 Å3

Primitive Unit Cell for Mo

a = 0.272 nm α = 109.47°

b = 0.272 nm β = 109.47°

c = 0.272 nm γ = 109.47°

volume = 15.6 Å3

Primitive Unit Cell Determination From Kikuchi Line Pairs

Primitive Unit Cell from Kikuchi Lines

a = 0.24 nm α = 61°

b = 0.24 nm β = 61°

c = 0.24 nm γ = 61°

volume = 10.1 Å3

Primitive Unit Cell for Ni

a = 0.248 nm α = 60°

b = 0.248 nm β = 60°

c = 0.248 nm γ = 60°

volume = 10.9 Å3

SummaryThe 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 diffractionto 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 symbolsACOM automated crystal orientation measurements

bcc body centred cubic (crystal structure)BKDP backscatter Kikuchi diffraction pattern

CET columnar to equiaxed transition (solidification)EBSD electron backscatter diffractionEDX energy dispersive X-ray spectrometry

fcc face centred cubic (crystal structure)FEG field emission gunFIB focused ion beamGB grain boundary

GBE grain boundary engineeringHAB high angle boundaryHAZ heat affected zone (welding)

hcp hexagonal close packed (crystal structure)HOLZ higher order Laue zone

KS Kurdjumov–Sachs (see ‘Appendix’)LAB low angle boundaryMR misorientation relationship (between product

phases)NW Nishiyama–Wassermann (see ‘Appendix’)

ODF orientation distribution function (texture)OIM orientation imaging microscopy

OR orientation relationship (between parent andproduct phases)

PTMC phenomenological theory of martensitecrystallography

SEM scanning electron microscope (or microscopy)SMA shape memory alloyTEM transmission electron microscope (or

microscopy)TRIP transformation induced plasticityWM weld metal

XRD X-ray diffraction2D two-dimensional3D three-dimensional

IntroductionThe electron backscatter diffraction (EBSD) technique,also termed automated crystal orientation measure-ments (ACOM), orientation imaging microscopy(OIM) and the Backscatter Kikuchi diffraction pattern(BKDP) technique, is utilised to determine the localcrystal structure and orientation of materials. It makesfull use of the versatility and multiscale capability of thescanning electron microscope (SEM). The principles andapplications of the technique can be found elsewhere(e.g. Schwartz, 2000; Dingley, 2004) and will be onlyshortly recalled here. Before leaving the material,backscattered electrons diffract at crystal lattice planesin the probe area. They are then intercepted by aphosphor screen (Fig. 1). Owing to Bragg diffractionconditions and to the sample to screen distance, bandscentred on diffracting planes are observed. By measuringthe location and spatial orientation of such bands onecan either determine the crystal structure or, if thecrystal structure is known, crystal orientation. Thespatial resolution is about 10–50 nm parallel to the tiltaxis, depending on the sample and operating conditions(Humphreys, 1999 and 2004; Dingley, 2004). Theangular accuracy of measurements is y1 and y0.5ufor misorientation between neighbouring areas (Dingley,2004; Humphreys, 2004) and can be improved down toy0.1u for particular applications if special care is taken(Humphreys, 2004). The technique has been developedsince the 1970s (Venables, 1973) and automatic mappinghas been readily available for about ten years. TheEBSD is used to investigate, e.g. texture and recrystalli-sation (Jazaeri et al., 2004), deformation mechanismsand local strains (Lehockey et al., 2000; Wilkinson,2000), interface characterisation (Randle, 2004) andcracking (Gourgues, 2002). Through cooperationbetween EBSD system providers and users, the techni-que has strongly developed in the past few years,including a dramatic increase in data acquisition speedthanks to digital cameras, increasing complexity of dataprocessing to extract more information from EBSD

Ecole des Mines de Paris, Centre des Materiaux PM Fourt, UMR CNRS7633, BP 87, 91003 Evry cedex, France

*Corresponding author, email [email protected]

� 2007 Institute of Materials, Minerals and Mining and ASM InternationalPublished by Maney for the Institute and ASM InternationalDOI 10.1179/174328007X160254 International Materials Reviews 2007 VOL 52 NO 2 65

data, including new pattern and map processing algo-rithms (Wright and Nowell, 2006; Brewer et al., 2006),coupling with chemical information or even reconstruct-ing parent grains as will be discussed below.

First reviews involving EBSD addressed a variety oftopics, often illustrated with a few examples (Dingleyand Randle, 1992; Mason and Adams, 1994; Randle,1994). Up to now, the number of papers mentioningEBSD is growing very rapidly (typically multiplied bytwo every year), showing that EBSD is now a routinelyused technique available in many laboratories. Thus,many reviews focused on one specific topic, such asapplicability 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 addressedthe application of EBSD to phase transformations. Thistopic is not new but it has developed only gradually. Inthe first review by Dingley and Randle (1992) only threeexamples of studies on multiphase materials were given.Applications of EBSD to solidification (Mason andAdams, 1994) and to phase identification (Randle, 1994)then began to develop. Most detailed reviews on topicsclose to phase transformations addressed phase identi-fication (Schwartz et al., 2000; Baba-Kishi, 2002). Thepresent author did not find any review paper addressingapplications of EBSD to solidification and more

generally to phase transformations in open literature,while the number of published studies is significant (togive a figure, more than 700 papers were read to writethe present review).

The present review aims to survey how EBSD is usedto address phase transformations. In this field, EBSDhas mainly been used so far to ‘revisit’ a number offeatures concerning phase transformations, the varietyof which is illustrated below, and for which crystal-lographic data were already available. This bothvalidates the EBSD technique and provides a significantnumber of data with rather simple sample preparation.The EBSD can now be used as a reference technique, yetwith limits that are discussed below, to investigate phasetransformations in the future.

Original results obtained with EBSD that were notaccessible using other techniques are also reviewed,highlighting specific advantages of EBSD in a number ofcases.

The review is organised according to transformationmechanisms, using tabular form in many cases forclarity. First, information is given on basic phenomenarelated to phase transformations (phase identification,thermodynamics and kinetics). The next two sections aredevoted to solidification and solid state phase transfor-mations respectively. Then, surface phenomena such asenvironmentally assisted reactions and thin film deposi-tion, which are of increasing practical interest, areaddressed. In the last section, coupling of EBSD withother experimental techniques and with numericalmodelling is discussed, illustrating promising ways toobtain better insight into phase transformationphenomena.

Phase identification and basicphenomena related to phasetransformations

Phase identificationElectron backscatter diffraction can be a powerful toolfor phase identification, in particular for new or complexcrystal structures or for mineral materials. The EBSD iscomplementary to longer established techniques basedon transmission electron microscopy (TEM), X-raydiffraction (XRD) and even light optical microscopy inthe case of minerals.

Crystal structure identification

This topic has been thoroughly addressed in the reviewby Baba-Kishi (2002). Here, more recent results andresults using other techniques together with EBSD arediscussed. The main advantage of EBSD versus localXRD (such as Kossel or pseudo-Kossel analysis) is itsability to perform rapid analysis, with high spatialresolution, at the expense of accuracy in crystalorientation and lattice parameter determination(Goehner and Michael, 1995; Dabritz et al., 2001).Lattice parameters can be evaluated either from theband width (which is proportional to the sine of thecorresponding Bragg angle) or from the size of higherorder Laue zone (HOLZ) rings in EBSD patterns (Baba-Kishi, 2002). The accuracy of measurements depends ondata acquisition conditions and on the chemicalcomposition of the analysed area. By using HOLZ ringsit can be better than 1%, if care is taken to correct for

(a)

(b)

a Electron diffraction according to Bragg’s law(2dhklsinh5nl); b EBSD pattern from a bainitic steel (bcccrystal structure)

1 Principle of EBSD analysis

Gourgues-Lorenzon Application of electron backscatter diffraction to the study of phase transformations

66 International Materials Reviews 2007 VOL 52 NO 2

distortions due to the gnomonic projection or to atomicnumber (Baba-Kishi, 1998; Michael, 1999 and 2000;Michael and Eades, 2000). However, for elements suchas Mo or W, the error is still about a few per cents(Michael and Eades, 2000). The location of HOLZ ringsin EBSD patterns can also be used to distinguishbetween polytypes, in particular in clay minerals(Kogure et al., 2005). Using the band width gives loweraccuracy [typically a few per cents (Michael andGoehner, 1993)] even with increasing the specimen toscreen distance or optimising the indexing algorithm(Vatne et al., 1998; Dingley, 2004). Extinction effects(Michael and Eades, 2000) and cell multiplicity (Vaillantet al., 2003) must be taken into account. The feasibilityof EBSD assisted phase identification (e.g. Michael andGoehner, 1993) essentially depends on the ‘signal tobackground noise’ ratio (Small et al., 2002), on back-ground acquisition (Michael, 2000; Small and Michael,2001) and on relief effects (Michael, 2000), not much onthe yield of backscattered electrons (Small and Michael,2002). Therefore, good results can be obtained withextraction replicas [e.g. for PbO2 (Michael, 2000) andU3O8 (Small and Michael, 2001)]. Particles over about0.3–1 mm in size can be readily analysed with EBSD(Straumal et al., 1999; Small and Michael, 2001).

Crystal symmetry has been addressed with EBSD fora long time (Baba-Kishi, 2002). 27 out of the 32 pointgroups can be identified using EBSD patterns.Identification methods of point and space groups aredetailed elsewhere (Baba-Kishi and Dingley, 1989;Michael 2000; Baba-Kishi, 2002). This field has stillbeen developed since these review papers [(see e.g. Kralet al., 2004) for iron rich phases in an Al–Si alloy], inparticular for minerals and quasicrystals. Super-structures of ordered intermetallic phases such as theL10 c phase in TiAl alloys are difficult to investigate byrapid, automated analysis, so that they are often ignoredif the distinction between them is not of utmost impor-tance for the considered application (Pouchou et al.,2004b). Special attention has been paid to minerals formany years (e.g. Dingley, 1984; Leinum et al., 2004) andin particular to polytype identification. Kogure (2003)developed a method based on band location andintensity, still using kinematic theory of electron–matterinteractions, which shows recognisable patterns char-acteristic of each polytype. This method gives goodresults for phyllosilicate minerals (Kogure, 2002 and2003; Kogure and Bunno, 2004; Kogure et al., 2005).Others established robust reflection tables (i.e. extinctionconditions) as e.g. for omphacite (Mauler et al., 1998).Identification of quasicrystal structures still generallyrequires manual indexation of patterns [e.g. forAl60Cu26Fe14 (Cheung et al., 2001)]. Special care mustbe taken to check the symmetry (including from insidethe bands) around zone axes, to distinguish ‘true’quasicrystals from their crystalline approximants(Ruhnow et al., 2002).

Coupling EBSD with chemical analysis

Energy dispersive X-ray spectrometry (EDX) microana-lysis is frequently available in the SEM together with theEBSD facility, allowing combination of chemical andcrystallographic information (although optimised oper-ating conditions are not the same). Starting fromsequential analysis of the same area, EBSD can be usedto facilitate EDX-based phase identification, especially

for off stoichiometry phases and for phases havingidentical or similar chemical compositions but differentcrystal structures (Camus, 2000; Kogure, 2002;Boettinger et al., 2003; Kogure and Bunno, 2004; Kralet al., 2004; Leinum et al., 2004). Up to date availablesystems now combine both crystallographic and chemi-cal analysis for automated phase identification (Michael,2000; Dingley, 2004; Nowell and Wright, 2004; Zhonget al., 2006). For rapid data acquisition and processing,the location of bands in the EBSD pattern is stored foreach data point, together with chemical analysis. Thechemical composition is then used to index every patternin an offline manner. This is especially useful when theidentity of phases is not known in advance, or if datacollection must be rapid (e.g. for in situ investigations).The spatial resolution is limited, however, to that ofEDX analysis (y1 mm), both for in plane dimensionsand along the sample normal.

Distinguishing between known phases

Minerals have been studied with EBSD due to theirfrequently low crystal symmetry and to the widecollection angle (y90u) provided by this technique. Insome instances, a list of reflections needs to be firstcalculated or corrected and then given to the EBSDsystem [e.g. omphacite in eclogite minerals (Mauler et al.,1998) and Al–Si–O triclinic phase in kyanite (Dingleyet al., 2004)]. In some cases manual adjustment is stillnecessary to insure right indexation of the EBSDpatterns [e.g. garnets and sulphides (Prior et al.,1999)]. While researchers in the past had to work withfilms to improve sensitivity and image contrast (Dingley,1984), new digital cameras now allow online working inthe SEM. The case of polytype minerals involves bothnumerical calculation of the patterns and visual identi-fication of individual patterns, provided that crystals aresuitably 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 EBSDcameras allow switching from manual to automatedEBSD [e.g. for iron ore and sinter (Magalhaes, 2002;Sasaki et al., 2005a)]. Advantages and challenges ofusing EBSD to investigate ceramic materials havealready been reviewed (Farrer et al., 2000) and will notbe recalled here. Recent studies addressed an increasingvariety of materials such as oxides (Michael andGoehner, 1993; Rogers et al., 1994; Randle, 1994;Korte et al., 2000; Cha et al., 2006), functional materials[YBCO (Koblischka et al., 2003; Koblischka-Venevaet al., 2003)], zeolites (Pennock et al., 2001), PbTiO3

domains (Yang et al., 1994), silicon (Her et al., 2000),eutectic fibres (Nakai et al., 2005; Lee et al., 2005),materials for nuclear applications (Medevielle et al.,1999) and applications are still rapidly growing. As anillustration, example studies of quasicrystals and metal-lic glasses are reported in Table 1.

Phase identification is also useful to understand in situsynthesis of composites through interfacial reactions.Good examples are given by AlN/Ti composites leadingto several (Ti,Al)Ny nitrides (Paransky et al., 1999,2000a and 2000b) and by sintered WC/VC/TiC/Cocermets (Arenas et al., 2005). Alignment of strengthen-ing particles during composite processing (Schuh andDunand, 2001), formation of intermediate phases duringtransient liquid phase bonding of a Ni base superalloy(Jalilian et al., 2006) and carbide formation in SiC/Ti


International Materials Reviews 2007 VOL 52 NO 2 67

alloy filamentary composites (Duda and Gourgues,2006) were also investigated with EBSD.

As SEM is much easier on electron conductingsamples, most EBSD studies have yet been carried outon metals and metal alloys. Besides many others, somespecifically address phase identification, as for exampleidentification of small precipitates [e.g. NiSn4

(Boettinger et al., 2003), MX particles in Ni base alloys(Ramirez and Lippold, 2004), discontinuous precipitatesin ancient components (Wanhill, 2005) and Laves phasesin austenitic alloys (Michael and Goehner, 1994; Robinoet al., 1997)], of topologically close packed precipitatesin tempered weldments (El-Dasher and Torres, 2004), ofeutectic 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; Nolzeet al., 2005). First principles calculations have been usedto find crystal structures and lattice parameters forfurther automatic indexing of EBSD patterns [e.g. innewly discovered Al2(Mg,Ca) ternary Laves phases(Zhong et al., 2006)]. The case of alloys particularlydifficult to investigate such as Pu–Ga alloys (Boehlertet al., 2001) and cerium (Boehlert et al., 2003a) should bementioned. Analysis of EBSD also allows convenientphase separation on fracture surfaces (not readilyavailable with TEM) (Foct and Akdut, 1993; Bacheet al., 1997a and 1997b) and for texture determination(not always easy by XRD) (Xu and Russell, 2004; Dunstand Mecking, 1996). The EBSD can also facilitateevidence of phase transformation (Sano et al., 2003b;Neishi et al., 2004; Zhu, 2004).

Discrimination by EBSD between phases having closeor even identical crystal structures is difficult. In somecases, the lattice parameter is used [e.g. to separate g9T

from e in Zn–Al–Cu alloys (Zhu et al., 2001, 2003a and2003b)]. In other cases, the quality of the patterns ismuch 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 andsecondary a phases in a titanium alloy (Germain et al.,2005a) were distinguished using backscattered electron

imaging. An alternative method using light opticalmicroscopy was also developed (Thomas et al., 2005).Discrimination between such phases also allows map-ping spatial and size distribution of them (see e.g.Schwarzer et al., 2000).

Equilibrium phase diagram assessmentRapid phase identification by EBSD, together withassessment of properties of individual constituents bylocal measurements has recently been reviewed in theframework of diffusion multiples (Zhao, 2006). Withthis technique, a whole isothermal section of one (orseveral) ternary diagram can be assessed after only onelong term heat treatment. This has been applied tovarious ternary alloys, assuming local equilibrium atinterfaces. However, the effect of local crystallographyon diffusion and on phase nucleation was not discussed(Zhao et al., 2001, 2002, 2003, 2004a, 2004b; Zhao, 2004;Zhong et al., 2006). Modification of existing phasediagrams can be suggested by EBSD results [e.g. for1200 and 1600uC isothermal sections of the quaternaryMo–Ti–Si–B diagram (Yang et al., 2005)]. Applicationof EBSD to local adjustment of the liquidus surface ofthe Ti–Al–(Nb) system is illustrated by identification ofthe solidification sequence (Takeyama et al., 2004).Except for this latter case, EBSD was mostly used as acomplementary technique to discriminate betweenphases having complex and close chemical compositionsbut different crystal structures. Rapid mapping facilitiesthat are now available should put EDX plus EBSDas leading experimental techniques for phase diagraminvestigations in the next future.

Electron backscatter diffraction and kineticissues of phase transformationsAnisotropy of ‘free’ surface and interfacial energy

‘Free’ surface energy

The equilibrium shape of single crystals is a goodtranslation of free surface energy into a measurableproperty. Provided that crystals are suitably orientedwith respect to the SEM, surface planes can be indexedwith EBSD, as e.g. ZnO well faceted fibres (Huang et al.,2004), clay minerals (Kogure et al., 2005; Kameda et al.,

Table 1 Phase identification assisted by EBSD in quasicrystals and metallic glasses

Material Phases of interestPhase identificationmethod Results Ref.

Cast Al–Cu–Fe alloys b-Al(Cu,Fe) (CsCl) Cu rich phases,e phases, icosahedral quasicrystallineand R phases, l-Al13Fe4 dendrites

EBSD z EDX Crystal orientations,orientation relationshipsbetween phases

Gui et al.,2001

Cast Al–20Cu–15Fe(at.-%)

Al60Cu26Fe14 (icosahedral), b-Al(Cu,Fe)(CsCl), near-l Al44Cu54Fe2

Manual indexing anduse of ‘Kikuchi’ atlas

Structural model of theicosahedral phaseconsistent with TEMresults

Cheung et al.,2001

AA6013 Al alloy Fe rich phase Symmetry in EBSDpatterns, comparisonwith XRD results

Not a quasicrystallinephase but crystallineapproximant

Ruhnow et al.,2002

Al–Cu–Fe–B b-Al(Cu,Fe) (CsCl), Fe2AlB2 (bodycentred orthorhombic), quasicrystallinematrix

Point analysis Identification of phases,orientation relationshipsbetween phases

Brien et al.,2004

Fe–Co–Zr–Mo–W–Bmetallic glass

ZrB2 (hexagonal) Automatic indexing withvarious crystal structuresand lattice parameters

Identification of thisresidual crystallinephase

Castellero et al.,2004

Zr–Cu–Al–Ni metallicglass

Zr–Cu–Al–Ni–O [face centred cubic(fcc)]

Use of band width Identification of phasestemming from oxygencontamination

Vaillant et al.,2003



2005) and tape cast ceramics (Markondeya Raj et al.,1999). Surface energy of SrTiO3 perovskite has beeninvestigated by trace or 3D plane analysis after boththermal grooving (Sano et al., 2003a) and coarseningwith TiO2 rich liquid (Sano et al., 2005). Interfacemigration assisted by an amorphous phase has beenstudied in sapphire single crystals bonded to sapphirepolycrystals as a function of the local orientation of‘free’ surface planes (Farrer et al., 2006). Relativeenergies of low index planes can be rather easilycompared by this way with minimum sample prepara-tion and on a larger data basis compared with TEMtechniques. On the other hand, assumptions have to bemade to accurately determine the spatial orientation ofthe free surface planes (see ‘Discussion’).

Internal interfaces

Interfaces are good candidates for heterogeneous phasenucleation, depending on their free energy. Electronbackscatter diffraction has been used in many ways inthis field. Interface wetting [e.g. Zn by Ga (Traskineet al., 2005), partially molten olivine aggregates (Fauland Fitz Gerald, 1999)] involve classification of ‘dry’and ‘wet’ interfaces according to e.g. the misorientationangle between neighbouring crystals (this being readilyaccessible with EBSD). The effect of lattice coincidencein these two cases is not obvious. The same result wasobtained with solid state spreading of copper on coppersubstrate (Missiaen et al., 2005). Thermal groovingcoupled with EBSD and near field microscopy givesaccess to interface energy anisotropy. Here again,coincidence site lattice criteria fail to qualitativelycompare 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 boundaryenergy correlates with none of usual criteria such ascoincidence site lattice, misorientation angle, tilt v. twistcharacter or plane boundary matching.

Segregation of solute atoms to boundaries has alsobeen investigated with EBSD in hydrogen containingAl–5Mg alloy (Horikawa and Yoshida, 2004) and Nbdoped rutile (TiO2) (Pang and Wynblatt, 2006).Coincidence site lattice boundaries are often resistantto solute atom segregation and thus to localisedcorrosion and fracture [e.g. in Ni (Cornen and LeGall, 2004), in boron containing AISI 304 stainless steel(Kurban et al., 2006) and for intergranular fracture ofFe–0.002C–0.06P (Williams et al., 2004)]. By readilyacquiring a high number of data, EBSD allows study ofthe ‘grain boundary character distribution’, which is inturn influenced by the interface energy distribution, as afunction of parameters such as chemical composition. InSn–Ag–Cu lead free solder alloys, Telang et al. (2004)showed that Ag (respectively Cu) tends to reduce(respectively increase) the difference in free energybetween various types of boundaries in the material.

Diffusion along interfaces

Interface diffusion may be characterised with the help ofEBSD as a function of the local interface structure. Themain difficulty is accurate determination of the localcrystallographic 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 angleboundaries (LABs) and S3 twin boundaries, allowing

only slow diffusion, are not sensitive to discontinuousordering. Vacancy migration is very difficult if no,111. direction is close to the GB plane, so that thesensitivity of high angle boundaries (HABs) to discon-tinuous ordering depends on both GB misorientationand local orientation of the GB plane (Bischoff et al.,1998; Semenov et al., 1998). Surface rearrangement inFeO is also strongly affected by neighbouring GBs,whatever the local free surface orientation (determinedby EBSD), due to preferential GB diffusion (Bahgatet al., 2005). Depending on the local crystallographicorientation of free surfaces, a Kirkendall effect due todifferences in solute atom diffusion can be observedafter phase trans formation [e.g. in Ti–9 wt-%Mo (Guoand Enomoto, 2006)].

Anisotropy of bulk diffusion

Anisotropy of bulk diffusion strongly depends on thecrystal structure. The EBSD was used to investigatediffusion of Cr in tetragonal Mo5Si3, for which thediffusivity along [100] and [010] directions is higher thanalong the [001] direction (Strom and Zhang, 2005).When single crystals are not readily available, diffusionin coarse grained materials after EBSD identification ofeach grain orientation is a convenient tool in this field[see e.g. oxygen tracer diffusion in (La2–xSrx)CuO4

(Claus et al., 1994)].

Solidification and semisolid state

Nucleation of solid phaseNucleation occurs at a very local scale, which cannot beaccessed with the SEM. However, one of its conse-quences (i.e. crystal orientation) can be efficientlystudied with EBSD, in particular when sample prepara-tion is tedious (e.g. for composite or heterogeneousmaterials such as welded joints), or if the microstructureis too coarse to be characterised with TEM or XRD. Byallowing access to local crystallography over large areas,the EBSD technique facilitates investigation of phenom-ena that are difficult to access by TEM, such asheterogeneous nucleation at a substrate surface or atscarcely distributed particles. Examples are numerousand 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. Specificorientation relationships (ORs) between nucleatingparticles and solidifying material have been observedin, e.g. aluminium inoculated with a TiC forming alloy[cube–cube OR (Tronche and Greer, 2001)] and in AISI409 ferritic stainless steel at TiN particles ({001}TiN//{001}ferrite and ,110.TiN//,100.ferrite) (Hunter andFerry, 2002a) leading to highly textured material.Equiaxed, randomly textured grains nucleate at segre-gated areas of the heat affected zone (HAZ) of Sc or Zrcontaining aluminium alloys (Kostrivas and Lippold,2004). Sb and Pb were shown to strongly inhibitnucleation of the solid phase in zinc based hot dipcoatings (Quiroga et al., 2004; Rappaz et al., 2004).

Solidification path

The EBSD has been intensively used for stainless steels,whose solidification path strongly depends on bothchemical composition and solidification rate. Theaustenite (fcc c) phase generally forms first in rapid



solidification, whereas ferrite (bcc d) forms first at lowersolidification rates. This has been illustrated in laser(Robino et al., 1998; Katayama et al., 1999; Brookset al., 2003; Iamboliev et al., 2003) and gas tungsten arc(Robino et al., 1998; Iamboliev et al., 2003) weldedalloys. As d and c phases exhibit particular ORs whenone forms by solid state transformation from the other,it is rather easy to determine by EBSD, with informationon both phase morphology and crystallography, whichphase was the first to form, if any. When a strong textureis observed, but not these particular ORs, one cansuppose that both d and c formed simultaneously duringsolidification. This could be the case in weld metal (WM)deposits (Bouche et al., 2000) (Fig. 2). The EBSDprovides information, which in these coarse grainedmaterials cannot by obtained with XRD, and on a muchmore reliable statistical basis than by TEM.

Information about abrupt changes in solidificationmode can be given by EBSD. By continuously varyingCO2 laser welding speed or base metal composition ofFe–18Cr–(10–14)Ni alloys, Fukumoto and Kurz (1997)showed that the change in solidification mode occurredwith no change in crystal orientation and no nucleationof new misoriented crystal, but after some undercooling.Owing to the higher distance between d and the cdendrite tips than between c and the d dendrite tips, theFA (d then c) to AF (c then d) transition occurred morereadily than the AF to FA transition.

The EBSD proved useful to investigate the solidifica-tion path of MCrAlY alloys deposited on a Ni basesuperalloy by continuous CO2 laser cladding (Bezenconet al., 2003), as soon as the lattice misfit could beaccommodated by LABs, the fcc c phase first formed byepitaxial growth. As soon as another primary phaseformed (e.g. b-NiAl), nucleation occurred and epitaxywas no longer possible. The solidification structure ofsmall areas in heterogeneous materials was also inves-tigated by EBSD at the right scale in laser deposited Ti–10 at.-%Cr alloys (Banerjee et al., 2002), in eutecticareas of Gd containing Ni–Cr–Mo alloy ingot (Robinoet al., 2003) and in Mg–Li–Ca cast alloys (Song andKral, 2005).

A recent example of application of EBSD to asolidification problem of great practical significancewas given by Sengupta et al. (2006), who studiedoscillation marks and hooks in continuously cast lowcarbon steel slabs. As the meniscus line still remained aHAB, it was clearly visible even after several phasetransformations occurred during cooling. It wasdeduced that solid phases did not nucleate at the sametime on both sides of the frozen meniscus. Owing to thelarge grain size and sample geometry, such informationcould only be accessed using EBSD.

Eutectic solidification

Nucleation of coarse eutectic grains was first studiedwith EBSD in white cast irons (Randle and Laird II,1993). A colony of hexagonal M7C3 carbides wassuggested to originate from a single nucleus. Most otherstudies addressed alloys undergoing dendritic, theneutectic solidification, to check whether the crystalorientation of the eutectic phase was the same as thatof its dendritic counterpart, i.e. if there was or notnucleation of that phase from the undercooled liquid. Inan arc melted hypereutectic Nb–Si alloy, Drawin et al.(2005) showed that Nb3Si shared a common crystal

orientation in eutectic colonies and in some dendriteneighbours. The vast majority of published workaddressed the solidification of Al–Si alloys modifiedwith Sr, Sb, Cr, Na and P and cast as small ingots. Thechange in morphology of eutectic silicon from lamellarto fibrous could not be unambiguously related to achange in OR between dendritic and eutectic (Al) phases(Dahle et al., 2001). While in unmodified alloys eutectic(Al) had most often the same crystal orientation as aneighbouring dendrite, this was not the case for

(a)

(b)

2 a light optical micrograph of type 316L stainless steel

WM and b {110} pole figure, in c austenite frame, of d

ferrite (individual dots) located at c LABs, showing

either KS ORs (surrounded by circles and triangles) or

near cube–cube ORs (surrounded by rectangles)

between d and c. After Bouche et al. (2000)



modified 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 thoughtto increase the efficiency of nucleating agents, leading toindependent nucleation of eutectic (Al) from the liquid,just as for a columnar to equiaxed transition (CET)(Nogita and Dahle, 2001a). In contrast with thesecommercial purity alloys, Heiberg and Arnberg (2001)and Heiberg et al. (2002) did not find any CET in highpurity Al–Si–(Sr) alloys; eutectic and dendritic (Al)phases shared the same crystal orientation and thus nobarrier to nucleation of eutectic (Al) from dendritic (Al)was found. Electron backscatter diffraction on both (Al)and (Si) phases (Heiberg and Arnberg, 2001) showed noparticular change in internal twinning of eutectic (Si)and no particular OR between both phases, althougheutectic (Si) had a ,110. fibre texture. Here again, theneed to characterise fine scale microstructures withincoarse grains obviously suggests EBSD as the mostsuitable technique to get statistically reliable andmetallurgically relevant information.

Peritectic solidification

Rather few studies have been dedicated to peritecticsolidification except for stainless steels (see section onsolidification path). In cast iron, no OR was foundbetween newly formed M3C and already existing M7C3

carbides at which they very likely nucleated (Randle andLaird II, 1993). The peritectic c2c9 solidification ofmodel and CMSX–4 single crystal nickel base super-alloys (Warnken et al., 2005) was studied at coarseshrinkage cavities; ball shaped c9 particles had a cube–cube OR with the dendritic c substrate.

Orientation relationships between seed (or substrate ormould) and solid

Chill or external zones of ingots or thin strip castingshave frequently been shown to exhibit a fine grained,randomly textured microstructure, except for some caseswhere a strong fibre texture was already observed with

EBSD (Summers et al., 2004). At a very local scale, arandom texture can be induced by nucleation at a roughsubstrate followed by locally textured growth [e.g. instainless steels (Hunter and Ferry, 2002b; Ferry andHunter, 2002)]. Numerous misoriented equiaxed grainswere also observed in molten silicon droplets solidifiedon a silicon wafer substrate (Nagashio et al., 2004)although liquid spreading did not allow columnargrowth perpendicular to the contact plane in thatparticular case.

Single crystal superalloys such as CMSX–4 andCM186LC exhibit a randomly textured chill zone.With EBSD one can check that the distribution ofmisorientation between grains follows the classical curvefor textureless cubic materials (Ardakani et al., 2000).

Epitaxy between the HAZ and the WM can be readilycharacterised with EBSD at the local (grain to grain)scale (Table 2). The EBSD was also used to evaluateORs between seed and solidified material in complexmicrostructures, as in fully lamellar c-TiAl alloys. Here,various grains appeared at the seed, sharing one ,110.

direction with it. In Ti–48Al the selected grain had thesame crystal orientation as the seed. In Ti–48Al–8Nb afew variants having one ,110] direction of lamellaeparallel to one of the seed were observed (Takeyamaet al., 2004).

Functionally graded materials may be obtained bylaser melt injection. Interfacial reactions and ORsbetween the injected ceramic powder particles and thehot metal matrix can be characterised with EBSD ata very local scale, allowing better insight into thesolidification mechanism. Ocelık et al. (2001) examinedone hundred interfaces between Al4C3 and SiC powderin the reaction layer of laser melt injected Al–SiCcomposites. In 25% of observed cases, {0001}SiC wasparallel to {0001}Al4C3

, according to the angle betweenthe {0001}Al4C3

plane and the temperature gradient. Incontrast with extrusion (where Al4C3 is not formed), noOR was observed between SiC particles and (Al) matrix.Specific ORs were observed in reaction zones of

Table 2 Orientation relationships found with EBSD in weld solidification

Base metal Weld metal OR between WM and HAZ Ref.

Be alloy Autogeneous electronbeam welding

Epitaxy at HAZ equiaxed grains Wright and Cotton,1995

Al alloys GTAW* with or withoutfiller metal

Equiaxed WM: no OR, no texture;dendritic WM: epitaxy on HAZ

Kostrivas and Lippold,2004

Gd containing Ni base alloy Autogeneous electronbeam and GTAW

Columnar WM in epitaxy with HAZ Robino et al., 2003

CMSX–4 Ni base superalloyzMCrAlY Laser cladding Cube–cube OR if primary solidificationinto c; no OR otherwise (b or b z c)

Bezencon et al., 2003

AISI 304 and 310S austenitic stainlesssteels

Pulsed YAG laser Cube–cube OR for solidification into c,no clear OR for solidification into d

Katayama et al., 1999,Iamboliev et al., 2003

AISI 304 austenitic stainless steel GTAW Kurdjumov–Sachs (KS) OR betweenferritic WM and austenitic HAZ

Iamboliev et al., 2003

Free machining stainless steel Autogeneous pulsedYAG laser

Epitaxy (no fusion boundary) if solidifiedinto c; no clear OR if solidified into d

Brooks et al., 2003

High purity Fe and Monel 70–30 filler GTAW Nishiyama–Wassermann (NW) and BainORs{

Nelson et al., 1999a

2.25Cr–1Mo steel and 625 Ni base filler GTAW Mostly Bain OR{ Nelson et al., 1999aA508 low alloy steel and AISI 309Laustenitic filler

GTAW Bain, sometimes NW OR Nelson et al., 1999a

AISI 409 ferritic stainless steel andMonel 70–30 filler

GTAW No OR (chill zone) Nelson et al., 1999b

*GTAW: gas tungsten arc welding.{In fact, cube–cube OR during solidification into austenite and then solid state transformation into ferrite in HAZ.



functionally graded Ti–6Al–4V/SiC or WC compositesproduced by laser melt injection, depending on the facetsof powder particles (Pei et al., 2002; de Hosson andOcelık, 2003). A functionally graded aluminium alloycontaining Al3Ti particles showed no OR betweenphases in centrifugally casting, leading to a morpholo-gical texture of Al3Ti platelets with no crystal texture inthe (Al) matrix (Watanabe et al., 2002).

Growth of solid phasesGrowth direction

Studies of EBSD on growth direction with respect to thethermal gradient have concentrated on directionalsolidification, where microstructures are frequentlycoarse grained (Table 3). In eutectic and peritecticmicrostructures, morphology and crystallographic ORsare intimately related, as reported below (section onmicrotextures). As an example of dendritic solidifica-tion, Nagashio and Kuribayashi (2005) associatedEBSD with light confocal microscopy (Fig. 3) toevidence the transition in growth direction from,211. to ,110. and then to ,100. for splatquenching of silicon onto silicon wafers. The transitionwas interpreted with facet planes and liquid/solid interfacial energy thanks to careful experimentalobservations.

Grain size and morphology

The EBSD technique is a good means to evaluate the grainsize and shape on a quantitative basis, grains being definedby boundaries of misorientation angle higher than a userfixed threshold. This implies that the ‘cleaning’ procedureused for EBSD data processing should be suitably chosenand clearly reported. Some examples in as solidifiedmicrostructures are given in Table 4. The EBSD isparticularly useful when the grain size is similar to thesize of the part, i.e. for so called ‘multicrystals’. This isthe case, for example, for lead free, coarse grained singleshear lap Sn–3.5Ag solder joints (Telang and Bieler, 2002,2005a and 2005b) and for Co–Cr–Mo laser cladding onrailway wheels (Farooq et al., 2006).

The EBSD may also reveal that individual particlesare in fact single crystals [e.g. coarse Bi particles in Bi–24.8In–18.0Sn eutectics (Ruggiero and Rutter, 1995)]or polycrystals composed of several grains [e.g. M7C3

carbides in high chromium white cast iron (Powell andRandle, 1997)].

Interrupted solidification tests allow investigatingmicrostructure formation, although the quenched liquidmay be difficult to distinguish with EBSD from thegrowing solid. The EDX may be here of great help tostudy solid/solid grain boundaries already formed beforequenching (Liu et al., 2005). In other cases, EBSDpatterns from the quenched liquid cannot be indexed, sothat the shape of the solid/liquid interface is easilyrevealed with this technique [e.g. in Fe–4.3Ni (Farynaet al., 2002)].

Phase connectivity is difficult to assess from lightoptical or electron microscopy imaging only. Byidentifying areas of the material sharing a commoncrystal orientation, EBSD provides interesting informa-tion even from two-dimensional (2D) sections, i.e.individual crystals of a 2D section may in fact belongto the same three-dimensional (3D) grain. Someexamples are given in Table 5. This is particularly usefulwhen individual grains are connected in 3D, but notin 2D (e.g. in EBSD maps or thin foil TEM images).Another side of the problem is grain clustering:misorientation gradients, which may influence productproperties, are readily revealed with EBSD as long as

3 Results of EBSD on determination of local dendrite

crystallography in splat quenched silicon: after

Nagashio and Kuribayashi (2005)

Table 3 Results of EBSD on solidification growth direction

Material Solidification process Solidification mode Crystal direction of solid growth Ref.

Ti–26Al–27Nb–0.03O(at.-%)

Induction float zonemelting

Directional solidification ,100.bcc Boehlert and Bingert,2001

Pb(Mg1/3Nb2/3)O3 z

PbTiO3

High pressureBridgman

Cellular [110]rhombohedral, sometimes 12–20ufrom it (trace analysis)

Soundararajan et al.,2004

Nb–33Ti–16Si (at.-%) Czochralski Cellular–dendritic [113]Nb; [001](Nb,Ti)3Si Sutliff and Bewlay,1996

AZ91 Mg alloy Bridgman Columnar ,1120. or ,2445. according tothermal gradient and growth rate;can be primary and ternary ,1120.

and secondary (,1120. z ,2445.)

Pettersen and Ryum,1989; Pettersen et al.,1990

Be alloy Electron beam welding Columnar ,1010. favoured Wright and Cotton,1995

Fe–3Si Twin roll casting Columnar Often close to ,100.bcc Takatani et al., 2000Al–Zn–Si Hot dip galvanising Dendritic–columnar

(Al)Neither ,100.Al nor ,110.Al,close to ,320.Al (trace analysis)

Semoroz et al., 2001

Zn Hot dip galvanising Dendritic (Zn) Mainly ,1010.hcp Semoroz et al., 2002bTi–6Al–4V Vacuum arc remelting Columnar ,100.bcc (leading to ,1120.hcp)

0 and , 45u from heat flowGlavicic et al., 2003c

Ni base Alloy 22 Gas tungsten arcwelding

Dendritic–columnar ,100.fcc (followed by partialrecrystallisation)

El-Dasher et al., 2006



mapping is possible. Grain clustering may be related tothe solidification texture, which increases the frequencyof LABs (West and Adams, 1997). Here, grain size andgrain connectivity strongly depend on the definition ofgrains given by the EBSD user.

Competitive grain growth

During crystal growth, a strong selection may occuramong 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 theundercooled melt. This competition is governed by thegrowth rate of individual grains, which is in turn relatedto the local crystal orientation with respect to the localheat flow.

During directional solidification, competitive graingrowth leading to a columnar zone with an increasinggrain size (e.g. Fig. 4) was clearly evidenced thanks to

Table 4 Electron backscatter diffraction characterisation of grain size and morphology of as solidified microstructures

Material Solidification process Grain size or morphology Ref.

2024 Al alloy Metal inert gas welding More than 80% of the WM 5

equiaxed grains of 50–100 mmin size

Lefebvre et al., 2005

Si Simulated melt spinning Equiaxed grains nucleate in thechill zone, followed by columnargrowth

Nagashio and Kuribayashi,2006

Si Splat cooling on Si wafer Many equiaxed grains near thecentre

Nagashio et al., 2004

AISI 316L stainless steel Autogenous CO2 laserwelding

Grain size 200 mm; cellular (size 3 mm)if the laser beam is focused, non-cellularif irradiation is uniform

Kell et al., 2005

2618 Al alloy Thixoforming Globular grains with HABs if cast atliquidus temperature

Xia and Tausig, 1998

Inconel 82 Ni base alloy Tungsten inert gas weldingwith low carbon steel

Grain size about 150–300 mm dependingon magnetic stirring

Kokawa et al., 1999

5052 and 5182 Al alloys Direct chill and twin rollcasting

Same grain size found with EBSD andlight microscopy (but not in the sameobservation plane)

Slamova et al., 2003

Al–0.15Fe–0.07Si Direct chill casting Same grain size (140 mm) found withEBSD and light microscopy

Samajdar and Doherty,1994

AZ91D and AM60BMg–Al alloys

High pressure die casting Grain size distribution before solutionannealing (not possible in light microscopy)

Bowles et al., 2004

Fe–15 at.-%Ga Roll casting Grain size 6.3–7.9 mm Saito et al., 2004Al–7Si–0.3Mg As cast with artificial

shrinkage porosityAverage grain size ,300 mm Buffiere et al., 2001

Al–7Si–0.4Mg Low temperature semiliquiddie casting

Cells clustered into single crystal coloniesdelimited by HABs

Han et al., 2001

Si–30Al Spray forming Grain size (y5 mm for Si and 250 mm for Al)in the divorced eutectic formed after slowcooling; the difference is due to nucleationconditions (Si from droplets, Al within theformed material)

Hogg et al., 2006

Table 5 Phase and grain connectivity determined with EBSD in as solidified microstructures

Material Solidification process Results obtained with EBSD Ref.

Al–1.25Mn Directional (cellular) Highly interpenetrated grains Sun and Ryum, 1992White cast irons As cast Hypereutectic alloy: M7C3 carbides

are single crystalline over large areas(shown by deep etching to beinterconnected); hypoeutectic alloy:M7C3 carbides are individual crystallites

Randle and Powell, 1993

High Cr white cast irons As cast Connectivity of carbides varies from onematerial to the other

Powell and Randle, 1997

Sn–17 wt-%Pb Quenched from semisolidstate

2D spatial connectivity is not correlatedto crystal orientation: 3D percolation issuggested; no coalescence (density ofLABs decreases with increasing time):Ostwald ripening

Wolfsdorf-Brenner et al., 1999

Sn–1.4 wt-%Cd Directionally solidifiedoscillating peritectic

a phase: multilayered grains connectedin 3D; b phase: connected even in 2D

Zeisler-Mashl et al., 1997

Ni–Cr–Co–Ti–Al–Mo–Sisuperalloy

Directionally solidified ingot Grain clustering with strong internalorientation gradients

West and Adams, 1997

Zn alloy Hot dip galvanising Polycrystalline ‘grains’ with domains ofsame crystal orientation possiblyconnected in 3D

Semoroz et al., 2002a

Ni–18.7 at.-%Sn Containerless anomalouseutectic

Ni3Sn (near single crystalline):connected network; Ni: individualtextureless particles

Li et al., 2005b



EBSD in an Al–1.25Mn alloy (Sun and Ryum, 1992)and in a beryllium alloy weld (Wright and Cotton,1995). A more or less strong ,100. texture was foundto gradually develop in X–750, CMSX–4 and CM186LCnickel base superalloys (Gandin et al., 1995; Ardakaniet al., 2000; D’Souza et al., 2000), in a twin roll cast Fe–3Si alloy (Takatani et al., 2000) and in austeniticstainless steels with simulated strip casting on Cusubstrates of controlled roughness (Hunter and Ferry,2002b and 2002c). In fact, the viscosity of the liquidcontrols the formation of secondary and tertiarydendrite arms (D’Souza et al., 2000). In case of lowviscosity, the competition between grains depends on therelative orientations of the primary dendrite arms [e.g. inCMSX–4 bicrystals, see (Wagner et al., 2004. Stanfordet al., 2004b)].

The origin of new undesirable ‘stray’ grains cannot beassessed from 2D measurements; in a laboratory nickelbase superalloy, serial sectioning coupled with EBSDmapping proved that stray grains nucleated at mouldwalls and not from dendrite fragmentation or constitu-tional undercooling (Stanford et al., 2004b). Stray grainformation was also characterised after electron beamand 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 toimprove the shape of isothermal curves using appro-priate modelling coupled with EBSD experimentalvalidation (e.g. (Kermanpur et al., 2000) on IN738 alloyand (Carter et al., 2000) for innovative single crystalcasting design)

By allowing crystal orientation mapping over largeareas, EBSD is particularly well suited to studies of the

CET during solidification. The CET occurs due to localmodification of thermal and/or chemical or mechanicalconditions near the tips of growing dendrites. Examplesmay be found for eutectic solidification (see sectionon nucleation in eutectic solidification), and also fordendritic and cellular solidification (Table 6).

In hot dip galvanising, grains nucleate with no textureand competitive grain growth depends on both dendritegrowth directions and grain orientation with respect tothe solid/liquid interface (here the grain thickness ismuch lower than the in plane grain size) (Semoroz et al.,2002a and 2002b; Quiroga et al., 2004).

Such EBSD investigations have also been applied tothe more complex case of two phase solidification in Fe–19Cr–11Ni stainless steels, solidified by autogeneous gastungsten arc welding interrupted by liquid tin quenching(Inoue et al., 2000). Competitive grain growth in each ofthe ferrite and austenite phases was eventually governedby the local crystal orientation of the HAZ at the fusionline (Fig. 5).

Dendrite fragmentation and semisolid state

Dendrite fragmentation may appear during recalescenceor after partial melting of the seed in single crystal

4 Competitive grain growth during solidification, illu-

strated with EBSD grain boundary map of X–750Ni

base superalloy: after Gandin et al. (1995)

Table 6 Studies on CET using EBSD

Material Solidification process CET mechanismInformation provided byEBSD Ref.

CMSX–4 Ni basesuperalloy

Laser metal forming Constitutional undercooling Number of nuclei per unitvolume

Gaumannet al., 2001

IN718 Ni base superalloy Vacuum arc remelting Constitutional undercooling ‘Tree rings’ (solidificationdefects) consist of equiaxedgrains

Xu et al.,2002a

Ni–1B Electrostatic levitationmelting

Cell fragmentation(undercooling ,200 K)

Remaining solid is recognisedthanks to twin orientations

Li et al.,2005a

Ni–1B Electrostatic andelectromagnetic levitationmelting

Dendrite fragmentation(undercooling: 70–200 K)

Grain size and shape; rotationof fragments between non-fragmented dendrites

Li et al.,2006

Cu, Cu–1 at.-%Ag, Fe–10 at.-%Ni, low carbonsteel

Magnetic levitation melting Magnetic stirring: surfaceoscillation or bulk convectionin liquid sphere

Evidence of equiaxed areas Yasudaet al., 2005

5 Competitive grain growth during solidification 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)



casting. For a high volume fraction of liquid, dendritefragments may rotate, so that a random texture is foundin that area after solidification [e.g. in CMSX–4 singlecrystals (Stanford et al., 2004a) and in Ni–1B lasermelted under electrostatic levitation (Li et al., 2005a)].In directionally solidified Ni–18.7 at.-%Sn having ananomalous eutectic microstructure, recalescence affectedthe Ni phase but not the Ni3Sn phase, so that Nifragments could not rotate easily and only LABs wereeventually observed with EBSD (Li et al., 2005b). Whenthe liquid fraction is rather low and no LABs areobserved between dendrite fragments, one may concludeto Ostwald ripening instead of coalescence [e.g. inreheated Al–7Si–0.3Mg alloy (Kliauga and Ferrante,2005)].

When a 6082 aluminium alloy is cast from thesemisolid state, grains tend to cluster into agglomerateshaving low energy (LAB or twin) boundaries. Thus,EBSD may distinguish ‘former’ aggregates after solidi-fication completion, showing intensive grain agglomera-tion if the mix is stirred, but very little in the absence ofstirring (Arnberg et al., 1999). Grain fragmentationduring agglomeration of silicon particles in thixoformedAl–30Si–5Cu–2Mg (wt-%) alloy has been shown usingEBSD to be of {111} type, leading to {111} agglomera-tion boundaries (Hogg and Atkinson, 2005). One mustnot forget, however, that EBSD does not distinguishbetween the former solid phase and the quenched liquid,which may solidify epitaxially on existing crystals, sothat great care must be taken while evaluating the grainboundary character distribution (Liu et al., 2005).

Solidification microtexture and resultingaverage textureSolidification microtexture

Orientation relationships between solid phases in assolidified microstructures have been investigated inmodified Al–Si alloys (see section on nucleation ineutectics). In as cast Al62.5–Cu25–Fe12.5 and Al65–Cu20–Fe15 alloys (Gui et al., 2001), no OR was found betweenl-Al13Fe4 single crystal dendrites and respectively theicosahedral quasicrystalline matrix and the polycrystal-line R-phase. In as welded austenitic stainless steel, theKurdjumov–Sachs OR (see ‘Appendix’) was foundbetween bcc d ferrite and fcc c austenite in lacy ferritemicrostructure (Inoue et al., 2000) whereas only acommon ,100. crystal direction, parallel to the growthdirection, was found between d and c phases in skeletalferrite microstructures (Inoue et al., 2000; Bouche et al.,2000). High resolution studies of solidification micro-textures are made possible thanks to EBSD. Forinstance, vacuum cast joints of white irons exhibitM7C3 carbides, surrounded by M3C with the samecrystal orientation, which are embedded in a ferritic ironmatrix (Wuhrer et al., 2004). Small, highly misorientedgrains have been observed in directionally solidified melttextured YBCO alloyed with YBa2CuO5 (Koblischka-Veneva et al., 2003; Koblischka et al., 2003). At (211)phase particles, the orientation of the (123) YBCOmatrix was strongly disturbed from its (001) texture,depending on the orientation of the individual (211)phases.

The EBSD is particularly useful if dendritic grains arevery coarse in size but with a very fine internal micro-structure. Few EBSD results addressed identification of

primary trunks from tertiary arms [e.g. in directionallysolidified Mg–9Al–1Zn alloy (Pettersen and Ryum,1989)]. Others focused on internal misorientation withindendritic grains. These may affect both morphology andinternal misorientations e.g. in ,112. dendrites of Al–4.3Cu–0.3Mg alloy in certain conditions (Henry et al.,1998b). In most cases, however, crystal orientationgradients are found within dendrites, due to fluid flowand shrinkage stresses (Doherty, 2003) or to gradient insolute concentration or to substrate induced thermalstresses (Semoroz et al., 2001). Some examples ofquantitative measurements using EBSD are given inTable 7.

Practical example: growth of ‘feathery’ grains

Very coarse, undesirable ‘feathery’ grains with fanshaped dendrites develop in certain conditions at theexpense of columnar grains in aluminium alloys. Theymostly appear during direct chill casting of alloyscontaining no refining elements, with high thermalgradients beyond the solidification front and underconvection (Rappaz and Henry, 1999). By EBSDmapping of wide areas at a fine scale compared to thedendrite arm width, Henry et al. showed that featherygrains were composed by parallel lamellae with alter-nating twin related crystal orientations; {111} bound-aries being alternatively (coherent and straight) and(incoherent and wavy) (Henry et al., 1997, 1998a and1998b). Within one main orientation, some subbound-aries were even found (Henry et al., 1997). Thecorresponding misorientation tended to accumulateleading to the fan shaped morphology (Henry et al.,1998b). The crystal direction parallel to the thermalgradient (,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 tothe thermal gradient. The detailed role of convection oncounterflow growth of ,110.Al twinned arms isreported elsewhere (Rappaz and Henry, 1999; Henryet al., 2004). Details about the anisotropy of primarydendrite arm spacing and 3D morphology can be foundin (Henry et al., 1998a).

Microtexture of eutectic and peritectic alloys

Eutectic and peritectic alloys often exhibit coarsecolonies of fine lamellae, so that high spatial resolutionis required over wide areas. Sample preparation is madedifficult by the difference in electrochemical and hard-ness properties of the various phases, so that EBSDstudies are still scarce. Some results on ORs found ineutectic and peritectic materials are illustrated inTable 8.

Average texture of as solidified products

The average texture is in many cases preferablyinvestigated by XRD. However, when the grain sizeexceeds a certain value (typically 50–100 mm), XRD canno longer provide statistically significant data. Neutrondiffraction can be used for grains up to y1 mm in size.For even coarser grains and for heterogeneous materialssuch as welded joints, EBSD can still be used thanks tostage motion in the SEM. In EBSD, the orientationdistribution function (ODF) is then directly calculated



Table 7 Electron backscatter diffraction measurements of internal misorientation in dendritic grains

Material Solidification processMisorientations measuredwith EBSD Ref.

Al–0.15Fe–0.07Si Direct chill casting Many misorientations upto 5u within dendrites

Samajdar and Doherty,1994

CMSX–4 Ni base single crystalsuperalloy

CO2 laser metal forming After 5 passes, arms becometrunks with 5–10u misorientationbetween dendrites

Gaumann et al., 1999

CMSX–4 Ni base single crystalsuperalloy

CO2 laser epitaxial cladding Slight misorientations betweendendrite trunks are viewedthanks to specifically developeddata processing

Cleton et al., 1999

CMSX–4 and CMSX–10N Nibase single crystal superalloys

Directional casting of turbineblades

Steady state growth: internalmisorientations of 2–3u do notcumulate; non-steady stategrowth: successive branchingcumulates misorientation up to y6u

D’Souza et al., 2005;Newell et al., 2005

99.9% pure Al Ingot casting (columnar zone) Misorientation of 4–10u over 3 mmalong the growth direction; internalLABs of 6–8u

Bhattacharyya et al.,2001

Al–Zn–Si alloy Hot dip galvanising Dendrite arms misoriented by4–10u mm21. Misorientations up to5u within grains, cumulate up to35u in coarser grains


High Cr white cast irons Electromagnetic stirring andcasting

Austenite grains are clusters ofsubgrains and internal LABs aresolute enriched and could originatefrom dendrite arm bending

Yang et al., 2003

Zn–0.2Al–0.15Sb Hot dip galvanising One nucleus only for dendrites in agiven grain; orientation domainsrelated by simple ORs in‘polycrystalline’ grains


Table 8 Electron backscatter diffraction measurements of orientation relationships in as solidified eutectic andperitectic microstructures*

MaterialSolidificationmode Microstructure OR between phases Growth direction Ref.

Ni–Cr–(Si) whitecast iron

Slow cooling(0.017 K s–1)

E for 0%Si, P for2%Si

0%Si: no OR betweenM3C formed at a givenM7C3

Strong [0001]M7C3

for 2%Si; no texturein M3C for 0%Si

Randle andLaird, II 1993

White iron Strip casting E Plate like Fe3C: [001]Fe3C//

normal direction // [001]a

[001]Fe3C// plane of

platesSong et al.,2003a

V–13 at.-%Si Directional E (broken lamellar) (011)V3Si // (112)V // lamellaeboundaries

[100]V3Si // [111]V Bei et al.,2004

Cr–16 at.-%Si Directional E (lamellar) (011)Cr3Si // (123)Cr // lamellaeboundaries, (001)Cr3Si // (011)Cr //lamellae boundaries

[100]Cr3Si // [111]Cr (closepacked directions)

Bei et al.,2003

Ni–45.5Al–9Mo(at.-%)

Directional E (NiAl matrix z

Mo fibres){011}Mo // {011}NiAl // interfaces ,100.Mo // ,100.NiAl Bei and

George, 2005Mg–33Al–Sr(wt-%)

Directional E (lamellar) (1101)Mg // (101)Mg17Al1210u from

interface[1120]Mg // [111]Mg17Al12

2–15u from growthdirection

Guldberg andRyum, 2000

Nb–22 at.-%Si Arc melting inCu crucible

E {111}Nb3Si // {111}Nb (one areastudied)

Drawin et al.,2005

Nb–16Si–1.5Zr(at.-%)

Arc melting inCu crucible

E No OR between Nb and Nb3Si Miura et al.,2005c

Al–7Si–(0–150 ppmSr)

Ingot casting E No Sr: two twin related Si variants;with Sr: various twin related Sivariants with one common ,110.

per colony, often parallel to ,100.

or ,110.Al; no clear OR betweenAl and Si

Heiberg andArnberg, 2001

Al2O3–19 mol.-%YAG

Directional(fibres)

E ,0001.Al2O3// ,112.YAG Nakai et al.,

2005Al2O3–16%YAG–18 mol.-%ZrO2

Micropulling E (lamellar) Three intricate single crystals pereutectic grain, ,2110.Al2O3

//,100.ZrO2

, YAG is much lesstextured

Murayamaet al., 2004a

Al2O3– 16%YAG–19 mol.-%ZrO2

Directional(rods)

E (‘geometric’ or‘Chinese scripts’)

No clear OR between fibretextured Al2O3 and ZrO2

Murayamaet al., 2004b

*E: eutectic; P: peritectic; YAG: yttrium–aluminium garnet.



from individual orientations by taking one point pergrain or by taking all data points and weightingorientation data with the respective area fraction ofgrains. If the grain size is low enough, EBSD and XRDresults can be successfully compared (e.g. Slamova et al.,2003; Saito et al., 2004). One must, however, keep inmind that EBSD is a surface analysis technique.Sectioning effects may be significant when grains arenot equiaxed, which is frequently the case in solidifica-tion microstructures.

Spatial information given by EBSD is necessary whenthe heat flow 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 com-plementary method to evaluate GBs of samples whilethe average texture is determined by XRD (Park et al.,1999). Some examples obtained in as solidified bulkmaterials are listed in Table 11.

A strong average texture induces particular ORsbetween grains, as e.g. in a ,100. textured directionally

Table 9 Solidification textures determined with EBSD in thin strip castings and hot dip coatings

Material Microstructure Average texture Ref.

Cast iron Grey, compacted ornodular

Inoculated materials: notexture in austenite andthus no texture in resulting ferrite

Campos et al., 2005

0.1%C steel (dendritic growth) Strong {100} texture Umezawa et al., 2003Fe–3Si ‘Upper’ and ‘lower’

columnar zones versusmid-thickness

,100. // local thermalgradient versus randomly textured

Takatani et al., 2000

Fe–15 at.-%Ga Strong ,100. texture withmany LABs

Saito et al., 2004

AISI 409 ferritic stainless steel Columnar zone ,001. fibre (ferrite) Ferry and Hunter, 2002AISI 304 austenitic stainless steel Columnar zone ,001. fibre (austenite) Ferry and Hunter, 2002AISI 409 ferritic stainless steel(simulated thin strip casting)

Chill zone and growthzone

Ti free (respectively Ti containing)steel: random texture (respectively,001. fibre) in chill zone, ,001.

increases in growth zone in bothcases

Hunter and Ferry, 2002a

AISI 304 austenitic stainless steel(simulated thin strip casting)

Chill zone and growthzone

,001. fibre increases duringgrowth

Hunter and Ferry, 2002b

Sn–3.5Ag and other Pb free solderalloys

Multicrystalline solderjoints

,110]Sn // heat flow, mainly‘special’ GBs

Telang et al., 2002;Telang and Bieler, 2005a,2005c

Al–Mg 5052 and 5182 alloys Elongated and equiaxedgrains

Less cube component than indirect chill castings


Al–43.4Zn–1.6Si (hot dip coating) No average texture: the coatingdoes not inherit that of steelsubstrate


Zn–0.2Al–0.15Sb (hot dip coating) 43% of grains have their {0001}planes less than 22.5u from thefree surface due to constrainedgrowth


Table 10 Average solidification textures determined with EBSD after welding or laser metal forming*

Material Process Microstructure Average texture Ref.

5182 and 6111 Al alloys Laser welding Columnar andequiaxed zones

,100. for columnar,random for equiaxed

Hector et al., 2004

Austenitic stainless steel GTA welding then liquid tinquenching

Cellular ,001. (ferrite) Inoue et al., 1995and 1998

AISI 409 ferritic stainlesssteel with Monel Ni–30Cu–Mn

Dissimilar GTA welded joints Growth area ,100. (austenite) Nelson et al.,1999b

Ni alloy 182 Multipass MMA welding Columnar ,100. Scott et al., 2005Ni alloy 82 Multipass GTA welding with

or without magnetic stirringStraight solidificationfront under magneticstirring, curved frontotherwise

,100. under magneticfield, random otherwise

Kokawa et al.,1999

Mg and AZ31, AZ61 andAZ91 Mg alloys

Autogeneous EB welding Weak texture Su et al., 2002

Mg alloys Autogeneous GTA welding Weak texture Wu et al., 2004A286 Fe based superalloy CO2 laser welding Weld metal centre Rotated cube Weiß et al., 2002CMSX–4 Ni base superalloy CO2 laser welding Welding at 30u from

,001.: many smallgrains

,001. // local thermalgradient

Hirose et al., 2003

CMSX–4 Ni base superalloy Multipass CO2 laser metalforming

Substrate and deposit ,001. fibre within 5u forsubstrate and within 10ufor deposit

Gaumann et al.,1999

*GTA: gas tungsten arc; MMA: manual metal arc; EB: electron beam.



solidified nickel base alloy ingot (West and Adams,1997); many subboundaries developed and grainsclustered into coarse entities having internal LABs andstrong orientation gradients. The size of such entitiesgrew faster than the grain size itself, due to stronglytextured (competitive) grain growth. In directionallysolidified CMSX–4 and CM186LC nickel base super-alloys, misorientation axes got close to the ,100. fibreduring growth; many LABs were also found, but‘special’ GBs such as S5, S13a and S17a (all misor-ientation around ,100. axes) were not favoured(Ardakani et al., 2000).

Hot cracking and GB resistanceHot cracking during solidification is of major practicalconcern. The EBSD was mainly applied to problemsassociated with welding. In nickel base alloy 718, HAZliquation was shown to occur at random GBs but not atcoincidence site lattice (CSL) boundaries, according tothe low sensitivity of CSL boundaries to boron atomsegregation (Guo et al., 1998) and to boride and carbideprecipitation (Qian and Lippold, 2003). In the [0001]Cu6Sn5 layer of solder interconnects, many HABsapparently provided penetration channels for the solderalloy (Lee et al., 2001). In free machining laser or gas

tungsten arc welded stainless steels, only alloys prone tofirst solidify into austenite were prone to hot cracking,according to the higher sensitivity of austenite toboundary segregation and cracking than that of ferrite(Brooks et al., 2003). In gadolinium containing Ni basealloy welded by electron beam or gas tungsten arcprocesses, epitaxial solidification evidenced with EBSDprovided a good resistance to hot cracking according toVarestraint tests (Robino et al., 2003).

Welding of nickel base single crystal superalloys maylead to hot cracking if the single crystals to be joined aremisaligned from each other or from the weldingdirection. The EBSD helped to establish adequatewelding conditions and to identify, if any, the highlymisoriented, newly nucleated grains that can induce hotcracking. Examples are found in laser welded CMSX–4(Hirose et al., 2003), in laser and electron beam weldedRene N5 (Vitek et al., 2003 and 2004) and in laserwelded MC2 (Wang et al., 2004) single crystals orbicrystals. Here, EBSD data on base metal orientationand WM microtexture were combined with analyticalmodels involving, e.g. local undercooling at grainboundaries.

Hot cracking in Al–4Cu alloy was also investigated byEBSD in terms of wetting of GBs by the remaining

Table 11 Solidification 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 Process Microstructure Average texture Ref.

Cu Directional solidification Columnar ,001. Grant et al., 1986AA1100 Al alloy Ingot casting Almost equiaxed Random Wang et al., 1990Al–1.25Mn Directional solidification Cellular ,001. Sun and Ryum, 1992AA 5052 and 5182 Al–Mgalloys

Direct chill and twin rollcasting

Equiaxed Copper z Brass z

cube z other texturecomponents


Ti–6Al–4V Vacuum arc remelted ingotcasting

Columnar ,100. (b phase) Glavicic et al., 2003c

Ti–48Al–2Cr–2Nb (at.-%) Ingot casting Columnar ,0001. of a phase Dupont et al., 1996Ni3Al Induction melting Columnar ,001. Hanada et al., 1986X–750 Ni base superalloy Directional solidification Columnar ,100. increases during

growthGandin et al., 1995

Fe–18.4 at.-%Ga Zone melting Columnar ,100. (ferrite) Summers et al., 2004CMSX–4 Ni base superalloy Directional solidification Columnar ,100. fibre Carter et al., 2000Duplex stainless steel Statically cast Columnar ,100. (ferrite) Calonne et al., 2000AISI 430 ferritic stainless steel Continuously cast slab Columnar zone

equiaxed zone{001},uv0. (columnar),random (equiaxed)

Hamada et al., 2003

Nb–33Ti–16Si (at.-%) Czochralski directionalsolidification

Cellular Weak ,113. for (Nb);,001. (almost singlecrystalline) for (Nb,Ti)3Si

Sutliff and Bewlay,1996

Nb–16 at.-%Si Arc melted ingot casting (Nb) dendritesz (Nb)/Nb3Sieutectic

[001] for eutectic Nb3Si;(Nb) randomly textured

Drawin et al., 2005

Nb–22 at.-%Si Arc melted ingot casting Nb3Si dendritesz (Nb)/Nb3Sieutectic

[001] for dendritic Nb3Si;(Nb) textured due to ORwith Nb3Si

Drawin et al., 2005

Cu6Sn5 Soldering Cu6Sn5 scalloplike grains

[0001] Lee et al., 2001

ZrB2/ZrC Spark plasma sintering ZrB2 weakly textured, ZrCrandomly textured

Shim et al., 2002

Al/Al3Ti Centrifugal solid particlecasting

Coarse Al grainsand Al3Ti platelets

Both Al and Al3Ti arerandomly textured

Watanabe et al.,2002

V–V3Si Directional solidification Eutectic ,111.V//,100.V3Si Bei et al., 2004Al2O3–YAG–ZrO2 eutectic Modified micropulling ‘Chinese scripts’

‘geometric’,2110. or ,1010.Al2O3

,,001. or ,220.ZrO2

,possibly ,100. or,111.YAG

,0001. or ,1010.Al2O3,

,001. or ,220.ZrO2,

,100. or ,111.YAG

Murayama et al.,2004b; Lee et al.,2005



liquid as a function of barium content and GB misor-ientation. By decreasing the liquid/solid interfacialenergy (deduced from minimum misorientation angleof wetted GBs and Read–Shockley equations) and thusdelaying grain coalescence, barium strongly increasedhot cracking sensitivity of this alloy (Fallet et al., 2006).

Electron backscatter diffraction andsolidification: summaryElectron backscatter diffraction is of particular interestin solidification investigations because of its ability tocharacterise the microstructures at multiple scales withsuitable statistical significance, from (sometimes very)coarse grains down to submicrometre sized phases suchas nucleating agents and eutectic colonies. Its angularand spatial resolution is generally high enough for thatpurpose. Geometric and statistical effects due tosectioning and sampling effects must be taken intoaccount or, if possible, avoided by carrying out 3Dinvestigations (see ‘Discussion’).

Solid state phase transformations

Orientation relationships between phasesMatrix phase transformations

The EBSD was generally used in this field to confirmTEM or XRD data or, alternatively, to get statisticallyreliable results. A huge variety of materials and phasetransformations have been addressed with EBSD asillustrated in Table 12 for ceramics, in Table 13 for non-ferrous metals and in Table 14 for intermetallic phasesand quasicrystals. Details about the most frequentlyobserved ORs are reported in the Appendix.

Most ORs were investigated at the scale of individualphases or by comparing the pole figures of productphases (formed from a single grain of the parent phase)to pole figures calculated using known ORs. Theysuccessfully compare with TEM data. Only few inves-tigations used the average pole figures (Boehlert andBingert, 2001).

Like eutectic microstructures, products of eutectoiddecomposition usually exhibit fine scale features and inmany cases only a few colonies may be observed in asingle TEM thin foil, whereas large areas may bescanned with EBSD. Four examples of results obtainedusing EBSD are given here:

(i) in Nb–(16–25)Si¡1.5Zr (at.-%), the Nb3Si partof the (NbzNb3Si) eutectic further decomposesupon cooling into tetragonal a-Nb5Si3zbcc(Nb). In binary Nb–Si alloys, eutectoid (Nb) issingle crystalline within a given eutectoid colonyand may share the same crystal orientation asthat of neighbouring eutectic (Nb) (Drawinet 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 natureof the OR depend on chemical composition andheat treatment (Miura et al., 2005b and 2005c)

(ii) in Al–36Mo–17Ti (at.-%), the b (A2) phasetransforms 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 defor-mation (Miura et al., 2005a) probably due to amemory effect on variants due to the orderedstructure of both product phases (Miura et al.,2004)

(iii) in Fe–12Mn–0.8C¡0.3V steels, decompositionof fcc austenite c into bcc ferrite a andtetragonal Fe3C cementite depends on thecomplex sequence of nucleation events (aformed at VC carbides formed at MnSsulphides) so that the KS OR between c anda is not systematically observed (Guo et al.,2001 and 2002)

(iv) in Mn–Si bearing hypo- and hypereutectoidsteels decomposed into pearlite under smallundercooling, the OR between a and Fe3Cstrongly depends on the 3D topology of phases.Given a colony nucleated at a c GB, the Pitsch–Petch OR (see ‘Appendix’) prevailed if the aphase of the pearlite colony was totally isolatedfrom the c grain where the colony did notdevelop, while the Bagaryatsky OR (see‘Appendix’) prevailed otherwise (Fig. 6). Inboth cases, Fe3C crystals at c GBs and in thecolony were found to share the same crystalorientation (Mangan and Shiflet, 1999).

In the last two examples, only association betweencareful serial sectioning and EBSD analysis allowed toget the key results. This point will be further addressedin the ‘Discussion’ section.

Precipitation

Most ORs between matrix and precipitates wereinvestigated with TEM. However, if precipitates arescarcely distributed (e.g. at boundaries of coarse grains)or if no high angular accuracy is required, EBSD mayreadily provide relevant data (Table 15). The EBSD isalso useful to study interactions between precipitationand damage cavitation, as much less sample preparationartefacts are usually induced than by TEM thin foilpreparation. Discontinuous precipitation has also beeninvestigated with EBSD. Results illustrated in Table 16are generally complementary to data obtained withTEM, although the evolution of the OR along the

Table 12 Orientation relationships determined with EBSD in solid state phase transformations of ceramic materials

Material Parent phase Product phase Orientation relationships Ref.

(001) MgO coatedwith In2O3

MgOzIn2O3 MgIn2O4 [001]MgO//[111]MgIn2O4and

[110]MgO//[110]MgIn2O4; no

OR between In2O3 and MgIn2O4

Korte et al., 2000

LaNbO4 Tetragonal Monoclinic Misorientation of 94u around[010] between product phasedomains

Jian and Wayman, 1995

Iron oxides Hematite Fe2O3 (H) Magnetite Fe3O4 (M) ,0001.H//,111.M and,1010.H//,110.M

Piazolo et al., 2004b



growing colonies might be analysed with EBSD only,especially over large distances (e.g. the last item inTable 16).

Decomposition of ferrite and austenite in ferrous alloys

Austenite (fcc c) and ferrite (bcc a or d) phases have beenwidely studied with EBSD. Several ‘classical’ ORsclustered around the 45u,001. Bain OR are recalledin the ‘Appendix’. There is still much debate about therelationship between OR and the displacive or diffusivecharacter of phase transformations in steels, in parti-cular concerning acicular ferrite, Widmanstatten ferrite

sideplates and bainite. This debate is well beyond thescope of the present review: to illustrate the variety andinterest of EBSD data about these as yet incompletelyunderstood phase transformations.

In duplex stainless steels, both d and c phases are stillpresent at room temperature, which facilitates the studyof their OR. As solidified microstructures are verycoarse, so that TEM based methods are not well suited.Note that c forms at high temperature (.1000uC) andthat high thermal stresses are expected to arise fromcooling due to the difference in thermal expansioncoefficient 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 Ni–Femetal alloys

Material Parent phaseProductphase Analysis scale Orientation relationships Ref.

Ti sheet a (hcp) b (bcc) Grains and GBs (in situ) Burgers; {334}b midribparallel to the commonclose packed plane

Seward et al.,2004

Ti–6Al–4V b (bcc) a (hcp) Macrozones Burgers for both primaryand secondary a

Le Biavantet al., 2002

Ti–8Al–(0–20)V b (bcc) a (hcp) Along one GB with gradientof chemical composition

Burgers (with oneexception)

Banerjeeet al., 2004

Ti–6Al–2Sn–4Zr–6Mo b (bcc) a (hcp) a colonies near b GBs Burgers Bhattacharyyaet al., 2003

Ti–5Ta–1.8Nb b (bcc) a (hcp) Widmanstatten colonies atGBs and primary a

More or less close toBurgers, neighbouringWidmanstatten and primarya phases having samecrystal orientation

Karthikeyanet al., 2005

Near-a a IMI834 Tialloy

b (bcc) a (hcp) Colonies of a phase Loss of Burgers OR;common close packedplanes preserved afterspheroidisation of the aphase

Germainet al., 2005b

Co b (fcc) a (hcp) Individual phases Near NW Wright et al.,2005

Cu–42 wt-%Zn b (bcc) a (fcc) At least b grains KS (from unpublishedpole figures)

Sakata et al.,2000

Cu–40Zn b (bcc) a (fcc) Widmanstatten colonies 1.7u from KS; no strict OR Stanford andBate, 2005

Cu–11 wt-%Ag b (Cu) a (Ag) Individual phases Cube–cube, i.e. samecrystal orientation

Li et al.,1994

Cu–Zn–Al b (bcc) a (fcc) Individual variants ofbainitic a phase

Pitsch Marukawaet al., 2000

Pu–2 at.-%Ga e (bcc) d (fcc) A few d variants One common ,110.d:possibly KS or NW

Boehlertet al., 2003b

Cu–12.55Al–4.84Ni(wt-%) shape memoryalloy (SMA)

P (DO3) 2H(orthorhombic)

Microtexture of diamondshaped entities

{001}2H // {110}P and[010]2H // ,001.P

Chen et al.,2000

Cu–7.3Al–8.5Mn (wt-%)SMA

L21 18R1

(monoclinic)Microtexture of lensshaped entities

Twin misorientationrelationships (MRs)between product variants

Wang et al.,2002

Fe–27.5Ni–17.7Co–3.8TiSMA

c (fcc) a9 (bcc) Local scale before andafter phase transformation

80% of ORs at (5ufrom NW

Bruckneret al., 1999

Fe–32 at.-%Ni bicrystals c (fcc) a9 (bcc) Near the GB NW Ueda et al.,2001a

Fe–32.85 wt-%Ni c (fcc) a9 (bcc) Individual variants Near GT close to themidrib; near KS close toretained austenite;gradient of OR in between

Shibataet al., 2005

Fe–29.6 wt-%Ni c (fcc) a9 (bcc) Former austenite grains,individual variants

Near NW Kitaharaet al., 2005

Ni/Ti/Ni multilayers c-Ni (fcc), a-Ti(hcp)

NiTi (B2) Average texture Probably KS for c/B2 andprobably Burgers for a/B2

Inoue et al.,2003

Ti–5Al–2Sn–4Zr–4Mo–2Cr–1Fe (b-Cez) alloy

b (bcc) a0

(orthorhombic)Individual crystals (twoperpendicular sections)

Habit plane 2u in averagefrom [312]

Zimmermannand Humbert,2002

Ni–(36–38)Al (at.-%) b (B2) indexedas bcc

c9 (L12)indexed as fcc

Individual crystals KS Sakata et al.,2001



the OR (which is measured at room temperature) is notknown yet. The OR was reported to be close to KS in ascast and as welded structures (Inoue et al., 1998; Pinol-Juez et al., 2000; Gourgues et al., 2004). In someinstances a unique OR, yet different from the wellestablished ones, was identified (Nolze, 2004 and 2006).Widmanstatten austenite tends to grow along thecommon close packed direction of the KS OR and toshare the same orientation as neighbouring allotrio-morphic (primary) austenite phase (Inoue et al., 1998),possibly with only one adjacent d grain into which it isgrowing (Pinol-Juez et al., 2000). Even massive austeniteforms in near KS OR with the parent d grain, at leastin autogeneous gas tungsten arc welded, then liquidtin quenched 21Cr–9.3Ni stainless steel (Inoue et al.,1995). Gas nitrided 22.5Cr–5.4Ni–1.9Mn–3.0Mo–0.16N

stainless steel, however, undergoes subsurface growth ofneedle shaped austenite having close packed planes aty15u from those of d ferrite (however, ferrite andaustenite textures were not measured in the samesample) (Tschiptschin et al., 2002).

Decomposition of ferrite into austenite has also beenstudied during heating in ferritic steels. To keep someaustenite phase retained after cooling at the end ofexperiments, the low carbon steel studied (0.06C) waswrapped into either nickel or austenitic stainless steelfoils before heating up to y900uC for a few minutes, tostabilise high temperature c by element diffusion(Bruckner et al., 2001; Park et al., 2002). The KS ORwas not strictly followed (departing by up to 10 or even25u). However, artefacts due to surface effects and to thelocal change in chemical composition still need further

Table 14 Orientation relationships determined with EBSD in solid state phase transformations of intermetallic alloysand quasicrystals

Material Phase transformation Analysis scale Orientation relationships Ref.

Al62.5–x–Cu25.3–Fe12.2–Bx Secondary phases in facecentred icosahedral (fci)matrix during sintering

Individual phases No OR between fci andsecondary phases

Brien et al.,2004

Ni base superalloy coatedwith NiAl

Pack cementation Individual phases(L12 phase indexedas fcc structure andB2 phase indexedas bcc structure)

{111}L12//{110}B2 and in

that plane either,112.L12

//,110.B2 or,011.L12

//,111.B2

Wollmer et al.,2003

Ni3Al coated with NiAl Pack cementation Individual phases (001)[110]L12//either

(011),111.B2 or(101),111.B2 or(014),041.B2

Zaefferer andGlatzel, 2002

Ni3Al coated with NiAl Precipitation of body centredtetragonal (bct) W2Ni

Individual phases (110)bct//(111)L12and

[001]bct//[110]L12

Zaefferer andGlatzel, 2002

Ti–25Al–24Nb (at.-%) a2 into O A few O variants Twin MR betweenvariants consistentwith a2 to O phasetransformation

Li et al., 2004

Ti–48Al–2Cr–2Nb (at.-%) a into massive c (indexedas fcc)

Individual phases (0001)a2//{111}c and

,1120.a2//,110.c z

identification of orderdomains

Pouchou et al.,2004a and2004b

Ti–48Al–2Cr–2Nb (at.-%) a (indexed as hcp) into c(indexed as fcc)

Individual phases Burgers Dupont et al.,1996

Ni–45 at.-%Al a2 into cz spheroidisation ofa2

Individual phases (0001)a2//{111}c and

maybe ,1120.a2//,110.c

(c indexed as fcc structure)

Buque andAppel 2002

Ti–25Al–10Nb–2V–1Mo (at.-%) b (B2) into a92 (DO19) Individual phases (011)b//(0001)a92and

[111]b//[2110]a92

Yang et al.,2003

Ti–46.5 at.-%Al hcp a into massive L10 czDO19 a2 (at GBs)

Lamellar grains Burgers OR with onegrain, growth into anotherone

Wang et al.,2002

Ni–36 at.-%Al b into c9 (partial, at GBs) Individual phases ,5u from KS with oneb grain, no OR with theother neighbouring b grain

Sakata et al.,2001

(Fe,Al,Ni)–10Cr a into A2 z B2 (ordering) Individual phases Cube–cube OR, raftingalong ,100. direction

Stallybrassand Sauthoff,2004

Ti–46.8Al–1.7Cr–1.8Nb (at.-%) a into c (L10) z a2 (DO19) Individual phases Blackburn (see ‘Appendix’) Dey et al.,2005

Udimet 720LI Ni basesuperalloy

Interactions betweenrecrystallisation of c matrixand c9 precipitates

Former c grains Loss of OR between c andc9: c9 keeps the cube–cubeOR with parent c grain orturns to twin OR with therecrystallised c grain

Lindsley andPierron, 2000

Mo z (210) single crystalMoSi2

Diffusion couple, formationof Mo5Si3

Individual phases [001] textured Mo5Si3(cross-sectional observations)

Tortorici andDayananda,1999

Ti–26Al–27Nb–0.03O bcc into O Average texture Results consistent with thefollowing OR: (001)O//(110)bcc

and [110]O//[111]bcc

Boehlert andBingert, 2001



analysis. Synthetic Fe–4Cr–0.008C heated up to 820uCfor 20 h and mapped with EBSD both before and afterthe heat treatment showed, in view of the interfacemigration velocity, that starting a phase and newly

formed c phase shared at least one common closepacked plane (Watanabe et al., 2005b).

The transformation of austenite into proeutectoidFe3C cementite was investigated with EBSD togetherwith 3D considerations in high-purity Fe–1.34C–13.1Mn (Mangan et al., 1999; Kral and Spanos, 2003).Seventy five per cent of the ‘dendritic’ Fe3C particlesexhibited the Pitsch, Farooque–Edmonds orThompson–Howell ORs with the neighbouring c matrix.Monolithic Fe3C plates also exhibited the Pitsch OR,while conglomerates of parallel laths exhibited theFarooque–Edmonds OR. Many cementite crystals stillexhibited no OR with neighbouring austenite. This wasattributed to nucleation outside the investigated volume.Similar results were found with Widmanstatten cemen-tite plates grown from austenite in an Fe–0.8C–12.3Mnsteel (Mangan et al., 1997).

Decomposition of austenite into ferrite, bainite ormartensite is a key point in the processing of most highstrength steel grades. Therefore, many results nowcomplete the database acquired with TEM basedmethods for many years. One major difficulty is theabsence of retained austenite in many steels of practicalinterest. Details are given here for three kinds of phasetransformations according to their temperature range:

(i) martensite

(ii) ‘high temperature’ phase transformations, i.e.formation of idiomorphic, allotriomorphic andWidmanstatten ferrite

(a) (b) (c)

6 Interrelationships between morphology and ferrite–

cementite OR in pearlite. Pitsch–Petch OR in a

hypoeutectoid Fe–C and b hypereutectoid Fe–C 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 auste-

nite grain (top) but is in fact connected as shown by

further serial sectioning (bottom). After Mangan and

Shiflet (1999)

Table 15 Determination of OR between matrix and precipitates using EBSD

Material Matrix Precipitate Results Ref.

Meteoritic minerals a (bcc) (Fe,Ni)3P No simple OR (consistentlywith TEM results)

Geist et al., 2005

Sintered Ti–4Fe–7.3MozTiB b (bcc) TiB (Widmanstatten) [010] growth of needles (OR:by TEM)

Feng et al., 2005

Zr cladded Zircaloy–2 in variousmetallurgical states

a (hcp) d (fcc) hydrides In general (0001)a//{111}d and,1120.a//,110.d; GB d with suchOR with only one neighbouringa grain; little effect of residual stresses

Une et al., 2004;Une and Ishimoto, 2006

SAF2507 superduplex stainlesssteel

c (fcc) s (decompositionof bcc d)

24u from the Nenno OR: here [101]c//[310]s Dobransky et al., 2004

Super austenitic stainless steel c (fcc) s (111)c//(110)s and [211]c//[110]s (notthe Nenno OR)

Lewis et al., 2006

Austenitic stainless steel c (fcc) M23C6 Cube–cube OR with one c grain,growth with no OR into the neighbouringc grain

Hong et al., 2001

Austenitic stainless steel c (fcc) M23C6 50% of particles in cube–cube OR,,20% next to creep cavities

Abdul Wahab and Kral,2005

Table 16 Determination of OR using EBSD for discontinuous precipitation

Material Parent phase Product phases OR Ref.

Cu–11 wt-%Ag b(Cu) (fcc) b(Cu)za(Ag) (all fcc) Cube–cube Li et al., 1994Cu–4 wt-%Ti a (fcc) a(Cu)zCu4Ti (orthorhombic) (111)a//(010)O and

[011]a//[501]O or(511)a//(010)O and[011]a//[501]O

Mangan and Shiflet, 1997

Re and Ru rich nickelbase alloy single crystal

czc9 (samecrystal orientation)

czc9ztopologicallyclose-packed phases

New c and c9 phaseskeep cube–cube OR

Lavigne et al., 2001 and2004

Nitrided Fe–(1–3)Cr a (bcc) azCrN a first cube–cube withparent a grain but twinboundaries developduring growth becauseof high volume increaseduring phase transformation

Sennour et al., 2004



(iii) ‘intermediate temperature’ phase transforma-tions, i.e. acicular and bainitic ferrite.

Martensite

Martensite results from a displacive phase transforma-tion and develops with a given OR with the parentaustenite grain into which it grows. Austenite formingelements may be added to steel composition to retainsome austenite, to facilitate investigation of the OR.Otherwise, the MRs between variants formed within agiven former austenite grain may be compared to thosecalculated using known ORs, e.g. KS/KS or NW/NWMRs. The most frequently (tried and) found ORs wereKS and NW for a9 (near bcc) martensite and Burgers forhcp e martensite (Table 17).

It is then possible to derive the crystal orientation ofparent austenite from those of martensite variantsformed within that austenite grain. This can beperformed by either graphical methods using {100} polefigures (Gourgues et al., 2000; Lambert-Perlade et al.,2004a; Cabus et al., 2004b) (Fig. 7) or by algebraiccalculations from MRs between variants (Suh et al.,2002). The former method makes no particular assump-tion about the OR (except that it is close to the BainOR), while the latter method assumes that the KS OR isstrictly followed, which is never exactly the case.

Allotriomorphic, idiomorphic and Widmanstatten ferrite

Orientation relationships between fcc and bcc phaseshave been investigated with high resolution EBSD inplessite, a mixture of fcc (taenite) and bcc (kamacite)phases found in iron and nickel rich meteorites. The ORvaries between KS and NW according to the particularmicrostructure and chemical composition of phases(Nolze and Geist, 2004). As kamacite may be deformed,such determination may be difficult; close packed planesare not strictly parallel and continuous variations of thelocal 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 Crclusters exhibited close packed planes (respectively closepacked directions) 1.27u (respectively 2u) in average fromthose of the fcc (Ni) matrix, i.e. the OR was up to 6u offKS and NW ORs (Adachi et al., 2005), irrespective ofthe deformation applied before ageing (Adachi andTsuzaki, 2005).

The OR between primary ferrite and austenite wasgenerally determined by deriving the orientation ofaustenite from those of several neighbouring martensitevariants after interrupted heat treatments (Suh et al.,2002). The assumption of KS OR is, however, asimplification as long as up to 10–20% (respectively50%) 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 (orNW) OR leads to an uncertainty double as high forMRs between product phases which can reach at least 8u(Gardiola et al., 2003). In fact, near KS or NW ORswere 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 aloading stress may weaken the OR, as e.g. in 0.15C–1.4Mn–0.25Si–B and 0.33C–1.5Mn–2Si–B steels trans-formed at 700uC under uniaxial compression (Suh et al.,2000; Kang et al., 2003). Primary ferrite grains mayshare a common orientation with neighbouring marten-site resulting from quenching (Cabus et al., 2004b) orexhibit MRs far from KS/KS (Dey et al., 2005).

Intragranular ferrite generally nucleates at inclusions,so that the austenite to ferrite OR strongly depends onthe nature of inclusions. V(C,N) precipitates may breakthe austenite–ferrite OR by introducing incoherentinterfaces with one of the ferrite (or more probablyaustenite) phases, leading to ORs (if any) far from theBain zone, e.g. Cho et al. (2002a and 2002b), Miyamoto

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

Table 17 Determination of ORs using EBSD between austenite and martensite in steels

Steel composition Martensite phase Investigation method OR Ref.

9Cr–1Mo–Nb–V a9 (ybcc) MR between a9 variants Near KS Nakashima et al., 20010.2C–12Cr–1Mo–V a9 (ybcc) MR between a9 variants KS Dronhofer et al., 20030.6C–1.5Si–1.5Mn a9 (ybcc) OR between retained c and a9 Near KS Regle et al., 20040.6C–1.5Si–1.5Mn a9 (ybcc) OR between retained c and a9 Close to NW and KS Cabus et al., 2004aInterstitial free and plaincarbon steels (0.2 to 0.6C)

a9 (ybcc) MRs between a9 variants Near KS Morito et al., 2003

AISI 301 0.13C austeniticstainless steel

a9 (ybcc) OR between a9 and c Near KS Lee et al., 2005

19.6Mn–3.1Si–2.9Al e (hcp) OR between e and c Burgers Godet et al., 2005



et al. (2003), Hernandez et al. (2003), Furuhara et al.(2003). Intragranular ferrite nucleated at deformationbands of strained austenite is also strongly texturedaccording 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 andferrite (Hurley et al., 1999; Kang and Lee, 2004).

Widmanstatten ferrite also exhibits ORs close to theBain zone with the parent austenite grain, e.g. in ironmeteorites (He et al., 2005), although the OR maycontinuously vary along the interphase interfaces (Heet al., 2006).

Acicular and bainitic ferrite

Mechanisms of austenite to bainite phase transforma-tions 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) decom-position of austenite, they also prevail for acicular ferrite(Fig. 8) and bainitic ferrite. Plate and lath bainite are amultiple scaled microstructure. Constitutive units arereadily studied by TEM; they cluster into packets (or‘sheaves’) whose size is close to the former austenitegrain size, so that the size and morphology of packets isbest studied using either SEM or light optical micro-scopy, and their crystallography using EBSD. Bainitepackets 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 isgenerally no longer present at room temperature, so thatORs are generally studied by reconstructing the averagecrystal orientation of individual austenite grains(Lambert-Perlade et al., 2004a) (Fig. 7) or by comparingMRs between packets to those calculated using, e.g. KSand NW ORs (Gourgues et al., 2000). Results obtainedwith EBSD (Table 18) generally well agree with thoseobtained with TEM at the same scale. By consideringthe {001} pole figures, e.g. those from Gourgues et al.(2000) and Verlinden et al. (2001) and the high

frequency of LABs in upper bainite packets, one findsthat no unique OR is generally followed: there arepreferred ORs and continuous (although minor innumber) data points between these preferred ORs. Thesame applies for acicular ferrite (Fig. 8c). Such data canonly be obtained by automated analysis over large areas,which are now made possible by EBSD. Thanks to fieldemission gun (FEG)-SEMs, local ORs along bainitelaths can also be checked. In a 0.6C–1.5Si–1.5Mn steel,the orientation gradient along bainitic laths maintainedthe KS OR with neighbouring film like austenite (Regleet al., 2004).

Owing to its limited angular accuracy, EBSD is notthe best tool to precisely determine an OR, for whichTEM based techniques appear best suited. However,FEG-SEMs now provide high spatial resolution, allow-ing local analysis over wide areas and thus goodstatistics. There is hardly a unique OR at roomtemperature, in particular in metals, because localresidual stresses or plastic rotation develop either duringthe phase transformation or during cooling. The inducedcrystal rotation or distortion may modify a genuine ORobeyed at the very beginning of the phase transforma-tion. Therefore, for most applications, the angularaccuracy of EBSD is generally high enough for ORdetermination.

As with other diffraction techniques, ORs may berepresented with pole figures, including higher indexpoles for which known ORs yield easily recognisablepatterns, which can be compared with experimental datacollected from a single parent grain (Nolze, 2004 and2006). ‘Convoluted’ pole figures may be calculated bythe EBSD software to improve accuracy and sharpnessand facilitate such comparisons (Nolze, 2004). TheRodrigues–Frank space is also increasingly used forORs between fcc and bcc phases (He et al., 2005). Eulerangles may also be useful in certain cases, provided thatan uncertainty interval is suitably given (Nolze et al.,2004).

(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 figures (no unique OR is found between

ferrite and austenite in either case)



Heterogeneous nucleationInvestigation of homogeneous nucleation requires a highdensity of nuclei and high resolution EBSD to get goodobservation conditions. The EBSD analysis of Fenanodendrites during crystallisation of Fe74Si11B14Ni1amorphous powders during isothermal annealing hasbeen reported (Godec et al., 2006). On the other hand,nucleation in solid state phase transformations is mostoften heterogeneous and relies on crystal structure andorientation of both parent and product phases, so thatheterogeneous nucleation has been extensively studiedwith EBSD. This section focuses on nucleation of bothprecipitates and matrix phases.

Heterogeneous nucleation of precipitates

Austenitic and duplex stainless steels suffer fromboundary precipitation of chromium rich phases afterparticular heat treatments or during high temperatureservice. By analysing a number of GBs with EBSD it wasshown in both duplex (Sato et al., 1999; Sato andKokawa, 1999; Dobransky et al., 2004) and austeniticAISI 304 (Zhou et al., 2001; Hong et al., 2001) stainlesssteels that secondary Cr23C6 and s phases hardlynucleated, or at least nucleated much more slowly atcoincident GBs (or near KS interphase interfaces).Comparing EBSD maps and corrosion tests at the samescale yielded statistically reliable data upon ‘sensitised’grain or phase boundaries. Other criteria, such as planematching boundaries or near coincident axial directiondid not seem to be selective enough. Even the wellknown Brandon criterion for coincident site latticeboundaries was not always selective enough, especiallyfor LABs (Zhou et al., 2001).

Precipitate nucleation has been studied with EBSD ina variety of materials for nuclear power generation. InNi–16Cr–9Fe–xC alloys, random GBs are favouritepaths for intergranular stress corrosion cracking andalso for precipitation of M23C6 (M,Cr) carbides(Alexandreanu et al., 2001). Here again, the GBstructure seems to influence the precipitation kinetics,morphology and size distribution of carbides (Liu et al.,1995). Hydridation of uranium and zirconium alloys isalso affected by the local GB structure; in as casturanium, hydrides form at twin boundaries and atLABs, which are readily imaged with EBSD but notwith light optical microscopy (Bingert et al., 2004).

The spheroidisation of pearlite in 0.36C–0.53Mn–0.22Si steel was further investigated with EBSD, bymonitoring LABs after thermomechanical treatmentsand imaging dissolution and reprecipitation of cementitecoupled with continuous recrystallisation of ferritegrains (Storojeva et al., 2004).

Discontinuous reactions have also been investigatedwith EBSD. In Fe–50 at.-%Co, discontinuous orderingstarts from GBs, but LABs and some coincident sitelattice boundaries seem much less sensitive (Bischoffet al., 1998; Semenov et al., 1998). The local extent ofthe reaction depends on both crystal misorientationand orientation of the GB plane (Bischoff et al., 1998).Such information can be gathered with EBSD (asso-ciated with determination of the local 3D boundarygeometry) over a statistically significant number ofgrains or GBs (more than 200 in this particularexample). This would not be possible by using otherdiffraction methods.T

ab

le18

Dete

rmin

ati

on

of

ori

en

tati

on

rela

tio

nsh

ips

usin

gE

BS

Db

etw

een

au

ste

nit

ean

dacic

ula

ro

rb

ain

itic

ferr

ite

inste

els

Mate

rial

Ch

em

ical

co

mp

osit

ion

(main

ele

men

ts)

Heat

treatm

en

tM

icro

str

uctu

reO

RR

ef.

Cast

iron

3. 2

C–1C

u–2S

i–0. 5

5M

nS

and

casting

Ausfe

rrite

(az

c)C

lose

toK

SFerr

yand

Xu,

2004

Cast

iron

3. 6

C–0. 3

Cu–2. 5

Si–

0. 6

Mn–0. 1

5M

oA

uste

mp

ering

Ausfe

rrite

(az

c)C

lose

toK

SM

arr

ow

and

Cetinel,

2000

Cast

iron

3. 6

C–0. 3

Cu–2. 5

Si–

0. 6

Mn–0. 1

5M

oA

uste

mp

ering

Ausfe

rrite

(az

c),

5u

from

KS

Marr

ow

et

al.,

2001

TR

IPste

el

0. 6

C–1. 5

Si–

1. 5

Mn

Ste

pq

uenchin

gB

ain

itez

reta

ined

auste

nite

Locally

rath

er

clo

se

toK

S(1u

from

neig

hb

ouring

pix

els

)R

eg

leet

al.,

2004;

Cab

us

et

al.,

2004a;

Cab

us,

2005

TR

IPste

el

Low

allo

y,

Si–

bearing

ste

el

Hot

rolli

ng

zste

pq

uenchin

g(4

00uC

)B

ain

itez

reta

ined

auste

nite

Not

exactly

KS

(bain

ite

isd

efo

rmed

)G

od

et

et

al.,

2001

TR

IPste

el

0. 4

C–1. 5

Si–

1. 5

Mn

Ste

pq

uenchin

g(4

00uC

)B

ain

itez

15–20%

reta

ined

auste

nite

Not

exactly

KS

God

et

et

al.,

2004

TR

IPste

el

0. 3

9C

–1. 3

7S

i–1. 4

5M

nS

tep

quenchin

g(4

00uC

)B

ain

itez

reta

ined

auste

nite

Clo

se

toK

Sor

NW

Verlin

den

et

al.,

2001

TR

IPste

el

0. 2

C–0. 5

Si–

1. 4

Mn–0. 7

Al

Cold

rolli

ng

zin

terc

riticalte

mp

ering

zste

pq

uenchin

gV

ery

clo

se

toK

S(b

oth

with

TE

Mand

EB

SD

)Z

aeff

ere

ret

al.,

2004

HS

LA

ste

el

0. 0

7C

–0. 3

Si–

1. 5

Mn–C

r–M

o–N

i–N

bTherm

ally

sim

ula

ted

coars

eg

rain

ed

HA

ZU

pp

er

bain

ite

Clo

ser

toN

Wth

an

toK

SG

ourg

ues

et

al.,

2000

Low

carb

on

ste

el

0. 0

7C

–0. 2

Si–

1. 6

Mn–C

r–N

i–N

b–Ti–

V–B

Weld

meta

ld

ep

osit

Acic

ula

rfe

rrite

Clo

ser

toN

Wth

an

toK

SG

ourg

ues

et

al.,

2000

Low

allo

yste

el

0. 2

C–0. 2

Si–

1. 4

Mn–C

r–M

o–N

i(A

533)

Contr

olle

dhot

rolli

ng

Up

per

bain

ite

Clo

ser

toN

Wth

an

toK

SG

ourg

ues

et

al.,

2000

HS

LA

ste

el

0. 0

7C

–0. 3

Si–

1. 5

Mn–C

r–M

o–N

i–N

bTherm

ally

sim

ula

ted

coars

eg

rain

ed

HA

ZU

pp

er

bain

ite

Not

necessarily

KS

or

NW

,als

oclo

se

tooth

er

less

cla

ssic

alO

Rs

Lam

bert

-Perlad

eet

al.,

2004a

Low

carb

on

ste

el

0. 0

9C

–0. 5

Si–

1. 9

Mn–B

–O

Weld

meta

ld

ep

osit

Acic

ula

rfe

rrite

Near

KS

(poin

tanaly

sis

)K

luken

et

al.,

1991

Low

carb

on

ste

els

0. 0

6to

0. 1

C–M

n–S

i–C

u–N

i–C

rS

tep

quenchin

gB

ain

ite

No

MR

betw

een

20

and

47u,

consis

tent

with

KS

or

NW

Dıa

z-F

uente

set

al.,

2003

Low

carb

on

ste

el

0. 2

C–2M

n–0. 3

V–N

–S

Ste

pq

uenchin

gA

cic

ula

rfe

rrite

MR

s,

5u

from

KS

/KS

variants

Miy

am

oto

et

al.,

2003



Similar studies have been carried out for discontin-uous (cellular) precipitation in Mg–10 wt-%Al (Mg zMg17Al12) (Bradai et al., 2002) and nickel base singlecrystal superalloy (c z c9 z topologically close packedphases) (Lavigne et al., 2004). Here, LABs (Lavigneet al., 2004) or GBs with low index misorientation axes(Bradai et al., 2002) were less sensitive to the involvedreaction. In Cu–4 wt-%Ti, Mangan and Shiflet (1997)combined EBSD with careful serial sectioning to showcomplex interactions between the moving boundary of(fcc azorthorhombic Cu4Ti) colonies and the twinboundaries of the starting microstructure.

Heterogeneous nucleation in matrix phase transformations

Nucleation of ‘major’ phases is of course also stronglyinfluenced by local crystallography. In white cast irons,phase transformation from eutectic cementite (Fe3C)into graphite involved nucleation of graphite at curvedferrite/Fe3C interfaces; however, no nucleation occurredat straight interfaces parallel to the [001] direction ofFe3C and to the normal direction of the product (Songet al., 2002).

Most reported EBSD studies on this topic focused onsteels. In situ light optical microscopy observations offerrite to austenite phase transformation of a coarsegrained Fe–4.8 at.-%Cr–0.008C alloy coated with SiO2

showed preferential nucleation of austenite at triplejunctions involving three random ferrite HABs; thehigher the number of ‘special’ boundaries connected tothe triple junction, the lower the probability foraustenite to be found there (Watanabe et al., 2005b).However, the use of coarse grained material (to get onlyone grain in thickness) does not prevent from freesurface effects and from rather low statistics of results.In a low carbon steel wrapped into an austenitic stainlesssteel foil and heat treated in molten salt baths, nopreferential nucleation of austenite was found near‘special’ grain boundaries (Bruckner et al., 2001).Nucleation of primary ferrite at ferrite/austenite phaseboundaries of a 0.15C–1.4Mn–0.25Si–0.006B steel at700uC was strongly favoured by an applied stress, due toa less strictly observed OR and thus to an increase in thephase boundary energy; this effect seemed stronger thanat austenite GBs (Suh et al., 2000).

Nucleation of intragranular ferrite at secondaryphases or inclusion particles has been widely studiedby TEM (although the probability to find a nucleationsite in a TEM thin foil is low) and by EBSD over a largevariety of inclusions (van der Eijk et al., 1999). Theeffect of deformation of the austenite phase on nuclea-tion of ferrite has also been studied with EBSD,especially in ultrafine grained ferrite formed at deforma-tion bands and cell boundaries of hot rolled austenite(Hurley et al., 2000, Hurley and Hodgson 2001). Incontrast, austenite LABs did not influence markedly itstransformation into martensite after accumulated rollbonding (Kitahara et al., 2004). Nucleation of acicularferrite at TiN particles may occur with an OR betweenevery individual ferrite phase and the TiN particle (Jinet al., 2003). In low carbon steels, the competitionbetween acicular ferrite and bainite at the austenite/ferrite phase boundaries depends on both the chemicalcomposition and the austenite grain size (Dıaz-Fuenteset al., 2003).

The formation of Widmanstatten ferrite sideplates atprimary ferrite crystals already formed at former

austenite GBs was shown thanks to EBSD and serialsectioning to occur not by interfacial instability but bynucleation and growth of individual plates. A distinctGB (and a 5–10u low angle MR) was found with EBSDbetween Widmanstatten sideplates and primary ferritefrom which they were growing (Spanos and Hall, 1996;Phelan and Dippenaar, 2004; Phelan et al., 2005).

As nucleation events are distributed everywherewithin the material, 3D observations are often necessary;TEM seems best suited to fine scale and finely dispersednucleation events; for scarcely distributed nucleationsites, 3D investigations involving EBSD can be bettersuited due to both statistical relevance of data and thepossibility to perform serial sectioning.

Evidence of variant selectionGiven an OR between parent and product phases, thereare a fixed number of crystal orientations of the productphase that can form from a given crystal of the parentphase. These are called ‘variants’. Not all possiblevariants are generally observed in metallographicsections 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 illustratedin Fig. 9. Variant selection is readily studied at the scaleof the former parent grains by TEM or EBSD and, froma statistical point of view, using the average texture ofthe material (obtained by, e.g. neutron diffraction, XRDor EBSD). Both approaches have successfully usedEBSD in a number of materials. At the scale ofindividual parent grains, the microtexture may readily

(a)

(b)

(c)

a no variant selection; b local, but no average variantselection; c local and average variant selection

9 Two-dimensional view of variant selection (one variant

per shape)



be investigated; at the global scale, such as with XRD,the experimental ODF is compared to that calculatedfrom the orientation of the parent phase by assuming anOR to be strictly obeyed (with or without variantselection criteria).

Martensitic transformations in shape memory and Fe–Nialloys

In Ni–Ti shape memory alloys (SMAs) fabricated byaccumulative roll bonding of Ni and Ti foils, NiTi doesnot directly form from Ni and Ti phases and intermediatecompounds such as Ni3Ti and Ti2Ni are involved.However, a KS OR is observed between Ni and NiTiand a Burgers OR is observed between Ti and NiTi,suggesting that intermediate phase transformationsinvolve variant selection (Inoue et al., 2003). Localvariant selection was shown in Fe–27.5Ni–17.7Co–3.8Tiquenched at –196uC (Bruckner et al., 1999). Variantselection was also suggested by average texture calcula-tions in undeformed (but not in deformed) Fe–28Ni–0.02C (wt-%) (Kestens et al., 2003) (with the Bain OR,however, which is not exactly relevant in that case). Thedetailed microtexture of fork and spear like martensite inCu–7.3Al–8.5Mn (wt-%) (among 24 possible variants of18R1 martensite) showed two groups of two variants ofcommon spatial but different crystal orientations (Wanget al., 2002). Self-accommodating variants, twin relatedby {121}2H and {101}2H planes respectively were found inspear like and fork like martensite of Cu–12.55Al–4.84Ni(wt-%) after transformation of DO3 austenite (Chen et al.,2000). At the scale of parent grains, not all possible variantsare generally found by EBSD in e.g. Fe–29.6 wt-%Ni(Kitahara et al., 2005) and Co thin films (Hesemannet al., 2001), where variants such that {0001}hcp//{111}fcc

at 20u from the surface of the film are favoured.The formation of lenticular martensite in Fe–(31–

32) at.-%Ni bicrystals was extensively investigated usingEBSD, in particular for symmetric ,211. tilt (Fig. 10)and 90u {211} twist boundaries. In single crystals ofsimilar chemical composition, all 12 possible variantswere observed, even when transformation occurredunder applied stress (Ueda et al., 2001b). For bicrystalshaving a tilt boundary and whatever the applied stress

and misorientation between GB and tensile axis, variantselection favoured martensite crystals having a habitplane parallel to the GB plane and enhancing accom-modation of the transformation strain across the GB(Ueda et al., 2001b). This stands generally for other tiltangles under no applied stress (Ueda et al., 2003a) and inprestrained 90u,211. bicrystals (Ueda et al., 2001a).For 90u {211} bicrystals, no strain accommodation waspossible through variant selection across the GB, so thatthe martensite start temperature was lower. However,variant selection was also found (Ueda et al., 2001b)together with local plastic deformation on the other sideof the GB (Ueda et al., 2001a). As residual stresses(resulting from only partial accommodation of trans-formation strains) were higher in the twist than in the tiltbicrystal, a better memory of the starting austenitecrystal orientation was observed after reverse transfor-mation of the twist bicrystal while many LABs appearedin the new austenite phase of the tilt bicrystal (Uedaet al., 2003b and 2004). Owing to the large size of bicry-stals together with the small size of individual marten-site variants, multiscale EBSD study was a key tool toinvestigate phase transformations in such materials.

Non-ferrous metal alloys

Some examples of variant selection evidenced (or notevidenced) by EBSD in titanium and zirconium alloysare given in Table 19 at various scales.

In hot rolled b (bcc) heat treated Cu–40Zn alloys,which then partially transformed into fcc a duringcooling, coarse a grains with strong internal misorienta-tions were found. The a phase formed from cold rolledand annealed (but not recrystallised) b showed only oneBain zone (i.e. near KS or NW ORs clustered aroundthe same 45u,100.b Bain OR). This suggests strongvariant selection that, surprisingly, decreased with thetransformation temperature (Yasuda et al., 1999). Suchvariant selection was also found for (azb) heat treatedCu–42 wt-%Zn, at least for a grains that were clusteredinto bands (Sakata et al., 2000).

In Al–36Mo–17Ti (at.-%), thermal cycling across theb (A2) into Al3Ti (DO22)zMo3Al (A15) eutectoid phasetransformation temperature tended to maintain theinitial orientation of the b phase, showing a memoryeffect on texture and thus involving variant selectionin both eutectoid and reverse phase transformations(Miura et al., 2004 and 2005a). In near-c Ti–46.8Al–1.7Cr–1.8Nb (at.-%), orientation of bothWidmanstatten and lamellar c crystals strongly dependson twinning in the parent a phase, leading to particularMRs between neighbouring Widmanstatten and lamel-lar c phases (Dey et al., 2005).

Steels and ferrous alloys

Variant selection in ferrite (a) to austenite (c) phasetransformation has only been scarcely studied in lowcarbon steels, as the c phase cannot be retained at roomtemperature. In a cold rolled 0.065C–1Mn steel, Parket al. (2002) found variant selection from average texturemeasurements. By measuring average textures of inter-stitial free steels before and after complete a to c thenback 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 bearingsteels, possibly due to some retained ferrite in thevicinity of TiN particles. However, such studies are very

10 Variant selection evidenced with EBSD in Fe–

32 at.-%Ni bicrystal containing 90u ,211. tilt bound-

ary and transformed under tension at 45u from tilt

axis. Only variants V29 and V3 are found in each aus-

tenite grain near GB. After Ueda et al. (2001b)



Tab

le19

Evid

en

ce

of

vari

an

tsele

cti

on

aid

ed

by

EB

SD

inh

cp

meta

lsan

dm

eta

lall

oys

(ite

ms

init

ali

cs

mo

resp

ecifi

call

yad

dre

ss

vari

an

tsele

cti

on

at

pare

nt

gra

inb

ou

nd

ari

es)

Mate

rial

Pare

nt

ph

ase

Pro

du

ct

ph

ase

Scale

of

EB

SD

investi

gati

on

Resu

lts

Ref.

Cold

rolle

dTi

ba

Avera

ge

and

localte

xtu

reIn

ad

ditio

nto

str

eng

thenin

gof

textu

reof

the

bp

hase,

variants

‘alm

ost

com

mon’to

ad

jacent

bg

rain

sare

sele

cte

dG

ey

and

Hum

bert

,2002

Ti

ba9

(lath

mart

ensite)

One

pare

nt

bg

rain

Fro

mM

Rs

betw

een

variants

,th

ere

isvariant

sele

ction

Wang

et

al.,

2003

Ti

ab

(pla

tes

zallo

trio

morp

hs)

Pare

nt

ag

rain

sV

ariant

sele

ction

pro

bab

lym

ain

lyd

uring

gro

wth

of

the

bp

hase

Sew

ard

et

al.,

2004

Cold

rolle

dz

bheat

treate

dIM

I834

Tiallo

yb

Prim

ary

and

second

ary

aM

acro

zones

(larg

eclu

ste

rsof

bg

rain

sof

sim

ilar

cry

sta

lorienta

tion)

No

part

icula

rvariant

sele

ction

for

prim

ary

a;

str

ong

variant

sele

ction

(only

one

textu

recom

ponent)

for

second

ary

aG

erm

ain

et

al.,

2005a

and

2005b

Ti–

6A

l–4V

ba

pla

tes

(diffu

sio

nal

mechanis

m)

Avera

ge

textu

reand

ind

ivid

ual

pare

nt

gra

ins

No

variant

sele

ction

inavera

ge;

at

least

thre

efa

mili

es

of

ap

late

sp

er

bg

rain

Hum

bert

et

al.,

1994

Up

to30%

hot

rolle

dTi–

6A

l–4V

ba

(diffu

sio

nal)

Avera

ge

textu

reand

ind

ivid

ual

pare

nt

gra

ins

No

variant

sele

ction

inavera

ge;

all

12

variants

found

ineach

pare

nt

bg

rain

Gey

et

al.,

1996

Hot

rolle

dz

heat–

treate

dTi–

6A

l–4V

ba

(diffu

sio

nal)

Avera

ge

textu

reand

alo

ng

ind

ivid

ualG

Bs

Evid

ence

of

variant

sele

ction

at

GB

stw

oaltern

ating

variants

of

prim

ary

a;

LA

Bb

etw

een

Wid

mansta

tten

and

prim

ary

aif

no

sp

ecia

lO

Rb

etw

een

bg

rain

s;

,0001

.a//

com

mon

,110

.b

ifexis

ting

Sta

nfo

rdand

Bate

,2004

Ti–

6A

l–2S

n–4Z

r–6M

ob

Wid

mansta

tten

and

GBa

Pare

nt

bg

rain

sW

idm

ansta

tten

variants

as

clo

se

as

possib

leto

prim

ary

aw

hile

ob

eyin

gth

eB

urg

ers

OR

with

the

pare

ntb

gra

ins

into

whic

hth

ey

are

gro

win

g.

Ifnot

possib

le,

para

llelclo

se

packed

directions

as

clo

se

as

possib

leto

the

pare

nt

GB

Bhattachary

ya

et

al.,

2003

Ti–

8A

l–xV

(laser

dep

osited

)b

GB

aA

long

one

hug

eG

Bover

the

whole

com

positio

nra

ng

eTw

oaltern

ating

variants

with

{0001} a

//to

the

sam

e{1

10} b

,m

isoriente

d10u

from

anoth

er;

OR

str

ictly

ob

eyed

on

one

sid

e,

as

clo

sely

as

possib

lew

ith

the

oth

er

pare

nt

gra

in

Banerjee

et

al.,

2004

Zircalo

y–4

ba

(diffu

sio

nal)

Avera

ge

textu

reThere

isvariant

sele

ction,

esp

ecia

llyw

hen

no

str

ess

isap

plie

dG

ey

et

al.,

2002



difficult and the majority of results concern transforma-tions from austenite to ferrite (or martensite) in steels.

Diffusional formation of primary ferrite

Globular ferrite growing from residual d ferrite of stripcast 0.1C–0.17Si–0.6Mn–P steels obviously shows astrong texture (with only internal LABs) within align-ments (Umezawa et al., 2003). If no d ferrite is retained(i.e. for the majority of ferritic steels), variant selectiondepends on the deformation state of parent austenite. Inweakly prestrained austenite of a 0.3Si–1.5Mn steel,coarse primary ferrite formed from coalescence of agrains of close crystal orientations (i.e. from the samevariant). For strains higher than y40%, neighbouring agrains formed as misoriented variants (Torizuka et al.,2000). In a 0.002C–1.66Mn–Si–Mo–Ni–Al steel vacuumcast into 2 mm thick sheets and then hot rolled, a strongtexture was found in individual former c grains, stronglydepending on the c crystal orientation, but wellpredicted by using all 24 KS variants, so that no variantselection could be evidenced (Hurley et al., 1999).

The diffusional formation of primary ferrite may alsobe significantly driven by free surface energy, such as incoarse grained ferritic steels obtained by intercriticalannealing (i.e. in the azc temperature range) in adecarburising atmosphere. Carbon depletion startingfrom free surfaces induced transformation of the twophase alloy into a fully ferritic microstructure.Abnormal grain growth then occurred due to the lowerfree surface energy of {100} grains and to some memoryof the initial texture and grain size effect, so that a coarsegrained microstructure with a desirable {100} texturewas finally obtained (Tomida, 2003; Tomida et al., 2003;Dzubinsky et al., 2004).

Transformation of austenite into Widmanstatten ferrite,bainite and martensite

Whatever the transformation mechanism, variant selec-tion in bainite and Widmanstatten ferrite has alreadybeen widely investigated with EBSD (Table 20). Owingto the coarse size of bainite packets with respect to theparent c grain size, a relatively low number of packetsare generally observed within a given c grain by 2Dsectioning. This leads to significant sampling effects. Thecomplex, non-convex and non-equiaxed shape of bainitepackets may also lead, even in the absence of variantselection, to an inhomogeneity in variant distributiondue to the morphological orientation of packets withrespect to the sample surface plane (Fig. 11). This purelygeometric phenomenon has recently been called ‘pseudovariant selection’ (Cabus, 2005). By assuming a givenshape and habit plane of bainite packets, one canattempt to process microtexture data to take pseudovariant selection into account in each parent austenitegrain (Cabus, 2005). Nevertheless, the vast majority ofliterature data does not take either these considerationsor even the (sometimes low) number of analysed c grainsinto account.

Variant selection is generally investigated at the scaleof the former c grain (i.e. from the resulting local textureor number of bainite variants). In some instances,however, such as in fatigue and cleavage crackpropagation, the relevant parameter is the misorienta-tion between neighbouring packets only. Whatever thebainitic or lath martensite microstructure, no misor-ientation angle of y20u was found between neighbour

packets, although it could possibly exist according tonear KS ORs (Fig. 12). Thus, as evidenced by localhistograms of misorientation angles, there are ‘forbid-den’ pairs of neighbours and thus ‘local’ variantselection, even if it may have no consequence on theaverage texture (Gourgues et al., 2000; Gourgues, 2003).

In hcp e martensite (Godet et al., 2005) showed onlytwo over the four possible {111}c parallel to {0001}e in a19.6Mn–3.1Si–2.9Al steel, suggesting that there couldalso be variant selection in this case. In AISI 304austenitic stainless steel tensile deformed at –60uC, emartensite appeared in parent grains as families ofparallel bands (one variant per family). Within thesebands, e martensite then probably partially transformedinto bcc a9 martensite having one {110} plane parallel tothe (0001)e plane. Six variants out of 24 were thusselected for each band family. Moreover, there wasfurther local variant selection among these six variants(Gey et al., 2005).

Variant selection at parent grain boundaries

Intergranular nucleation of a new matrix phase involvesat least three contributions to the change in free energy:

(i) GB interfacial energy

(ii) chemical variation in free energy due to phasetransformation

(iii) interface and strain energy of coupled new phaseand individual matrix grains.

(i) and (iii) are variant dependent, so that new variantsmay tend to obey a given OR with both parent grains.This is best studied with EBSD, especially if the parentgrain size is coarse. Examples from hexagonal metalsand metal alloys are given in italics in Table 19.

In Cu–40Zn with {001},110. textured bcc b, fcc avariants either of close crystal orientations or in twinMR formed on either side of the b GBs. Coarse acolonies nucleated on either side of the same GBgenerally 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 theaverage texture (Stanford and Bate, 2005). In Ni–43Crheat treated in the fcc c phase range and then cooleddown slightly below the solvus of the bcc a phase, whenexisting, the only variant selected was that having a KSOR with both c grains; otherwise, selected variantsobeyed the KS OR with one c grain, and had their closepacked plane of the OR as close as possible to the c GBplane (Adachi and Tsuzaki, 2005; Adachi et al., 2005).

In cold rolled low alloy (0.065C–0.05Si–0.99Mn) steelannealed in the c temperature range, EBSD resultssuggested that a memory of the initial a crystalorientation still existed, with selection of a variants inKS OR with the neighbouring c grains (frequently in KSOR themselves with the same initial a crystal) (Brucknerand Gottstein, 2001). Such variant selection was alsoobserved in a 0.15C–0.3Si–1.42Mn steel after hot torsion(Novillo et al., 2004). In austenitic 0.0015C–22Cr–(8–9)Ni stainless steels, gas tungsten arc welding followedby liquid tin quenching showed that at least at thebeginning of bcc d to fcc c phase transformation, cvariants at d GBs were more frequently in KS ORwith both neighbouring d grains than with one d grainonly (Inoue et al., 1998). The same result was foundin annealed and quenched duplex stainless steels(Gourgues et al., 2004; Monlevade et al., 2006) (Fig. 13).



Tab

le20

Evid

en

ce

of

vari

an

tsele

cti

on

aid

ed

by

EB

SD

info

rmati

on

of

bain

itic

or

Wid

man

sta

tten

ferr

ite*

Allo

yco

mp

osit

ion

Fin

al

mic

rostr

uctu

reA

naly

sis

tech

niq

ue

Resu

lts

Vari

an

tsele

cti

on

Ref.

3. 2

C–1C

u–0. 5

5M

n–2S

iA

scast

gre

yiron:

bain

itez

reta

ined

cN

um

ber

of

variants

per

cg

rain

Severa

lvariants

per

cg

rain

Not

enoug

hd

ata

toconclu

de

Ferr

yand

Xu,

2004

Ni–

Fe-r

ich

mete

oritic

min

era

lW

idm

ansta

tten

aO

ne

hug

ec

gra

inanaly

sed

All

12

near

NW

variants

were

found

No

He

et

al.,

2006

Low

allo

y,

Sib

earing

(TR

IP)

Bain

itez

reta

ined

cIn

div

idualorienta

tion

of

variants

Variants

sele

cte

daccord

ing

toactive

slip

syste

ms

Yes

God

et

et

al.,

2001

0. 3

9C

–1. 3

7S

i–1. 4

5M

n(T

RIP

)Lath

bain

itez

reta

ined

cN

um

ber

of

morp

holo

gic

alvariants

;avera

ge

textu

rew

ithin

pare

nt

cg

rain

Low

er

num

ber

of

morp

holo

gic

alvariants

for

ste

pq

uenchin

gfr

om

defo

rmed

c;m

axim

um

inte

nsity

of

textu

revaries

from

one

cg

rain

toanoth

er

Verlin

den

et

al.,

2001

0. 1

9C

–1. 4

6S

i–1. 5

7M

nand

0. 3

1C

–0. 3

4S

i–1. 5

7M

n–1. 2

3A

l(T

RIP

)B

ain

itez

reta

ined

cA

vera

ge

textu

reof

ccalc

ula

ted

from

that

of

bain

ite

{001},

100

.c

weaker

(resp

ectively

str

ong

er)

than

pre

dic

ted

for

Al–

Si(r

esp

ectively

Alfr

ee)

ste

el

Possib

lyyes

De

Meyer

et

al.,

2001

0. 6

C–1. 5

Si–

1. 5

Mn

(TR

IP)

Bain

ite

z.

20%

czm

art

ensite

Num

ber

of

variants

per

cg

rain

(over

afe

wc

gra

ins)

Less

than

the

24

possib

leK

Svariants

;clo

se

packed

pla

nes

of

KS

OR

are

para

llelto

only

one

or

two

{111} c

pla

nes;

possib

lesam

plin

geff

ects

?

Possib

lyyes

Reg

leet

al.,

2004;

Cab

us

et

al.,

2004a

0. 7

9C

–1. 5

6S

i–1. 9

8M

n–1. 0

1A

l–0. 2

4M

o–1. 0

1C

r–1. 5

1C

o(T

RIP

)C

arb

ide

free

bain

ite

Tra

ce

of

bain

ite

packets

,m

orp

holo

gy

of

cry

sta

llog

rap

hic

packets

Tra

ces

are

para

llelto

maxim

alshear

pla

nes;

packets

are

bett

er

alig

ned

iftr

ansfo

rmed

und

er

com

pre

ssio

n

Yes

Hase

et

al.,

2004

0. 6

C–1. 5

Si–

1. 5

Mn

(TR

IP)

Bain

itez

.20%

czm

art

ensite

Avera

ge

aand

cte

xtu

res

takin

gp

seud

ovariant

sele

ction

into

account

Clo

se

packed

pla

nes

of

near

KS

OR

are

para

llelto

one

or

two

dom

inating

{111} c

pla

nes.

Yes

Cab

us,

2005

0. 4

C–1. 5

Si–

1. 5

Mn

(TR

IP)

Bain

itez

15–20%

cfr

om

cd

efo

rmed

by

0. 2

or

0. 8

Num

ber

of

KS

variants

per

pare

nt

cg

rain

All

24

variants

are

found

for

e50. 2

,not

all

for

e50. 8

;in

tern

alm

isorienta

tion

incre

ases

with

incre

asin

gd

efo

rmation

of

auste

nite

Yes

God

et

et

al.,

2004

0. 2

2C

–1. 6

Si–

1. 5

Mn–0. 0

45N

b(T

RIP

)B

ain

itez

reta

ined

cN

Wvariants

v.

active

part

iald

islo

cation

slip

syste

ms

Ina

giv

en

cg

rain

,b

oth

variants

associa

ted

toactive

slip

syste

mand

op

posite

syste

mare

found

Possib

lyyes

Jonas

et

al.,

2005

0. 0

4C

–0. 2

Si–

1. 5

Mn–N

i–N

b(H

SLA

)E

long

ate

db

ain

ite

alo

ng

the

hot

rolli

ng

direction

MR

sb

etw

een

bain

ite

‘colo

nie

s’

Low

(,15u)

mis

orienta

tions:

one

colo

ny

per

cg

rain

.P

ossib

lyone

colo

ny

51

to2

clo

sely

oriente

dK

Svariants

Possib

lyyes

Mats

uoka

et

al.,

1999

0. 0

7C

–0. 3

2S

i–1. 5

Mn–C

r–M

o–N

b–V

(HS

LA

)Lath

bain

ite

from

coars

eg

rain

ed

cM

Rs

betw

een

packets

com

pare

dto

KS

or

NW

rela

ted

MR

sC

lose

packed

pla

nes

of

OR

para

llelto

diffe

rent

{111} c

pla

nes

inneig

hb

ouring

packets

;th

ere

are

locally

forb

idd

en

MR

s

Locally

yes

Gourg

ues

et

al.,

2000;

Lam

bert

-Perlad

eet

al.,

2004a

0. 2

C–0. 2

5S

i–1. 3

8M

n–C

r–M

o–N

i–A

l–N

b–Ti–

V(A

533)

Tem

pere

db

ain

ite

MR

sb

etw

een

packets

com

pare

dto

KS

or

NW

rela

ted

MR

sU

pp

er

bain

ite:

clo

se

packed

pla

nes

of

OR

para

llel

tod

iffe

rent

{111} c

pla

nes

inneig

hb

ouring

packets

;lo

wer

bain

ite:

clo

se

tom

art

ensite

mic

rote

xtu

re(s

ee

section

on

mic

rote

xtu

res)

Locally

yes

Gourg

ues

et

al.,

2000

0. 0

5C

–0. 5

Si–

1. 6

Mn–V

(HS

LA

)B

ain

itez

reta

ined

cA

vera

ge

textu

re,

NW

OR

sE

xp

erim

enta

lte

xtu

renot

the

sam

eas

calc

ula

ted

one

Yes

Hum

bert

et

al.,

2002b

0. 1

5C

–2. 2

5C

r–1M

o,

0. 0

5C

–9N

i,0. 0

7C

–0. 4

Si–

1. 4

Mn–V

Up

per

bain

ite

(sim

ula

ted

coars

eg

rain

ed

HA

Zs)

MR

sb

etw

een

packets

,siz

eof

cle

avag

efa

cets

Up

per

bain

ite:

many

inte

rnalLA

Bs;

low

er

bain

ite:

many

HA

Bs;

there

are

locally

forb

idd

en

MR

s.

Cle

avag

efa

cets

of

sam

esiz

eas

cg

rain

s

Locally

yes

Gourg

ues,

2003

0. 2

C–0. 5

Si–

1. 4

Mn–0. 7

Al(T

RIP

)Ferr

itez

bain

ite

shellz

reta

ined

cLocalM

Rs

LA

Bs

betw

een

ferr

ite

and

bain

ite:

bain

ite

orienta

tion

dic

tate

db

yth

at

of

ferr

ite

Yes

Zaeff

ere

ret

al.,

2004

*TR

IP:

transfo

rmation

ind

uced

pla

sticity

aid

ed

ste

els

;H

SLA

:hig

hstr

eng

thlo

wallo

y.



In summary, EBSD investigations of various metalalloy systems showed that at GBs of the parent phase,variant selection may occur, favouring those variantseither obeying as strictly as possible the OR with bothparent grains, or having a special OR with the GB plane.

Examples of practical applications of variantselectionGrain boundary engineering (GBE) through phasetransformations

Grain boundary engineering is a method by which,through well controlled metallurgical and thermome-chanical processing, ‘special’ GBs are strongly favouredleading to improved product properties (see e.g.Watanabe, 1984). This has been made possible byextensive EBSD characterisation (Gourgues, 2002).The GBE is generally achieved through series of hotworking and annealing treatments, making use of grainboundary motion, recrystallisation and annealing twin-ning. However, variant selection in phase transforma-tions could be another way to produce ‘special’ GBs

between grains of product phases through controlledphase transformations. The feasibility of GBE wasshown in orthorhombic Ti–Al–Nb alloys by variousmetallurgical routes (Li et al., 2004; Boehlert et al., 2004;Li and Boehlert, 2005a). According to the DO19 a2 orordered B2 parent phases, special MRs were foundbetween orthorhombic O grains. Some MRs betweenvariants were favoured (e.g. 65u,001. or 90u misor-ientations). Other MRs seemed to be locally forbidden(e.g. 30u,001. starting from the a2 phase). Localtexture could thus possibly be tailored through variantselection, even for random average textures.

The GBE might also be achieved by phase transfor-mation under particular conditions, such as in para-magnetic fcc austenite into ferromagnetic (pearlitic) bccferrite in a medium carbon steel (Zhang et al., 2005) andin a 1.0C–Si–Mn–Cr steel (Zhang et al., 2006). A highapplied magnetic induction (12 to 14 T) both increases

11 Sectioning effects inducing pseudo variant selection,

here in case of rod shaped phases: area intercepted by

sectioning plane (in white) is schematically repre-

sented in dark grey; variants having their long axis clo-

sest to sectioning plane have high apparent fraction

12 Histogram of misorientation angles in low carbon

steels, showing apparently ‘forbidden’ pairs of neigh-

bouring 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)

a b

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)



the transformation temperature and strongly decreasesthe amount of LABs between ferrite crystals. Grainboundary engineering on one phase (or more) at a timemight also be achieved in two phase alloys such asin azb9 Cu–40 wt-%Zn alloys (Lee et al., 2003).Conversely, variant selection could possibly be used toavoid certain ‘low strength’ GBs in product phase, suchas 90u MRs between hcp a grains in Ti–6Al–4V (Bieleret al., 2005a); this would be very useful to avoidextensive cavitation of such GBs during upset forging.

Preventing growth and coarsening of ferritic steels

Among the practical issues of phase transformations,structure refinement is achieved by monitoring not onlythe number of nucleated grains, but also the evolution ofmicrotexture during or after phase transformation. Asan example, it is still very difficult to achieve a grain sizelower than y5 mm in ferritic steels, although the highnumber of nucleated grains should lead to a finer ferritegrain size. This is attributed to coarsening, a phenom-enon which is intimately related to the microtexture ofthe initially formed ferrite. Thus, coarsening could belimited by better control of the phase transformationstage, where EBSD is of great help as illustrated inTable 21. The EBSD was used here to investigate, over asignificant number of grains, the deviation from strictOR (and thus decreasing probability that ferrite grainsof the same crystal orientation nucleate close to eachother and eventually coalesce) and to quantitativelydefine the grain size by a threshold criterion involvingthe misorientation angle.

Microtexture: relationships betweenmorphology and local crystallographyOwing to anisotropic interfacial energy or to transfor-mation strains, there can be strong correlation betweencrystal orientation and morphology resulting from solidstate phase transformations (see e.g. habit planes ofmartensite or of certain precipitates). The morphologyof phases may be observed using conventional lightmicroscopy or SEM imaging techniques. However, ifproduct phases come in intricate or complex shapedentities, or if only 2D trace analysis is possible, suchtechniques may give a confusing appearance of productphases. One must then distinguish between what appearsby imaging (here denoted as ‘morphological’ entities)and ‘true crystals’ surrounded by user defined bound-aries (here denoted as ‘crystallographic’ entities). Theright scale is generally that of the SEM/EBSD technique.Several cases have been encountered using EBSD,namely:

(i) several morphological units may belong to thesame crystallographic unit, as in e.g. pearlitecolonies of pearlitic steels (Aernoudt et al.,2005), in misoriented intragranular ferritenucleated at a given inclusion, in acicular ferritein certain low carbon steels (Dıaz-Fuentes et al.,2003), in hcp a phase colonies from bcc b phasesin Ti–6Al–2Sn–4Zr–6Mo (azb) titanium alloy[close Burgers variants in that case (seeBhattacharyya et al., 2003)] and in plates orconglomerates of laths in proeutectoid Fe3C ofa Fe–1.34C–13.1Mn steel (Mangan et al., 1999)

(ii) several crystallographic units may be morpho-logically parallel and become undistinguishablefrom each other in 2D metallographic sections.

This is the case of groups of variants inmartensitic Cu–15.4Al–8.9Mn (at.-%) SMA(Wang et al., 2002). This is also the case for‘blocks’ of lath martensite or even bainite insteels (see below)

(iii) crystallographic units may correspond to a few,very intricate morphological entities, whichappear as ‘knitted’ or ‘woven’ (Fig. 14a). Thisis clearly the case in upper bainite steelmicrostructures (Gourgues et al., 2000;Nohava et al., 2003; Lambert-Perlade et al.,2004a) and also possibly (by closely looking atmicrographs) in hcp a colonies in Ti–5Ta–1.8Nb (Karthikeyan et al., 2005). This micro-texture appears when variants of close crystalorientations, but highly misoriented in mor-phology are selected. Although there are in factmany crystals in such a crystallographic entity,these are separated by LABs only, which do notstrongly affect properties such as resistance tocleavage or fatigue crack propagation. Thisleads to coarser unit crack path and lowertoughness properties (Gourgues et al., 2000;Kim et al., 2000; Dıaz-Fuentes et al., 2003;Nohava et al., 2003; Lambert-Perlade et al.,2004a). As a result, no obvious correlationbetween morphology and crystal orientationcan be found in this case (Gourgues et al., 2000;Nohava et al., 2003)

(iv) intricate, both crystallographically and mor-phologically misoriented units may be found.This is the case of, e.g. Widmanstatten cemen-tite in Fe–0.8C–12.3Mn steel (Mangan et al.,1997) and in acicular ferrite of steel welddeposits (Gourgues et al., 2000) (Fig. 8)

(v) irregular entities, where no particular correla-tion between morphology and crystal orienta-tion can be evidenced, such as primary hcp aformed from bcc b in Ti–8Al–6V (Banerjee et al.,2004) and individual pearlite colonies in fullypearlitic steels (Aernoudt et al., 2005).

In some instances, coupled information on crystal andmorphological orientations may give information aboutthe phase transformation scheme during metal proces-sing, e.g. plate hcp a plates in extruded Zr–2.5Nbpressure tubes; in this example, some pro-monotectoid aphase already formed before extrusion, whereas discreteclusters of a particles having their ,0001. axes parallelto the tube axis appeared during extrusion only(Griffiths et al., 1998, Holt and Zhao, 2006).

The microtexture of lath martensite in steels mayreadily be determined with EBSD, at least from 2Dmaps, 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 ofmartensite microtexture, which was built from EBSDresults only, is based on the KS OR, even though thisOR is not strictly followed in lath martensite. It hasrecently been extended, with some modifications, tobainite in Fe–9Ni steels transformed between 450 and350uC (Furuhara et al., 2006). Laths sharing almost thesame crystal and morphological orientation are gatheredtogether into so called ‘subblocks’. Subblocks having thesame morphological orientation but slightly differentcrystal orientations (same parallel close packed planes



Tab

le21

Ele

ctr

on

backscatt

er

dif

fracti

on

investi

gati

on

of

gro

wth

an

dco

ars

en

ing

of

ferr

itic

ste

els

rela

ted

toau

ste

nit

eto

ferr

ite

ph

ase

tran

sfo

rmati

on

Ste

el

co

mp

osit

ion

Th

erm

om

ech

an

ical

treatm

en

tS

tart

ing

cm

icro

str

uctu

reO

RR

esu

lts

on

co

ars

en

ing

Ref.

0. 1

5C

–0. 2

5S

i–1. 4

Mn–0. 0

06B

1150uC

for

3m

inth

en

10%

unia

xia

lcom

pre

ssio

nstr

ain

at

700uC

,¡

50

sd

well

befo

recoolin

g

Tra

nsfo

rmation

str

ess

free

and

und

er

str

ess

KS

,w

eaker

for

und

er

str

ess

than

for

str

ess

free

Aff

ects

main

lyfe

rrite

nucle

ation

Suh

et

al.,

2000

0. 1

7C

–0. 3

Si–

1. 5

Mn

1200uC

,1

min

then,

com

pre

ssed

at

750uC

zcoolin

gP

lastically

defo

rmed

(20–50%

)N

ot

sp

ecifie

dFerr

ite

gra

ins

more

eq

uia

xed

,H

AB

more

num

ero

us

with

incre

asin

gp

lastic

str

ain

of

c(b

ut

less

than

30

gra

ins

stu

die

din

cert

ain

sam

ple

s)

Torizuka

et

al.,

2000

0. 0

022C

–0. 2

2S

i–1. 6

6M

n–M

o–N

i47%

pla

stic

str

ain

at

850uC

zair

coolin

gH

eavily

defo

rmed

KS

Most

ferr

ite

gra

ins

are

surr

ound

ed

by

HA

Bs

(but

KS

/KS

MR

snot

cle

arly

vis

ible

on

pole

fig

ure

s)

Hurley

et

al.,

1999

0. 1

Cp

lain

carb

on

ste

el

Hot

rolle

dto

str

ain

of

1. 5

¡d

well

for

10

sth

en

wate

rq

uenchin

gN

ot

sp

ecifie

dE

xte

nsiv

ecoale

scence

of

ferr

ite

gra

ins

(LA

Bs

dis

ap

pear)

Kelly

et

al.,

2002

0. 1

7C

–0. 4

5S

i–1. 5

Mn–A

l–V

Hot

tors

ion

Auste

nite

gra

insiz

eof

14

or

84mm

Not

sp

ecifie

dC

oale

scence

of

ferr

ite

during

coolin

g,

contr

olle

db

y2D

(raft

s)

or

3D

meeting

of

ag

rain

s;

EB

SD

giv

es

the

ag

rain

siz

ed

istr

ibution

Bela

diet

al.,

2004

0. 1

5C

–0. 3

Si–

1. 4

2M

n–N

b–V

Hot

tors

ion

(sim

ula

ting

roug

hin

gand

finis

hin

gro

lling

)D

efo

rmed

or

recry

sta

llised

KS

Defo

rmed

c:fe

wLA

Bs

(,15u)

due

tovariant

sele

ction

or

pla

stic

rota

tion;

recry

sta

llised

c:m

any

LA

Bs,

ag

rain

siz

econtr

olle

db

ycoale

scence

favoure

db

ysuch

variant

sele

ction

Novill

oet

al.,

2004

0. 1

5C

–0. 2

5S

i–1. 4

Mn–B

and

0. 3

3C

–2. 1

Si–

1. 5

Mn–B

1200uC

dow

nto

700uC

,10%

com

pre

ssio

nz

coolin

gd

ow

nto

400uC

with

or

without

str

ess

KS

Shift

off

KS

OR

incre

ases

ifth

elo

ad

issusta

ined

,le

ss

coale

scence

of

neig

hb

ouring

ag

rain

s(b

ut

many

OR

s.

15u

from

KS

inth

ep

ap

er)

Kang

et

al.,

2003

0. 0

82C

–0. 3

6S

i–1. 5

Mn–N

b–V

Multip

ass

hot

tors

ion

Heavily

defo

rmed

Not

sp

ecifie

dFerr

ite

gra

ins

meet

firs

tat

cG

Bs;

there

iscoale

scence

behin

dth

etr

ansfo

rmation

front;

EB

SD

giv

es

ferr

ite

fraction

and

siz

ed

istr

ibution

and

mig

rating

inte

rface

are

ap

er

unit

volu

me

Cotr

ina

et

al.,

2004

0. 0

32C

–0. 1

5S

i–0. 7

4M

n–N

b1150uC

for

5m

inth

en

0. 8

com

pre

ssiv

estr

ain

at

845uC

at

various

str

ain

rate

sth

en

wate

rq

uenchin

g

Defo

rmed

Str

ain

ed

at

0. 0

01

s–1:

dynam

icsoft

enin

gvia

str

ain

ind

uced

transfo

rmation,

rand

om

lyoriente

da

gra

ins,

little

coale

scence;

0. 1

s–1:

most

aG

Bs

are

HA

Bs,

finer

final

ag

rain

siz

e

Eg

hb

ali

and

Ab

dalla

h-Z

ad

eh,

2006

0. 1

9C

–1. 5

Si–

1. 5

Mn–A

l–(0

. 003

or

0. 0

1)N

(TR

IP)

Sim

ula

ted

continuous

annealin

gR

ecry

sta

llised

with

more

or

less

num

ero

us

AlN

part

icle

sN

ot

sp

ecifie

dFin

er

ferr

ite

gra

insiz

eand

hig

her

volu

me

fraction

of

reta

ined

c(b

oth

measure

dw

ith

EB

SD

)w

ith

incre

asin

gth

ed

ensity

of

AlN

(measure

dw

ith

TE

M)

Baik

et

al.,

2006

0. 1

5C

–1. 5

Si–

1. 5

Mn

(TR

IP)

950

or

1200uC

then

hot

tors

ion

at

various

tem

pera

ture

sD

efo

rmed

Not

sp

ecifie

dThe

ferr

ite

gra

insiz

e(E

BS

Dm

easure

ments

)d

ep

end

son

the

therm

alm

echanic

altr

eatm

ent;

best

results

ifd

efo

rmed

at

Ar 3

tem

pera

ture

God

et

et

al.,

2006



but different ,111. directions parallel to the ,110.

close packed directions of parent austenite) are in turnclustered into ‘blocks’, so that particular MRs betweenvariants (e.g. 60u,111. twin MR) are found betweenblocks. These blocks are parts of ‘packets’. Within onepacket, all laths are morphologically parallel; however, apacket consists in a variety (up to six) of intricate, highlymisoriented crystals. Martensite blocks are highlyintricate over the whole martensite packets (Gourgueset al., 2000; Nakashima et al., 2001; Dronhofer et al.,2003) although they may look equiaxed in 2D sections

(Nakashima et al., 2001). No particular neighbourselection was found among the six possible blocks in agiven packet (Morito et al., 2003). In martensite formedfrom fine grained austenite, one packet may dominate(at least in 2D sections) (Morito et al., 2005), or less thansix variants may be found in every packet (Kitaharaet al., 2006). Such results confirm those previouslyobtained with TEM, yet with much higher statisticalsignificance.

The determination of crystallographic units needscareful selection of the threshold angle used in EBSD todefine their boundaries. In fatigue and cleavage sen-sitive materials, this is related to crack arrest, e.g. inaustempered ductile cast iron, whose packet boundariesdefined with EBSD may in fact stop fatigue crackpropagation (Marrow et al., 2001). The size of theseunits can be used to compare steel microstructures suchas bainite and martensite (Tsunekage and Tsubakino,2002). Note, however, that cracks only arrest atcontinuous boundaries, while 2D sections also take intoaccount small packets locally embedded in larger ones.Consequently, the true unit crack path may be muchlarger than that measured from 2D EBSD maps [e.g. inlath martensite steel microstructures (Gourgues, 2003)].Local orientation gradients also disturb the definition ofrelevant boundaries. They are common along bainitelaths [e.g. in high carbon steels (Regle et al., 2004) andalong the LAB network within crystallographic units ofpearlitic steels (Aernoudt et al., 2005)].

Resulting average texturesThanks to the development of high speed systems,EBSD is now increasingly used for average texturemeasurements, avoiding the problem of calculating theODF from pole figures (as for XRD or neutrondiffraction). The EBSD is also used to infer the textureof the parent phase from that of low temperatureproduct phase. Here, spatial information provided byEBSD is very useful. Such ‘texture history’ is ofoutstanding value to understand and improve proces-sing routes to get optimal texture of final product at lowcosts.

Retrieving texture of parent phase

To infer the ODF of the parent phase from that of theproduct phase, one can work directly with individualgrains (i.e. by calculating individual orientations ofparent phase grains from resulting variants of theproduct phase). This is here referred to as a ‘local’approach. Another possibility is to work with averageODFs only. Here, EBSD is of particular use if the parentphase is coarse grained (e.g. b grains hundreds ofmicrons in size in heat treated titanium alloys). This willbe referred to as a ‘global’ approach.

The ‘local’ approach was first used in materials wherethe parent grains were still easily reconstructed withimaging techniques. One can then select appropriatevariants of the product phase, determine their crystalorientation by EBSD point or map analysis and thencalculate the orientation of the parent grain by assumingan OR between parent and product phases. This workswell in titanium and zirconium alloys, where the BurgersOR is rather strictly obeyed. Two or three variants aregenerally needed to calculate every grain orientation ofthe parent b phase (Humbert et al., 1995). This methodwas successfully used for Ti–6Al–4V, a number of

a

b

a partially transformed upper bainite with highlymisoriented sets of parallel units sharing close crystalorientation as shown in {001} pole figure: afterLambert-Perlade et al. (2004); b fully transformed lathmartensite, where each block ‘B’ delineated by whitelines always contains same pair of low misoriented var-iants ‘V’: after Morito et al. (2003)

14 Microtexture evidenced using EBSD in product phase



triplets of a plates giving about 100 orientations offormer b grains (Humbert et al., 1994; Stanford andBate, 2004) and by using both primary and colony aphase in equiaxed b grains (Humbert et al., 1996;Moustahfid et al., 1997a) and coarse a colonies of pureTi (Gey and Humbert, 2002). The method requires,however, that GBs of the parent phase be readilyrecognised. It works well even if there is variantselection, but also requires that the OR be strictlyobeyed. This is not the case in steels, where no uniqueOR is generally found; the uncertainty in the ORstrongly decreases the accuracy of results concerning theparent phase: a departure of .5u from the OR preventsfrom finding the right orientation of the parent grain(Decocker et al., 2003). In steels, provided that there areenough ferrite crystals formed within a former austenitegrain, it is possible to determine the orientation of thatformer c grain by an iterative graphical method using{001} pole figures (Gourgues et al., 2000; Cabus et al.,2004b). Such methods are rather tedious, however.

To get statistically reliable data, automated analysiswas also developed, with criteria to determine whetherthe chosen set of variants in fact stems from the sameparent grain. Several ways exist, e.g. one calculation ofdeparture 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 ofneighbouring product variants [e.g. in Ti–6Al–4V alloys(Glavicic et al., 2003b and 2004b)], improved by useof weighting coefficients representing the reliability ofindividual parent grain orientation data (Glavicic et al.,2003a). With such improvements, EBSD maps of theformer parent phase may even be automaticallygenerated in a robust manner and used to investigate,e.g. the solidification or forging texture of the parentphase, even after it completely disappeared duringsubsequent processing steps (e.g. in near-a IMI834(Germain et al., 2004) and in Ti–6Al–4V (Glavicicet al., 2004a) titanium alloys). A method to simplyreconstruct parent grains from EBSD data, based on arigorous algebraic analysis, that also works for fcc to bcctransformations (e.g. in steel martensite with highinternal plastic strain) has been recently developed(Cayron et al., 2006), although not yet able to calculatethe crystal orientation of the reconstructed parentgrains.

The ‘global’ approach requires little (if no) variantselection to avoid local negative values of the ODF(Humbert and Gey, 1999). In addition, the parent phaseshould not exhibit lower crystal symmetry than theproduct phase (Gey et al., 1999). In these conditions,EBSD data may be used to calculate the ODF ofproduct phase, and then (by numerical computations)that of the parent phase. Classical tools used in XRDmay readily be used. More than 2700 data points wereacquired with EBSD in Ti–6Al–4V alloy for this purpose(Humbert and Gey, 1999). A positivity criterion mayalso be introduced to allow calculations even with weakvariant selection [e.g. in metastable b Ti alloys (Geyet al., 1999; Humbert et al., 2001), tentatively inZircaloy–4 alloy (Gey et al., 2002) and in 99.85%Ti(Gey and Humbert, 2002)]. The quality of the resultsstrongly depends on the accuracy of the ODF of theproduct phase and of possible variant selection. Thismethod is much less tedious than non-automated local

approach and much less complicated than automatedlocal approach.

The calculated ODF of the parent phase may be usedin turn to calculate the ODF of the product phase byassuming no variant selection and a given OR (Humbertet al., 1994; Moustahfid et al., 1997a; Gey et al., 2002;Stanford and Bate, 2004; Glavicic et al., 2004b). Toconclude about variant selection from comparisonbetween experimental and calculated ODFs of theproduct phase, one must however bare in mind that:

(i) not all product variants were generally measuredby point analysis

(ii) analysis of 2D sections may bias the results dueto sampling effects or pseudo variant selection

(iii) local variant selection may have no effect on theresulting average texture (Stanford and Bate,2005).

Methods using only some well known texture compo-nents of the parent phase should be avoided unlessresults are experimentally confirmed by, e.g. especiallydesigned heat treatments retaining a significant part ofthe parent phase down to room temperature (Yasudaet al., 1999).

Correlation between average texture and phasetransformations

Little literature is available on average textures deter-mined by EBSD related to solid state phase transforma-tions, except for hexagonal metals and alloys (often dueto the coarse grain size of parent grains, which excludesuse of XRD) and for steels. There is a study on NiTiSMA sheets, where the final {223},110. texture resultsfrom both rolling and variant selection (Inoue et al.,2003). The effect of processing parameters on the finaltexture of product phase have also been investigated inCu–39Zn–2.6Pb (azb) brass, where appropriate extru-sion in the b phase range leads to an optimised balanceof a texture components controlling ductility andmachinability respectively (Mapelli and Venturini,2006). A strong ,110. texture influencing magneticproperties appears when Fe–9Si–13B bulk metallic glasscrystallises under a high magnetic induction (Watanabeet al., 2005a). Cyclic nitriding of 22.5Cr–5.4Ni duplexstainless steels leads to a fully austenitic case withdesirable corrosion resistant {100},001.z{110},112.

texture, while avoiding detrimental columnar grainstructure (Garzon and Tschiptschin, 2004). In diffusionbonded Ti–45Al, Ti depletion near the bond interfacelead to partial transformation of lamellar DO19 a2 phaseinto 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 parallelto the bonding direction (Buque and Appel, 2002). Incommercially pure titanium with initial {2205},1120.

texture, the transformation from hcp a into bcc b waseventually dominated by the growth of huge allotrio-morphic b grains leading to a final {001},110. texture,even if other texture components also initially appeared(Seward et al., 2004). In acicular ferrite of steel WMdeposits, the strong ,100. solidification texture of bccd ferrite was shown by Kluken et al. (1991) in theirpioneering EBSD point analysis study to lead to threemain texture components for fcc c. As near KS ORsprevail for both d–c and c–a phase transformations, apart of the final acicular ferrite (a) microstructurerecovered the initial solidification texture. In a hot



rolled low carbon microalloyed steel, the final texture offerrite was found to be random for a low number ofpasses or a low strain per pass; it turned to typicaltexture of recrystallised ferrite with increasing strain,suggesting strain induced transformation from austeniteto ferrite, followed by deformation and recrystallisationof ferrite (Seo et al., 2000).

The average texture of phases is readily determined byEBSD in multiphase materials, without any need fordeconvolution of average pole figures, e.g. in steelscontaining 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 assesswhether the texture of retained austenite accuratelyrepresents that of all starting austenite grains presentbefore phase transformation, and that EBSD patterns ofall phases are correctly indexed (Field et al., 1996). Thestability of retained austenite during plastic deforma-tion can also be studied for each texture componentseparately (Wasilkowka et al., 2006). Microtexture dataobtained with EBSD could here also be used inadvanced micromechanical models, to get local stressesmore accurately than by classical Taylor and Sachsapproximations.

Texture components and/or pattern quality of theparent phase provide information about its metallurgicalstate before phase transformation. By separating recrys-tallised from deformed austenite based on their wellknown texture components and by distinguishingbetween various bcc products such as primary ferrite,bainite and martensite, it was made possible to assesswhich product phase formed from a given state ofaustenite in a low carbon steel (Mesplont and DeCooman, 2003), in hot rolled dual phase steels(Waterschoot et al., 2002) and in low alloy TRIP aidedsteels (Hutchinson et al., 1998; De Meyer et al., 2001).Primary ferrite tended to form from deformed austenitewhereas bainite formed from deformed and also possiblyfrom recrystallised austenite. Local inhomogeneity inthe parent phase may strongly influence the local textureof the product phase. For instance, locally severelysheared ,110. austenite of a 0.16C–0.61Mn steeltransforms into a ,111. fibre of ferrite (Ping et al.,2005).

When comparing experimentally measured textureswith calculated ones (with assumptions about OR andvariant selection), one can find that there is nosignificant variant selection at that scale [as e.g. inspontaneous reverse transformation of warm deformedsteel (Yokota et al., 2005)]. One may even find little orno resulting texture at all [e.g. in 0.2C–0.2Si–1.3Mn–0.1Ti steel hot rolled and transformed under highmagnetic induction (Maruta and Shimotomai 2002)].Several criteria such as active slip systems or elasticstrain energy (see section on modelling for furtherdetails) have been used to include variant selection intoaverage texture calculations (Bruckner and Gottstein,2001; Humbert et al., 2002b; Moustahfid et al., 1997b;Humbert and Gey, 2003). Agreement between experi-ment and modelling has still to be improved even whentaking pseudo variant selection into account.

Solid state phase transformations: summaryWith increasing development of EBSD systems, in par-ticular for FEG-SEMs, crystallographic investigation of

solid state phase transformations is now extensively usedfrom very early growth of small, scarcely distributednuclei up to growth and coalescence of phases. At thescale of parent grains, quantitative description ofmicrotexture as ‘crystallographic’ entities, now alsoavailable for coarse grained structures, is of greatpractical significance as far as e.g. plasticity or fractureproperties are concerned. The EBSD may even replaceXRD determination of textures, especially for verycoarse grains and when several phases of close crystalstructures coexist in the investigated microstructure.Data of EBSD may be gathered and processed withroutine procedures, so that results little depend on theuser’s interpretation (except for the data ‘cleaning’procedure, which should be clearly reported). Thenumber of EBSD studies of solid state phase transfor-mations in metallic materials is exponentially increasing.With the help of EDS to facilitate phase identification,similar use of EBSD is expected for non-metallicmaterials such as ceramics and natural minerals in thefuture.

Environmentally assisted and surfacereactionsSurfaces play an increasing role in the properties ofmaterials, and in particular of functional materials.Although surface reactions are usually not referred to as‘phase transformations’, they are also considered herefor their strong similarities with phase transformationsin ‘closed’ systems, for their practical implications andbecause to the author’s knowledge, there is no recentreview of the wide use of EBSD in this field in openliterature.

Environmentally assisted surface reactionsMicrostructure and microtexture of oxide layers

Application of EBSD to the structural investigation ofoxide layers requires good spatial resolution. Oxidescales usually have a complex structure and exhibitstrong backscattered electron contrast with the under-lying metal substrate, so that cross-section examinationsrequire careful sample preparation and high perfor-mance EBSD systems with, e.g. automated backgroundacquisition during mapping.

A significant practical application of EBSD in thisfield is the investigation of oxide scales on steel products,whose structure and mechanical properties are of primeimportance for hot rolling, cold rolling and wiredrawing. Both FeO1–x (wustite), Fe3O4 (magnetite) andFe2O3 (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 withEBSD (Burke and Higginson, 2000; Birosca andHigginson, 2003). Interstitial free and low carbon steelsare of primary concern. According to oxidation condi-tions (temperature, atmosphere and cycling conditions)and steel composition, the internal wustite layer may beeither columnar (Burke and Higginson, 2000; Kim andSzpunar, 2001 and 2002; West et al., 2005) or equiaxed(Birosca and Higginson, 2003; Birosca et al., 2004). Astrong ,100. texture may be encountered in wustitewhatever that of the steel substrate (Kim and Szpunar,2001 and 2002; Higginson et al., 2002). A cube–cube ORbetween wustite and magnetite may also prevail,possibly due to the defect structure of wustite (West



et al., 2005), but is not always found (Birosca andHigginson, 2003). Silicon significantly affects the struc-ture and texture of the oxide layers (Kim and Szpunar,2002; Higginson et al., 2002). The oxide texture may becorrelated with porosity and thus mechanical propertiesof oxide layers (Higginson et al., 2002). Scales producedin ‘industrial’ conditions have also been characterisedwith EBSD (Burke and Higginson, 2000). The limits ofsuch analysis are spatial resolution (for very thin scalesto be observed in cross-sections) and statistical reliabilityof data. However, sample preparation is much lesstedious than for TEM cross-sections and usually doesnot need to use advanced techniques such as focused ionbeam (FIB) milling.

Oxide scales have also been studied in cross-sectionsof T40 and Ti–3Al–2.6V titanium alloys, where rutileTiO2 grows faster in Ar rich atmospheres than in N2 richatmospheres and a tendency to (0002)Ti//(100)TiO2 wasobserved (Lenarduzzi et al., 2002). Thermal barriercoatings on nickel base superalloys have also beenstudied with EBSD, for various coating processes. Thealumina scale may, or may not be strongly ,0001.

textured. This controls internal stresses and finalproperties of the thermal barrier coatings (Karadgeet al., 2006). The development of internal stress andstrain fields was investigated with EBSD after oxidationof buried AlGaAs layers; residual stresses and plasticzone geometry were calculated by a finite element

method and compared to the distribution of patternquality (Keller et al., 2004).

Another way to investigate the microtexture of layersis to carry out EBSD analysis of oxidised surfacesdirectly (Fig. 15). This provides data over a wide area,although only at the external surface. Oxidation ofrecrystallised {100},001. (cube) textured nickel lead totwo types of areas:

(i) rough areas with coarse cube or {111} texturedgrains and smaller, possibly faceted ‘intergranu-lar’ grains

(ii) smooth regions having the desired epitaxial cubeor rotated cube texture (Woodcock et al., 2002a,2002b and 2004).

Role of interfaces and free surfaces

As environmentally assisted mechanisms are closelyrelated to diffusion, interfaces and free surfaces stronglyinfluence morphology and growth kinetics of products.As there is already review literature on EBSD studies ofintergranular cracking (Gourgues, 2002), only corrosionis addressed here (Table 22). Most results were obtainedby analysis of the corroded surface and of parallel planesprepared by serial sectioning, sometimes confirmed bycross-section analysis.

The crystal orientation of free surface planes, which isreadily determined with EBSD, also influences the layergrowth kinetics. The relevant parameter is generally the

(a) (b) (c)

a prior EBSD mapping of surface to be oxidised; b exposure to oxidising environment; c characterisation of oxidisedsurface (e.g. with near field or interferometry techniques)

15 Principle of EBSD investigation of oxidation

Table 22 Some EBSD studies of intergranular corrosion

Material Corrosion conditions EBSD results Ref.

Ni–39–40Fe (at.-%) 1000uC for 5 h in O2

atmosphereRandom GBs are sensitive and LABs are not sensitiveto corrosion; the sensitivity of coincident site lattice GBsincreases with oxygen pressure and with departure fromS3, S11, S19 and S27 coincidence

Yamaura et al.,1999 and 2000

Ni–39 at.-%Fe 800–927uC for 18–24 hin air

Sensitivity increases with applied stress; 65% of randomGBs in the sample is enough to oxide over the full width

Yamaura et al.,2003

Low carbon ship steels Seawater environment Not all GBs are corroded, some can only be imaged byEBSD

Katrakova andMucklich, 2000

AA6061 aluminium alloy Intergranular attack inseawater environment

LABs are immune; intergranular attack stops when thereis a loss in connectivity of sensitive HABs

Minoda andYoshida, 2002

Sensitised AISI 316LNstainless steel

Intergranular attack inoxalic acid

LABs and twin boundaries are not sensitive; misorientationangle of sensitive GBs spreads between 30 and 55u; suchboundaries form a continuous network

Kunıkova et al.,2004

Nickel base alloy 718 900uC for 30 h in air Twin boundaries are immune; random GBs are oxidised Yang et al.,2005



angle between the local free surface and low-indexcrystal planes such as {0001} planes in oxidised Grade 1titanium (Konig and Davepon, 2001) and {100} planesin nickel base alloy 690 subjected to plasma assistednitriding (He et al., 2003; Czerwiec et al., 2003).Transmission electron microscopy results are difficultto obtain, whereas EBSD may be conducted before theenvironmentally assisted reaction, without affecting thesample geometry. This has been done for Co51.6Ga48.3

oxidised into Ga2O3, for which the oxide growth kineticson {211} substrate planes was about five times higherthan that on {100} planes (Koops et al., 2002). In nickelbase alloys, atomic force microscopy of corrodedsurfaces (characterised by EBSD before corrosion)allowed quantitative assessment of the dissolution rateas a function of the local surface orientation (Gray et al.,2006; Schuh et al., 2003) and crystallographic investiga-tion of fine scaled surface features of individualcorroded grains (Schuh et al., 2003).

Strong interactions between substrate GBs and freesurfaces have been evidenced thanks to EBSD forwustite reduction into iron in CO/CO2 atmospheres bythe following reactions

CO adð Þz2 h:zV ’’

FezOXO?CO2 adð Þ (1)

FeXFe?Fe0z2 h

:zV ’’

Fe (2)

Reaction (1) leads to local depletion in oxygen and thento nucleation of metallic iron by reaction (2). It alsoleads to surface rearrangement, in particular near GBs(Bahgat et al., 2004a). Surface rearrangement leads tolocal roughness depending on the individual wustitegrain orientation (Bahgat et al., 2004b and 2005). Evenwhen still not visible in the SEM, iron nuclei can beclearly identified by EBSD, since EBSD is sensitive tothe very surface of the specimens (Sasaki et al., 2005b).Iron particles nucleate at surface ledges and their sizeand number strongly depend on the local wustite grainorientation (Bahgat et al., 2004a and 2004b). Thegrowth of iron particles also depends on the localrearranged surface (Sasaki et al., 2005b). Such studiesmake full use of the non-destructive, highly resolved inthickness EBSD technique.

Other results on environmentally assisted reactions

A variety of reactions have been explored with EBSDfor either phase identification or determination of ORand microtexture (Table 23). Another interesting exam-ple is given by in situ reaction synthesis of alumina fromreaction between molten aluminium and surroundingSiO2 quartz tube (Murthy et al., 2005). Al2O3 and Alwere found as fully interconnected colonies with onlytwin boundaries between Al2O3 grains, which should bebeneficial to mechanical properties of the final product ifcomplete synthesis could be obtained.

Thin film depositionEBSD has been used at all stages of process develop-ment for thin film deposition, from feasibility demon-stration to quality control of the final product.

Process feasibility

Electron backscatter diffraction has been used to findout processing conditions yielding the desired phase,such as amorphous versus crystalline silicon on singlecrystal silicon substrate (Gao et al., 2000), crystalline

silicon by metal assisted nucleation in amorphous Si:Hlayer (Chang et al., 2004) and silicide mediated versuslaser assisted crystallisation of silicon on glass (Kimet al., 2004). Quantitative determination of the amountof given phases or polytypes may also be given by EBSDanalysis of deposited films, such as SiC deposition onto4H and 6H SiC substrates (Chaussende et al., 2004;Latu-Romain et al., 2005). Once the right phase isobtained, the next point is to control its crystal qualityand orientation. Crystal quality may be assessed byinspection of GBs or by looking at EBSD patternquality (Kim et al., 2004). Controlling the film texture(e.g. through epitaxial growth combined with variantselection) can be more difficult than controlling thenature of polytype (Chaussende et al., 2004). Exceptwhen deposited films were thick enough [e.g. TiN innickel base superalloys (Jeong et al., 2002b)], only freesurfaces of films were generally investigated, making fulluse of the sensitivity of EBSD to extreme surface layersonly.

Some results given by EBSD analysis about thefeasibility of obtaining suitably oriented films on varioussubstrates are illustrated in Table 24. Extensive mappingwas not always necessary, simple eye observation ofchanges in EBSD patterns by rastering the electronbeam over the entire sample surface being preferred inmany cases.

Orientation relationships between layers and substrate

The OR between substrate and deposited layers has beeninvestigated with EBSD in a variety of cases, mainly bysurface analysis of films (Table 25). In some cases,however, sampling or phase size effects may causemissing of variants that were indeed found by XRD(Cain and Lange, 1994).

Layer structure and resulting texture

Spatial information provided by EBSD has been usedto determine the grain size, variant morphology andclustering and even grain morphology on polished cross-sections. Data are now available for various materialsand deposition processes (Table 26). The resultingtexture is usually analysed with XRD but has also beeninvestigated with EBSD (Table 27).

Information on local roughness has been used to linkthin film morphology to EBSD determined crystal struc-ture and orientation of substrate and film. 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), andsputter deposited Nb, Cu, Co and Permalloy epitaxiallayers (Loloee et al., 2001).

Surface reactions: a summaryEssential features of the EBSD technique in the field ofsurface reactions are as follows:

(i) its sensitivity to extreme surface layers allowssurface characterisation of as deposited extre-mely thin films (down to y20 nm in thickness)

(ii) its non-destructive character is essential to deter-mine ORs between substrate and layers forpolycrystalline substrates

(iii) the possibility is given to scan over large areas ata fine scale.



Tab

le23

Ele

ctr

on

backscatt

er

dif

fracti

on

stu

die

so

fen

vir

on

men

tall

yassis

ted

su

rface

reacti

on

s

Mate

rial

En

vir

on

men

tS

urf

ace

reacti

on

EB

SD

resu

lts

Ref.

Pure

Mg

0. 0

1M

NaC

lz10

–4M

Na

2C

r 2O

7

aq

ueous

solu

tion

Fila

menta

rycorr

osio

nC

orr

osio

nin

itia

tes

only

on

{0001}

oriente

dg

rain

s.

Surf

ace

pro

pag

ation

alo

ng

,1120

.and

,1010

.

directions

Schm

utz

et

al.,

2003

Ti–

8at.

-%M

oN

itrid

ing

environm

ent

Inte

rnalTiN

(hcp

a)

nitrid

ing

Burg

ers

OR

with

matr

ix,

1–3

variants

per

bcc

bg

rain

of

the

sub

str

ate

Guill

ou

et

al.,

2004

Ti–

16

at.

-%M

oN

itrid

ing

environm

ent

Inte

rnalTiN

1–x

(d,

‘fcc’)

nitrid

ing

Near-

KS

OR

,M

Rs

betw

een

part

icle

sare

oft

en

60u,

111

.

Guill

ou

et

al.,

2004

Pure

iron

and

two

low

carb

on

low

allo

yste

els

Borid

ing

with

or

without

carb

urisin

gIn

tern

alfo

rmation

of

tetr

ag

onalFeB

2

part

icle

sS

ing

lecry

sta

lline

Fe

2B

part

icle

sin

borid

ed

Fe;

poly

cry

sta

lline

Fe

2B

part

icle

sin

borid

edz

carb

urised

ste

els

Kulk

aet

al.,

2006

Dup

lex

sta

inle

ss

ste

els

Nitrid

ing

at

1200uC

Surf

ace

dis

solu

tion

of

bcc

dp

hase

Identification

of

the

cp

hase

and

of

dis

ap

peara

nce

of

dp

hase

Pad

ilha

et

al.,

1999

Fe–4

at.

-%N

i–(2

%Tior

3%

Cr)

Nitrid

ing

environm

ent

(thin

sheet)

Part

ially

revers

ible

bulk

transfo

rmation

into

nitrid

es

and

resultin

gg

rain

refinem

ent

Phase

identification

(EB

SD

),g

rain

siz

eand

morp

holo

gy

(TE

M)

Chezan

et

al.,

2004

Fe–18

wt-

%C

rP

lasm

anitrid

ing

Nitrid

ep

recip

itation

and

cellu

lar

pre

cip

itation

Cry

sta

llog

rap

hic

continuity

betw

een

sub

str

ate

gra

ins

and

gra

ins

of

the

nitrid

ed

layer

Miy

am

oto

et

al.,

2006

Fe–28M

n–6S

i–5

wt-

%C

r900uC

for

1h

ina

vacuum

of

10

–2

Pa

Evap

ora

tion

of

Mn

causin

gexte

rnal

fcc

cto

bcc

atr

ansfo

rmation

Phase

identification

of

aFukaiet

al.,

2005

Nib

ase

allo

y22

NaC

lzH

Claq

ueous

solu

tions

Com

petition

betw

een

passiv

ation

and

meta

ld

issolu

tion

3M

HC

l:d

issolu

tion

accord

ing

toth

elo

calnorm

alto

free

surf

aces:

incre

asin

gra

tes

for

{111},

{100},

{110}

1M

HC

l:re

sid

ualoxid

ation

com

pete

sw

ith

dis

solu

tion;

resultin

gra

te{1

11},

{110},

{100}

(quantita

tive

descrip

tion

inin

vers

ep

ole

fig

ure

s)

Gra

yet

al.,

2006

Nib

ase

allo

y600

0. 1

NH

Cld

rop

let

Dis

solu

tion

and

oxid

ation

,100

.b

and

son

corr

od

ed

{110}

surf

aces.

Dis

solu

tion

rate

:{1

11},

{110},

{100}

(quantita

tive

descrip

tion

inin

vers

ep

ole

fig

ure

s)

Schuh

et

al.,

2003



Tab

le24

So

me

EB

SD

resu

lts

on

qu

ali

tyo

fth

infi

lmd

ep

osit

sfo

rfe

asib

ilit

yd

em

on

str

ati

on

Su

bstr

ate

Film

Dep

osit

ion

pro

cess

Resu

lts

Ref.

(100)

ZrO

2–9. 5

%Y

2O

3(c

ub

ic)

ZrO

2A

queous

pre

curs

orz

cert

ain

annealin

gcond

itio

ns

Sam

eE

BS

Dp

attern

over

the

entire

sam

ple

surf

ace

Mill

er

et

al.,

1993

(100)

Cu

(fcc)

Cu

and

Co–N

im

ultila

yers

(0. 1

5nm

per

layer)

Pote

ntiosta

tic

ele

ctr

od

ep

ositio

nE

pitaxy

(cub

e–cub

eO

R)

Alp

er

et

al.,

1993

Rolle

dand

polis

hed

Ni–

Wallo

yC

eO

2S

ol–

geld

ipcoating

Cub

e–cub

eorienta

tion

with

poly

cry

sta

lline

sub

str

ate

Van

Driessche

et

al.,

2003

(0001)

GaN

,N

ith

en

Au

Meta

llisation

Cry

sta

lq

ualit

yof

both

layers

invarious

cond

itio

ns;

suitab

leep

itaxy

ifN

i,th

en

Au

are

dep

osited

Davyd

ov

et

al.,

2004

(1120)

Al 2

O3

(sap

phire)

Nb

DC

mag

netr

on

sp

utt

ering

at

750uC

Clo

ser

than

,1u

toep

itaxy

Lolo

ee

et

al.,

2001

Tl 2

Ba

2C

a2C

u3O

xLaA

lO3

DC

mag

netr

on

sp

utt

ering

Cub

e–cub

eep

itaxy

Bra

mle

yet

al.,

1998

(001)

and

(111)

Mg

O*

In2O

3P

uls

ed

laser

dep

ositio

nz

anneal

Ep

itaxy,

OR

bein

g1. 7

¡0. 5u

,111

.*

Johnson

et

al.,

1999a

(100)

SrT

iO3

(Pb

0. 5

2Z

r 0. 4

8)T

iO3

Puls

ed

laser

dep

ositio

nC

ub

e–cub

eep

itaxy{

Ham

ed

iet

al.,

1998

Siof

various

orienta

tions

Si

Ele

ctr

on

cyclo

tron

resonance

chem

icalvap

our

dep

ositio

n(1

00)

Si:

ep

itaxy;

(210)

Si:

ep

itaxy

with

defe

cts

;(3

11),

(111),

(221):

no

ep

itaxy

Rau

et

al.,

2004

(0001)

Al 2

O3

(sap

phire)

Al 2

O3

Solid

sta

teconvers

ion

of

Al

All

convert

ed

Al 2

O3

part

icle

sare

of

sam

ecry

sta

lorienta

tion

as

sub

str

ate

(nanohete

roep

itaxy)

Park

et

al.,

2005

Anod

ised

poly

cry

sta

lline

Ti

Pb

O2

Ele

ctr

od

ep

ositio

nFeasib

ililit

yonly

on

{0001}

Tig

rain

s,

too

difficult

oth

erw

ise

Devill

iers

et

al.,

2004

*In

vestig

ation

incro

ss-s

ection.

{ Surf

ace

investig

ation

by

ele

ctr

on

channelli

ng

patt

ern

analy

sis

(clo

se

toth

eE

BS

Dte

chniq

ue).

Tab

le25

Ele

ctr

on

backscatt

er

dif

fracti

on

investi

gati

on

of

ori

en

tati

on

rela

tio

nsh

ips

betw

een

thin

dep

osit

ed

layers

an

dsu

bstr

ate

Su

bstr

ate

Film

Dep

osit

ion

pro

cess

Resu

lts

Ref.

(1120)

Al 2

O3

(sap

phire)

Nb

DC

mag

netr

on

sp

utt

ering

at

750uC

(110) N

b//

(1120) A

l 2O

3and

[111] N

b//

[0001]

Al 2

O3

by

,1u

Lolo

ee

et

al.,

2001

Nb

(of

pre

ced

ing

row

)(b

cc)

Cu

(fcc)

DC

mag

netr

on

sp

utt

ering

at

350uC

or

(150uC

zannealat

350uC

)N

WO

R,

with

two

variants

Lolo

ee

et

al.,

2001

(0001)

Al 2

O3

(sap

phire)

rota

ted

by

10u

tow

ard

(1010)

GaN

(30

nm

)C

hem

icalvap

our

dep

ositio

n(1

010) G

aN

//(1

210) A

l 2O

3i.e.

90u

aro

und

,0001

.Tra

ger-

Cow

an

et

al.,

2001

(0001)

and

(1120)

Al 2

O3

(sap

phire)

ZrO

2–10

mol.-%

Y2O

3A

queous

pre

curs

or

(0001):

thre

evariants

(001) Z

rO2

//(0

001) A

l 2O

3and

,100

.Z

rO2

//,

1210

.A

l 2O

3

with

one

dom

inating

variant;

(1120):

four

variants

with

various

OR

s,

som

eoth

ers

dete

cte

db

yX

RD

only

Cain

and

Lang

e,

1994;

Cain

et

al.,

1995

Poly

cry

sta

lline

Cu

Cu

dro

ple

tsA

nnealat

1050uC

inH

2/H

eatm

osp

here

There

are

pre

ferr

ed

initia

lO

Rs

but

with

limited

effect

on

sp

read

ing

.E

pitaxy

at

the

end

of

sp

read

ing

(GB

mig

ration).

Mis

sia

en

et

al.,

2005

GaN

Ni

Ele

ctr

on

beam

dep

ositio

n[1

10] N

i//

[1120] G

aN

or

[1210] G

aN

Davyd

ov

et

al.,

2004

(110)

TiO

215

nm

siz

ed

Au

part

icle

sIn

situ

meta

llisation

and

anneal

at

527uC

80%

of

101

analy

sed

part

icle

shave

(111)

,10u

from

(110) T

iO2;

two

variants

are

found

with

(111) A

u//

(110) T

iO2

and

(I)

[110] A

u//

[001] T

iO2

and

(II)

[110] A

u//

[001] T

iO2

Cosand

ey,

1997

(110)

TiO

212

nm

siz

ed

Au

part

icle

sIn

situ

meta

llisation

at

20uC

(zanneal)

or

502uC

20uC

:(1

11) A

u//

(110) T

iO2b

y3u;

two

variants

are

found

(I)

[110] A

u//

[001] T

iO2

and

(II)

[110] A

u//

[001] T

iO2

502uC

:(1

12) A

u//

(110)

TiO

2b

y2u

and

[110] A

u//

[001] T

iO2

or

[110] A

u//

[001] T

iO2

or

twin

rela

ted

with

these

Cosand

ey

et

al.,

2001



Tab

le26

Usin

gE

BS

Dto

dete

rmin

eth

estr

uctu

reo

fd

ep

osit

ed

layers*

Su

bstr

ate

Film

Dep

osit

ion

pro

cessz

ob

serv

ati

on

co

nd

itio

ns

Resu

lts

Ref.

(001)

Mg

OFe

2O

3P

uls

ed

laser

dep

ositio

nz

(IP

)Four

self-a

ccom

mod

ating

variants

gro

up

ed

into

recta

ng

ula

rd

om

ain

s(w

ith

deta

iled

mic

rote

xtu

re)z

possib

lein

tern

altw

innin

gJohnson

et

al.,

1999b

(100)

Sicoate

dw

ith

Ti,

then

Ni,

then

(111)

Pd

Sn–3. 5

%A

g(b

-Sn

phase)

Sta

ck

ele

ctr

op

latingz

(CS

)(2

20)

textu

re,

avera

ge

gra

insiz

ey

21mm

zevolu

tion

during

annealin

gE

zaw

aet

al.,

2004

(?)

YB

a2C

u3O

7–

dD

Csp

uttering

at

780uC

z(I

P)

Gra

insiz

ed

istr

ibution

(y1mm

2),

desirab

le[0

01]

textu

reob

tain

ed

at

98. 5

%Fairhurs

tet

al.,

2000

Pure

poly

cry

sta

lline

Cu

of

various

textu

res

Cu

(50mm

)E

lectr

od

ep

ositio

nz

(CS

)C

oars

eep

itaxia

lcolu

mnar

gra

ins,

com

petitive

gro

wth

ztw

innin

gC

ho

and

Szp

unar,

2002

,111

.S

icoate

dw

ith

60

nm

Cu

Cu

(2. 5

mm

)E

lectr

od

ep

ositio

nz

(IP

)G

rain

siz

ey

1. 5

mm

much

hig

her

than

siz

eof

ind

ivid

ualsp

here

sR

ead

et

al.,

2004

Nic

kelb

ase

sup

era

lloy

TiN

(6mm

)P

hysic

alvap

our

dep

ositio

nz

(CS

)S

mall

(0. 1

5–1. 5

mm

)colu

mnar

gra

ins,

gra

insiz

ed

istr

ibution

Jeong

et

al.,

2002b

Mo

Dia

mond

Chem

icalvap

our

dep

ositio

nin

recycle

dg

as

at

830uC

z(I

P,

CS

)C

om

petitive

gro

wth

and

twin

nin

gand

associa

ted

textu

reevolu

tion

inth

ickness

Mao

et

al.,

2005

(1120)A

l 2O

3(s

ap

phire)

coate

dw

ith

(110)

Nb

Perm

allo

y(N

i–16Fe),

then

Cu

DC

mag

netr

on

sp

utteringz

(IP

)C

uand

Perm

allo

y:

two

variants

with

180u,

111

.M

R,

4–5mm

insiz

eLolo

ee

et

al.,

2001

Poly

cry

sta

lline

Ni 3

Al

Dia

mond

Pla

sm

aassis

ted

chem

icalvap

our

dep

ositio

nw

ith

positiv

eb

ias

enhanced

nucle

ationz

(IP

)N

ucle

ation

density

dep

end

son

sub

str

ate

gra

inorienta

tion

Chen

and

Chang

,2005

(001)

SrT

iO3

coate

dw

ith

IrD

iam

ond

Pla

sm

aassis

ted

chem

icalvap

our

dep

ositio

nw

ith

bia

senhanced

nucle

ationz

(IP

)N

ucle

ation

str

uctu

res:

sam

eE

BS

Dp

attern

as

Irb

ut

are

infa

ct

futu

red

iam

ond

dom

ain

s;

the

reaction

isauto

cata

lytic

Schre

ck

et

al.,

2003

,111

.S

i nD

iam

ond

Pla

sm

aassis

ted

chem

icalvap

our

dep

ositio

nw

ith

bia

senhanced

nucle

ationz

(serial

sections

para

llelto

IP)

Colu

mnar,

mostly

ep

itaxia

lg

rain

sC

hen

and

Rud

olp

h,

2003

No

sub

str

ate

SiC

(3C

)Flu

idis

ed

bed

dep

ositio

nfr

om

CH

3S

iCl 3

(CS

)C

olu

mnar

gra

ins

from

the

eq

uia

xed

chill

zone;

inte

rnaltw

innin

g;

alm

ost

no

avera

ge

textu

reH

ela

ryet

al.,

2006

Ti

Nanostr

uctu

red

Co–20

at.

-%N

iE

lectr

od

ep

ositio

n(C

S,

IP)

5%

fcc

(Co)

phase

with

OR

tohcp

matr

ix;

gra

insiz

e,

GB

chara

cte

risation;

cry

sta

lorienta

tion

gra

die

nt

incolu

mnar

gra

ins

Basto

set

al.,

2006

AIS

I316

sta

inle

ss

ste

el

Pd

Ele

ctr

od

ep

ositio

nz

(CS

)G

rain

siz

ed

istr

ibution

(140

nm

inavera

ge),

gro

wth

from

sub

str

ate

gra

ins

far

from

GB

sB

era

et

al.,

2004

*IP

:in

pla

ne

ob

serv

ations;

CS

:ob

serv

ation

of

cro

ss-s

ections.



For in plane analysis, a balance must be found betweenspatial resolution and sampling effects and the rough-ness of the analysed surface must be low. Cross-sectionanalysis may require specific sample preparation (e.g. byFIB milling techniques) to avoid edge effects.

Discussion: coupling EBSD with otherinvestigation methodsAs EBSD mapping has become in most cases a routinetechnique, it has widely been used together with otherexperimental characterisation techniques for multiscaleinvestigation of materials. The case of EBSD/EDXcoupling for phase identification has already beenaddressed in the present paper. On the other hand,information on coupled crystal orientation and mor-phology is used in advanced models, which are now evenable to take into account individual or clustered crystalsto optimise process conditions or product properties.

Coupling EBSD with other experimentaltechniquesValidation of experimental results

In mineralogy samples, the orientation of individualcrystals is generally investigated with the light micro-scope. Advantages and drawbacks of EBSD and lightmicroscopy respectively, as well as coupled use of bothhave already been reviewed (Trimby and Prior, 1999).The main advantages of EBSD are its ability to analysesmall grains, optically ‘isotropic’ crystals and transpar-ent materials. Grain boundaries are more quantitativelycharacterised than by light microscopy (which is notsensitive to LABs) or backscattered electron imaging(Trimby and Prior, 1999). However, a robust reflectiontable must be constructed for each analysed mineral(Mauler et al., 1998).

The EBSD technique has also been used together withFIB imaging. In Al–0.5Cu, the ion channelling con-trast was shown with EBSD to rely on the angularmisorientation between the local normal to the samplesurface and the nearest ,111. crystal direction (Barret al., 1992).

Coupled analysis with EBSD and near field micro-scopy has been performed for less than a decade forphase identification [e.g. to distinguish ferrite fromaustenite in multiphase steels (Wendrock et al., 2001;Ros-Yanez et al., 2001 and 2002)], and to investigate GBgrooving [e.g. shallow thermal grooves at LABs orcoincident site lattice boundaries of polycrystalline MgO(Farrer et al., 2000)]. The high spatial resolution ofatomic force microscopy has been used to checkaccuracy of EBSD determination of GB traces in TiO2

polycrystals (Pang and Wynblatt, 2006), and to checkthat sapphire crystals obtained by solid state conversionwere of sufficient height (here y100 nm) for theirorientation to be determined with EBSD independentlyof that of the sapphire substrate (Park et al., 2005).

Multiscale analysis

Although EBSD makes full use of the large magni-fication range of the SEM, there is still a need for finerscale analysis and for analysis of higher amounts ofmaterial to reduce sampling effects. The coupled use ofvarious techniques for that purpose is discussed in thissection.T

ab

le27

Usin

gE

BS

Dto

dete

rmin

eavera

ge

textu

reo

fd

ep

osit

ed

layers

Su

bstr

ate

Film

Dep

osit

ion

pro

cess

Resu

lts

Ref.

Poly

(meth

ylm

eth

acry

late

)coate

dw

ith

Cu

Ni

Ele

ctr

od

ep

ositio

nin

sulfam

ate

(S)

or

Watts

bath

(W)

(S):

,100

.colu

mnar

zone;

(W):

fine,

poorly

ind

exed

mic

rostr

uctu

re,

weaker

,110

.

Buchheit

et

al.,

2002

Alcoate

dw

ith

Zn

then

with

Cu

Ni

Ele

ctr

od

ep

ositio

n,

110

.colu

mnar,

many

low

mis

orienta

tions

within

colu

mns

Arn

ould

et

al.,

2003

Ti

Co–20

at.

-%N

iE

lectr

od

ep

ositio

nS

trong

{1120} a

and

{220} b

textu

reB

asto

set

al.,

2006

Mg

OTl 2

Ba

2C

a2C

u3O

xD

Cm

ag

netr

on

sp

uttering

(001)

fib

reand

many

HA

Bs:

poor

film

pro

pert

ies

Bra

mle

yet

al.,

1998

Sicoate

dw

ith

SiO

2th

en

with

Tith

en

with

Pt

then

with

La(N

O3) 3

zp

ossib

leb

uff

er

layers

(Pb

,Zr)

TiO

3S

ol–

gelcoating

Str

ong

(100)

textu

re,

no

textu

rein

pla

ne

Choiet

al.,

2004

and

2005

Mo–9S

i–18

at.

-%B

MoS

i 2z

transfo

rmation

into

Mo

5S

i 3d

uring

annealin

g

Pack

cem

enta

tionz

annealin

gM

oS

i 2:

[001]

at

exte

rnalsurf

ace;

Mo

5S

i 3:

[001]

colu

mnar

Ito

et

al.,

2003

Oxid

ised

(100)

Sicoate

dw

ith

100

nm

Cu

then

with

282

nm

Al

Al 2

Cu

Ele

ctr

on

beam

evap

ora

tion

Cellu

lar

gro

wth

with

pre

fere

ntial(1

10)

textu

reS

on

et

al.,

2001

No

sub

str

ate

TiO

2(r

utile

)Tap

ecastingz

sin

tering

TiO

2:

(001)

textu

re,

[001]

gro

wth

direction

Cosand

ey

et

al.,

1999

No

sub

str

ate

Al 2

O3

Tap

ecastingz

sin

tering

(0001)

para

llelto

both

film

and

pla

ne

of

pla

tes

Mark

ond

eya

Rajet

al.,

1999



Additional information provided by coupling EBSD withnear field microscopy

Near field microscopy gives access to local 3D surfacemorphology and material properties at a very fine scale.Shreck et al. (2003) were able to detect diamond nucleion iridium substrate by Kelvin probe microscopy,although the local crystal structure was still determinedby EBSD to be that of iridium. Magnetic forcemicroscopy readily detected magnetisation domains atGBs of AISI 304 austenitic stainless steel, which wereconfirmed by fine scale EBSD mapping to be martensiteparticles (Takaya et al., 2004). Local surface modifica-tion after thermal grooving [e.g. in SrTiO3 (Sano et al.,2003a)] gives information about free surface and GBenergy.

Local surface relief produced on polished surfaces byphase transformation (e.g. from bcc b to orthorhombica’’ in Ti–9 wt-%Mo (Guo and Enomoto, 2006), fromaustenite into Widmanstatten ferrite (here characterisedwith a specific procedure by light microscopy) (Hall andAaronson, 1994) or into bainite (Ohmori, 2002) in steel)suggests surface reconstruction or previous twinning ofthe parent phase near single crystal, tent shaped plates(i.e. a diffusional mechanism) and no diffusion nearplates showing an invariant plane strain morphology.More generally, the macroscopic strain induced bydisplacive solid state phase transformations at polishedsurfaces can be determined in 3D using near fieldmicroscopy, whereas local crystallography in the samearea is determined with EBSD. Such precious data areessential for validation of phenomenological theoriesof martensite crystallography (PTMCs) (see Modellingsection).

The measurement of local properties coupled withEBSD determination of the local crystal structure andorientation has been recently reviewed in the frame-work of phase diagram determination (Zhao, 2006).Nanoindentation on individual phases identified withEBSD was performed in Pd–Rh–Pt diffusion multiples(Zhao et al., 2002), on Ag3Sn and Cu6Sn5 intermetallicphases in Sn–Ag–Cu solder interconnects (Li et al.,2005b) and in various layers formed on a nickel basesuperalloy coated with NiAl by pack cementation(Wollmer et al., 2003). The anisotropy of propertiesmay be quantified thanks to information about localcrystal orientation [e.g. in the NiAl phase of NiAl–Moeutectic (Bei and George, 2005)]. There are cases forwhich a simple rule of mixtures between the variousphases worked well for the investigated microstructure[e.g. hardness and elastic modulus of a V–V3Si eutectic(Bei et al., 2004)]. In other instances, no agreement couldbe found, e.g. for elastic modulus and for hardness(Zhao et al., 2002). Correlation between nanohardnessand 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 SEM-EBSD investigations of the same phenomena; auto-mated indexing of Kikuchi bands is now possible in theTEM, allowing orientation imaging at very fine scales.This section focuses on complementary use of SEM-EBSD and TEM techniques. Transmission electronmicroscopy investigations are needed for fine scalecharacterisation of deformation structures, such as

dislocation clustering into LABs that are observed withEBSD but do not affect the martensitic transformation[e.g. in Cu–Al–Ni SMA (Rodriguez, 2004)], and if thereare local deformation bands in the parent phase, inwhich particular variant selection may then occur [e.g.in Cu–42 wt-%Zn (Sakata et al., 2000)]. Interactionsbetween the local texture and very fine scale precipita-tion also require TEM observations [e.g. precipitationin Zircaloy–4 (Loge et al., 2000)]. The effect of GBmisorientation on discontinuous precipitation in Al–2.8Mg–1 at.-%Ga was determined with EBSD, whereasthe ORs between phases had to be determined withTEM (Hirth and Gottstein, 1998). In precipitation aidedmatrix phase transformations, the OR between matrixphases may be determined with EBSD while the ORswith fine nucleating agents are still studied in the TEM[e.g. ferritic steels (Furuhara et al., 2003)].

Fine scale microstructural features (such as thosedifferentiating ferrite from bainite in low alloy TRIPsteels) were first studied by TEM, giving qualitative orquantitative criteria for further (and easier) investigationby SEM-EBSD. In this particular case (Fig. 16),orientation gradient and internal LABs were observedin bainite, but not in ferrite (Zaefferer et al., 2004). Theinternal structure of c phases in c-TiAl gave comple-mentary information to EBSD determined ORs betweenlamellar and Widmanstatten c phases in this alloy (Deyet al., 2005). The gradual misorientation determinedby EBSD within lenticular a’ martensite of Fe–32.85 wt-%Ni (Fig. 17) was shown by TEM to be linkedto a change in the internal structure of martensite (andlocal accommodation of transformation induced latticestrains) from dislocation network to microtwinning(Shibata et al., 2005). Internal microtwinning in self-accommodating martensite of Cu–12.55Al–4.84 wt-%Ni(Chen et al., 2000) and in Cu–7.3Al–8.5 wt-%Mn (Wanget al., 2002) was detected in the TEM but not by SEM-EBSD, so that only a part of the self-accommodatingvariants could be identified in each martensite unit byEBSD. TEM based techniques remain necessary if veryfine scale features or dislocation structures have to beinvestigated.

Other diffraction techniques

X-ray diffraction is a reference technique for texturedetermination, so that the comparison of resultsobtained by XRD and EBSD respectively, sincepioneering studies of e.g. Schwarzer and Weiland ondual phase steels (Schwarzer and Weiland, 1988), hasalready been reviewed (Dingley and Randle, 1992). Inaddition to providing spatial information, EBSD is wellsuited for coarse grained materials. Lattice parametersare better determined with XRD, and a large area can beanalysed at a time. The probability to miss particularvariants or phases is much lower with XRD than withEBSD [e.g. in cubic ZrO2 deposited onto sapphire (Cainand Lange, 1994)]. For moderately coarse microstruc-tures or for very low amounts of phases, neutrondiffraction coupled with EBSD is a well suited tool. Thepioneering study of Grant et al. (1986) focused ondirectionally solidified copper, where optical microscopyrevealed a columnar grain structure, neutron diffractionshowed a ,100. fibre texture that was confirmed bylocal electron channelling pattern analysis. In anaustenitic stainless steel WM deposit, Bouche et al.(2000) showed by both neutron diffraction (providing



statistics over y1 cm3 of material), point EBSD analysisof submicron sized bcc ferrite and local TEM observa-tions that the OR between austenite and ferrite was notonly the classical near KS OR, but could be much closerto a cube–cube OR, at least for ferrite particles locatedat austenite LABs. Cold rolled duplex stainless steelUranus 45N was shown by neutron diffraction to haveferrite and austenite phase textures identical to those oftheir single phase steel counterparts. In fact, a loss of theOR between ferrite and austenite was found with EBSD,due to complex deformation structures imaged in theTEM (Baudin et al., 2002). Electron backscatter diffr-action may also suggest ORs that are useful for global

texture calculations to be coupled to hot stage XRDtexture characterisation of the product phase [e.g. ina low carbon steel (Bruckner and Gottstein, 2001)]. In(Ni,Co)O single crystals, neutron diffraction gaveaverage results on crystal quality (here, mosaicity),XRD gave details on lattice parameters and EBSDprovided spatial information on crystal orientation(Brewer et al., 2002). The ORs between Ni and NiOwere obtained by carrying out EBSD (sensitive to NiOonly) and XRD (sensitive to the Ni substrate) in thesame area (Woodcock et al., 2004).

As XRD and TEM are well known techniques theycan easily be combined to get quantitative data oncrystal structure and orientation. Neutron diffraction ismuch less commonly used but provides useful bulkcharacterisation. Transmission electron microscopy isstill necessary for fine scale imaging and crystal charac-terisation, although sample preparation is destructiveand more tedious and analysed areas are small.

In situ investigations

Very few EBSD analyses associated with in situ inves-tigations have been published yet. Hot stage microscopyassociated with crystallographic EBSD characterisationof initial and/or final state has already provided newinteresting data (Table 28). With the development ofhigh speed, highly sensitive EBSD systems this is a

a

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 EBSDmap of a ferrite grain: angular deviation from the crys-tal orientation of the grain centre (from 0 in white up to4u in black), showing bainite areas in dark

16 Coupled use of EBSD and TEM to characterise bai-

nite in a low alloy TRIP aided steel: hatched particles

are retained austenite, other ferrite grains are in

white. After Zaefferer et al. (2004)

a

b

a information obtained with TEM reported on a micro-graph; b EBSD map of misorientation with respect topoint X

17 Coupled EBSD and TEM investigation of the internal

structure of plate martensite in Fe–32.85 at.-%Ni: a

misorientation profile is superimposed, showing mis-

orientation up to 3u, following the change in OR

between austenite (A) and martensite (M). After

Shibata et al. (2005)



promising way to get information about phase trans-formation mechanisms, at least at the sample surface.Environmental SEMs may be equipped with EBSDanalysis. Nothing seems to have been published yetabout in situ EBSD investigation of surface reactions butthe feasibility of EBSD analysis in various environ-mental and thermal conditions has already beendemonstrated in water and nitrogen environments forboth conducting and non-conducting materials(Garmestani and Harris, 1999; Habesch, 2000). In situphase transformation of low alloy TRIP aided steelsconfirmed that retained austenite gradually transformedupon straining, coarse equiaxed particles being lessstable that elongated ones in the area monitored byEBSD (Oh et al., 2002; Park et al., 2002).

Electron backscatter diffraction in hot stage SEM hasbeen made possible by a low effect of temperature onpattern quality for various materials up to 650 or even700uC (Garmestani and Harris, 1999; Seward et al.,2002) and by the recent development of fast EBSDsystems (Wright et al., 2005). Published studies mainlyconcentrated on recrystallisation and grain growth, e.g.in aluminium (Ferry, 1998; Huang et al., 2002) andnickel and deformed NaCl (Piazolo et al., 2004a). Somestudies have already been published on phase transfor-mations, e.g. in hcp a into bcc b and then back into hcpa transformations of titanium (Seward et al., 2002). Byheating titanium, bcc b phase transformed from hcp amay appear as plates with a Burgers OR and a tentshaped surface relief (Fig. 18) (Seward et al., 2004).Orientation relationships close to NW were identified inhcp a into fcc b and then back into hcp a transforma-tions of cobalt (Wright et al., 2005). Phase transforma-tions in iron oxides such as that from hematite intomagnetite have also been investigated using hot stageEBSD (Piazolo et al., 2004b). The main difficulties inhot stage EBSD mapping are temperature measurements(Seward et al., 2002) and the high kinetics of phasedevelopment, which may restrict in situ monitoring toonly a small area, possibly leading to sampling effects ifno repeated experiments are to be made.

Three-dimensional considerations

Electron diffraction cannot give information aboutcrystal orientation in the bulk of the material; 3D-XRD techniques are being developed for this pur-pose but still require a high flux synchrotron X-rayfacility to get the 3D shape of individual crystals andof orientation gradients (Fu et al., 2003; Barabashet al., 2006). The spatial resolution is coarser (abouta few mm) than that of EBSD but the angular re-solution is high (y0.05u) (Juul Jensen, 2000). Beingnon-destructive, 3D-XRD may be used for in situ inves-tigation of e.g. recrystallisation (Juul Jensen, 2000)and possibly phase transformations. However, it is farfrom being readily available, so that other methodsare generally used to get 3D information about crystalmorphology.

Three-dimensional investigations

The reconstruction of the 3D morphology is difficult(Fig. 19) and involves both careful experimental section-ing and complex 3D image processing. For coarsegrained materials, it may be useful to analyse bothparallel sides of the sample and to assume that no othercrystal is embedded in the bulk [e.g. in single shear lapT

ab

le28

Investi

gati

on

of

ph

ase

tran

sfo

rmati

on

sb

yE

BS

Dasso

cia

ted

wit

hin

sit

um

icro

sco

py

Mate

rial

Ho

tsta

ge

devic

eIn

form

ati

on

pro

vid

ed

by

ho

tsta

ge

devic

eIn

form

ati

on

pro

vid

ed

by

EB

SD

Ref.

Sp

lat

coolin

gand

melt

sp

innin

gof

molten

Si

Infr

are

dm

icro

scop

yS

pre

ad

ing

of

conta

ct

zone

The

conta

ct

zone

consis

tsof

fine,

eq

uia

xed

gra

ins

Nag

ashio

et

al.,

2004;

Nag

ashio

and

Kurib

ayashi,

2006

Form

ation

of

prim

ary

and

Wid

mansta

tten

ferr

ite

inlo

wcarb

on

ste

el

Laser

confo

cal

mic

roscop

yTim

ere

solv

ed

monitoring

nucle

ation

and

gro

wth

of

ind

ivid

ualp

hases

Mis

orienta

tion

betw

een

prim

ary

and

Wid

mansta

tten

ferr

ite

Phela

nand

Dip

penaar,

2004;

Phela

net

al.,

2005

Fe–32

at.

-%N

ib

icry

sta

lsLig

ht

op

ticalm

icro

scop

yM

onitoring

revers

etr

ansfo

rmation

from

mart

ensite

into

auste

nite

Fin

alm

icro

textu

re:

back

toorig

inalauste

nite

cry

sta

lorienta

tions

tog

eth

er

with

form

ation

of

LA

Bs

Ued

aet

al.,

2004

Fe–4. 1

8at.

-%C

rLig

ht

op

ticalm

icro

scop

yN

ucle

ation

sites

of

auste

nite

during

heating

Eff

ect

of

pare

nt

GB

mis

orienta

tion,

sub

seq

uent

ab

norm

al

gro

wth

and

twin

nin

gof

auste

nite

Wata

nab

eet

al.,

2004

and

2005b

Cu–A

l–B

eS

MA

X-r

ay

diffr

action*

Inte

rnalstr

esses

(one

sele

cte

dg

rain

)C

rysta

lorienta

tion

of

neig

hb

ouring

gra

ins

Kaouache

et

al.,

2004

*Tensile

sta

ge

devic

e.



Sn–3.5Ag solder joints (Telang and Bieler, 2005a)].Habit planes of plates may be determined by analysis oftwo perpendicular sections (Fig. 19c) such as in the bto a’’ phase transformation of titanium based b-Cezalloy (Zimmermann and Humbert, 2002). Electronbackscatter diffraction analysis of interfaces and facets

has been recently reviewed (Randle, 2004) and will notbe detailed here.

Another way to get 3D information on phasemorphology and connectivity is deep etching performedafter EBSD analysis (Fig. 19b). The morphology ofeutectic silicon was studied as a function of alloyingelements and local crystallography of phases in Al–Sihypoeutectic alloys (Nogita and Dahle, 2001a and2001b). Proeutectoid cementite in Fe–1.34C–13.1Mnwas shown to appear as both monolithic single crystalsand polycrystalline conglomerates of parallel laths, theOR with the austenite matrix being different from onecase to the other (Mangan et al., 1999). The morpho-logy of intergranular cementite in Fe–1.3C–13Mn wasstudied by TEM observation of deep etched materialand by EBSD investigation of OR with the austenitematrix (Kral and Spanos, 2003). Deep etching is alsouseful to investigate 3D connectivity of phases, e.g. ineutectic M7C3 carbides of white cast irons. These appearas interconnected colonies of parallel rods. Colonies aresingle crystalline in hypereutectic alloys and polycrystal-line in hypoeutectic alloys (Randle and Powell, 1993).3D analysis also gives access to nucleation sites, forexample in successive nucleation of MnS particles atoxides, of VC carbides at MnS sulphides, and of pearliteat VC carbides in intragranular pearlite of hypereutectic0.8C–12Mn–V steel (Guo et al., 2002).

The surface geometry may be determined by use ofstereo pairs as is already done on fracture surfaces(Hebesberger et al., 2000). Provided that the surface

(a)

(b)

(c)

a backscattered electron image (A1, A2, A3: b allotrio-morphs; P1: intragranular b); b pole figures of {111}band {11.0}a; c pole figures of {110}

band {00.1}a for

grains A3 and a218 In situ EBSD investigation of ORs between growing

allotriomophic b phase and starting a phase at 882uC:

after Seward et al. (2004)

(a)

(c)

(b)

(d)

(e)

19 3D morphological investigations to assess the hidden

volume a of the iceberg by b deep etching, c non-

parallel plane sectioning, d serial sectioning and e

one plane trace analysis: a practical example is given

in Fig. 6



relief does not impede EBSD analysis by shadowingeffects, phase identification on fracture surface ofmultiphase materials [e.g. in c za2 TiAl alloys(Hebesberger et al., 2000)] is possible. Grain boundarygeometry (Randle, 2004) provides additional data forthe understanding of segregation phenomena [e.g. inNiz7 at. ppm S (Cornen and Le Gall, 2004)] andprecipitation.

The most widely used technique to get 3D informa-tion from EBSD is serial sectioning (Fig. 19d) either toget the 3D morphology alone (‘uncoupled’ use inTable 29) or even to get an EBSD map of all or partof the slices (‘coupled’ use in Table 29). Manual orautomatic metallographic polishing is the most conven-tional method. Ion milling is now in development (Chenand Rudolph, 2003). Dual beam SEMs now allow moreor less automated sequences of FIB milling followed byEBSD analysis in the same apparatus (Groeber et al.,2006; Zaafarani et al., 2006; Konrad et al., 2006). As thespecimen has to be moved between successive millingand EBSD mapping sequences, absolute spatial locationand orientation of the sample must be adjusted for eachslice (King et al., 2000) and distortion due to, e.g.electron beam drift during EBSD mapping is to bestrictly avoided. Data processing is now much easier,thanks to the increase in computer power and thedevelopment 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 oftraces (Fig. 19e) to determine facet orientation in crystalgrowth, interphase interfaces, habit planes and interac-tions between cracks and microstructure of productphases (Table 30) for both metallic and non-metallicmaterials. Most studies determine probable crystal planefamilies to which the observed traces could belong.Several methods exist to assess the reliability of theseresults. If crystal planes are considered, one cannormalise the results (e.g. fraction of interfaces whosetraces are closer to experimental ones than a user definedthreshold) by the frequency that would be obtained ifthese planes were randomly oriented with respect to thecrystal. This is particularly useful if the plane multi-plicity is high due to crystal symmetry. For example, in asimulated 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 morefrequently close to the trace of these planes than arandomly oriented plane would have been (Gourgues,2003). The same kind of calculations was carried out forthe growth direction of bainite in a 0.6C–1.5Si–1Mnsteel (Cabus, 2005). Such normalising takes the actualcrystallographic orientation of phases into account andthus reduces the bias induced by the crystallographictexture. Habit planes are generally expressed in theframe of the parent phase, so that normalising has to becarried out for each grain orientation of the parentphase separately, which can be tedious when this phaseis totally absent from the resulting microstructure.

Stereological methods based on extensive data analy-sis over a number of non-parallel sections are nowavailable to up to date computer systems and providestatistically based information on interfaces [e.g. in GBsegregation of Nb in TiO2 (Pang and Wynblatt, 2006)].Other methods assuming tetrakaidecahedron shaped

grains help getting from 2D sections to 3D investiga-tions of ‘effective’ grain size after phase transformationin hot rolled steel (Bhattacharjee and Davis, 2002).Another way to investigate the 3D connectivity of lowmisoriented 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 bainiteand martensite in steel HAZs come with a high den-sity of HABs in 2D sections, areas of close crystalorientations within a given parent grain are actuallyconnected to each other in 3D, so that the size ofcleavage facets is much coarser (in this case, close to thehuge austenite grain size) and the toughness is muchlower than predicted from the ‘crystallographic’ grainsize calculated from individual 2D EBSD sections,although embedded misoriented crystals induce someroughness in cleavage fracture surfaces (Gourgues,2003).

In summary, although the vast majority of EBSDresults focus on 2D considerations only, one must notforget how to get to a 3D view, which is relevant tomaterial properties and reduces sampling effects such aspseudo variant selection. This is particularly true forcomplex shaped microstructures such as bainite andmartensite, and for all studies involving nucleation orvariant selection. The fast development of new 3Danalysis techniques should make it possible to increas-ingly include 3D considerations into the crystallographyof many phase transformations.

Coupling EBSD results with quantitativemodellingMany modelling approaches now use EBSD data as anexperimental basis. Some examples are given in thissection to illustrate the specific use of EBSD for thatpurpose.

Modelling phase transformations

Geometry considerations have been used for a decade tointerpret EBSD results of interphase interface proper-ties, phase connectivity and stereology (Table 31). Suchmodels should now benefit from 3D investigations asmentioned in the previous section. Another field ofmodelling is coupling EBSD data with heat and/or fluidflow calculations, especially for solidification (Table 32).In many instances, heat and fluid flow models aresimplified either to speed up calculations or to avoidintroduction of parameters that are difficult to calibrate(e.g. thermal exchange coefficients).

Little literature is available concerning couplingEBSD data and modelling of phase transformationkinetics, except for CET (see section on solidification).A simple model for diffusion anisotropy was usedto discuss results of oxygen tracer diffusion inLa2–xSrxCuO4¡d (Claus et al., 1996). Grain boundarymigration coupled with diffusion anisotropy allowedto explain EBSD data on heterogeneous kinetics ofdiscontinuous ordering in Fe–50 at.-%Co (Bischoffet al., 1998). Simple analytic kinetic models were usedand their results compared with crystal connectivitydetermined with EBSD to investigate fragmentation ofthe nickel skeleton in containerless eutectic solidificationof Ni–18.7 at.-%Sn (Li et al., 2005b), oscillation ofperitectic solidification in Sn–1.4 wt-%Cd (Zeisler-Mashl and Lograsso, 1997) and dendrite tip under-cooling in laser treated Fe–Cr–Ni alloys (Fukumoto and



Tab

le29

3D

mic

rostr

uctu

ral

investi

gati

on

su

sin

gE

BS

D

Mate

rial

Ph

ase

tran

sfo

rmati

on

Co

up

led

or

un

co

up

led

EB

SD

an

aly

sis

Resu

lts

(new

info

rmati

on

)R

ef.

Al–

10S

iE

ute

ctic

solid

ific

ation

Uncoup

led

Rad

ialg

row

thof

eute

ctic

Sifr

om

Sip

oly

hed

raD

ahle

et

al.,

2005

Al–

1S

i–0. 1

7Ti

Solid

ific

ation

(feath

ery

gra

ins)

Coup

led

Dend

rite

gro

wth

direction,

twin

nin

gp

lanes

Henry

et

al.,

1998

2618

alu

min

ium

allo

yS

olid

ific

ation

(thix

ofo

rmin

g)

Uncoup

led

Glo

bula

rm

orp

holo

gy

as

alread

ysug

geste

db

y2D

analy

sis

,H

AB

sX

iaand

Tausig

,1998

AL–6X

Nsup

era

uste

nitic

sta

inle

ss

ste

el

Inte

rgra

nula

rp

recip

itation

of

sp

hase

Coup

led

(EB

SD

every

tenth

slic

e)

Morp

holo

gy,

cry

sta

llog

rap

hy,

GB

pla

ne,

OR

betw

een

sand

matr

ixLew

iset

al.,

2006

Auste

nitic

sta

inle

ss

ste

el

for

hyd

rog

en

refo

rmin

gP

recip

itation

of

M23C

6C

oup

led

All

cre

ep

cavitie

sare

connecte

dto

M23C

6;

these

M23C

6

are

less

freq

uently

incub

e–cub

eO

Rw

ith

the

matr

ixth

an

ifnot

connecte

dto

cre

ep

cavitie

s

Ab

dulW

ahab

and

Kra

l,2005

Cu–4

wt-

%Ti

Dis

continuous

pre

cip

itation

from

ain

toaz

Cu

4Ti

Coup

led

Exte

nsiv

ein

form

ation

ab

out

morp

holo

gy

and

cry

sta

llog

rap

hy

of

colo

nie

sM

ang

an

and

Shifle

t,1997

Fe–C

pla

incarb

on

ste

els

Eute

cto

idp

earlite

form

ation

Coup

led

3D

cry

sta

llog

rap

hy

of

pearlite

colo

nie

s,

OR

betw

een

ferr

ite

and

cem

entite

linked

tonucle

ation

sites

Mang

an

and

Shifle

t,1999

Fe–0. 8

C–12M

n–0. 3

VE

ute

cto

idp

earlite

form

ation

Uncoup

led

3D

imag

ing

:nucle

ation

cond

itio

ns;

EB

SD

:no

OR

betw

een

auste

nite

and

pearlitic

ferr

ite

Guo

et

al.,

2002

Fe–0. 8

C–12. 3

Mn

Form

ation

of

Wid

mansta

tten

cem

entite

pla

tes

Coup

led

Inte

rlocked

pla

tes

are

infa

ct

diffe

rent

cry

sta

lsand

not

bifurc

ations

of

the

sam

ecry

sta

l;in

form

ation

ab

out

nucle

ation,

gro

wth

and

OR

s

Mang

an

et

al.,

1997

Low

carb

on

ste

el

Tra

nsfo

rmation

of

auste

nite

into

inte

rgra

nula

rfe

rrite

Coup

led

Poly

cry

sta

lline

ferr

ite

(inclu

din

gLA

Bs);

all

cry

sta

lsare

inconta

ct

with

aM

nS

nucle

ating

part

icle

;th

enum

ber

of

ferr

ite

cry

sta

lsp

er

MnS

incre

ases

with

the

siz

eof

the

MnS

part

icle

Yokom

izo

et

al.,

2003

Hig

hp

urity

Fe–0. 1

2C

–3. 2

8N

iTra

nsfo

rmation

of

auste

nite

into

inte

rgra

nula

rp

rim

ary

and

Wid

mansta

tten

ferr

ite

Coup

led

Peak

morp

holo

gy:

pyra

mid

alsin

gle

cry

sta

ls;

lath

sand

second

ary

pla

tes:

poly

cry

sta

lsw

ith

inte

rnalLA

Bs

(rep

eate

dnucle

ation);

one

cry

sta

lorienta

tion

far

from

auste

nite

GB

s

Sp

anos

et

al.,

2005;

Kra

land

Sp

anos,

2005

Hig

h-p

urity

Fe–0. 1

2C

–3. 2

8N

iTra

nsfo

rmation

of

auste

nite

into

ferr

ite

sid

ep

late

sU

ncoup

led

Prim

ary

ferr

ite

film

and

sid

ep

late

ssep

ara

ted

by

aLA

B:

there

isin

deed

nucle

ation

of

Wid

mansta

tten

ferr

ite,

not

only

unsta

ble

gro

wth

of

the

ferr

ite

film

Sp

anos

and

Hall,

1996

Auste

mp

ere

dd

uctile

cast

iron

Tra

nsfo

rmation

of

auste

nite

into

ausfe

rrite

Coup

led

Fatig

ue

cra

cks

arr

est

at

packet

bound

aries;

sta

ge

Icra

cks

are

conta

ined

in{1

11}

pla

nes

of

auste

nite

Marr

ow

et

al.,

2002

0. 0

7C

–0. 8

Mn–3. 5

Ni–

1. 6

Cu–0. 6

Mo

(HS

LA

–100)

Tra

nsfo

rmation

of

auste

nite

into

‘coars

e’m

art

ensite

Coup

led

Tap

ere

d3D

morp

holo

gy

and

cry

sta

lin

dic

es

of

inte

rface

pla

nes

Row

enhors

tet

al.,

2006

Ni–

45. 6

at.

-%A

lIn

terg

ranula

rseg

reg

ation

Uncoup

led

The

GB

energ

yd

ep

end

son

the

GB

pla

ne

even

for

rand

om

GB

sA

mouyalet

al.,

2005

Dia

mond

on

sili

con

Cry

sta

lg

row

thC

oup

led

,p

ara

llel

toth

efilm

pla

ne

Colu

mnar

{111}

gro

wth

Chen

and

Rud

olp

h,

2003



Tab

le30

Tra

ce

an

aly

sis

fro

mE

BS

Dre

su

lts

(excep

tth

ose

co

ncern

ing

the

gro

wth

dir

ecti

on

inso

lid

ificati

on

,see

co

rresp

on

din

gsecti

on

)

Mate

rial

Ph

ase

tran

sfo

rmati

on

Facet

An

aly

sis

co

nd

itio

ns

Resu

lts

Ref.

Pb

(Mg

0. 3

3N

b0. 6

7)O

3z

Pb

TiO

3R

eactive

sin

tering

Cry

sta

lfr

ee

surf

aces

Tra

ce

analy

sis

(no

deta

ilp

rovid

ed

){1

00}

facets

Liet

al.,

1998

Kaolin

ite

and

dic

kite

min

era

lsC

rysta

lg

row

thC

rysta

lfr

ee

surf

aces

Tra

ce

analy

sis

Orienta

tion

of

late

ralfa

cets

Kog

ure

et

al.,

2005;

Kam

ed

aet

al.,

2005

SrT

iO3

inTiO

2rich

liquid

Coars

enin

gof

cry

sta

lsC

rysta

lfr

ee

surf

aces

Tra

ce

analy

sis

zste

reolo

gic

alm

od

el

Shap

echang

ein

to{1

00}

facets

and

,100

.zone

axes

during

coars

enin

gS

ano

et

al.,

2005

2. 2

5C

r–1M

oste

el

Auste

nite

into

bain

ite

Cle

avag

ecra

cks

Tra

ces

plo

tted

onto

ste

reog

rap

hic

pro

jection

Com

patib

lew

ith

{100}

pla

nes

of

bain

ite

Bouyne

et

al.,

1998

Thre

elo

wcarb

on

ste

els

Auste

nite

into

acic

ula

rfe

rrite

and

bain

ite

Cle

avag

ecra

cks

Tra

ce

analy

sis

,cra

ck

arr

est

cond

itio

ns

{100}

traces,

cra

ck

devia

tion

for

mis

orienta

tion

ang

le.

15u

Dıa

z-F

uente

set

al.,

2003

Dup

lex

sta

inle

ss

ste

el

Ferr

ite

into

auste

nite

Fatig

ue

cra

cks

Tra

ce

analy

sis

Str

ong

eff

ect

of

the

two

phase

mic

rostr

uctu

reon

cry

sta

lorienta

tion

of

traces

Gourg

ues

et

al.,

2004

0. 7

8C

mic

roallo

yed

ste

el

Auste

nite

into

pearlite

Cle

avag

ecra

cks

Orienta

tion

units

(5sin

gle

cry

sta

lfe

rrite

inp

earlite

colo

nie

s)

The

siz

eof

orienta

tion

units

isth

esam

eas

that

of

cle

avag

efa

cets

corr

ecte

dfr

om

2D

/3D

ste

reolo

gy

Cotr

ina

et

al.,

2003

Auste

mp

ere

dd

uctile

cast

iron

Auste

nite

into

ausfe

rrite

Fatig

ue

cra

cks

2D

and

3D

(serialsectionin

g)

pro

pag

ation

pla

nes

{111}

pla

nes

of

pare

nt

(and

reta

ined

)auste

nite

Marr

ow

et

al.,

2002

Mo

5S

i 3(C

r,Ti)

Solid

ific

ation

(seg

reg

ate

dzones)

Cle

avag

enear

ind

enta

tion

mark

sTra

ce

analy

sis

(001)

cry

sta

lp

lanes

Str

om

and

Zhang

,2005

Hig

hstr

eng

thlo

wallo

yste

el

Auste

nite

into

up

per

bain

ite

Str

aig

ht

inte

rfaces

of

lath

gro

up

sTra

ce

analy

sis

{557}

and

{223}

auste

nite

pla

nes

more

pro

bab

leth

an

{111}

auste

nite

pla

nes

Lam

bert

-Perlad

eet

al.,

2004a

0. 8

C–12. 3

Mn

ste

el

Auste

nite

into

pearlite

Hab

itp

lanes

Work

on

EB

SD

patt

ern

s(0

01) c

//{1

25} c

with

Pitsch–P

etc

hO

R,

(101) c

//{2

11} c

with

Isaic

hev

OR

;(0

01) c

//{1

21} c

with

Bag

ary

ats

ky

OR

dep

end

ing

on

the

ind

ivid

ualcolo

ny

Mang

an

and

Shifle

t,1998

Cu–3

wt-

%Ti

Cellu

lar

pre

cip

itation

Hab

itp

lanes

Work

on

EB

SD

patt

ern

s(1

11) a

//(0

10) b

Mang

an

and

Shifle

t,1998

Ti

hcp

ain

tob

cc

bH

ab

itp

lane

of

bIn

situ

trace

analy

sis

zshap

econsid

era

tions

Near

to{3

34} b

,conta

ins

the

[0001] a

//[1

10] b

Sew

ard

et

al.,

2004

Hig

hstr

eng

thlo

wallo

yste

el

Auste

nite

into

bain

ite

Str

aig

ht

inte

rface

of

lath

gro

up

sTra

ce

analy

sis

{557}

or

{223}

but

not

{111}

pla

nes

of

auste

nite

Gourg

ues,

2003

Ti–

25A

l–24

at.

-%N

ba

2in

toO

GB

pla

nes

Auto

mate

dtr

ace

analy

sis

of

MR

and

inte

rphase

inte

rfaces

(110)

for

39%

of

twin

rela

ted

cry

sta

lsLiet

al.,

2004

TiO

2d

op

ed

with

Nb

GB

seg

reg

ation

GB

pla

ne

Tra

ce

analy

sis

zste

reolo

gic

alm

od

el

The

am

ount

of

seg

reg

ate

dN

bis

invers

ely

pro

port

ional

toth

efr

eq

uency

of

GB

s;

Nb

seem

sto

flatt

en

the

GB

energ

yd

istr

ibution

Pang

and

Wynb

latt

,2006

0. 6

C–1. 5

Si–

1. 5

Mn

ste

el

Auste

nite

into

bain

ite

Str

aig

ht

inte

rfaces

of

lath

gro

up

sTra

ce

analy

sis

znorm

alis

ing

66%

of

traces

at

,10u

from

,110

.p

roje

ction

onto

sam

ple

surf

ace

(50%

for

rand

om

lyoriente

dp

lanes)

Cab

us,

2005



Tab

le31

Mo

dellin

gp

hase

geo

metr

yu

sin

gE

BS

Dd

ata

Ph

ysic

al

ph

en

om

en

on

of

inte

rest

Mate

rial

Mo

del

Use

of

or

co

mp

ari

so

nw

ith

EB

SD

data

Ref.

Hete

roep

itaxy

ZrO

2/Y

2O

3onto

Al 2

O3

Coin

cid

ence

site

latt

ice

bound

aries

More

OR

sp

red

icte

dth

an

those

ob

serv

ed

by

EB

SD

Cain

and

Lang

e,

1994;

Cain

et

al.,

1995

Directionalsolid

ific

ation

CM

SX

–4

and

CM

186LC

Ni

base

sup

era

lloys

Coin

cid

ence

site

latt

ice

bound

aries

With

the

ob

serv

ed

,001

.fib

rete

xtu

re,

not

all

pre

dic

ted

coin

cid

ence

site

latt

ice

bound

aries

are

ob

serv

ed

Ard

akaniet

al.,

2000

Fre

esurf

ace

energ

yS

rTiO

3In

terp

reta

tion

of

results

of

ato

mic

forc

em

icro

scop

yR

esults

were

coup

led

toE

BS

Dcry

sta

lorienta

tion

data

tod

ete

rmin

eanis

otr

op

icfr

ee

surf

ace

energ

yS

ano

et

al.,

2003a

Solid

sta

tesp

read

ing

Cop

per

onto

cop

per

Em

bed

ded

ato

mm

od

el

For

tim

es

up

to30

ps,

the

mod

elw

ork

sw

ell

for

morp

holo

gy

of

phases,

but

not

with

cry

sta

lalig

nm

ent

ob

serv

ed

by

EB

SD

Read

et

al.,

2004

Rela

tive

HA

Benerg

yN

irich

NiA

lE

mb

ed

ded

ato

mm

od

el

EB

SD

zscannin

gp

rob

em

icro

scop

yg

ive

valu

es

of

0. 2

up

to1. 1

;th

em

od

elg

ives

0. 3

up

to0. 9

Am

ouyalet

al.,

2005

GB

netw

ork

No

part

icula

rm

ate

rial

Geom

etr

yof

GB

netw

ork

How

toextr

act

the

rand

om

GB

netw

ork

from

EB

SD

data

Kin

get

al.,

2000

GB

wett

ing

and

finite

siz

escalin

gG

ain

Zn

Latt

ice

mod

elfo

rsam

plin

geff

ects

sim

ilar

toth

ose

of

EB

SD

measure

ments

Eff

ect

of

sam

ple

wid

thon

the

dep

thof

inte

rgra

nula

rin

vasio

nof

Zn

by

Ga

Tra

skin

eet

al.,

2005

Variant

sele

ction

Bain

ite

inste

els

Cro

ss-s

ection

eff

ects

on

textu

red

ete

rmin

ation

(i.e

.p

seud

ovariant

sele

ction)

Even

while

takin

gp

seud

ovariant

sele

ction

into

account,

avera

ge

textu

res

still

show

variant

sele

ction

Cab

us,

2005

Directionalsolid

ific

ation

Ni–

Cr–

Co–Ti–

Al–

Mo–S

isup

era

lloy

Eff

ect

of

textu

restr

eng

thenin

gon

gra

inclu

ste

ring

EB

SD

measure

dg

rain

clu

ste

ring

ag

rees

with

geom

etr

iceff

ects

ind

uced

by

textu

restr

eng

thenin

gW

est

and

Ad

am

s,

1997

Tab

le32

Co

up

lin

gE

BS

Dd

ata

wit

hh

eat/

flu

idfl

ow

calc

ula

tio

ns

Ph

ysic

al

ph

en

om

en

on

of

inte

rest

Mate

rials

an

dp

rocesses

Mo

del

Use

of

EB

SD

data

Ref.

Menis

cus

shap

eS

lab

casting

of

ultra

low

carb

on

ste

els

Bic

kerm

an

(analy

tical)

fluid

flow

eq

uations

The

actu

alshap

eof

frozen

menis

cus

dete

rmin

ed

with

EB

SD

ag

rees

with

mod

eloutp

ut

Seng

up

taet

al.,

2006

Direction

of

dend

rite

gro

wth

Tw

inro

llcasting

of

Fe–3S

i3D

dend

ritic

gro

wth

with

sim

plif

ied

geom

etr

y,

takin

gfluid

flow

into

account

EB

SD

dete

rmin

ed

density

of

nucle

iin

chill

zone

isa

mod

elin

put;

the

dend

rite

gro

wth

direction

(mod

eloutp

ut)

com

pare

sw

ell

with

that

measure

dw

ith

EB

SD

Takata

niet

al.,

2000

Form

ation

of

feath

ery

gra

ins

during

solid

ific

ation

Direct

chill

casting

of

AA

1050

alu

min

ium

allo

yin

gots

Flu

idflow

inm

ould

:eff

ect

of

fluid

convection

Localm

icro

textu

rep

red

icte

db

yth

em

od

elis

com

pare

dto

EB

SD

data

Henry

et

al.,

2004

Com

petitive

gra

ing

row

thd

uring

solid

ific

ation

Directionalsolid

ific

ation

of

IN738LC

,IN

718

and

sin

gle

cry

sta

lnic

kelb

ase

sup

era

lloys,

solid

ific

ation

of

Zn

(hot

dip

galv

anis

ing

)

Heat

transfe

r,d

end

rite

or

gra

ing

row

th(c

ellu

lar

auto

mato

nz

finite

ele

ment

analy

sis

),coup

led

or

not

with

tem

pera

ture

calc

ula

tions

Pre

dic

ted

localte

xtu

re,

gra

insiz

eand

shap

eare

com

pare

dw

ith

EB

SD

data

for

pro

cess

op

tim

isation

Kerm

anp

ur

et

al.,

2000;

Cart

er

et

al.,

2000;

Sem

oro

zet

al.,

2002b

;N

ew

ell

et

al.,

2005;

Xu

et

al.,

2002a

and

2002b

Colu

mnar

toeq

uia

xed

transitio

nand

str

ay

gra

info

rmation

insolid

ific

ation

Weld

ing

and

laser

meta

lfo

rmin

gof

nic

kelb

ased

sup

era

lloys;

hot

dip

galv

anis

ation

with

Zn

allo

y

Sim

plif

ied

therm

alm

od

el(e

.g.

Rosenth

al

eq

uations

for

weld

ing

)g

ives

coolin

gra

teand

tem

pera

ture

gra

die

nt;

akin

etic

mod

elis

used

inp

ost-

pro

cessin

gcalc

ula

tions

Density

of

nucle

i(inp

ut

for

the

mod

el);

the

pre

dic

ted

volu

me

fraction

of

eq

uia

xed

gra

ins

iscom

pare

dto

EB

SD

ob

serv

ations

Gaum

ann

et

al.,

2001;

Vitek

et

al.,

2004;

Quirog

aet

al.,

2004



Kurz, 1997). Agglomeration of silicon particles in semi-solid Al–Si alloy evidenced by EBSD investigations wasalso suggested by the failure of a liquid film migrationmodel to fit experimental data (Hogg and Atkinson,2005).

Modelling local crystallography and variant selection

Crystallographic models of ORs have been only scarcelyused together with EBSD data, except for counting thenumber of possible variants or calculating the MRsbetween variants (for instance, the present author foundat least 11 EBSD related papers with detailed descrip-tion of MRs between variants for KS or NW ORs).

Phenomenological theories of martensite crystallogra-phy are widely used to describe crystallographic featuressuch as ORs, habit planes and macroscopic transfor-mation eigenstrains. The traditional way to comparepredictions with experiment is TEM investigation of thinfoils, but EBSD may provide statistically significantdatasets for both ORs and (if coupled with surfaceanalysis techniques such as near field microscopy)transformation eigenstrains. EBSD is much less suitedto habit plane determination unless ‘habit’ planes aredefined by straight interphase interfaces (and may not be‘true’ habit planes). Predictions of PTMCs have beencompared with EBSD measurements for habit planes ofa’’ phase in titanium based b-Cez alloy (in fact EBSDresults suggest that the highest value of lattice invariantshear should be taken) (Zimmermann and Humbert,2002). ‘Habit planes’ close to {223} or {557} austeniteplanes were found for groups of upper bainite laths in asimulated HAZ of low carbon steel (Lambert-Perladeet al., 2004a). Both a Pitsch type OR and a macro-scopic shear eigenstrain of 0.20 were determined in Cu–39.3 at.-%Zn (from bcc b to fcc a bainite, treated as 9Rmartensite in the PTMC) (Marukawa et al., 2000), aswere habit plane and transformation eigenstrain deter-mined in Ti–9 wt-%Mo alloy (from bcc b into orthor-hombic a’’ phase) (Guo et al., 2000). The OR versuslattice invariant shear mechanism was discussed inlenticular a’ martensite of Fe–32.85 wt-%Ni (Shibataet al., 2005).

Coupled use of EBSD results and modelling generallyaims at accounting for variant selection in solid statephase transformations. Various criteria have beendeveloped to model how a limited number of variantsappear under certain conditions due to local stress orstrain fields.

In the active slip model, common plane and directionbetween parent and product phases should describe theslip system (of perfect or even partial dislocations) ofhighest Schmid factor. This local Schmid factor isgenerally calculated using the applied loading witheither a Sachs assumption (homogeneous stress in thematerial) or a more or less constrained Taylor assump-tion (homogeneous strain in the material) (Table 33).Active slip models give general trends and often showlimited agreement with experiments, as local stress andstrain fields in polycrystalline materials strongly varyfrom one grain to another, especially at grain bound-aries where nucleation often occurs.

Another criterion is the total eigenstrain calculated forthe simultaneous formation of at least two variants. Thiscriterion is used to describe self-accommodation by localvariant selection within the parent grain. Very goodagreement was found between groups of variants T

ab

le33

Pre

dic

tio

ns

of

acti

ve

sli

pm

od

els

for

vari

an

tsele

cti

on

co

mp

are

dw

ith

EB

SD

exp

eri

men

tal

resu

lts

Mate

rial

Tra

nsfo

rmati

on

co

nd

itio

ns

OR

Slip

syste

msz

localis

ati

on

assu

mp

tio

nC

rite

rio

nR

esu

lts

Ref.

Ti–

6A

l–4V

bcc

bin

tohcp

aaft

er

com

pre

ssio

nB

urg

ers

{110},

111

.b

and

{112},

111

.bz

Sachs

Maxim

um

resolv

ed

shear

str

ess

Qualit

ative

ag

reem

ent

with

exp

erim

enta

lavera

ge

textu

reM

ousta

hfid

et

al.,

1997b

Cu–A

l–B

eallo

yb

1auste

nite

into

mart

ensite

(tensio

n)

24

variants

(OR

not

sp

ecifie

d)

Localstr

esses

from

ela

stic

str

ain

sm

easure

db

yX

RD

;slip

syste

ms

not

sp

ecifie

dS

chm

idfa

cto

rS

mall

valu

es

of

crite

rion

lead

tono

phase

transfo

rmation

Kaouache

et

al.,

2004

Fe–32

at.

-%N

ib

icry

sta

lsfc

causte

nite

into

lenticula

rb

cc

mart

ensite

(tensio

n)

NW

(24

coup

les

of

variantz

hab

itp

lane)

Macro

scop

icshear

direction

and

hab

itp

lane

norm

al

Min

imum

constr

ain

ed

macro

scop

icstr

ain

at

GB

Ag

reem

ent

with

exp

erim

ent

on

identity

of

sele

cte

dvariants

Ued

aet

al.,

2001a

Ste

elw

ith

bain

itez

reta

ined

auste

nite

fcc

auste

nite

(c)

into

bcc

bain

itic

ferr

ite;

hot

rolli

ng

red

uction

of

0. 2

at

750uC

Near

KS

{111},

110

.c,

fully

constr

ain

ed

Taylo

rm

od

el

Schm

idfa

cto

rFeasib

ility

dem

onstr

ate

d,

pro

mis

ing

results

God

et

et

al.,

2001

0. 6

Cb

ain

itic

ste

el

fcc

auste

nite

(c)

into

bcc

bain

itic

ferr

ite;

channeld

iecom

pre

ssio

nz

ste

pq

uenchin

g

Uniq

ue,

clo

se

toK

Sand

NW

{111},

110

.c,

fully

constr

ain

ed

Taylo

rand

Sachs

mod

els

Com

mon

clo

se-p

acked

pla

nes

para

llelto

pla

nes

of

activate

dslip

syste

ms

Only

part

ialag

reem

ent

with

exp

erim

ent

Cab

us

et

al.,

2004a

Low

allo

yTR

IPaid

ed

bain

itic

ste

el

fcc

auste

nite

(c)

into

bcc

bain

itic

ferr

ite;

25–50%

red

uction

by

hot

rolli

ng

at

750uC

NW

,K

S{1

11},

110

.cz

corr

esp

ond

ing

Shockle

yp

art

ial

dis

locations;

Taylo

rm

od

el

Maxim

um

resolv

ed

shear

str

ess

‘Positiv

e’and

‘neg

ative’slip

variants

are

accounte

dfo

rb

ysp

read

ing

ab

out

cert

ain

NW

variants

Jonas

et

al.,

2005

Low

allo

yand

hig

hM

nTR

IPaid

ed

ste

els

fcc

auste

nite

(c)

into

bod

ycentr

ed

tetr

ag

onalor

hcp

mart

ensite

und

er

tensio

n

KS

and

Burg

ers

resp

ectively

{111},

110

.c,

Sachs

Assum

ption

Com

mon

clo

se

packed

pla

nes

para

llelto

pla

nes

of

activate

dslip

syste

ms

Good

ag

reem

ent

with

exp

erim

ent

on

identity

of

sele

cte

dvariants

God

et

et

al.,

2005



minimising the total eigenstrain (calculated with aPTMC) and groups actually found with EBSD in spearlike martensite of Cu–7.3Al–8.5 wt-%Mn (Wang et al.,2002), in plate martensite at a symmetrical 180u,211.

tilt boundary of a Fe–32 at.-%Ni bicrystal (Ueda et al.,2003a), in groups of three variants of hcp a phase intitanium (Wang et al., 2003). By contrast, lath marten-site subblocks evidenced with EBSD in Fe–C alloys werenot efficient self-accommodating structures according tothis criterion (Morito et al., 2003). Accommodation oflarge strains imposed by hot rolling was found to takeplace by variant selection in a low carbon bainitic steel(Matsuoka et al., 1999); however, in that study thelattice Bain strain was surprisingly chosen as thetransformation eigenstrain.

More complex criteria for strain accommodationwithin a given parent grain involve elastic interactionenergy calculated with the transformation eigenstrain(or more surprisingly lattice Bain strains in some cases)associated with candidate variants. Consistent resultsbetween observed variants and negative interactionenergy were found in austenitic AISI 301 austeniticstainless steel in tension and in compression, under theSachs assumption (Lee et al., 2005). By using a thres-hold value for the interaction energy criterion, goodaverage texture predictions were obtained for compactstrip processed high strength low alloy steel by usinganisotropic elasticity of phases and either the latticeBain strain (Humbert et al., 2002b) or the macroscopictransformation eigenstrain (Humbert et al., 2002a). InFe–32 at.-%Ni bicrystals, the interaction energy termcan be overwhelmed by the necessity for strain com-patibility at the GB according to the particular GBmisorientation (Ueda et al., 2001b and 2003a).

Coupled effects of transformation eigenstrain andphase geometry have been taken into account bymodelling local stress and strain fields based on theEshelby inclusion problem. The matrix is generallytaken to be the parent phase with isotropic oranisotropic elastic–plastic properties. Variants are mod-elled as oblate ellipsoids extending along their macro-scopic ‘habit’ plane. Mechanical coupling betweenphases is achieved under self-consistency assumptions.The model outputs are the interaction strain energy, andsometimes also the plastic strain in the parent phase as afunction of candidate variants. Such calculations werecompared to variant selection experimentally evidencedwith EBSD to account for the identity of variants instress free materials and as a function of applied stressfor, e.g. martensite formation in carburised steels(Karaman et al., 1998), for microtexture of upperbainite packets in low carbon steel HAZ (Gourgues,2003; Lambert-Perlade et al., 2004a) and for averagetexture affected by variant selection in Zircaloy–4 alloy(Humbert and Gey, 2003). There is still much to do inthis field, in particular to get accurate data on theconstitutive behaviour of phases under such extremeconditions (e.g. elevated temperature, possibly high localstrain rates and high strains). 3D EBSD coupled withlocal measurements of phase property (Zhao, 2006)could be a promising way to further improve thesemodels.

Modelling average transformation textures

The prediction of average transformation textures is ofutmost importance to infer product properties from

processing conditions. A lot of work has been carriedout in this field using EBSD data either alone or togetherwith XRD data (Table 34). Most studies in this fieldconcentrate either on variant selection effects on averagetexture or on accuracy of quantitative texture predic-tion. However, the texture of the parent phase isgenerally difficult to assess, even if some phase isretained, unless specific calculation methods are usedto retrieve it (see section on average textures in solidstate phase transformations).

Modelling resulting properties

In service properties of transformed microstructuresmay be tentatively predicted using EBSD data aboutmicrotexture, macrotexture and morphology of indivi-dual phases together with homogenisation models tocalculate ‘average’ or ‘macroscopic’ properties. Thesimplest homogenisation model used is the rule ofmixtures, which successfully predicted, e.g. the compres-sion peak stress of eutectic Al2O3–YAG–ZrO2 rods as afunction of the texture of individual phases (Murayamaet al., 2004b). More complex microtextures may inducefailure of this model to account for experimentalmeasurements, e.g. in wrought duplex stainless steels,where areas maintaining the KS OR between bothphases behave as ‘hard’ particles in a much softer matrix(Iza-Mendia et al., 1998).

More advanced micromechanical models have alsobeen used to predict yield properties of heterogeneousmaterials such as columnar and equiaxed zones of Ti–6Al–4V ingots under Taylor assumption and withcrystal plasticity models (Glavicic et al., 2003c and2004a). Local stresses arising from upset forging of Ti–6Al–4V were also calculated with a finite elementmethod, allowing local Taylor factors to be calculatedthanks to a simple micromechanical model (Bieler et al.,2005b) and cavity initiation sites to be related to localcrystal orientation and spheroidisation mechanisms(Bieler and Semiatin 2002, Bieler et al., 2005a and2005b). Micromechanical models of crystal plasticityhave been used to assess strain localisation in bainiticand martensitic microstructures of A508Cl.3 low alloysteel under tension (Sekfali et al., 2002) and yield andfracture properties of cast and aged duplex stainlesssteels (Bugat et al., 2001). In the two latter cases, localmeasurements of surface strains together with EBSDmapping of initial state were used to mesh the ‘actual’surface microstructure and to compare experimentalmeasurements of strains with model predictions. TheOR between parent and product phases, and MRbetween product variants play a key role in both sliplocalisation and cleavage cracking properties. Moresimply, the crystallographic packet size, which is theunit crack path for cleavage microcracking could also beused with a Hall–Petch type equation to predict thefracture toughness of low carbon acicular ferrite steels asa function of the packet size (Dıaz-Fuentes et al., 2003).It was also quantitatively used to predict fracturetoughness of a bainitic steel HAZ microstructure(Lambert-Perlade et al., 2004b). A local micromechani-cal model was used together with a transformationinduced superplasticity model to predict the evolution ofTi–6Al–4V/TiBw composite tensile loaded during ther-mal cycling around the matrix transformation tempera-tures (Schuh and Dunand, 2001).



Tab

le34

Mo

dellin

gavera

ge

tran

sfo

rmati

on

textu

res

usin

gd

ata

gen

era

ted

wit

hE

BS

D

Mate

rial

Ph

ase

tran

sfo

rmati

on

Exp

eri

men

tal

data

Mo

del

Resu

lts

Ref.

Hig

hp

urity

iron

fcc

cin

tob

cc

aA

vera

ge

textu

re(b

oth

EB

SD

and

XR

D)

Sta

rtin

gfr

om

cte

xtu

re,

24

KS

variants

,no

variant

sele

ction

There

are

mis

sin

gvariants

inexp

erim

enta

lvers

us

pre

dic

ted

OD

F,

att

rib

ute

dto

gra

ing

row

thb

ut

not

tovariant

sele

ction

Ab

iko

et

al.,

2000

Low

carb

on

ste

el

bcc

ain

tofc

cc

Avera

ge

textu

reof

aand

caft

er

heat

treatm

ent

Sta

rtin

gfr

om

ate

xtu

re,

24

KS

variants

,no

variant

sele

ction

One

textu

recom

ponent

exp

erim

enta

llym

issin

g,

anoth

er

too

str

ong

vers

us

pre

dic

tions,

thus

there

isvariant

sele

ction

Park

et

al.,

2002

Low

carb

on

ste

el

fcc

cin

tob

cc

aA

vera

ge

textu

reS

tart

ing

from

typ

icalte

xtu

recom

ponents

of

defo

rmed

c,24

KS

variants

,no

variant

sele

ction

The

ap

hase

nucle

ate

sfr

om

defo

rmed

(not

recry

sta

llised

)c

Hurley

and

Hod

gson,

2001

Low

carb

on

ste

els

bcc

ain

tofc

cc

back

into

aE

BS

D:

gra

instr

uctu

re;

XR

D:

avera

ge

textu

reS

tart

ing

from

ate

xtu

re,

12

NW

variants

Pre

dic

tions

consis

tent

with

exp

erim

ent

for

one

ste

el,

insuff

icie

nt

textu

rem

em

ory

pre

dic

ted

for

two

oth

er

ste

els

Ryd

eet

al.,

1999

Low

carb

on

ste

el

bcc

ain

tofc

cc

EB

SD

:O

R;

XR

Dand

neutr

on

diffr

action:

avera

ge

textu

reS

tart

ing

from

cte

xtu

re,

24

KS

variants

;variant

sele

ction:

assum

ing

rolli

ng

str

ain

and

Taylo

rhyp

oth

esis

,b

oth

active

slip

and

transfo

rmation

work

crite

ria

were

teste

d

Mod

elp

red

ictions

consis

tent

with

exp

erim

ent

only

ifb

oth

crite

ria

are

com

bin

ed

Bru

ckner

and

Gott

ste

in,

2001

HS

LA*

ste

el(c

om

pact

str

ipp

rod

uction)

fcc

cin

tob

cc

aE

BS

D:

OR

;X

RD

:avera

ge

textu

reof

aand

reta

ined

cS

tart

ing

from

cte

xtu

re,

12

NW

variants

;variant

sele

ction:

ela

stic

str

ain

energ

y(B

ain

str

ain

or

macro

scop

ictr

ansfo

rmation

eig

enstr

ain

)

Possib

levariant

sele

ction:

pre

dic

ted

textu

res

are

sharp

er

than

exp

erim

enta

lones

Hum

bert

et

al.,

2002a

and

2002b

Low

allo

yTR

IPste

el

fcc

cin

tob

ain

itic

bcc

aE

BS

D:

OD

Fs

for

aand

reta

ined

c;X

RD

:volu

me

fraction

of

c

Thre

eB

ain

,12

NW

or

24

KS

variants

,no

variant

sele

ction

Pre

dic

ted

textu

rew

ith

rig

ht

com

ponents

but

too

weak

vers

us

exp

erim

ent

De

Meyer

et

al.,

2001

Dualp

hase

ste

el

fcc

cin

tob

cc

a,

here

both

prim

ary

a,

bain

itic

aand

mart

ensite

EB

SD

:in

div

idualO

DF

of

pro

duct

phases;

XR

D:

textu

reof

reta

ined

c

Sta

rtin

gfr

om

various

cte

xtu

res,

thre

eB

ain

variants

,no

variant

sele

ction

Prim

ary

afo

rms

from

defo

rmed

c;b

ain

ite

and

mart

ensite

pre

fera

bly

form

from

recry

sta

llised

cH

utc

hin

son

et

al.,

1998;

Wate

rschoot

et

al.,

2002

Low

carb

on

mic

roallo

yed

ste

el

fcc

cin

top

rim

ary

and

bain

itic

bcc

aE

BS

D:

ind

ivid

ualO

DFs

of

pro

duct

phases;

XR

D:

Sta

rtin

gfr

om

various

cte

xtu

res;

24

KS

variants

;no

variant

sele

ction

Prim

ary

and

bain

itic

afo

rmfr

om

defo

rmed

c;re

tain

ed

cis

part

ially

recry

sta

llised

Mesp

lont

and

De

Coom

an,

2003

0. 3

C–9N

iste

el

bcc

ain

tofc

cc

into

near-

bcc

a’m

art

ensite

EB

SD

:O

DF,

mic

rostr

uctu

reand

mic

rote

xtu

re;

XR

D:

avera

ge

textu

re

Sta

rtin

gfr

om

various

cte

xtu

recom

ponents

;24

KS

variants

,no

variant

sele

ction

Mod

elp

red

ictions

are

consis

tent

with

exp

erim

ent:

no

variant

sele

ction

Yokota

et

al.,

2005

AIS

I304

sta

inle

ss

ste

el

fcc

cin

tohcp

eand

near

bcc

a’m

art

ensite

EB

SD

:lo

cald

efo

rmation

mechanis

ms

(inclu

din

gp

hase

transfo

rmation);

XR

D:

volu

me

fraction

of

phases

and

avera

ge

textu

reof

auste

nite

Sta

rtin

gfr

om

exp

erim

enta

lc

textu

re;

24

variants

ded

uced

from

aP

TM

C,

coup

led

variant

sele

ction

and

cry

sta

lp

lasticity

of

auste

nite,

localis

ation

rule

by

aself-c

onsis

tent

schem

efo

rth

eauste

nite

poly

cry

sta

l

Mod

elp

red

ictions

are

part

ially

consis

tent

with

exp

erim

ent

concern

ing

the

orienta

tion

of

auste

nite

gra

ins

that

transfo

rmfirs

t;d

esp

ite

that

the

mod

elis

not

yet

ab

leto

take

em

art

ensite

into

account

Petit

et

al.,

2006



Coupling EBSD with other advanced techniques:a summaryThe following key issues should be considered in thenext future.

Think in 3D

Not only should experimental techniques be furtherdeveloped, but models should be improved, inasmuch asthey are frequently based on 2D assumptions about, forexample, the morphology of newly formed phases andthe determination of nucleation sites from 2D observa-tions. Crystal connectivity should be necessarily con-sidered from a 3D point of view. Phenomena such asvariant selection should include 3D considerations, todifferentiate ‘true’ variant selection from stereologyartefacts. In situ investigations are still in progress,to be combined with 3D considerations as detailedabove.

Model improvements

Micromechanical modelling of phase transformationsis a favourite frame to use EBSD data combiningcrystallographic and spatial information. However, themost advanced micromechanical models are not oftenused together with EBSD. As an example, PTMCsare often used with approximations on mechanical pro-perties (e.g. stiffness, strength, strain rate and tempera-ture effects) of parent and product phases. They areoften used as if they were descriptive, although theyare phenomenological in nature. On the other hand,localisation and homogenisation rules used in multi-scale modelling of resulting properties could also beimproved.

Concluding remarksAn exponential increase continues in the number ofpublished papers on application of EBSD to phasetransformations, a topic that is still developing rapidly.From ‘revisiting’ a number of features of phasetransformations, EBSD has progressed and now pro-vides original results in a number of specific areas. Asfor other topics related to EBSD, a careful literaturereview is required before starting a new study. The vastmajority of the literature is devoted to metallicmaterials; promising results already exist for ceramicsdespite experimental difficulties. It would be interestingto cross-reference what is commonly found with metallicand ceramic materials.

Electron backscatter diffraction is now a maturetechnique. It is easy to use (except for minerals or for 3Dinvestigations), although handling the amount of dataproduced by 2D or 3D EBSD mapping is increasinglydifficult. Coupling EBSD with in situ investigations,local property measurement and advanced modelling isnow required to get deeper insight into phase transfor-mation mechanisms.

The development of high speed systems and com-puter aided volume reconstruction techniques stronglysuggests that many results on phase transformationcrystallography and mechanisms should be revisitedusing 3D characterisation of partially or fully trans-formed microstructures, which provide input datafor process optimisation and prediction of productproperties.T

ab

le34

Co

nti

nu

ed

Mate

rial

Ph

ase

tran

sfo

rmati

on

Exp

eri

men

tal

data

Mo

del

Resu

lts

Ref.

Ti–

6A

l–4V

bcc

bin

tohcp

aE

BS

Dand

XR

D:

avera

ge

textu

reS

tart

ing

from

bte

xtu

re;

Burg

ers

variants

Ag

reem

ent

with

exp

erim

ent

dep

end

son

bor

(az

b)

initia

lsta

teand

bd

efo

rmation

sta

teb

efo

rep

hase

transfo

rmation

Hum

bert

et

al.,

1994;

Gey

et

al.,

1996;

Mousta

hfid

et

al.,

1997a;

Sta

nfo

rdand

Bate

,2004

Ti

hcp

ain

tob

cc

bE

BS

D:

avera

ge

textu

res

Sta

rtin

gfr

om

ate

xtu

re;

Burg

ers

variants

One

com

ponent

und

ere

stim

ate

din

the

mod

el,

due

tog

row

thof

ballo

trio

morp

hs

Sew

ard

et

al.,

2004

IMI8

34

Tiallo

yb

cc

bin

tohcp

aE

BS

D:

avera

ge

textu

res

Sta

rtin

gfr

om

bte

xtu

re;

Burg

ers

variants

with

or

without

ela

stic

energ

ycrite

rion

based

on

the

Bain

str

ain

{0001} a

and

{110} b

pole

fig

ure

sare

sig

nific

antly

diffe

rent:

there

isvariant

sele

ction;

accounte

dfo

rb

yth

eela

stic

energ

ycrite

rion

Germ

ain

et

al.,

2005b

;H

um

bert

et

al.,

2006

Cu–40Z

nb

cc

bin

tocolo

nie

sof

fcc

aE

BS

D:

mic

rote

xtu

re;

XR

D:

avera

ge

textu

reC

ontr

ibution

of

Bain

str

ain

tore

duction

inre

sid

ualstr

esses

from

rolli

ng

The

rig

ht

Bain

zone

isp

red

icte

db

yth

em

od

el

Yasud

aet

al.,

1999

Ni–

(36–38)

at.

-%A

lB

2b

(ind

exed

as

bcc)

into

L1

2c’

aft

er

hot

com

pre

ssio

nE

BS

D:

avera

ge

textu

reS

tart

ing

from

bte

xtu

re,

24

KS

variants

,111

.b

fib

reg

ives

the

rig

ht

fib

res

for

the

textu

reof

c’S

akata

et

al.,

2001

*H

SLA

:hig

hstr

eng

thlo

wallo

y.



Appendix

Orientation relationshipsThe most commonly encountered ORs between phasesin solid state transformations are reported in Table 35.

Acknowledgements

Technical assistance from Mrs Odile Adam for papertracking is gratefully acknowledged. Many thanks aredue to Professor Pineau for his kind and continuoussupport to achieve the present work. The present paperis dedicated to the memory of late Professor Flower,who kindly gave me my first opportunity to makeextensive EBSD measurements in his research group atImperial College.

References1. A. Abdul Wahab, M. V. Kral: ‘Three dimensional analysis of

creep voids’, Microsc. Microanal., 2005, 11, (Suppl. 2), 224–225.

2. K. Abiko, S. Takaki, T. Yokota, S. Satoh: ‘Formation of giant

columnar grains in high-purity iron by hot-rolling’, Mater. Trans.

JIM, 2000, 41, 102–108.

3. Y. Adachi, K. Tsuzaki: ‘Coherent to incoherent transition of

intergranular bcc-precipitates by pre-/post deformations in a Ni–

43Cr alloy’, ISIJ Int., 2005, 45, 1703–1710.

4. Y. Adachi, K. Hakata, K. Tsuzaki: ‘Crystallographic analysis of

grain boundary Bcc-precipitates in a Ni–Cr alloy by FESEM/

EBSD and TEM/Kikuchi line methods’, Mater. Sci. Eng. A, 2005,

A412, 252–263.

5. E. Aernoudt, A. Walentek, M. Seefeldt, B. Verlinden, P. Van

Houtte: ‘Towards a description of complex pearlite structures’,

Z. Metallkd., 2005, 96, 1032–1037.

6. B. Alexandreanu, B. Capell, G. S. Was: ‘Combined effect of special

grain boundaries and grain boundary carbides on IGSCC of Ni–

16Cr–9Fe–xC alloys’, Mater. Sci. Eng. A, 2001, A300, 94–104.

7. M. Alper, P. S. Aplin, K. Attenborough, D. J. Dingley, R. Hart,

S. J. Lane, D. S. Lashmore, W. Schwarzacher: ‘Growth and

characterization of electrodeposited Cu/Cu–Ni–Co alloy super-

lattices’, J. Magn. Magn. Mater., 1993, 126, 8–11.

8. Y. Amouyal, E. Rabkin, Y. Mishin: ‘Correlation between grain

boundary energy and geometry in Ni-rich NiAl’, Acta Mater.,

2005, 53, 3795–3805.

9. M. G. Ardakani, N. D’Souza, B. A. Shollock, M. McLean:

‘Directional and single-crystal solidification of Ni-base super-

alloys: Part II. Coincidence site lattice character of grain

boundaries’, Metall. Mater. Trans. A, 2000, 31A, 2887–2893.

10. F. Arenas, E. Barrios, D. Field, L. Bejar: ‘Analytical electron

microscopy investigation of hard metals’, Microsc. Microanal.,

2005, 11, (Suppl. 2), 1958 (CD-ROM).

11. L. Arnberg, A. Bardal, H. Sund: ‘Agglomeration in two semisolid

type 6082 aluminium alloys’, Mater. Sci. Eng. A, 1999, A262, 300–

303.

12. O. Arnould, O. Hubert, J. Duval, F. Hild: ‘Predictive study of

aging modes of an electrodeposited Ni/Cu assembly’, Rev.

Mecamat I, 2003, 30, 33–43 (in French).

13. K. Z. Baba-Kishi, D. J. Dingley: ‘Application of backscatter

Kikuchi diffraction in the scanning electron microscope to the

study of NiS2’, J. Appl. Crystallogr., 1989, 22, 189–200.

14. K. Z. Baba-Kishi: ‘Measurement of crystal parameters on

backscatter Kikuchi diffraction patterns’, Scanning, 1998, 20,

117–127.

15. K. Z. Baba-Kishi: ‘Review: electron backscatter Kikuchi diffrac-

tion in the scanning electron microscope for crystallographic

analysis’, J. Mater. Sci., 2002, 37, 1715–1746.

16. M. R. Bache, H. M. Davies, W. J. Evans: ‘Characterisation of

hydrogen induced fracture in the titanium alloy IMI685’, Proc.

9th Int. Conf. on ‘Fracture’, (ed. B. L. Karihaloo et al.), Vol. 1,

351–358; 1997a, Oxford, Pergamon.

17. M. R. Bache, W. J. Evans, H. M. Davies: ‘Electron back scattered

diffraction (EBSD) analysis of quasi-cleavage and hydrogen

induced fractures under cyclic and dwell loading in titanium

alloys’, J. Mater. Sci., 1997b, 32, 3435–3442.

18. M. Bahgat, Y. Sasaki, S. Hijino, M. Iguchi, K. Ishii: ‘The effect of

grain boundaries on iron nucleation during wustite reduction

process’, ISIJ Int., 2004a, 44, 2023–2028.

19. M. Bahgat, Y. Sasaki, K. Ishii: ‘Correlation between surface

structure and iron nucleation in the wustite reduction’, Steel Res.

Int., 2004b, 75, 113–121.

20. M. Bahgat, Y. Sasaki, M. Iguchi, K. Ishii: ‘The effect of grain

boundaries on the surface rearrangement during wustite reduction

within its range of existence’, ISIJ Int., 2005, 45, 657–661.

21. S. C. Baik, S.-H. Park, O. Kwon, D.-I. Kim, K. H. Oh: ‘Effects of

nitrogen on the mechanical properties of cold rolled TRIP-aided

steel sheets’, ISIJ Int., 2006, 46, 599–605.

22. R. Banerjee, P. C. Collins, H. L. Fraser: ‘Phase evolution in laser-

deposited titanium–chromium’, Metall. Mater. Trans. A, 2002,

33A, 2129–2138.

23. R. Banerjee, D. Bhattacharyya, P. C. Collins, G. B. Viswanathan,

H. L. Fraser: ‘Precipitation of grain boundary a in a laser

deposited compositionally graded Ti–8Al–xV alloy – an orienta-

tion microscopy study’, Acta Mater., 2004, 52, 377–385.

24. O. M. Barabash, R. I. Barabash, S. A. David, G. E. Ice: ‘Residual

stresses, thermomechanical behavior and interfaces in the weld

joint of Ni-based superalloys’, Adv. Eng. Mater., 2006, 8, 202–205.

25. D. L. Barr, L. R. Harriott, W. L. Brown: ‘Focused ion beam

observation of grain structure and precipitates in aluminum thin

films’, J. Vac. Sci. Technol. B, 1992, B10, 3120–3125.

26. A. Bastos, S. Zaefferer, D. Raabe, C. Schuh: ‘Characterization of

the microstructure and texture of nanostructured electrodeposited

NiCo using electron backscatter diffraction (EBSD)’, Acta

Mater., 2006, 54, 2451–2462.

27. T. Baudin, J. Jura, W. Swiatnicki, M. H. Mathon, R. Penelle:

‘Multi-scale characterisation of the microstructure of a deformed,

then recrystallised austenitic–ferritic steel’, Proc. Materiaux 2002,

Table 35 Commonly encountered ORs in EBSD studies

Name and acronymCrystal structureof one phase

Crystal structure ofthe other phase Parallel planes Parallel directions

Burgers bcc hcp {011}bcc//{0001}hcp ,111.bcc//,1120.hcp

Kurdjumov–Sachs (KS) bcc fcc {011}bcc//{111}fcc ,111.bcc//,110.fcc

Nishiyama–Wassermann (NW) bcc fcc {011}bcc//{111}fcc ,011.bcc//,211.fcc

Pitsch bcc fcc {011}bcc//{001}fcc ,111.bcc//,110.fcc

Greninger–Troiano (GT) bcc fcc {011}bcc ,1u from {111}fcc Midway between KSand closest NW

Nishiyama–Wassermann (NW) fcc hcp {111}fcc//{0001}hcp ,112.fcc//,1100.hcp

Blackburn c (L10) a2 (DO19) {111}c//{0001}a2,110.c//,1120.a2

Pitsch–Petch a (bcc) c (Tetragonal Fe3C) {001}c//{215}a ,100.c 2.6u from ,311.a

and ,010.c 2.6u from,131.a

Bagaryatsky a (bcc) c (Tetragonal Fe3C) {001}c//{112}a ,100.c//,110.a and,010.c//,111.a

Pitsch c (fcc) c (Tetragonal Fe3C) ,100.c//,554.c and,010.c//,010.c and,001.c//,225.c



Tours, France, October 2002, Universite Technologique de

Belfort-Montbeliard, 4 pp. (CD-ROM) (in French).

28. H. Bei, E. P. George, E. A. Kenik, G. M. Pharr: ‘Directional

solidification and microstructures of near-eutectic Cr–Cr3Si

alloys’, Acta Mater., 2003, 51, 6241–6252.

29. H. Bei, E. P. George, E. A. Kenik, G. M. Pharr: ‘Microstructures

and mechanical properties of V–V3Si eutectic composites’,

Z. Metallkd., 2004, 95, 505–512.

30. H. Bei, E. P. George: ‘Microstructures and mechanical properties

of a directionally solidified NiAl–Mo eutectic alloy’, Acta Mater.,

2005, 53, 69–77.

31. H. Beladi, G. L. Kelly, A. Shokouhi, P. D. Hodgson: ‘The

evolution of ultrafine ferrite formation through dynamic strain-

induced transformation’, Mater. Sci. Eng. A, 2004, A371, 343–

352.

32. D. Bera, S. C. Kuiry, S. Seal: ‘Kinetics and growth mechanism of

electrodeposited palladium nanocrystallites’, J. Phys. Chem. B,

2004, B108, 556–562.

33. C. Bezencon, A. Schnell, W. Kurz: ‘Epitaxial deposition of

MCrAlY coatings on a Ni-base superalloy by laser cladding’, Scr.

Mater., 2003, 49, 705–709.

34. D. Bhattacharjee, C. L. Davis: ‘Influence of processing history on

mesotexture and microstructure–toughness relationship in con-

trol-rolled and normalised steels’, Scr. Mater., 2002, 47, 825–831.

35. A. Bhattacharyya, E. El-Danaf, S. R. Kalidindi, R. D. Doherty:

‘Evolution of grain-scale microstructure during large strain simple

compression of polycrystalline aluminum with quasi-columnar

grains: OIM measurements and numerical simulations’, Int. J.

Plast., 2001, 17, 861–883.

36. D. Bhattacharyya, G. B. Viswanathan, R. Denkenberger, D.

Furrer, H. L. Fraser: ‘The role of crystallographic and geometrical

relationships between a and b phases in a a/b titanium alloy’, Acta

Mater., 2003, 51, 4679–4691.

37. T. R. Bieler, S. L. Semiatin: ‘The origins of heterogeneous

deformation during primary hot working of Ti–6Al–4V’, Int. J.

Plast., 2002, 18, 1165–1189.

38. T. Bieler, R. L. Goetz, S. L. Semiatin: ‘Anisotropic plasticity and

cavity growth during upset forging of Ti–6Al–4V’, Mater. Sci.

Eng. A, 2005a, A405, 201–213.

39. T. R. Bieler, P. D. Nicolaou, S. L. Semiatin: ‘An experimental and

theoretical investigation of the effect of local colony orientations

and misorientation on cavitation during hot working of Ti–6Al–

4V’, Metall. Mater. Trans. A, 2005b, 36A, 129–140.

40. J. F. Bingert, R. J. Hanrahan, Jr, R. D. Field, P. O. Dickerson:

‘Microtextural investigation of hydrided a-uranium’, J. Alloy.

Compd., 2004, 365, 138–148.

41. S. Birosca, R. L. Higginson: ‘Study of scale growth on steel

substrates using electron back scatter diffraction’, Mater. Sci.

Forum, 2003, 426–432, 3611–3616.

42. S. Birosca, D. Dingley, R. L. Higginson: ‘Microstructural and

microtextural characterization of oxide scale on steel using

electron backscatter diffraction’, J. Microsc., 2004, 213, 235–240.

43. E. Bischoff, V. Semenov, E. Rabkin, W. Gust: ‘Determination of

the grain boundary misorientation for the analysis of the

discontinuous ordering reactions in Fe–50at.%Co’, Mater. Sci.

Forum, 1998, 273–275, 243–248.

44. C. J. Boehlert, J. F. Bingert: ‘Microstructure, tensile, and creep

behavior of O z BCC Ti2AlNb alloys processed using induction-

float-zone melting’, J. Mater. Process. Technol., 2001, 117, 400–

408.

45. C. J. Boehlert, R. K. Schulze, J. N. Mitchell, T. G. Zocco, R. A.

Pereyra: ‘Initial electron backscattered diffraction observations of

a plutonium alloy’, Scr. Mater., 2001, 45, 1107–1115.

46. C. J. Boehlert, J. D. Farr, R. K. Schulze, R. A. Pereyra, J. A.

Archuleta: ‘Initial electron back-scattered diffraction observations

of cerium’, Philos. Mag., 2003a, 83, 1735–1744.

47. C. J. Boehlert, T. G. Zocco, R. K. Schulze, J. N. Mitchell, R. A.

Pereyra: ‘Electron backscatter diffraction of a plutonium–gallium

alloy’, J. Nucl. Mater., 2003b, 312, 67–75.

48. C. J. Boehlert, S. Civelekoglu, R. C. Gundakaram, J. F. Bingert:

‘The grain boundary character distribution in BCC and OzBCC

Ti–Al–Nb alloy microstructures’, Proc. 10th World Conf. on

‘Titanium’, (ed. G. Lutjering, J. Albrecht), Vol. 4, 2145–2152;

2004, Weinheim, Wiley-VCH.

49. W. J. Boettinger, M. D. Vaudin, M. E. Williams, L. A. Bendersky,

W. R. Wagner: ‘Electron backscattered diffraction and energy

dispersive X-ray spectroscopy study of the phase NiSn4’,

J. Electron. Mater., 2003, 32, 511–515.

50. G. Bouche, J. L. Bechade, M. H. Mathon, L. Allais, A. F.

Gourgues, L. Naze: ‘Texture of welded joints of 316L stainless

steel, multi-scale orientation analysis of a weld metal deposit’,

J. Nucl. Mater., 2000, 277, 91–98.

51. E. Bouyne, H. M. Flower, T. C. Lindley, A. Pineau: ‘Use of

EBSD technique to examine microstructure and cracking in a

bainitic steel’, Scr. Mater., 1998, 39, 295–300.

52. A. Bowles, K. Nogita, M. Dargush, C. Davidson, J. Griffiths:

‘Grain size measurements in Mg–Al high pressure die castings

using electron back-scattered diffraction (EBSD)’, Mater. Trans.,

2004, 45, 3114–3119.

53. D. Bradai, P. Zieba, E. Bischoff, W. Gust: ‘Correlation between

grain boundary misorientation and the discontinuous precipita-

tion reaction in Mg–10wt.% Al alloy’, Mater. Chem. Phys., 2002,

78, 222–226.

54. A. P. Bramley, A. J. Wilkinson, A. P. Jenkins, C. R. M.

Grosvenor: ‘Microstructural studies of Tl2Ba2Ca2Cu3Ox thin

films on LaAlO3 and MgO substrates’, J. Supercond., 1998, 11,

71–72.

55. L. N. Brewer, V. P. Dravid, M. Velazquez, A. Revcolevschi: ‘Solid

solution directionally solidified eutectic oxide composites: Part II.

Co1–xNixO single crystal growth and characterization’, J. Mater.

Res., 2002, 17, 768–773.

56. L. N. Brewer, M. A. Othon, L. M. Young, T. M. Angeliu:

‘Misorientation mapping for visualization of plastic deformation

via electron back-scattered diffraction’, Microsc. Microanal.,

2006, 12, 85–91.

57. V. Brien, V. Khare, F. Herbst, P. Weisbecker, J.-B. Ledeuil, M. C.

de Weerd, F. Machizaud, J.-M. Dubois: ‘Influence of boron

content on the microstructure of sintered Al62.5–xCu25.3Fe12.2Bx

alloys (x50, 3, 5)’, J. Mater. Res., 2004, 19, 2974–2980.

58. J. A. Brooks, C. V. Robino, T. J. Headley, J. R. Michael: ‘Weld

solidification and cracking behavior of free-machining stainless

steel’, Weld. J., 2003, 82, 51S–64S.

59. G. Bruckner, A. Kontges, G. Gottstein: ‘Microstructure and

texture development during the phase transformation in an Fe–

Ni–Co–Ti shape memory alloy’, Steel Res., 1999, 70, 188–192.

60. G. Bruckner, J. Pospiech, I. Seidl, G. Gottstein: ‘Orientation

correlation during diffusional aRc phase transformation in a

ferritic low carbon steel’, Scr. Mater., 2001, 44, 2635–2640.

61. G. Bruckner, G. Gottstein: ‘Transformation textures during

diffusional aRcRa phase transformations in ferritic steels’, ISIJ

Int., 2001, 41, 468–477.

62. T. E. Buchheit, D. A. Lavan, J. R. Michael, T. D. Christenson,

S. D. Leith: ‘Microstructural and mechanical properties investiga-

tion of electrodeposited and annealed LIGA nickel structures’,

Metall. Mater. Trans. A, 2002, 33A, 539–554.

63. J. Y. Buffiere, S. Savelli, P. H. Jouneau, E. Maire, R. Fougeres:

‘Experimental study of porosity and its relation to fatigue

mechanisms of model Al–Si7–Mg0.3 cast Al alloys’, Mater. Sci.

Eng. A, 2001, A316, 115–126.

64. S. Bugat, J. Besson, A.-F. Gourgues, F. N’Guyen, A. Pineau:

‘Microstructure and damage initiation in duplex stainless steels’,

Mater. Sci. Eng. A, 2001, A317, 32–36.

65. C. Buque, F. Appel: ‘Diffusion bonding of gamma-based titanium

aluminides’, Z. Metallkd., 2002, 93, 784–789.

66. D. P. Burke, R. L. Higginson: ‘Characterisation of multi-

component scales by electron back scattered diffraction

(EBSD)’, Scr. Mater., 2000, 42, 277–281.

67. C. Cabus, H. Regle, B. Bacroix: ‘Phase transformation textures in

steels’, Proc. Int. Conf. on ‘Advanced high strength sheet steels for

automotive applications’, (ed. M. A. Baker), 259–267; 2004a,

Warrendale, PA, AIST.

68. C. Cabus, H. Regle, B. Bacroix: ‘Phase transformation textures in

steels’, J. Phys. IV, 2004b, 120, 137–144.

69. C. Cabus: ‘Study and modelling of phase transformation textures

in drawing steels’, PhD dissertation, University Paris 13, Paris,

France, 2005 (in French).

70. M. G. Cain, F. F. Lange: ‘Heteroepitaxy of cubic zirconia on

basal and prismatic planes of sapphire’, J. Mater. Res., 1994, 9,

674–687.

71. M. G. Cain, F. F. Lange, M. H. Lewis, S. Bjorkert: ‘Substrate and

fibre coatings form aqueous, zirconia-based liquid precursors’,

Proc. Int. Symp. on ‘Novel synthesis and processing of ceramics’,

(ed. F. R. Sale), 7–31; 1995, London, The Institute of Materials.

72. V. Calonne, A. F. Gourgues, A. Pineau: ‘Influence of thermal

ageing on fatigue crack growth behaviour in cast duplex stainless

steels’, Proc. ECF–13, (ed. M. Fuentes et al.), 8 pp.; 2000,

Amsterdam, Elsevier Science (CD-ROM).

73. M. F. de Campos, L. C. R. Lopes, P. Magina, F. C. L. Tavares,

C. T. Kunioshi, H. Goldenstein: ‘Texture and microstructure



studies in different types of cast irons’, Mater. Sci. Eng. A, 2005,

A398, 164–170.

74. P. P. Camus: ‘Hardware and software optimization for orienta-

tion mapping and phase identification’, in ‘Electron backscatter

diffraction in materials science’, (ed. A. J. Schwartz et al.), 127–

134; 2000, New York, Kluwer Academic/Plenum Publishers.

75. P. Carter, D. C. Cox, C. A. Gandin, R. C. Reed: ‘Process

modelling of grain selection during the solidification of single

crystal superalloy castings’, Mater. Sci. Eng. A, 2000, A280, 233–

246.

76. A. Castellero, M. Motyka, A. L. Greer, M. Baricco: ‘Synthesis

and crystallisation of Fe61Co7Zr10Mo5W2B15 bulk metallic

glasses’, Mater. Sci. Eng. A, 2004, A375–A377, 250–254.

77. C. Cayron, B. Artaud, L. Briottet: ‘Reconstruction of parent

grains from EBSD data’, Mater. Charact., 2006, 57, 386–401.

78. W.-Y. Cha, T. Miki, Y. Sasaki, M. Hino: ‘Identification of

titanium oxide phases equilibrated with liquid Fe–Ti alloy based

on EBSD analysis’, ISIJ Int., 2006, 46, 987–995.

79. Y. J. Chang, J. H. Oh, K. H. Kim, J. Jang, D. I. Kim, K. H. Oh:

‘Electron backscattered diffraction study of poly-Si by Ni-

mediated crystallization of amorphous silicon using a SiO2

nanocap’, J. Vac. Sci. Technol. A, 2004, A22, 650–654.

80. D. Chaussende, P. Chaudouet, L. Auvray, M. Pons, R. Madar:

‘Electron back scattering diffraction (EBSD) as a tool for the

investigation of 3C–SiC nucleation and growth on 6H or 4H’,

Mater. Sci. Forum, 2004, 457–460, 387–390.

81. H. G. Chen, L. Chang: ‘Diamond nucleation on Ni3Al substrate

using bias enhanced nucleation method’, Diam. Relat. Mater.,

2005, 14, 183–191.

82. H.-W. Chen, V. Rudolph: ‘The 3-D structure of polycrystalline

diamond film by electron backscattering diffraction (EBSD)’,

Diam. Relat. Mater., 2003, 12, 1633–1639.

83. X. Chen, J. Gui, R. Wang, J. Wang, J. Liu, F. Chen, D. Wang:

‘Orientation relationships of martensite variants determined by

electron backscatter diffraction’, Micron, 2000, 31, 17–25.

84. Y. L. Cheung, K. C. Chan, Y. H. Zhu: ‘Characterization of the

icosahedral phase in as-cast quasicrystalline Al65Cu20Fe15 alloy’,

Mater. Charact., 2001, 47, 299–305.

85. A. R. Chezan, C. B. Craus, N. G. Chechenin, T. Vystavel,

L. Niesen, J. T. M. De Hosson, D. O. Boerma: ‘On the formation

of ultra-fine grained Fe-base alloys via phase transformations’,

Mater. Sci. Eng. A, 2004, A367, 176–184.

86. J.-Y. Cho, D.-W. Suh, J.-H. Kang, H.-C. Lee: ‘Evaluation of the

orientation distribution of intragranular ferrite grains dynamically

formed during deformation in a V-added low carbon steel by

EBSD’, Mater. Sci. Forum, 2002, 408–412, 1239–1244.

87. J.-Y. Cho, J. A. Szpunar: ‘The effect of substrate texture and

electroplating conditions on the texture and surface morphology

of copper electrodeposits’, Mater. Sci. Forum, 2002, 408–412,

1609–1614.

88. J.-Y. Cho, D.-W. Suh, J.-H. Kang, H.-C. Lee: ‘Orientation

distribution of proeutectoid ferrite nucleated at prior austenite

grain boundaries in vanadium-added steel’, ISIJ Int., 2002, 42,

1321–1323.

89. J.-J. Choi, G.-T. Park, C.-S. Park, J.-W. Lee, H.-E. Kim: ‘Effects

of lanthanum nitrate buffer layer on the orientation and piezo-

electric property of Pb(Zr,Ti)O3 thick film’, J. Mater. Res., 2004,

19, 3671–3678.

90. J.-J. Choi, G.-T. Park, C.-S. Park, H.-E. Kim: ‘Ferroelectric and

piezoelectric properties of highly oriented Pb(Zr,Ti)O3 film grown

on Pt/Ti/SiO2/Si substrate using conductive lanthanum nickel

nitrate buffer layer’, J. Mater. Res., 2005, 20, 726–733.

91. J. Claus, G. Borchardt, S. Weber, S. Scherrer: ‘EBSP and SIMS

studies of oxygen tracer diffusion in the high temperature

superconductor La2–xSrxCuO4’, Mater. Sci. Forum, 1994, 157–

162, 1161–1166.

92. J. Claus, G. Borchardt, S. Weber, J. M. Hiver, S. Scherrer:

‘Combination of EBSP measurements and SIMS to

study crystallographic orientation dependence of diffusivities

in a polycrystalline material: oxygen tracer diffusion in

La2–xSrxCuO4¡d’, Mater. Sci. Eng. B, 1996, B38, 251–257.

93. F. Cleton, P. H. Jouneau, S. Henry, M. Gaumann, P. A. Buffat:

‘Crystallographic orientation assessment by electron backscat-

tered diffraction’, Scanning, 1999, 21, 232–237.

94. M. Cornen, R. Le Gall: ‘Direct measurement of impurity

segregation concentration at grain boundaries for polycrystalline

materials using EBSD and 3D reconstruction of SEM images of

etch grooves’, MRS Proc., 2004, 819, 133–138.

95. F. Cosandey: ‘High spatial resolution EBSD study of nanosized

epitaxial particles’, Microsc. Microanal., 1997, 3, 559–560.

96. F. Cosandey, P. Markondeya Raj, W. R. Cannon: ‘Texture

determination of ceramic materials by EBSD’, Microsc.

Microanal., 1999, 5, 224–225.

97. F. Cosandey, L. Zhang, T. E. Madey: ‘Effect of substrate

temperature on the epitaxial growth of Au on TiO2(110)’, Surf.

Sci., 2001, 474, 1–13.

98. E. Cotrina, B. Lopez, J. M. Rodriguez-Ibabe: ‘Influence of

thermomechanical treatment on the austenite–pearlite transfor-

mation in a high carbon Nb-microalloyed steel’, Proc. Int. Conf.

on ‘Austenite formation and decomposition’, (ed. E. B. Damm),

213–225; 2003, Warrandale, PA, ISS–TMS.

99. E. Cotrina, A. Iza-Mendia, B. Lopez: ‘Study of the ferrite grain

coarsening behind the transformation front by electron back-

scattered diffraction techniques’, Metall. Mater. Trans. A, 2004,

35A, 93–102.

100. T. Czerwiec, H. He, A. Saker, L. T. Huu, C. Dong, C. Frantz,

H. Michel: ‘Reactive magnetron sputtering as a way to improve

the knowledge of metastable f.c.c. nitrogen solid solutions formed

during plasma assisted nitriding of Inconel 690’, Surf. Coat.

Technol., 2003, 174–175, 131–138.

101. S. Dabritz, E. Langer, W. Hauffe: ‘Kossel and pseudo Kossel

CCD patterns in comparison with electron backscattering

diffraction diagrams’, Appl. Surf. Sci., 2001, 179, 38–44.

102. A. K. Dahle, K. Nogita, J. W. Zindel, S. D. McDonald, L. M.

Hogan: ‘Eutectic nucleation and growth in hypoeutectic Al–Si

alloys at different strontium levels’, Metall. Mater. Trans., 2001,

32, 949–960.

103. A. K. Dahle, K. Nogita, S. D. McDonald, C. Dinnis, L. Lu:

‘Eutectic solidification and microstructure development in Al–Si

alloys’, Mater. Sci. Eng. A, 2005, A413–A414, 243–248.

104. A. V. Davydov, L. A. Bendersky, W. J. Boettinger, D. Josell,

M. D. Vaudin, K.-S. Chang, I. Takeuchi: ‘Combinatorial

investigation of structural quality of Au/Ni contacts on GaN’,

Appl. Surf. Sci., 2004, 223, 24–29.

105. R. Decocker, L. Kestens, R. Petrov, Y. Houbaert: ‘Revealing a

parent phase structure after transformation based on crystal-

lographic relations’, Mater. Sci. Forum, 2003, 426–432, 3751–

3756.

106. J. T. M. De Hosson, V. Ocelık: ‘Functionally graded materials

produced with high power lasers’, Mater. Sci. Forum, 2003, 426–

432, 123–130.

107. M. De Meyer, L. Kestens, B. C. De Cooman: ‘Texture

development in cold rolled and annealed C–Mn–Si and C–Mn–

Al–Si TRIP steels’, Mater. Sci. Technol., 2001, 17, 1353–1359.

108. D. Devilliers, T. Baudin, M. T. D. Thi, E. Mahe: ‘Selective

electrodeposition of PbO2 on anodised-polycrystalline titanium’,

Electrochim. Acta, 2004, 49, 2369–2377.

109. S. R. Dey, A. Hazotte, E. Bouzy, S. Naka: ‘Development of

Widmanstatten laths in a near-c TiAl alloy’, Acta Mater., 2005,

53, 3783–3794.

110. M. Dıaz-Fuentes, A. Iza-Mendia, I. Guttierrez: ‘Analysis of

different acicular ferrite microstructures in low-carbon steels by

electron backscattered diffraction. Study of their toughness

behavior’, Metall. Mater. Trans. A, 2003, 34A, 2505–2516.

111. D. J. Dingley: ‘Diffraction from sub-micron areas using electron

backscattering in a scanning electron microscope’, Scan. Electron

Microsc., 1984, 2, 569–575.

112. D. Dingley, V. Randle: ‘Review – Microtexture determination by

electron back-scatter diffraction’, J. Mater. Sci., 1992, 27, 4545–

4566.

113. D. J. Dingley: ‘Progressive steps in the development of electron

backscatter diffraction and orientation imaging microscopy’,

J. Microsc., 2004, 213, 214–224.

114. J. Dobransky, P. J. Szabo, T. Berecz, V. Hrotko, M. Portko:

‘Energy-dispersive spectroscopy and electron backscatter diffrac-

tion analysis of isothermally aged SAF 2507 type superduplex

stainless steel’, Spectrochim. Acta B, 2004, 59B, 1781–1788.

115. R. D. Doherty: ‘Comments on ‘Mechanical deformation of

dendrites by fluid flow during the solidification of undercooled

melts’, Scr. Mater., 2003, 49, 1219–1222.

116. S. Drawin, P. Petit, D. Boivin: ‘Microstructural properties of Nb–

Si alloys investigated using EBSD at large and small scale’,


117. A. Dronhofer, J. Pesicka, A. Dlouhy, G. Eggeler: ‘On the nature

of internal interfaces in tempered martensite ferritic steels’,

Z. Metallkd., 2003, 94, 511–520.

118. N. D’Souza, M. G. Ardakani, M. McLean, B. A. Shollock:

‘Directional and single-crystal solidification of Ni-base super-

alloys: Part I. The role of curved isotherms on grain selection’,




119. N. D’Souza, M. Newell, K. Devendra, P. A. Jennings, M. G.

Ardakani, B. A. Shollock: ‘Formation of low angle boundaries in

Ni-based superalloys’, Mater. Sci. Eng. A, 2005, A413–A414, 567–

570.

120. C. Duda, A.-F. Gourgues: ‘Electron backscatter diffraction

characterisation of liquid route processed Ti6242S/SCS–6 com-

posites’, Mater. Sci. Eng. A, 2006, A435–A436, 530–539.

121. D. Dunst, H. Mecking, ‘Analysis of experimental and theoretical

rolling textures of two-phase titanium alloys’, Z. Metallkd., 1996,

87, 498–507.

122. J. N. DuPont, J. R. Michael, B. D. Newbury: ‘Welding metallurgy

of Alloy HR–160’, Weld. Res. Suppl., 1999, 78, 408S–415S.

123. M. L. Dupont, T. Baudin, R. Penelle, S. Naka, M. Thomas:

‘Texture and microstructure evolution of a two-phase c/a2

titanium aluminide according to heat treatments’, J. Phys. IV

(France), Suppl. to J. Phys. III, 1996, 6, C2–235 to C2–240.

124. M. Dzubinsky, Y. Sidor, F. Kovac: ‘Kinetics of columnar

abnormal grain growth in low-Si non-oriented electrical steel’,

Mater. Sci. Eng. A, 2004, A385, 449–454.

125. B. Eghbali, A. Abdallah-zadeh: ‘Strain-induced transformation in

a low carbon microalloyed steel during hot compression testing’,

Scr. Mater., 2006, 54, 1205–1209.

126. B. S. El-Dasher, S. G. Torres: ‘Effect of stress mitigation on

precipitation kinetics of Alloy 22 welds’, JOM, 2004, 56, 148–149.

127. B. S. El-Dasher, T. S. Edgecumbe, S. G. Torres: ‘The effect of

solution annealing on the microstructural behavior of Alloy 22

welds’, Metall. Mater. Trans. A, 2006, 37A, 1027–1038.

128. H. Ezawa, M. Seto, H. Katsumata: ‘Pb-free bumping for high-

performance SoCs’, Proc. 2004 Electron. Components Technol.

Conf., Piscataway, NJ, USA, June 2004, IEEE, 655–660.

129. R. J. Fairhurst, H.-Y. Zhai, J. K. Meen, D. Elthon:

‘Crystallographic study of superconducting YBCO thin films by

EBSD’, Physica C, 2000, 341C–348C, 2019–2020.

130. A. Fallet, G. Chichignoud, C. L. Martin, M. Suery, P. Jarry:

‘Influence of barium addition on the microstructure and the

rheological behaviour of partially solidified Al–Cu alloys’, Mater.

Sci. Eng. A, 2006, A426, 187–193.

131. M. U. Farooq, U. Klement, G. Nolze: ‘Microstructural char-

acterisation of a Co–Cr–Mo laser clad applied on railway wheels’,

Int. J. Mater. Res., 2006, 97, 838–844.

132. J. K. Farrer, J. R. Michael, C. B. Carter: ‘EBSD of ceramic

materials’, in ‘Electron backscatter diffraction in materials

science’, (ed. A. J. Schwartz et al.), 299–318; 2000, New York,

Kluwer Academic/Plenum Publishers.

133. J. K. Farrer, C. B. Carter, N. Ravishankar: ‘The effects of

crystallography on grain-boundary migration in alumina’,

J. Mater. Sci., 2006, 41, 661–674.

134. M. Faryna, W. Wołczynski, T. Okane: ‘Microanalytical techni-

ques applied to phase identification and measurement of solute

redistribution at the solid/liquid interface of frozen Fe–4.3Ni

doublets’, Microchim. Acta, 2002, 139, 61–65.

135. U. H. Faul, J. D. Fitz Gerald: ‘Grain misorientation in partially

molten olivine aggregates: an electron backscatter diffraction

study’, Phys. Chem. Miner., 1999, 26, 187–197.

136. H. Feng, Y. Zhou, D. Jia, Q. Meng: ‘Microstructural character-

ization of spark plasma sintered in situ TiB reinforced Ti matrix

composite by EBSD and TEM’, Mater. Trans., 2005, 46, 575–580.

137. M. Ferry: ‘Materials analysis using electron backscattered

diffraction in the SEM’, Proc. Materials 98, (ed. M. Ferry),

439–444; 1998, Wollongong, Wollongong University Press.

138. M. Ferry, A. Hunter: ‘Factors affecting the ,001. fiber texture

in strip-cast stainless steels’, Mater. Sci. Forum, 2002, 408–412,

1395–1400.

139. M. Ferry, W. Xu: ‘Microstructural and crystallographic features

of ausferrite in as-cast gray iron’, Mater. Charact., 2004, 53, 43–

49.

140. D. P. Field, S. I. Wright, D. J. Dingley: ‘Multi-phase texture

analysis by orientation imaging microscopy’, Proc. 11th Int. Conf.

on ‘Textures of materials’, (ed. Z. Liang et al.), 94–99; 1996,

Beijing, International Academic Publishers.

141. J. Foct, N. Akdut: ‘Cleavage-like fracture of austenite in duplex

stainless steel’, Scr. Metall. Mater., 1993, 29, 153–158.

142. X. Fu, H. F. Poulsen, S. Schmidt, S. F. Nielsen, E. M. Lauridsen,

D. J. Jensen: ‘Non-destructive mapping of grains in three

dimensions’, Scr. Mater., 2003, 49, 1093–1096.

143. H. Fukai, S. Suzuki, N. Masahashi, S. Hanada, T. Maruyama,

H. Kubo, Y. Waseda: ‘Improvement of oxidation resistance of an

Fe–Mn–Si–Cr shape memory alloy by annealing under vacuum’,

Mater. Trans., 2005, 46, 1745–1748.

144. S. Fukumoto, W. Kurz: ‘The d to c transition in Fe–Cr–Ni alloys

during laser treatment’, ISIJ Int., 1997, 37, 677–684.

145. T. Furuhara, T. Shinyoshi, G. Miyamoto, J. Yamaguchi,

N. Sugita, N. Kimura, N. Takemura, T. Maki: ‘Multiphase

crystallography in the nucleation of intragranular ferrite on MnS

z V(C,N) complex precipitate in austenite’, ISIJ Int., 2003, 43,

2028–2037.

146. T. Furuhara, H. Kawata, S. Morito, T. Maki: ‘Crystallography of

upper bainite in Fe–Ni–C alloys’, Mater. Sci. Eng. A, 2006, A431,

228–236.

147. T. Furuhara, H. Kawata, S. Morito, T. Maki: ‘Crystallography of

upper bainite in Fe–Ni–C alloy’, Mater. Sci. Eng. A, 2006, A431,

228–236.

148. C.-A. Gandin, M. Rappaz, D. West, B. L. Adams: ‘Grain texture

evolution during the columnar growth of dendritic alloys’, Metall.

Mater. Trans., 1995, 26A, 1543–1551.

149. J. Gao, J. Wang, N. Sakai, K. Iwanaga, K. Muraoka,

H. Nakashima, D. Gao, K. Furukawa: ‘Study of the effects of

discharge conditions and substrate temperature on Si epitaxial

deposition using sputtering-type electron cyclotron resonance

plasma’, J. Vac. Sci. Technol. A, 2000, A18, 873–878.

150. B. Gardiola, C. Esling, M. Humbert, K.-E. Hensger: ‘EBSD study

of the c to a phase transformation in a CSP–HSLA steel’, Adv.

Eng. Mater., 2003, 5, 583–587.

151. H. Garmestani, K. Harris: ‘Orientation determination by EBSP in

an environmental scanning electron microscope’, Scr. Mater.,

1999, 41, 47–53.

152. C. M. Garzon, A. P. Tschiptschin: ‘New high temperature gas

nitriding cycle that enhances the wear resistance of duplex

stainless steels’, J. Mater. Sci., 2004, 39, 7101–7105.

153. M. Gaumann, S. Henry, F. Cleton, J.-D. Wagniere, W. Kurz:

‘Epitaxial laser metal forming: analysis of microstructure forma-

tion’, Mater. Sci. Eng. A, 1999, A271, 232–241.

154. M. Gaumann, C. Bezencon, P. Canalis, W. Kurz: ‘Single-crystal

laser deposition of superalloys: processing–microstructure maps’,

Acta Mater., 2001, 49, 1051–1062.

155. V. Geist, G. Wagner, G. Nolze, O. Moretzki: ‘Investigations of

the meteoritic mineral (Fe,Ni)3P’, Cryst. Res. Technol., 2005, 40,

52–64.

156. L. Germain, N. Gey, M. Humbert, P. Bocher, M. Jahazi: ‘Texture

and microtexture analysis of an IMI 834 alloy after thermo-

mechanical processing’, Proc. 10th World Conf. on ‘Titanium’, (ed.

G. Lutjering, J. Albrecht), 1291–1298; 2004, Weinheim, Wiley-VCH.

157. L. Germain, N. Gey, M. Humbert, A. Hazotte, P. Bocher,

M. Jahazi: ‘An automated method to analyze separately the

microtextures of primary ap grains and the secondary as inherited

colonies in bimodal titanium alloys’, Mater. Charact., 2005a, 54,

216–222.

158. L. Germain, N. Gey, M. Humbert, P. Bocher, M. Jahazi:

‘Analysis of sharp microtexture heterogeneities in a bimodal

IMI 834 billet’, Acta Mater., 2005b, 53, 3535–3543.

159. N. Gey, M. Humbert, M. J. Philippe, Y. Combres: ‘Investigation

of the a- and b- texture evolution of hot rolled Ti–64 products’,

Mater. Sci. Eng. A, 1996, A219, 80–88.

160. N. Gey, M. Humbert, J. J. Fundenberger: ‘Comparison between

indirect methods to determine high-temperature textures of parent

phases’, Z. Metallkd., 1999, 90, 738–743.

161. N. Gey, M. Humbert: ‘Characterization of the variant selection

occurring during the aRbRa phase transformations of a cold

rolled titanium sheet’, Acta Mater., 2002, 50, 277–287.

162. N. Gey, E. Gautier, M. Humbert, A. Cerqueira, J. L. Bechade,

P. Archambault: ‘Study of the a/b phase transformation of Zy–4

in presence of applied stresses at heating: analysis of the inherited

microstructures and textures’, J. Nucl. Mater., 2002, 302, 175–184.

163. N. Gey, M. Humbert: ‘Specific analysis of EBSD data to study

the texture inheritance due to the bRa phase transformation’,

J. Mater. Sci., 2003, 38, 1289–1294.

164. N. Gey, B. Petit, M. Humbert: ‘Electron backscattered diffraction

study of e/a’ martensitic variants induced by plastic deformation

in 304 stainless steel’, Metall. Mater. Trans. A, 2005, 36A, 3291–

3299.

165. M. G. Glavicic, P. A. Kobryn, T. R. Bieler, S. L. Semiatin: ‘An

automated method to determine the orientation of the high-

temperature beta phase from measured EBSD data for the low-

temperature alpha phase in Ti–6Al–4V’, Mater. Sci. Eng. A,

2003a, A351, 258–264.

166. M. G. Glavicic, P. A. Kobryn, T. R. Bieler, S. L. Semiatin: ‘A

method to determine the orientation of the high-temperature beta

phase from measured EBSD data for the low-temperature alpha

phase in Ti–6Al–4V’, Mater. Sci. Eng. A, 2003b, A346, 50–59.



167. M. G. Glavicic, P. A. Kobryn, F. Spadafora, S. L. Semiatin:

‘Texture evolution in vacuum arc remelted ingots of Ti–6Al–4V’,

Mater. Sci. Eng. A, 2003c, A346, 8–18.

168. M. G. Glavicic, P. A. Kobryn, R. L. Goetz, K. O. Yu, S. L.

Semiatin: ‘Texture evolution during primary processing of

production-scale vacuum arc remelted ingots of Ti–6Al–4V’,

Proc. 10th World Conf. on ‘Titanium’, (ed. G. Lutjering,

J. Albrecht), 1299–1306; 2004a, Weinheim, Wiley-VCH.

169. M. G. Glavicic, P. A. Kobryn, S. L. Semiatin: ‘Validation of an

automated EBSD method to deduce the b-phase texture in Ti–

6Al–4V with a colony-a microstructure’, Mater. Sci. Eng. A,

2004b, A385, 372–376.

170. M. Godec, D. Nolan, M. Jenko: ‘Characterisation of crystal-

lisation in amorphous soft magnetic Fe74Si11B14Ni1 powders by

EBSD method’, Mater. Sci. Eng. B, 2006, B129, 31–38.

171. S. Godet, P. J. Jacques, J. A. Szpunar, J. J. Jonas, F. Delannay:

‘Microtextural analysis of the variant selection phenomenon

during the bainitic transformation’, Rev. Met. JA, 2001, 62 (in

French).

172. S. Godet, J. C. Glez, J. He, J. J. Jonas, P. J. Jacques: ‘Grain-scale

characterization of transformation textures’, J. Appl. Crystallogr.,

2004, 37, 417–425.

173. S. Godet, A. Petein, P. J. Jacques: ‘High resolution EBSD

characterisation of the phase transformations and orientation

relationships in ultra high performance steels’, Rev. Metall., 2005,

102, 166–167.

174. S. Godet, P. Harlet, P. J. Jacques: ‘Grain refinement of TRIP-

assisted multiphase steels through strain-induced phase transfor-

mation’, Steel Res. Int., 2006, 77, 271–275.

175. R. P. Goehner, J. R. Michael: ‘Applied crystallography in the

scanning electron microscope using a CCD detector’, in

‘Advances in X–ray analysis’, (ed. P. Predecki et al.), 539–545;

1995, New York, Plenum Press.

176. R. P. Goehner, J. R. Michael: ‘Phase identification in a scanning

electron microscope using backscattered electron Kikuchi pat-

terns’, J. Res. Natl Inst. Stand. Technol., 1996, 101, 301–308.

177. X. Gomez, J. Echeberria: ‘Microstructure and mechanical proper-

ties of carbon steel A210–superalloy Sanicro 28 bimetallic tubes’,

Mater. Sci. Eng. A, 2003, A348, 180–191.

178. A.-F. Gourgues, H. M. Flower, T. C. Lindley: ‘Electron

backscattering diffraction study of acicular ferrite, bainite, and

martensite steel microstructures’, Mater. Sci. Technol., 2000, 16,

26–40.

179. A. F. Gourgues: ‘Overview: EBSD and cracking’, Mater. Sci.

Technol., 2002, 18, 119–133.

180. A.-F. Gourgues: ‘Microtexture induced by the bainitic transfor-

mation in steels during welding. Effect on the resistance to

cleavage cracking’, Mater. Sci. Forum, 2003, 426–432, 3629–3634.

181. A. F. Gourgues, V. Calonne, S. Bugat: ‘EBSD crystallographic

characterisation of microstructure and cracking of cast duplex

stainless steels’, in ‘L’analyse EBSD: principes et applications (in

French)’, (ed. J.-L. Pouchou), 101–109; 2004, Les Ulis, EDP

Sciences.

182. E. Grant, D. J. Jensen, B. Ralph: ‘A determination of the texture

of a directionally solidified sample of high-purity copper’,

J. Mater. Sci., 1986, 21, 1688–1692.

183. J. J. Gray, B. S. El Dasher, C. A. Orme: ‘Competitive effects of

metal dissolution and passivation modulated by surface structure:

an AFM and EBSD study of the corrosion of alloy 22’, Surf. Sci.,

2006, 600, 2488–2494.

184. M. Griffiths, R. A. Holt, J. Li, S. Saimoto: ‘Microtexture analysis

of Zr–2.5Nb pressure tubing’, Proc. 31st Annu. Tech. Meet. Int.

Metallogr. Soc., (ed. D. O. Northwood et al.), 293–302; 1998,

Materials Park, OH, ASM International.

185. M. A. Groeber, B. K. Haley, M. D. Uchic, D. M. Dimiduk,

S. Ghosh: ‘3D reconstruction and characterization of polycrystal-

line microstructures using a FIB-EBSD system’, Mater. Charact.,

2006, 57, 259–273.

186. J. Gui, J. Wang, R. Wang, D. Wang, J. Liu, F. Chen: ‘On some

discrepancies in the literature about the formation of icosahedral

quasi-crystal in Al–Cu–Fe alloys’, J. Mater. Res., 2001, 16, 1037–

1046.

187. A. Guillou, J. P. Bars, I. Thibon, D. Ansel: ‘Orientation

relationships in nitrided titanium alloys’, Proc. 10th World

Conf. on ‘Titanium’, (ed. G. Lutjering, J. Albrecht), 957–962;

2004, Weinheim, Wiley-VCH.

188. S. Guldberg, N. Ryum: ‘Microstructure and crystallographic

orientation relationship in directionally solidified Mg–Mg17Al12

eutectic’, Mater. Sci. Eng. A, 2000, A289, 143–150.

189. H. Guo, M. C. Chaturvedi, N. L. Richards: ‘Effect of nature of

grain boundaries on intergranular liquation during weld thermal

cycling of nickel base alloy’, Sci. Technol. Weld. Join., 1998, 3,

257–259.

190. H. Guo, K. Okuda, M. Enomoto: ‘Surface relief of a’’ martensite

in a Ti–Mo alloy’, Metall. Mater. Trans. A, 2000, 31A, 599–605.

191. H. Guo, M. Enomoto: ‘Surface reconstruction associated with aprecipitation in a Ti–Mo alloy’, Scr. Mater., 2006, 54, 1409–1413.

192. Z. Guo, T. Furuhara, T. Maki: ‘The influence of (MnS z VC)

complex precipitate on the crystallography of intergranular

pearlite transformation in Fe–Mn–C hypereutectoid alloys’, Scr.

Mater., 2001, 45, 525–532.

193. Z. Guo, N. Kimura, S. Tagashira, T. Furuhara, T. Maki:

‘Kinetics and crystallography of intragranular pearlite transfor-

mation nucleated at (MnS z VC) complex precipitates in

hypereutectoid Fe–Mn–C alloys’, ISIJ Int., 2002, 42, 1033–1041.

194. S. M. Habesch: ‘Electron backscattered diffraction analyses

combined with environmental scanning electron microscopy:

potential applications for non-conducting, uncoated mineralogi-

cal samples’, Mater. Sci. Technol., 2000, 16, 1393–1398.

195. M. G. Hall, H. I. Aaronson: ‘Formation of invariant plane-strain

and tent-shaped surface reliefs by the diffusional ledge mechan-

ism’, Metall. Mater. Trans. A, 1994, 25A, 1923–1931.

196. J. Hamada, Y. Matsumoto, F. Fudanoki, S. Maeda: ‘Effect of

initial solidified structure on ridging phenomenon and texture in

type 430 ferritic stainless steel sheets’, ISIJ Int., 2003, 43, 1989–

1998.

197. L. H. Hamedi, M. Guilloux-Viry, A. Perrin, M. H. Cherkani: ‘On

the epitaxial growth of PZT films by pulsed laser deposition’, Ann.

Chim. Sci. Mater., 1998, 23, 377–380.

198. S.-W. Han, S. Kumai, A. Sato: ‘Origin of improved ductility in

semi-liquid die-cast Al–7%Si–0.4%Mg alloys’, Mater. Trans.,

2001, 42, 342–349.

199. S. Hanada, T. Ogura, S. Watanabe, O. Izumi, T. Masumoto:

‘Application of the selected area channeling pattern method to the

study of intergranular fracture in Ni3Al’, Acta Metall., 1986, 34,

13–21.

200. K. Hase, C. Garcia-Mateo, H. K. D. H. Bhadeshia: ‘Bainite

formation influenced by large stress’, Mater. Sci. Technol., 2004,

20, 1499–1505.

201. H. He, T. Czerwiec, C. Dong, H. Michel: ‘Effect of grain

orientation on the nitriding rate of a nickel base alloy studied by

electron backscatter diffraction’, Surf. Coat. Technol., 2003, 163–

164, 331–338.

202. Y. He, S. Godet, J. J. Jonas: ‘Representation of misorientations in

Rodrigues-Frank space: application to the Bain, Kurdjumov–

Sachs, Nishiyama–Wassermann and Pitsch orientation relation-

ships in the Gibeon meteorite’, Acta Mater., 2005, 53, 1179–1190.

203. Y. He, S. Godet, P. J. Jacques, J. J. Jonas: ‘Crystallographic

relations between face- and body-centred cubic crystals under

near-equilibrium conditions: Observations from the Gibeon

meteorite’, Acta Mater., 2006, 54, 1323–1334.

204. T. Hebesberger, R. Pippan, O. Kolednik, C. O. A.

Semprimoschnig, H. Clemens: ‘Crystallographic fractometry: a

new method of fracture surface analysis applied on TiAl fracture

surfaces’, Prakt. Metallogr., 2000, 37, 301–314.

205. L.G. Hector, Jr, Y.-L. Chen, S. Agarwal, C. L. Briant: ‘Texture

characterization of autogenous Nd:YAG laser welds in AA5182

and AA6111–T4 aluminum alloys’, Metall. Mater. Trans. A, 2004,

35A, 3032–3038.

206. G. Heiberg, L. Arnberg: ‘Investigation of the microstructure of

the Al–Si eutectic in binary aluminium–7wt% silicon alloys by

electron backscatter diffraction (EBSD)’, J. Light Met., 2001, 1,

43–49.

207. G. Heiberg, K. Nogita, A. K. Dahle, L. Arnberg: ‘Columnar to

equiaxed transition of eutectic in hypoeutectic aluminium–silicon


208. D. Helary, O. Dugne, X. Bourrat, P. H. Jouneau, F. Cellier:

‘EBSD investigation of SiC for HTR fuel particles’, J. Nucl.

Mater., 2006, 350, 332–335.

209. S. Henry, P. Jarry, P.-H. Jouneau, M. Rappaz: ‘Electron

backscattered diffraction investigation of the texture of feathery

crystals in aluminum alloys’, Metall. Mater. Trans. A, 1997, 28A,

207–213.

210. S. Henry, P. Jarry, M. Rappaz: ‘,110. dendrite growth in

aluminum feathery grains’, Metall. Mater. Trans. A, 1998, 29A,

2807–2817.

211. S. Henry, T. Minghetti, M. Rappaz: ‘Dendrite growth morphol-

ogies in aluminum alloys’, Acta Mater., 1998, 46, 6431–6443.



212. S. Henry, G.-U. Gruen, M. Rappaz: ‘Influence of convection on

feathery grain formation in aluminum alloys’, Metall. Mater.

Trans. A, 2004, 35A, 2495–2501.

213. T.-H. Her, R. J. Finlay, C. Wu, E. Mazur: ‘Femtosecond laser-

induced formation of spikes on silicon’, Appl. Phys. A, 2000, A70,

383–385.

214. D. Hernandez, M. Dıaz-Fuentes, B. Lopez, J. M. Rodriguez-

Ibabe: ‘Study of grain boundary ferrite nucleation in V

microalloyed steels by EBSD’, Mater. Sci. Forum, 2003, 426–

432, 1151–1156.

215. H. T. Hesemann, P. Mullner, E. Arzt: ‘Stress and texture

development during martensitic transformation in cobalt thin

films’, Scr. Mater., 2001, 44, 25–30.

216. R. L. Higginson, B. Roebuck, E. J. Palmiere: ‘Texture develop-

ment in oxide scales on steel substrates’, Scr. Mater., 2002, 47,

337–342.

217. M. Hillert et al.: ‘Preface to the viewpoint set on: bainite’ and

following papers by various authors, Scr. Mater., 2002, 47, (3)

(the whole issue).

218. A. Hirose, D. Nakamura, H. Yanagawa, K. F. Kobayashi:

‘Microstructure and mechanical property of laser welds of single

crystal nickel base superalloy CMSX–4’, Mater. Sci. Forum, 2003,

426–432, 4007–4012.

219. S. Hirth, G. Gottstein: ‘Misorientation effects on discontinuous

precipitation in Al–Ag–Ga’, Acta Mater., 1998, 46, 3975–3984.

220. S. C. Hogg, H. V. Atkinson: ‘Inhibited coarsening of a spray-

formed and extruded hypereutectic aluminum–silicon alloy in the

semisolid state’, Metall. Mater. Trans. A, 2005, 36A, 149–159.

221. S. C. Hogg, A. Lambourne, A. Ogilvy, P. S. Grant:

‘Microstructural characterisation of spray formed Si–30Al for

thermal management applications’, Scr. Mater., 2006, 55, 111–

114.

222. R. A. Holt, P. Zhao: ‘Micro-texture of extruded Zr–2.5Nb tubes’,

J. Nucl. Mater., 2006, 335, 520–528.

223. H. U. Hong, B. S. Rho, S. W. Nam: ‘Correlation of the M23C6

precipitation morphology with grain boundary characteristics in

austenitic stainless steel’, Mater. Sci. Eng. A, 2001, A318, 285–292.

224. K. Horikawa, K. Yoshida: ‘Visualization of hydrogen distribution

in tensile–deformed Al–5%Mg alloy investigated by means of

hydrogen microprint technique with EBSP analysis’, Mater.

Trans., 2004, 45, 315–318.

225. L. Huang, S. Wright, S. Yang, D. Shen, B. Gu, Y. Du: ‘ZnO well-

faceted fibers with periodic junctions’, J. Phys. Chem. B, 2004,

B108, 19901–19903.

226. Y. Huang, F. J. Humphreys, I. Brough: ‘The application of a hot

deformation SEM stage, backscattered electron imaging and

EBSD to the study of thermomechanical processing’, J. Microsc.,

2002, 208, 18–23.

227. M. Humbert, H. Moustahfid, F. Wagner, M. J. Philippe:

‘Evaluation of the high temperature texture of the b phase of a

TA6V sample from the individual orientations of grains of the low

temperature a phase’, Scr. Metall. Mater., 1994, 30, 577–582.

228. M. Humbert, F. Wagner, H. Moustahfid, C. Esling:

‘Determination of the orientation of a parent b grain from the

orientations of the inherited a plates in the phase transformation

form body-centred cubic to hexagonal close-packed’, J. Appl.

Crystallogr., 1995, 28, 571–576.

229. M. Humbert, N. Gey: ‘Use of a method based on a correlation

function to reconstruct the parent textures from the inherited

textures in phase transformation’, Proc. 12th Int. Conf. on

‘Textures of materials’, (ed. J. A. Szpunar), 147–152; 1999,

Ottawa, NRC Research Press.

230. M. Humbert, N. Gey, B. Gardiola, C. Esling: ‘Restitution of high

temperature parent textures of bcc and hcp polycrystals by a non-

linear positivity method’, Acta Mater., 2001, 49, 445–451.

231. M. Humbert, B. Gardiola, C. Esling, G. Flemming, K. E.

Hensger: ‘Analysis and modelling of a variant selection mechan-

ism occuring by phase transformation of a HSLA steel produced

by compact strip production’, Mater. Sci. Forum, 2002a, 408–412,

445–450.

232. M. Humbert, B. Gardiola, C. Esling, G. Flemming, K. E.

Hensger: ‘Modelling of the variant selection mechanism in the

phase transformation of HSLA steel produced by compact strip

production’, Acta Mater., 2002b, 50, 1741–1747.

233. M. Humbert, N. Gey: ‘Elasticity-based model of the variant

selection observed in the b to a phase transformation of a

Zircaloy–4 sample’, Acta Mater., 2003, 51, 4783–4790.

234. M. Humbert, L. Germain, N. Gey, P. Bocher, M. Jahazi: ‘Study

of the variant selection in sharp textured regions of bimodal IMI

834 billet’, Mater. Sci. Eng. A, 2006, A430, 157–164.

235. F. J. Humphreys: ‘Determination of microtexture by EBSD at

high spatial resolution in a FEGSEM’, Proc. 12th Int. Conf. on

‘Textures of materials’, (ed. J. A. Szpunar), 74–78; 1999, Ottawa,

NRC Research Press.

236. F. J. Humphreys: ‘Characterisation of fine-scale microstructures

by electron backscatter diffraction (EBSD)’, Scr. Mater., 2004, 51,

771–776.

237. A. Hunter, M. Ferry: ‘Texture enhancement by inoculation during

casting of ferritic stainless steel strip’, Metall. Mater. Trans. A,

2002a, 33A, 1499–1507.

238. A. Hunter, M. Ferry: ‘Evolution of microstructure and texture

during casting of AISI 304 stainless steel strip’, Metall. Mater.

Trans. A, 2002b, 33A, 3747–3754.

239. A. Hunter, M. Ferry: ‘Comparative study of texture development

in strip-cast ferritic and austenitic stainless steels’, Scr. Mater.,

2002c, 47, 349–355.

240. P. J. Hurley, P. D. Hodgson, B. C. Muddle: ‘Analysis and

characterisation of ultra-fine ferrite produced during a new steel

strip rolling process’, Scr. Mater., 1999, 40, 433–438.

241. P. J. Hurley, B. C. Muddle, P. D. Hodgson: ‘Microstructure and

microtexture of ultrafine ferrite formed in 0.1%C steel using new

strip rolling process’, Mater. Sci. Technol., 2000, 16, 1376–1379.

242. P. J. Hurley, P. D. Hodgson: ‘Formation of ultra-fine ferrite in

hot rolled strip: potential mechanisms for grain refinement’,

Mater. Sci. Eng. A, 2001, A302, 206–214.

243. B. Hutchinson, L. Ryde, E. Lindh, K. Tagashira: ‘Texture in hot

rolled austenite and resulting transformation products’, Mater.

Sci. Eng. A, 1998, A257, 9–17.

244. T. Iamboliev, S. Katayama, A. Matsunawa: ‘Interpretation of

phase formation in austenitic stainless steel welds’, Weld. J., Dec.

2003, 337S–347S.

245. H. Inoue, T. Koseki, S. Ohkita, T. Tanaka: ‘Effect of solidifica-

tion on subsequent ferrite-to-austenite massive transformation in

an austenitic stainless steel weld metal’, ISIJ Int., 1995, 35, 1248–

1257.

246. H. Inoue, T. Koseki, S. Okita, M. Fuji: ‘Solidification and

transformation behaviour of Cr–Ni stainless steel weld metals

with ferritic single-phase solidification mode: study of solidifica-

tion and transformation of Cr–Ni stainless steel weld metals (4th

report)’, Weld. Int., 1998, 12, 282–296.

247. H. Inoue, T. Koseki, S. Ohkita, M. Fuji: ‘Formation mechanism

of vermicular and lacy ferrite in austenitic stainless steel weld

metals’, Sci. Technol. Weld. Join., 2000, 5, 385–396.

248. H. Inoue, M. Ishio, T. Takasugi: ‘Texture of TiNi shape memory

alloy sheets produced by roll-bonding and solid phase reaction

from elementary metals’, Acta Mater., 2003, 51, 6373–6383.

249. K. Ito, T. Hayashi, T. Murakami, M. Yamaguchi: ‘Oxidation

behavior of Mo-based alloys coated with silicide using the halide-

activated pack cementation method’, Mater. Sci. Forum, 2003,

426–432, 1745–1750.

250. A. Iza-Mendia, A. Pinol-Juez, J. J. Urcola, I. Gutierrez:

‘Microstructural and mechanical behavior of a duplex stainless

steel under hot working conditions’, Metall. Mater. Trans. A,

1998, 29A, 2975–2985.

251. F. Jalilian, M. Jahazi, R. A. L. Drew: ‘Microstructural evolution

during transient liquid phase bonding of Inconel 617 using Ni–Si–

B filler metal’, Mater. Sci. Eng. A, 2006, A423, 269–281.

252. H. Jazaeri, F. J. Humphreys: ‘Quantifying recrystallization by

electron backscatter diffraction’, J. Microsc., 2004, 213, 241–246.

253. B. Y. Jeong, R. Gauvin, S. Yue: ‘Characterization of dual phase

steels by electron backscattered diffraction techniques’, ISS Mech.

Work. Steel Process. Conf., 2002, 44, 173–178.

254. B. Y. Jeong, S. Yue, R. Gauvin, R. A. L. Drew: ‘Microstructure

of TiN coatings by EBSD techniques’, Microsc. Microanal.,

2002b, 8, (Suppl. 2), 674–675.

255. B. Y. Jeong, R. Gauvin, S. Yue: ‘EBSD study of martensite in a

dual phase steel’, Microsc. microanal., 2002c, 8, (Suppl. 2), 700–

701.

256. L. Jian, C. M. Wayman: ‘Electron back scattering study of

domain structure in monoclinic phase of a rare-earth orthoniobate

LaNbO4’, Acta Metall. Mater., 1995, 43, 3893–3901.

257. H.-H. Jin, J.-H. Shim, Y. W. Cho, H.-C. Lee: ‘Formation of

intragranular acicular ferrite grains in a Ti-containing low carbon

steel’, ISIJ Int., 2003, 43, 1111–1113.

258. M. T. Johnson, C. B. Carter, J. Michael: ‘SEM analysis of oxide

thin films and reactions’, J. Am. Ceram. Soc., 1999a, 82, 1644–

1646.

259. M. T. Johnson, J. R. Michael, S. R. Gilliss, C. B. Carter: ‘Iron

oxide on (001) MgO’, Philos. Mag. A, 1999b, 79A, 2887–2898.



260. J. J. Jonas, Y. He, S. Godet: ‘The possible role of partial

dislocations in facilitating transformations of the Nishiyama–

Wassermann type’, Scr. Mater., 2005, 52, 175–179.

261. J. Jura, J. Pospiech, J. Bonarski, T. Baudin, C. Quesne, R. Penelle:

‘Microtexture inhomogeneity in hot rolled two-phase steel’, Proc.

12th Int. Conf. on ‘Textures of materials’, (ed. J. A. Szpunar),

1278–1283; 1999, Ottawa, NRC Research Press.

262. J. Jura, T. Baudin, M. H. Mathon, W. Swiatnicki, R. Penelle:

‘Microstructure and texture analysis in a cold-rolled austenitic–

ferritic steel with duplex structure’, Mater. Sci. Forum, 2002, 408–

412, 1359–1364.

263. D. Juul Jensen: ‘Three-dimensional orientation imaging’, in

‘Electron backscatter diffraction in materials science’, (ed. A. J.

Schwartz et al.), 91–104; 2000, New York, Kluwer Academic/

Plenum Publishers.

264. J. Kameda, A. Yamagishi, T. Kogure: ‘Morphological character-

istics of ordered kaolinite: investigation using electron back-

scattered diffraction’, Am. Mineral., 2005, 90, 1462–1465.

265. J.-H. Kang, D.-W. Suh, J.-Y. Cho, K. H. Oh, H.-C. Lee: ‘Effect of

external stress on the orientation distribution of ferrite’, Scr.

Mater., 2003, 48, 91–95.

266. J.-H. Kang, H.-C. Lee: ‘The orientation distribution of ferrite

grains dynamically and statically transformed from heavily

deformed austenite’, Mater. Trans., 2004, 45, 2219–2223.

267. B. Kaouache, S. Berveiller, K. Inal, A. Eberhardt, E. Patoor:

‘Stress analysis of martensitic transformation in Cu–Al–Be

polycrystalline and single-crystalline shape memory alloy’,

Mater. Sci. Eng. A, 2004, A378, 232–237.

268. M. Karadge, X. Zhao, M. Preuss, P. Siao: ‘Microtexture of the

thermally grown alumina in commercial thermal barrier coatings’,

Scr. Mater., 2006, 54, 639–644.

269. I. Karaman, H. Sehitoglu, H. J. Maier, M. Balzer: ‘Stress-state

effects on the stress-induced martensitic transformation of

carburized 4320 steels’, Metall. Mater. Trans. A, 1998, 29A,

427–437.

270. T. Karthikeyan, A. Dasgupta, A. J. Khan, S. Saroja,

M. Vijayalakshmi, D. Bhattacharjee, V. S. Ragunathan: ‘Study

of texture in a TiTaNb alloy using electron back scattered

diffraction technique’, Mater. Sci. Eng. A, 2005, A393, 294–302.

271. S. Katayama, A. Matsunawa, T. Iamboliev: ‘Formation mechan-

ism of rapidly quenched microstructure of laser welds metals in

austenitic stainless steels’, Proc. 5th Conf. on ‘Trends in welding

research’, (ed. J. M. Vitek et al.), 93–98; 1999, Materials Park,

OH, ASM International.

272. D. Katrakova, F. Mucklich: ‘Investigation of the corrosion of

steels in marine environment using orientation imaging micro-

scopy’, Prakt. Metallogr., 2000, 37, 643–656.

273. J. Kell, J. R. Tyrer, R. L. Higginson, R. C. Thomson:

‘Microstructural characterization of autogenous laser welds on

316L stainless steel using EBSD and EDS’, J. Microsc., 2005, 217,

167–173.

274. R. R. Keller, A. Roshko, R. H. Geiss, K. A. Bertness, T. P.

Quinn: ‘EBSD measurement of strains in GaAs due to oxidation

of buried AlGaAs layers’, Microelectron. Eng., 2004, 75, 96–102.

275. G. L. Kelly, H. Beladi, P. D. Hodgson: ‘Ultrafine grained ferrite

formed by interrupted hot torsion deformation of plain carbon

steel’, ISIJ Int., 2002, 42, 1585–1590.

276. A. Kermanpur, N. Varahram, P. Davami, M. Rappaz: ‘Thermal

and grain-structure simulation in a land-based turbine blade

directionally solidified with the liquid metal cooling process’,

Metall. Mater. Trans. B, 2000, 31B, 1293–1304.

277. L. Kestens, R. Petrov, Y. Houbaert: ‘Orientation selective

martensite transformation in an Fe–28Ni alloy’, ISIJ Int., 2003,

43, 1444–1452.

278. B.-K. Kim, J. A. Szpunar: ‘Orientation imaging microscopy for

the study of high temperature oxidation’, Scr. Mater., 2001, 44,

2605–2610.

279. B.-K. Kim, J. A. Szpunar: ‘Anisotropic microstructure of iron

oxides formed during high temperature oxidation of steel’, Mater.

Sci. Forum, 2002, 408–412, 1711–1716.

280. D.-I. Kim, K. H. Oh, H.-C. Lee, Y. J. Chang, W. S. Sohn, J. Jang:

‘Characterization of crystallographic properties of SMC poly Si

using electron backscattered diffraction’, J. Microsc., 2004, 215,

121–126.

281. M. C. Kim, Y. J. Oh, J. H. Hong: ‘Characterization of boundaries

and determination of effective grain size in Mn–Mo–Ni low alloy

steel from the view of misorientation’, Scr. Mater., 2000, 43, 205–

211.

282. W. E. King, J. S. Stolken, M. Kumar, A. J. Schwartz: ‘Strategies

for analyzing EBSD datasets’, in ‘Electron backscatter diffraction

in materials science’, (ed. A. J. Schwartz et al.), 153–170; 2000,

New York, Kluwer Academic/Plenum Publishers.

283. H. Kitahara, T. Kimura, N. Tsuji, Y. Minamino: ‘Structure of

martensite transformed from severely deformed austenite in Fe–

28.5at.%Ni’, in ‘Ultrafine grained materials III’, (ed. Y. T. Zhu et

al.), 369–374; 2004, Warrendale, PA, TMS.

284. H. Kitahara, R. Ueji, M. Ueda, N. Tsuji, Y. Minamino:

‘Crystallographic analysis of plate martensite in Fe–28.5at.% Ni

by FE-SEM/EBSD’, Mater. Charact., 2005, 54, 378–386.

285. H. Kitahara, R. Ueji, N. Tsuji, Y. Minamino: ‘Crystallographic

features of lath martensite in low-carbon steel’, Acta Mater., 2006,

54, 1279–1288.

286. A. M. Kliauga, M. Ferrante: ‘Liquid formation and microstruc-

tural evolution during re-heating and partial melting of an

extruded A356 aluminium alloy’, Acta Mater., 2005, 53, 345–356.

287. A. O. Kluken, Ø. Grong, J. Hjelen: ‘The origin of transformation

textures in steel weld metals containing acicular ferrite’, Metall.

Trans. A, 1991, 22A, 657–663.

288. A. Koblischka-Veneva, M. R. Koblischka, K. Ogasawara,

M. Murakami: ‘Position-dependent texture analysis of melt-

textured YBCO by means of electron backscatter diffraction’,

Physica C, 2003, 392C–396C, 607–612.

289. M. R. Koblischka, A. Koblischka-Veneva, E. S. Reddy, G. J.

Schmitz, K. Ogasawara, M. Murakami: ‘Orientations of

Y2BaCuO5 and YBCO within melt-textured and directional

solidified samples studied by EBSD’, Physica C, 2003, 392C–

396C, 589–595.

290. T. Kogure: ‘Identification of polytypic groups in hydrous

phyllosilicates using electron back-scattering patterns’, Am.

Mineral., 2002, 87, 1678–1685.

291. T. Kogure, J. Hybler, H. Yoshida: ‘Coexistence of two polytypic

groups in cronstedtite from Lostwithiel, England’, Clays Clay

Miner., 2002, 50, 504–513.

292. T. Kogure: ‘A program to assist Kikuchi pattern analyses’,

J. Crystallogr. Soc. Jpn, 2003, 45, 391–395 (partly in Japanese).

293. T. Kogure, M. Bunno: ‘Investigation of polytypes in lepidolite

using electron back-scattered diffraction’, Am. Miner., 2004, 89,

1680–1684.

294. T. Kogure, A. Inoue, D. Beaufort: ‘Polytype and morphology

analyses of kaolin minerals by electron back-scattered diffraction’,

Clays Clay Miner., 2005, 53, 201–210.

295. H. Kokawa, Y. S. Sato, A. Ishida, T. Arakawa, K. Hirano: ‘Effect

of magnetic stirring and grain structure on ultrasonic character-

istics in Inconel overlay-welds’, Proc. 5th Conf. on ‘Trends in

welding research’, (ed. J. M. Vitek et al.), 67–71; 1999, Materials

Park, OH, ASM International.

296. U. Konig, B. Davepon: ‘Microstructure of polycrystalline Ti and

its microelectrochemical properties by means of electron-

backscattering diffraction (EBSD)’, Electrochim. Acta, 2001, 47,

149–160.

297. J. Konrad, S. Zaefferer, D. Raabe: ‘Investigation of orientation

gradients around a hard Laves particle in a warm-rolled Fe3Al-

based alloy using a 3D EBSD-FIB technique’, Acta Mater., 2006,

54, 1369–1380.

298. U. Koops, D. Hesse, M. Martin: ‘High-temperature oxidation of

CoGa: influence of the crystallographic orientation on the

oxidation rate’, J. Mater. Res., 2002, 17, 2489–2498.

299. C. Korte, J. K. Farrer, N. Ravishankar, J. R. Michael,

H. Schmalzried, C. B. Carter: ‘On the influence of applied fields

on spinel formation’, MRS Proc., 2000, 586, 151–156.

300. A. D. Kostrivas, J. C. Lippold: ‘Simulating weld-fusion boundary

microstructures in aluminum alloys’, JOM, Feb. 2004, 56, 65–72.

301. M. V. Kral, G. Spanos: ‘Crystallography of grain boundary

cementite dendrites’, Acta Mater., 2003, 51, 301–311.

302. M. V. Kral, H. R. McIntyre, M. J. Smillie: ‘Identification of

intermetallic phases in a eutectic Al–Si casting alloy using electron

backscatter diffraction pattern analysis’, Scr. Mater., 2004, 51,

215–219.

303. M. V. Kral, G. Spanos: ‘Three-dimensional analysis and

classification of grain-boundary-nucleated proeutectoid ferrite

precipitates’, Metall. Mater. Trans. A, 2005, 36A, 1199–1207.

304. M. Kulka, A. Pertek, L. Klimek: ‘The influence of carbon content

in the borided Fe-alloys on the microstructure of iron borides’,

Mater. Charact., 2006, 56, 232–240.

305. T. Kunıkova, H. Wendrock, K. Wetzig, D. Hrivnakova: ‘EBSD

investigation of intergranular corrosion attack on low interstitial

stainless steel’, Mater. Corros., 2004, 55, 437–443.

306. M. Kurban, U. Erb, K. T. Aust: ‘A grain boundary characteriza-

tion study of boron segregation and carbide precipitation in alloy

304 austenitic stainless steel’, Scr. Mater., 2006, 54, 1053–1058.



307. A. Lambert-Perlade, A. F. Gourgues, A. Pineau: ‘Austenite to

bainite phase transformation in the heat-affected zone of a high

strength low alloy steel’, Acta Mater., 2004a, 52, 2337–2348.

308. A. Lambert-Perlade, A. F. Gourgues, J. Besson, T. Sturel,

A. Pineau: ‘Mechanisms and modelling of cleavage fracture in

simulated heat-affected zone microstructures of a high-strength

low alloy steel’, Metall. Mater. Trans. A, 2004b, 35A, 1039–1053.

309. L. Latu-Romain, D. Chaussende, P. Chaudouet, F. Robaut,

G. Berthome, M. Pons, R. Madar: ‘Study of 3C-SiC nucleation

on (0001) 6H–SiC nominal surfaces by the CF–PVT method’,

J. Cryst. Grow., 2005, 275, e609–e613.

310. O. Lavigne, C. Ramusat, P. Caron, D. Boivin, J.-L. Pouchou:

‘Application of EBSD analysis to the study of microstructural

instabilities in single crystal superalloys’, Rev. Met. JA, 2001, 140

(in French).

311. O. Lavigne, C. Ramusat, S. Drawin, P. Caron, D. Boivin, J.-L.

Pouchou: ‘Relationships between microstructural instabilities and

mechanical behaviour in new generation nickel-based single

crystal superalloys’, Proc. Conf. Superalloys 2004, (ed. K. A.

Green et al.), 667–675; 2004, Warrendale, PA, TMS.

312. K. Le Biavant, S. Pommier, C. Prioul: ‘Ghost structure effect on

fatigue crack initiation and growth’, Proc. Conf. ‘Titanium’99’,

(ed. I. V. Gorynin, S. S. Ushkov), 481–486; 1999, Saint-

Petersburg, CRISM.

313. K. Le Biavant, S. Pommier, C. Prioul: ‘Local texture and fatigue

crack initiation in a Ti–6Al–4V titanium alloy’, Fatigue Fract.

Eng. Mater. Struct., 2002, 25, 527–545.

314. J.-H. Lee, J.-H. Park, Y.-H. Lee, Y.-S. Jim, D. H. Shin: ‘Stability

of channels at a scalloplike Cu6Sn5 layer in solder interconnec-

tions’, J. Mater. Res., 2001, 16, 1227–1230.

315. J. H. Lee, A. Yoshikawa, Y. Murayama, Y. Waku, S. Hanada,

T. Fukuda: ‘Microstructure and mechanical properties of Al2O3/

Y3Al5O12/ZrO2 ternary eutectic materials’, J. Eur. Ceram. Soc.,

2005, 25, 1411–1417.

316. S. H. Lee, J.-Y. Kang, H. N. Han, K. H. Oh, H.-C. Lee, D.-W.

Suh, S.-J. Kim: ‘Variant selection in mechanically-induced

martensitic transformation of metastable austenitic steel’, ISIJ

Int., 2005, 45, 1217–1219.

317. S. Y. Lee, Y. B. Chun, J. W. Han, S. K. Hwang: ‘Effect of

thermomechanical processing on grain boundary characteristics in

two-phase brass’, Mater. Sci. Eng. A, 2003, A363, 307–315.

318. F. Lefebvre, S. Ganguly, I. Sinclair: ‘Micromechanical aspects of

fatigue in a MIG welded aluminium airframe alloy, Part 1:

microstructural characterization’, Mater. Sci. Eng. A, 2005, A397,

338–345.

319. E. M. Lehockey, Y. Lin, O. E. Lepik: ‘Mapping residual plastic

strain in materials using electron backscatter diffraction’, in

‘Electron backscatter diffraction in materials science’, (ed. A. J.

Schwartz et al.), 247–264; 2000, New York, Kluwer Academic/

Plenum Publishers.

320. J. R. Leinum, K. Moen, J. Hjelen, T. Malvik: ‘EBSD – a

supplementary technique in automatic characterisation of geolo-

gical samples with chemically similar minerals’, Proc. 13th Eur.

Microsc. Cong., (ed. D. Schryvers, T. S. Timmermans), Vol. 2,

563–564; 2004, Antwerp, The Belgian Society of Microscopy.

321. E. Lenarduzzi, P. Bounie, C. Schuman, M.-J. Philippe, D. Petelot:

‘Titanium oxidation during thermal treatment: inhibiting role of

nitrogen and epitaxial orientation relations evidenced by EBSD’,

Adv. Eng. Mater., 2003, 5, 587–593.

322. L. Levin, A. Tokar, A. Berner: ‘Microstructural characterization

of c-TiAl base alloy by electron probe X-ray microanalysis and

electron backscatter diffraction’, J. Mater. Sci., 2000, 35, 3923–

3929.

323. A. C. Lewis, J. F. Bingert, D. J. Rowenhorst, A. Gupta, A. B.

Geltmacher, G. Spanos: ‘Two- and three-dimensional micro-

structural characterization of a super-austenitic stainless steel’,

Mater. Sci. Eng. A, 2006, A418, 11–18.

324. D. Li, S. I. Wright, C. J. Boehlert: ‘The grain boundary character

distribution of a fully-orthorhombic Ti–25Al–24Nb(at.%) alloy’,

Scr. Mater., 2004, 51, 545–550.

325. D. Li, C. J. Boehlert: ‘Processing effects on the grain-boundary

character distribution of the orthorhombic phase in Ti–Al–Nb

alloys’, Metall. Mater. Trans. A, 2005a, 36A, 2569–2584.

326. D. Li, C. Liu, P. P. Conway: ‘Characteristics of intermetallics and

micromechanical properties during thermal ageing of Sn–Ag–Cu

flip-chip solder interconnects’, Mater. Sci. Eng. A, 2005b, A391,

95–103.

327. J. Li, Z. He, S. Saimoto, H. Sang: ‘Anomalous transformation

behaviour of off-eutectic Cu–Ag near the eutectic temperature’,

Proc. Int. Conf. on ‘Solid-solid phase transformations’, (ed. W. C.

Johnson et al.), 195–200; 1994, Warrendale, PA, TMS.

328. M. Li, T. Ishikawa, K. Nagashio, K. Kuribayashi, S. Yoda:

‘Experimental evidence of crystal fragmentation from highly

undercooled Ni99B1 melts processed on an electrostatic levitator’,

Metall. Mater. Trans. A, 2005a, 36A, 3254–3257.

329. M. Li, K. Nagashio, T. Ishikawa, S. Yoda, K. Kuribayashi:

‘Microtexture and macrotexture formation in the containerless

solidification of undercooled Ni–18.7at.% Sn eutectic melts’, Acta

Mater., 2005b, 53, 731–741.

330. M. Li, T. Ishikawa, K. Nagashio, K. Kuribayashi, S. Yoda: ‘A

comparative EBSP study of microstructure and microtexture

formation from undercooled Ni99B1 melts solidified on an

electrostatic levitator and an electromagnetic levitator’, Acta

Mater., 2006, 54, 3791–3799.

331. T. Li, A. M. Scotch, H. M. Chan, M. P. Harmer, S.-E. Park, T. R.

Schrout, J. R. Michael: ‘Single crystals of Pb(Mg1/3Nb2/3)O3–

35 mol% PbTiO3 from polycrystalline precursors’, J. Am. Ceram.

Soc., 1998, 81, 244–248.

332. B. Lindsley, X. Pierron: ‘Sub-solvus recrystallization mechanisms

in UdimetH alloy 720LI’, Proc. Superalloys 2000, (ed. T. M.

Pollock et al.), 59–68; 2000, Warrendale, PA, TMS.

333. D. Liu, H. V. Atkinson, R. L. Higginson: ‘Disagglomeration in

thixoformed wrought aluminium alloy 2014’, Mater. Sci. Eng. A,

2005, A392, 73–80.

334. H. Liu, M. Gao, D. G. Harlow, R. P. Wei: ‘Grain boundary

character, and carbide size and spatial distribution in a ternary

nickel alloy’, Scr. Metall. Mater., 1995, 32, 1807–1812.

335. R. E. Loge, J. W. Signorelli, Y. B. Chastel, M. Y. Perrin, R. A.

Lebensohn: ‘Sensitivity of a-Zy4 high temperature deformation

textures to the b-quenched precipitate structure and to recrys-

tallization: application to hot extrusion’, Acta Mater., 2000, 48,

3917–3930.

336. R. Loloee, W. P. Pratt, Jr, M. A. Crimp: ‘Crystallographic

characterization of sputter-deposited epitaxial Nb–Cu–Co and

Nb–Cu–Permalloy multilayers using electron back-scatter diffrac-

tion patterns’, Philos. Mag., 2001, 81, 261–273.

337. M. S. de Magalhaes, P. R. G. Brandao: ‘Electron backscattering

diffraction patterns (EBSDP): a new approach to iron ore and

sinter research’, Proc. 2nd Int. Conf. on ‘Iron ore industry’,

Kiruna, Sweden, June 2002, Lulea University, 217–233.

338. M. A. Mangan, P. D. Lauren, G. J. Shiflet: ‘Three-dimensional

reconstruction of Widmanstatten plates in Fe–12.3Mn–0.8C’,

J. Microsc., 1997, 188, 36–41.

339. M. A. Mangan, G. J. Shiflet: ‘Three dimensional investigation of

Cu–Ti discontinuous precipitation’, Scr. Mater., 1997, 37, 517–522.

340. M. A. Mangan, G. J. Shiflet: ‘Application of electron back-

scattered diffraction to habit planes in plates’, Scr. Mater., 1998,

39, 763–770.

341. M. A. Mangan, M. V. Kral, G. Spanos: ‘Correlation between the

crystallography and morphology of proeutectoid Widmanstatten

cementite precipitates’, Acta Mater., 1999, 47, 4263–4274.

342. M. A. Mangan, G. J. Shiflet: ‘The Pitsch–Petch orientation

relationship in ferrous pearlite at small undercooling’, Metall

Mater. Trans. A, 1999, 30A, 2767–2781.

343. W. Mao, H. Zhu, L. Chen, H. Feng, F. Lu: ‘Grain orientation

dependence on distance to surface of CVD diamond film’, Mater.

Sci. Technol., 2005, 21, 1383–1386.

344. C. Mapelli, R. Venturini: ‘Dependence of the mechanical proper-

ties of an a/b brass on the microstructural features induced by hot

extrusion’, Scr. Mater., 2006, 54, 1169–1173.

345. P. Markondeya Raj, F. Cosandey, W. R. Cannon, P.

Mainwarning: ‘Particle orientation and texture formation in tape

cast ceramic materials’, Proc. 12th Int. Conf. on ‘Textures of

materials’, (ed. J. A. Szpunar), 1476–1481; 1999, Ottawa, NRC

Research Press.

346. T. J. Marrow, H. Cetinel: ‘Short fatigue cracks in austempered

ductile cast iron (ADI)’, Fatigue Fract. Eng. Mater. Struct., 2000,

23, 425–434.

347. T. J. Marrow, H. Cetinel, N. Wardman, T. Brough, H. Bolyan:

‘Observation of retained austenite by electron backscatter

diffraction in austempered ductile cast iron (ADI)’, Proc. 20th

ASM Heat Treat. Soc. Conf., (ed. K. Funatani, G. E. Totten),

491–496; 2001, Materials Park, OH, ASM International.

348. T. J. Marrow, H. Cetinel, M. Al-Zalmah, S. Macdonald, P. J.

Withers, J. Walton: ‘Fatigue crack nuclei in austempered ductile

cast iron’, Fatigue Fract. Eng. Mater. Struct., 2002, 25, 635–648.

349. K. Marukawa, I. Kumagai, K. Takezawa: ‘Surface morphological

study of the transformation strain of martensites and bainites in

copper alloys’, Mater. Sci. Forum, 2000, 327–328, 417–420.



350. K. Maruta, M. Shimotomai: ‘Magnetic field-induced alignment of

steel microstructures’, J. Cryst. Grow., 2002, 237–239, 1802–1805.

351. T. A. Mason, B. L. Adams: ‘The application of orientation

imaging microscopy’, JOM, Oct. 1994, 46, 43–45.

352. S. Matsuoka, K. Sakata, O. Furukimi, T. Obara: ‘Orientational

morphology of low carbon steel rolled in nonrecrystallized

austenite region’, Proc. Int. Conf. on ‘Solid–solid phase transfor-

mations’99’, (ed. M. Koiwa et al.), 1537–1540; 1999, Sendai, The

Japan Institute of Metals.

353. A. Mauler, K. Kunze, J.-P. Burg, P. Philippot: ‘Identification of

electron backscatter diffraction patterns in a monoclinic solid-

state solution series: exemple of omphacite’, Mater. Sci. Forum,

1998, 273–275, 705–710.

354. A. Medevielle, I. Hugon, O. Dugne: ‘Electron backscatter

diffraction: applications for nuclear materials’, J. Microsc.,

1999, 195, 233–238.

355. C. Mesplont, B. C. De Cooman: ‘Effect of austenite deformation

on crystallographic texture during transformations in micro-

alloyed bainitic steel’, Mater. Sci. Technol., 2003, 19, 875–886.

356. J. R. Michael, R. P. Goehner: ‘Crystallographic phase identifica-

tion in the scanning electron microscope: backscattered electron

Kikuchi patterns imaged with a CCD-based detector’, MSA Bull.,

1993, 23, 168–175.

357. J. R. Michael, R. P. Goehner: ‘Advances in backscattered-electron

Kikuchi patterns for crystallographic phase identification’, Proc.

52nd Annu. Meet. Microsc. Soc. America, (ed. G. W. Bailey, A. J.

Garratt-Read), 596–597; 1994, San Francisco, CA, San Francisco

Press.

358. J. R. Michael: ‘Phase identification using EBSD in the SEM: what

can be done today and what we hope to do tomorrow’, Microsc.

Microanal., 1999, 5, 220–221.

359. J. R. Michael, J. A. Eades: ‘Use of reciprocal lattice layer spacing

in electron backscatter diffraction pattern analysis’,

Ultramicroscopy, 2000, 81, 67–81.

360. J. R. Michael: ‘Phase identification using electron backscatter

diffraction in the scanning electron microscope’, in ‘Electron

backscatter diffraction in materials science’, (ed. A. J. Schwartz

et al.), 75–89; 2000, New York, Kluwer Academic/Plenum

Publishers.

361. K. T. Miller, C. J. Chan, M. G. Cain, F. F. Lange: ‘Epitaxial

zirconia thin films from aqueous precursors’, J. Mater. Res., 1993,

8, 169–177.

362. T. Minoda, H. Yoshida: ‘Effect of grain boundary characteristics

on intergranular corrosion resistance of 6061 aluminum alloy

extrusion’, Metall. Mater. Trans. A, 2002, 33A, 2891–2898.

363. J. M. Missiaen, R. Voytovych, B. Gilles, N. Eustathopoulos:

‘Solid state spreading in the Cu/Cu system’, J. Mater. Sci., 2005,

40, 2377–2381.

364. S. Miura, H. Shimamura, J. Fujinaka, T. Mohri: ‘Effects of

microstructure on high temperature mechanical properties of

Al3Ti–Mo3Al two-phase intermetallic alloys’, Intermetallics, 2004,

12, 771–777.

365. S. Miura, H. Shimamura, K. Ohkubo, T. Mohri: ‘Investigation on

the microstructure and high temperature mechanical properties of

Al3Ti–Mo3Al two-phase alloys’, Mater. Sci. Forum, 2005a, 475–

479, 837–840.

366. S. Miura, M. Aoki, Y. Saeki, K. Ohkubo, Y. Mishima, T. Mohri:

‘Effects of Zr on the eutectoid decomposition behavior of Nb3Si

into (Nb)/Nb5Si3’, Metall. Mater. Trans. A, 2005b, 36A, 489–496.

367. S. Miura, K. Ohkubo, T. Mohri: ‘Effect of microstructure and Zr

addition on the crystallographic orientation relationships among

phases related to the eutectoid decomposition of Nb3Si in near

eutectic Nb–Si alloy’, MRS Proc., 2005c, 842, 279–284.

368. G. Miyamoto, T. Shinyoshi, J. Yamaguchi, T. Furuhara, T. Maki,

R. Uemori: ‘Crystallography of intragranular ferrite formed on

(MnSzV(C,N)) complex precipitate in austenite’, Scr. Mater.,

2003, 48, 371–377.

369. G. Miyamoto, A. Yonemoto, Y. Tanaka, T. Furuhara, T. Maki:

‘Microstructure in a plasma-nitrided Fe–18mass% Cr alloy’, Acta

Mater., 2006, 54, 4771–4779.

370. E. F. Monlevade, L. G. S. Falleiros: ‘Orientation relationships

associated with austenite formation from ferrite in a coarse-

grained duplex stainless steel’, Metall. Mater. Trans. A, 2006, 37A,

939–949.

371. S. Morito, H. Tanaka, R. Konishi, T. Furuhara, T. Maki: ‘The

morphology and crystallography of lath martensite in Fe–C


372. S. Morito, H. Saito, T. Ogawa, T. Furuhara, T. Maki: ‘Effect of

austenite grain size on the morphology and crystallography of lath

martensite in low carbon steels’, ISIJ Int., 2005, 45, 91–94.

373. S. Morito, X. Huang, T. Furuhara, T. Maki, N. Hansen: ‘The

morphology and crystallography of lath martensite in alloy steels’,

Acta Mater., 2006, 54, 5323–5331.

374. H. Moustahfid, N. Gey, M. Humbert, M. J. Philippe: ‘Study of

the b–a phase transformations of a Ti–64 sheet induced from a

high-temperature b state and a high-temperature azb state’,

Metall. Mater. Trans. A, 1997a, 28A, 51–61.

375. H. Moustahfid, M. Humbert, M. J. Philippe: ‘Modeling of the

texture transformation in a Ti–64 sheet after hot compression’,

Acta Metall., 1997b, 45, 3785–3790.

376. Y. Murayama, S. Hanada, J. H. Lee, A. Yoshikawa, T. Fukuda:

‘Microstructure and high-temperature strength of directionally

solidified Al2O3/YAG/ZrO2 eutectic composite’, Mater. Trans.,

2004a, 45, 303–306.

377. Y. Murayama, S. Hanada, J. H. Lee, A. Yoshikawa, T. Fukuda:

‘Texture control and high-temperature strength of directionally

solidified Al2O3/YAG/ZrO2 eutectic composite rods’, Mater.

Trans., 2004b, 45, 2697–2702.

378. V. S. R. Murthy, K. Kawahara, Y. Saito, T. Matsuzaki,

T. Watanabe: ‘Orientation and grain boundary microstructure

of alumina in Al/Al2O3 composites produced by reactive metal

penetration’, J. Am. Ceram. Soc., 2005, 88, 2902–2907.

379. K. Nagashio, H. Murata, K. Kuribayashi: ‘Spreading and

solidification behavior of molten Si droplets impinging on

substrates’, Acta Mater., 2004, 52, 5295–5301.

380. K. Nagashio, K. Kuribayashi: ‘Growth mechanism of twin-

related and twin-free facet Si dendrites’, Acta Mater., 2005, 53,

3021–3029.

381. K. Nagashio, K. Kuribayashi: ‘Experimental verification of

ribbon formation process in chill-block melt spinning’, Acta

Mater., 2006, 54, 2353–2360.

382. M. Nakai, H. Kaiden, J. H. Lee, A. Yoshikawa, K. Sugiyama,

T. Fukuda: ‘Eutectic Al2O3/Y3Al5O12 fibers modified by the

substitution of Sc2O3, Fe2O3 or Cr2O3’, J. Eur. Ceram. Soc., 2005,

25, 1405–1410.

383. H. Nakashima, D. Terada, F. Yoshida, H. Hayakawa, H. Abe:

‘EBSP analysis of modified 9Cr–1Mo martensitic steel’, ISIJ Int.,

2001, 41, Supplement, S97–S100.

384. K. Neishi, T. Uchida, N. Ashie, A. Yamauchi, K. Nakamura,

Z. Horita, T. G. Langdon: ‘Superplasticity of a Cu–Zn–Sn alloy

processed by equal-channel angular pressing’, Mater. Sci. Forum,

2004, 447–448, 483–488.

385. T. W. Nelson, J. C. Lippold, M. J. Mills: ‘A fundamental

investigation of the evolution of boundaries and interfaces along

the fusion boundary in dissimilar metal welds’, Proc. 5th Conf. on

‘Trends in welding research’, (ed. J. M. Vitek et al.), 221–226;

1999a, Materials Park, OH, ASM International.

386. T. W. Nelson, J. C. Lippold, M. J. Mills: ‘Nature and evolution of

the fusion boundary in ferritic–austenitic dissimilar weld metals,

Part 1: nucleation and growth’, Weld. Res. Suppl., Oct. 1999b,

329s–337s.

387. M. Newell, K. Devendra, P. A. Jennings, N. D’Souza: ‘Role of

dendrite branching and growth kinetics in the formation of low

angle boundaries in Ni-base superalloys’, Mater. Sci. Eng. A,

2005, A412, 307–315.

388. K. Nogita, A. K. Dahle: ‘Determination of eutectic solidification

mode in Sr-modified hypoeutectic Al–Si alloys by EBSD’, Mater.

Trans., 2001a, 42, 207–214.

389. K. Nogita, A. K. Dahle: ‘Eutectic growth mode in strontium,

antimony and phosphorus modified hypoeutectic Al–Si foundry

alloys’, Mater. Trans., 2001b, 42, 393–396.

390. K. Nogita, A. K. Dahle: ‘Eutectic solidification in hypoeutectic

Al–Si alloys: electron backscatter diffraction analysis’, Mater.

Charact., 2001c, 46, 305–310.

391. K. Nogita, S. D. McDonald, J. W. Zindel, A. K. Dahle: ‘Eutectic

solidification mode in sodium modified Al–7mass%Si–

3.5mass%Cu–0.2mass%Mg casting alloys’, Mater. Trans., 2001,

42, 1981–1986.

392. J. Nohava, P. Haushild, M. Karlık, P. Bompard: ‘Electron

backscattering diffraction analysis of secondary cleavage cracks in

a reactor pressure vessel steel’, Mater. Charact., 2003, 49, 211–

217.

393. G. Nolze, V. Geist: ‘A new method for the investigation of

orientation relationships in meteoritic plessite’, Cryst. Res.

Technol., 2004, 39, 343–352.

394. G. Nolze: ‘Characterization of the fcc/bcc orientation relationship

by EBSD using pole figures and variants’, Z. Metallkd., 2004, 95,

744–755.

395. G. Nolze, V. Geist, R. S. Neumann, M. Buchheim: ‘Investigation

of orientation relationships by EBSD and EDS on the example of



the Watson iron meteorite’, Cryst. Res. Technol., 2005, 40, 791–

804.

396. G. Nolze: ‘Improved determination of fcc/bcc orientation

relationships by use of high-indexed pole figures’, Cryst. Res.

Technol., 2006, 41, 72–77.

397. E. Novillo, D. Hernandez, I. Gutierrez, B. Lopez: ‘Analysis of

ferrite grain growth mechanism during c–a transformation in a

niobium alloyed steel using EBSD’, Mater. Sci. Eng. A, 2004,

A385, 83–90.

398. M. M. Nowell, S. I. Wright: ‘Phase differentiation via combined

EBSD and XEDS’, J. Microsc., 2004, 213, 296–305.

399. V. Ocelık, J. A. Vreeling, J. T. M. De Hosson: ‘EBSP study of

reaction zone in SiC/Al metal matrix composite prepared by laser

melt injection’, J. Mater. Sci., 2001, 36, 4845–4849.

400. S. T. Oh, K. K. Park, H.-N. Han, S.-H. Park, K. H. Oh:

‘Transformation behavior of retained austenite in hydroformed

TRIP steel’, Mater. Sci. Forum, 2002, 408–412, 1341–1346.

401. Y. Ohmori: ‘Crystallographic aspects of bainite transformation in

steels’, Scr. Mater., 2002, 47, 201–206.

402. A. F. Padilha, V. Randle, I. F. Machado: ‘Microstructure and

microtexture changes during solution nitriding to produce

austenitic case on ferritic–austenitic duplex stainless steel’,

Mater. Sci. Technol., 1999, 15, 1015–1018.

403. Y. Pang, P. Wynblatt: ‘Effects of Nb doping and segregation on

the grain boundary plane distribution in TiO2’, J. Am. Ceram.

Soc., 2006, 89, 666–671.

404. Y. Paransky, A. Berner, I. Gotman: ‘Microstructure of reaction

zone at the Ti–AlN interface’, Mater. Lett., 1999, 40, 180–186.

405. Y. Paransky, I. Gotman, E. Y. Gutmanas: ‘Reactive phase

formation at AlN–Ti and AlN–TiN interfaces’, Mater. Sci. Eng.

A, 2000, A277, 83–94.

406. Y. M. Paransky, A. I. Berner, I. Y. Gotman, E. Y. Gutmanas:

‘Phase recognition in AlN–Ti system by energy dispersive

spectroscopy and electron backscatter diffraction’, Microchim.

Acta, 2000, 134, 171–177.

407. C.-M. Park, G. Bruckner, G. Gottstein: ‘Orientation relationships

and variant selection during a- to c- phase transformation in low

carbon steel’, Mater. Sci. Forum, 2002, 408–412, 1191–1196.

408. H. Park, H. M. Chan, R. P. Vinci: ‘Patterning of sapphire

substrates via a solid state conversion process’, J. Mater. Res.,

2005, 20, 417–423.

409. J. Y. Park, K. H. Oh, H. Y. Ra: ‘Microstructure and crystal-

lographic texture of strip-cast 4.3wt%Si steel sheet’, Proc. 12th Int.

Conf. on ‘Textures of materials’, (ed. J. A. Szpunar), 1065–1070;

1999, Ottawa, NRC Research Press.

410. K. K. Park, S. T. Oh, S. M. Baeck, D.-I. Kim, J. H. Han, H. N.

Han, S.-H. Park, C. G. Lee, S.-J. Kim, K. H. Oh: ‘In situ

deformation behavior of retained austenite in TRIP steel’, Mater.

Sci. Forum, 2002, 408–412, 571–576.

411. Y. T. Pei, V. Ocelik, J. T. M. De Hosson: ‘SiCp/Ti6Al4V

functionally graded materials produced by laser melt injection’,

Acta Mater., 2002, 50, 2035–2051.

412. G. M. Pennock, A. Barnhoorn, A. J. Bons, M. R. Drury: ‘EBSD

of zeolites’, J. Mater. Sci. Lett., 2001, 20, 1099–1101.

413. B. Petit, N. Gey, M. Cherkaoui, B. Bolle, M. Humbert:

‘Deformation behavior and microstructure/texture evolution of

an annealed 304 AISI stainless steel sheet. Experimental and

micromechanical modeling’, Int. J. Plast., 2007, 23, 323–341.

414. R. Petrov, L. Kestens, Y. Houbaert: ‘Characterization of the

microstructure and transformation behaviour of strained and

nonstrained austenite in Nb–V-alloyed C–Mn steel’, Mater.

Charact., 2004, 53, 51–61.

415. K. Pettersen, N. Ryum: ‘Crystallography of directionally solidi-

fied magnesium alloy AZ91’, Metall. Trans. A, 1989, 20A, 847–

852.

416. K. Pettersen, O. Lohne, N. Ryum: ‘Dendritic solidification of

magnesium alloy AZ91’, Metall. Trans. A, 1990, 21A, 221–230.

417. D. Phelan, R. Dippenaar: ‘Widmanstatten ferrite plate formation

in low-carbon steels’, Metall. Mater. Trans. A, 2004, 35A, 3701–

3706.

418. D. Phelan, N. Stanford, R. Dippenaar: ‘In situ observations of

Widmanstatten ferrite formation in a low-carbon steel’, Mater.

Sci. Eng. A, 2005, A407, 127–134.

419. S. Piazolo, M. W. Jessell, D. J. Prior, P. D. Bons: ‘The integration

of experimental in situ EBSD observations and numerical

simulations: a novel technique of microstructural process analy-

sis’, J. Microsc., 2004a, 213, 273–284.

420. S. Piazolo, G. G. E. Seward, N. Seaton, D. J. Prior: ‘The potential

of combined in situ heating experiments and detailed EBSD

analysis in the investigation of grain scale processes such as

recrystallization and phase transformation’, Mater. Sci. Forum,

2004b, 467–470, 1407–1412.

421. Y. Ping, Y. W. Yue, S. Z. Qing: ‘Texture developments during

ferrite refinement through deformation-enhanced ferrite transfor-

mation and dynamic recrystallization in low carbon steel’, Mater.

Sci. Forum, 2005, 475–479, 165–168.

422. A. Pinol-Juez, A. Iza-Mendia, I. Gutierrez: ‘d/c interface

boundary sliding as a mechanism for strain accommodation

during hot deformation in a duplex stainless steel’, Metall. Mater.

Trans. A, 2000, 31A, 1671–1677.

423. J. L. Pouchou, A. Denquin, A. Ferrini: ‘Contribution of EBSD to

understanding of massive c transformation in TiAl’, Microchim.

Acta, 2004a, 145, 177–182.

424. J.-L. Pouchou, A. Ferrini, A. Denquin, D. Boivin, Y. Renollet,

C. Gallais: ‘Local crystallographic analysis and large-scale

orientation mapping: two very different examples of use of

EBSD analysis’, in ‘L’analyse EBSD: principes et applications (in

French)’, (ed. J.-L. Pouchou), 51–78; 2004b, Les Ulis, EDP

Sciences.

425. G. Powell, V. Randle: ‘The effect of Si on the relationship between

orientation and carbide morphology in high chromium white

irons’: J. Mater. Sci., 1997, 32, 561–565.

426. D. J. Prior, A. P. Boyle, F. Brenker, M. C. Cheadle, A. Day,

G. Lopez, L. Peruzzo, G. J. Potts, S. Reddy, R. Spiess, N. E.

Timms, P. Trimby, J. Wheeler, L. Zetterstrom: ‘The application of

electron backscatter diffraction and orientation contrast imaging

in the SEM to textural problems in rocks’, Am. Mineral., 1999, 84,

1741–1759.

427. J. Qi, W. Yang, Z. Sun: ‘Mechanisms of microstructure evolution

during deformation of undercooled austenite in a low carbon

steel’, J. Univ. Sci. Technol. Beijing, 2002, 24, 97–102 (partly in

Chinese).

428. M. Qian, J. C. Lippold: ‘The effect of annealing twin-generated

special grain boundaries on HAZ liquation cracking of nickel-

base superalloys’, Acta Mater., 2003, 551, 3351–3361.

429. A. Quiroga, S. Claessens, B. Gay, M. Rappaz: ‘A novel

experiment for the study of substrate-induced nucleation in

metallic alloys: application to Zn–Al’, Metall. Mater. Trans. A,

2004, 35A, 3543–3550.

430. A. J. Ramirez, J. C. Lippold: ‘High temperature behavior of Ni-

base weld metal Part I. Ductility and microstructural character-

ization’, Mater. Sci. Eng. A, 2004, A380, 259–271.

431. V. Randle, G. Laird II: ‘A microtexture study of eutectic carbides

in white cast irons using electron back-scatter diffraction’,

J. Mater. Sci., 1993, 28, 4245–4249.

432. V. Randle, G. L. F. Powell: ‘Application of electron backscatter

diffraction to orientation measurements of individual carbides in a

white cast iron’, J. Mater. Sci. Lett., 1993, 12, 779–781.

433. V. Randle: ‘Application of electron backscatter diffraction to steel

products’, Ironmaking Steelmaking, 1994, 21, 209–214.

434. V. Randle: ‘Application of electron backscatter diffraction to

grain boundary characterisation’, Int. Mater. Rev., 2004, 49, 1–11.

435. M. Rappaz, S. Henry: ‘Why twinned dendrites in cast aluminum

alloys ?’, Proc. Solidification 1999, (ed. W. H. Hofmeister et al.),

131–141; 1999, Warrendale, PA, TMS.

436. M. Rappaz, A. Quiroga, A. Semoroz: ‘Effect of lead and

antimony on the grain structure of directionally solidified Zn–Al

alloys’, Proc. Symp. on ‘Solidification processes and microstruc-

tures – A Symposium in honor of Wilfried Kurz’, (ed. M. Rappaz

et al.), 225–230; 2004, Warrendale, PA, TMS.

437. B. Rau, I. Sieber, B. Selle, S. Brehme, U. Knipper, S. Gall,

W. Fuhs: ‘Homo-epitaxial Si absorber layers grown by low-

temperature ECRCVD’, Thin Solid Films, 2004, 451–452, 644–648.

438. D. T. Read, Y. W. Cheng, R. Geiss: ‘Morphology, microstructure,

and mechanical properties of a copper electrodeposit’,

Microelectron. Eng., 2004, 75, 63–70.

439. H. Regle, N. Maruyama, N. Yoshinaga: ‘Texture of multiphased

steel sheets’, Proc. Int. Conf. on ‘Advanced high strength sheet

steels for automotive applications’, (ed. M.A. Baker), 239–246;

2004, Warrendale, PA, AIST.

440. C. V. Robino, J. R. Michael, M. J. Cieslak: ‘Solidification and

welding metallurgy of Thermo-Span alloy’, Sci. Technol. Weld.

Join., 1997, 2, 220–230.

441. C. V. Robino, J. R. Michael, M. C. Maguire: ‘The solidification

and welding metallurgy of galling-resistant stainless steels’, Weld.

J. Res. Suppl., 1998, 77, 446s–457s.

442. C. V. Robino, J. R. Michael, J. J. Stephens, J. N. DuPont, D. B.

Williams, R. E. Mizia: ‘Solidification and weldability of

gadolinium-containing nickel-based alloys’, Proc. 6th Conf. on



‘Trends in welding research’, (ed. S. A. David et al.), 627–632;

2003, Materials Park, OH, ASM International.

443. P. P. Rodriguez, A. Ibarra, A. Iza-Mendia, V. Recarte, J. I. Perez-

Landazabal, J. San Juan, M. L. No: ‘Influence of thermo-

mechanical processing on the microstructure of Cu-based shape

memory alloys produced by powder metallurgy’, Mater. Sci. Eng.

A, 2004, A378, 263–268.

444. K. A. Rogers, K. P. Trumble, B. J. Dalgleish, I. E. Reimanis:

‘Role of oxygen in microstructure development at solid-state

diffusion-bonded Cu/a–Al2O3 interfaces’, J. Am. Ceram. Soc.,

1994, 77, 2036–2042.

445. T. Ros-Yanez, Y. Houbaert, A. Mertens: ‘Characterization of

TRIP-assisted multiphase steel surface topography by atomic

force microscopy’, Mater. Charact., 2001, 47, 93–104.

446. T. Ros Yanez, Y. Houbaert: ‘Characterisation of multiphase steel

surface topography by atomic force microscopy’, Prakt.

Metallogr., 2002, 39, 202–210.

447. D. J. Rowenhorst, A. Gupta, C. R. Feng, G. Spanos: ‘3D

crystallographic and morphological analysis of coarse martensite:

combining EBSD and serial sectioning’, Scr. Mater., 2006, 55, 11–

16.

448. M. A. Ruggiero, J. W. Rutter: ‘Origin of microstructure in 350K

eutectic of Bi–In–Sn ternary system’, Mater. Sci. Technol., 1995,

11, 136–142.

449. M. Ruhnow, I. Haase, H. Wendrock: ‘Structures similar to a

quasicrystal in technical aluminum alloys’, Z. Metallkd., 2002, 93,

117–122.

450. L. Ryde, D. Artymovicz, W. B. Hutchinson: ‘Transformation

textures and texture memory in low carbon steels’, Proc. 12th Int.

Conf. on ‘Textures of materials’, (ed. J. A. Szpunar), 1031–1036;

1999, Ottawa, NRC Research Press.

451. C. Saito, Y. Furuya, T. Okazaki, T. Matzusaki, T. Watanabe:

‘Microstructure and magnetostriction of rapid-solidified Fe–

15at%Ga alloy’, Mater. Trans., 2004, 45, 193–198.

452. T. Sakata, H. Y. Yasuda, Y. Umakoshi: ‘Formation process of

transformation texture from the b to a phase in Cu–42mass%Zn

alloy’, Scr. Mater., 2000, 43, 411–416.

453. T. Sakata, H. Y. Yasuda, Y. Umakoshi: ‘Control of micro-

structure and orientation distribution in Ni–Al –based (b/c’) two

phase alloys by thermomechanical processing’, Acta Mater., 2001,

49, 4231–4239.

454. I. Samajdar, R. D. Doherty: ‘Grain boundary misorientation in

DC-cast aluminum alloy’, Scr. Metall. Mater., 1994, 31, 527–530.

455. T. Sano, D. M. Saylor, G. S. Rohrer: ‘Surface energy anisotropy

of SrTiO3 at 1400uC in air’, J. Am. Ceram. Soc., 2003a, 86, 1933–

1939.

456. T. Sano, H. Mori, E. Ohmura, I. Miyamoto: ‘Femtosecond laser

quenching of the e phase of iron’, Appl. Phys. Lett., 2003b, 83,

3498–3500.

457. T. Sano, C.-S. Kim, G. S. Rohrer: ‘Shape evolution of SrTiO3

crystals during coarsening in a titania-rich liquid’, J. Am. Ceram.

Soc., 2005, 88, 993–996.

458. Y. Sasaki, K. Ohkawara, M. Iguchi, K. Ishii, M. Hino:

‘Measuring strains for hematite phase in sinter by electron

backscattering diffraction method’, ISIJ Int., 2005a, 45, 582–586.

459. Y. Sasaki, M. Bahgat, M. Iguchi, K. Ishii: ‘The preferable growth

direction of iron nuclei on wustite surface during reduction’, ISIJ

Int., 2005b, 45, 1077–1083.

460. Y. S. Sato, H. Kokawa, T. Kuwana: ‘Effect of nitrogen on sigma

transformation in duplex stainless steel weld metal at high

temperatures’, Proc. 5th Conf. on ‘Trends in welding research’,

(ed. J. M. Vitek et al.), 131–136; 1999, Materials Park, OH, ASM

International.

461. Y. S. Sato, H. Kokawa: ‘Preferential precipitation site of sigma

phase in duplex stainless steel weld metal’, Scr. Mater., 1999, 40,

659–663.

462. Y. S. Sato, H. Kokawa, K. Ikeda, M. Enomoto, S. Jogan,

T. Hashimoto: ‘Microtexture in the friction-stir weld of an

aluminum alloy’, Metall. Mater. Trans. A, 2001, 32A, 941–948.

463. D. M. Saylor, G. S. Rohrer: ‘Measuring the influence of grain-

boundary misorientation on thermal groove geometry in ceramic

polycrystals’, J. Am. Ceram. Soc., 1999, 82, 1529–1536.

464. P. Schmutz, V. Guillaumin, R. S. Lillard, J. A. Lillard, G. S.

Frankel: ‘Influence of dichromate ions on corrosion processes

on pure magnesium’, J. Electrochem. Soc., 2003, 150, B99–

B110.

465. M. Schreck, T. Bauer, S. Gsell, F. Hormann, H. Bielefeldt,

B. Strizker: ‘Domain formation in diamond nucleation on

iridium’, Diam. Relat. Mater., 2003, 12, 262–267.

466. C. Schuh, D. C. Dunand: ‘Whisker alignment of Ti–6Al–4V/TiB

composites during deformation by transformation superplasti-

city’, Int. J. Plast., 2001, 17, 317–340.

467. C. A. Schuh, K. Anderson, C. Orme: ‘Rapid assessment of

anisotropic surface processes: experiments on the corrosion of

Inconel 600’, Surf. Sci., 2003, 544, 183–192.

468. R. A. Schwarzer, H. Weiland: ‘Texture analysis by the measure-

ment of individual grain orientations–electron microscopical

methods and application on dual-phase steel’, Textures

Microstruct., 1988, 8–9, 551–577.

469. R. A. Schwarzer, A. K. Singh, J. Sukkau: ‘Discrimination and

mapping of phase distributions by automated crystal orientation

measurement’, Mater. Sci. Technol., 2000, 16, 1389–1392.

470. A. J. Schwartz, M. Kumar, B. L. Adams (eds.): ‘Electron

backscatter diffraction in materials science’; 2000, New York,


471. P. Scott, M. Foucault, B. Brugier, J. Hickling, A. McIlree:

‘Examination of stress corrosion cracks in alloy 182 weld metal

after exposure to PWR primary water’, Proc. 12th Int. Symp. on

‘Environmental degradation of materials in nuclear systems-water

reactors’, (ed. T. R. Allen et al.), 497–507; 2005, Warrendale, PA,

TMS.

472. S. Sekfali, C. Rey, B. Marini: ‘Modelling the behaviour of bainite

and martensite’, Proc. Materiaux 2002, Tours, France, October

2002, Universite Technologique de Belfort-Montbeliard, 4 (CD-

ROM) (in French).

473. V. Semenov, E. Rabkin, E. Bischoff, W. Gust: ‘The effect of the

grain boundary misorientation on the kinetics of the discontin-

uous ordering reaction in Fe–50at.%Co’, Acta Mater., 1998, 46,

2289–2298.

474. A. Semoroz, Y. Durandet, M. Rappaz: ‘EBSD characterization of

dendrite growth directions, texture and misorientations in hot-

dipped Al–Zn–Si coatings’, Acta Mater., 2001, 49, 529–541.

475. A. Semoroz, L. Strezov, M. Rappaz: ‘Orientation domains and

texture in hot-dipped galvanized coatings’, Metall. Mater. Trans.

A, 2002a, 33A, 2695–2701.

476. A. Semoroz, L. Strezov, M. Rappaz: ‘Numerical simulation of Zn

coating solidification’, Metall. Mater. Trans. A, 2002b, 33A,

2685–2694.

477. J. Sengupta, H.-J. Shin, B. G. Thomas, S.-H. Kim: ‘Micrograph

evidence of meniscus solidification and sub-surface microstructure

evolution in continuous-cast ultralow-carbon steels’, Acta Mater.,

2006, 54, 1165–1173.

478. M. Sennour, P. H. Jouneau, C. Esnouf: ‘TEM and EBSD

investigation of continuous and discontinuous precipitation of

CrN in nitrided pure Fe–Cr alloys’, J. Mater. Sci., 2004, 39, 4521–

4531.

479. D.-H. Seo, J.-K. Choi, W.-Y. Choo: ‘Ferrite grain refinement by

multi-pass rolling at intercritical temperature in low carbon steel’,

Proc. Thermec 2000, (ed. T. Chandra et al.), 6 pp.; 2000,

Amsterdam, Elsevier Science (CD-ROM).

480. G. G. E. Seward, D. J. Prior, J. Wheeler, S. Celotto, D. J. M.

Halliday, R. S. Paden, M. R. Tye: ‘High-temperature electron

backscatter diffraction and scanning electron microscopy imaging

techniques: in situ investigation of dynamic processes’, Scanning,

2002, 24, 232–240.

481. G. G. E. Seward, S. Celotto, D. J. Prior, J. Wheeler, R. C. Pond:

‘In situ SEM-EBSD observations of the hcp to bcc phase

transformation in commercially pure titanium’, Acta Mater.,

2004, 52, 821–852.

482. A. Shibata, S. Morito, T. Furuhara, T. Maki: ‘Local orientation

change inside lenticular martensite plate in Fe–33Ni alloy’, Scr.

Mater., 2005, 53, 597–602.

483. S. H. Shim, K. Niihara, K. H. Auh, K. B. Shim: ‘Crystallographic

orientation of ZrB2–ZrC composites manufactured by the spark

plasma sintering method’, J. Microsc., 2002, 205, 238–244.

484. M. Slamova, M. Karlık, F. Robaut, P. Slama, M. Veron:

‘Differences in microstructure and texture of Al–Mg sheets

produced by twin-roll continuous casting and by direct-chill

casting’, Mater. Charact., 2003, 49, 231–240.

485. J. A. Small, J. R. Michael: ‘Phase identification of individual

crystalline particles by electron backscatter diffraction’,

J. Microsc., 2001, 201, 59–69.

486. J. A. Small, J. R. Michael, D. S. Bright: ‘Improving the quality of

electron backscatter diffraction (EBSD) patterns from nanopar-

ticles’, J. Microsc., 2002, 206, 170–178.

487. K. A. Son, N. Missert, J. C. Barbour, J. J. Hren, R. G. Copeland,

K. G. Minor: ‘Growth and oxidation of thin film Al2Cu’,

J. Electrochem. Soc., 2001, 148, B260–B263.



488. G. S. Song, M. V. Kral: ‘Characterization of cast Mg–Li–Ca

alloys’, Mater. Charact., 2005, 54, 279–286.

489. J. M. Song, T. S. Lui, L. H. Chen: ‘A study on inhomogeneous

distribution of temper graphite particles in strip-cast Fe–C–Si

alloys’, Metall. Mater. Trans. A, 2002, 33A, 1263–1273.

490. J. M. Song, L. H. Chen, T. S. Lui: ‘Examination on the growth

textures of eutectic cementite of various morphologies’, Mater.

Sci. Eng. A, 2003, A347, 5–8.

491. R. Soundararajan, R. N. Das, R. Tjossem, A. Bhandyopadhyay,

K. G. Lynn, E. E. Eisser, J. Lazaroff: ‘Growth and characteriza-

tion of single-crystal lead magnesium niobate–lead titanate via

high-pressure vertical Bridgman method’, J. Mater. Res., 2004, 19,

609–615.

492. G. Spanos, M. G. Hall: ‘The formation mechanism(s), morphol-

ogy, and crystallography of ferrite sideplates’, Metall. Mater.

Trans. A, 1996, 27A, 1519–1534.

493. G. Spanos, A. W. Wilson, M. V. Kral: ‘New insights into the

Widmanstatten proeutectoid ferrite transformation: integration of

crystallographic and three-dimensional morphological observa-

tions’, Metall. Mater. Trans. A, 2005, 36A, 1209–1218.

494. C. Stallybrass, G. Sauthoff: ‘Ferritic Fe–Al–Ni–Cr alloys with

coherent precipitates for high-temperature applications’, Mater.

Sci. Eng. A, 2004, A387–A389, 985–990.

495. N. Stanford, A. Djakovic, B. A. Shollock, M. McLean,

N. D’Souza, P. A. Jennings: ‘Seeding of single crystal superalloys

– role of seed melt-back on casting defects’, Scr. Mater., 2004a,

50, 159–163.

496. N. Stanford, A. Djakovic, B. Shollock, M. McLean, N. D’Souza,

P. Jennings: ‘Defect grains in the melt-back region of CMSX–4

single crystal seeds’, Proc. Superalloys 2004, (ed. K. A. Green

et al.), 719–726; 2004b, Warrendale, PA, TMS.

497. N. Stanford, P. S. Bate: ‘Crystallographic variant selection in Ti–

6Al–4V’, Acta Mater., 2004, 52, 5215–5224.

498. N. Stanford, P. S. Bate: ‘Crystallographic variant selection in a–bbrass’, Acta Mater., 2005, 53, 859–867.

499. L. Storojeva, D. Ponge, R. Kaspar, D. Raabe: ‘Development of

microstructure and texture of medium carbon steel during heavy

warm deformation’, Acta Mater., 2004, 52, 2209–2220.

500. B. B. Straumal, N. F. Vershinin, R. Dimitriou, W. Gust,

T. Watanabe, Y. Igarashi, X. Zhao: ‘The grain structure of

vacuum arc deposited Co thin films’, Mater. Sci. Forum, 1999,

294–296, 787–790.

501. E. Strom, J. Zhang: ‘Mechanical anisotropy and segregation in

Mo5Si3 studied by EBSD’, Intermetallics, 2005, 13, 367–372.

502. S. F. Su, J. C. Huang, H. K. Lin, N. J. Ho: ‘Electron beam

welding behavior in Mg–Al based alloys’, Metall. Mater. Trans.

A, 2002, 33A, 1461–1473.

503. D.-W. Suh, J.-Y. Cho, J.-H. Kang, K. H. Oh, H.-C. Lee: ‘Effects

of uniaxial stress on the nucleation behavior of ferrite from

deformed austenite’, Proc. Thermec 2000, (ed. T. Chandra et al.),

6 pp.; 2000, Amsterdam, Elsevier Science (CD-ROM).

504. D.-W. Suh, J.-H. Kang, K.H. Oh, H.-C. Lee: ‘Evaluation of the

deviation angle of ferrite from the Kudjumov-Sachs relation-

ship in a low carbon steel by EBSD’, Scr. Mater., 2002, 46, 375–

378.

505. E. Summers, T. A. Lograsso, J. D. Snodgrass, J. Slaughter:

‘Magnetic and mechanical properties of polycrystalline Galfenol’,

Proc. Int. Symp. on ‘Smart structures and materials’, (ed. D. C.

Lagoudas), Vol. 5387, 448–459; 2004, Bellingham, VA, USA,

SPIE.

506. C.-C. Sun, N. Ryum: ‘Crystallographic aspect of cellular

solidification’, Mater. Charact., 1992, 29, 381–386.

507. J. A. Sutliff, B. P. Bewlay: ‘Orientation imaging of a Nb–Ti–Si

directionally solidified in situ composite’, Proc. Microsc.

Microanal. 1996 Conf., (ed. J. M. Corbett et al.), 350–351; 1996,

San Francisco, CA, San Francisco Press.

508. H. Takatani, C. A. Gandin, M. Rappaz: ‘EBSD characterisation

and modelling of columnar dendritic grains growing in the

presence of fluid flow’, Acta Mater., 2000, 48, 675–688.

509. S. Takaya, T. Suzuki, Y. Matsumoto, K. Demachi, M. Uesaka:

‘Estimation of stress corrosion cracking sensitivity of type 304

stainless steel by magnetic force microscope’, J. Nucl. Mater.,

2004, 327, 19–26.

510. M. Takeyama, Y. Yamamoto, M. Nagaki, K. Hashimoto,

T. Matsuo: ‘Effect of Nb on lamellar orientation control of single

crystal gamma TiAl alloys with fully lamellar microstructure’,

Proc. Int. Symp. on ‘Niobium for high temperature applications’,

(ed. Y. W. Kim, T. Carneiro), 253–265; 2004, Warrendale, PA,

TMS.

511. A. U. Telang, T. R. Bieler, S. Choi, K. N. Subramanian:

‘Orientation imaging studies of Sn-based electronic solder joints’,

J. Mater. Res., 2002, 17, 2294–2306.

512. A. U. Telang, T. R. Bieler, J. P. Lucas, K. N. Subramanian, L. P.

Lehman, Y. Xing, E. J. Cotts: ‘Grain-boundary character and

grain growth in bulk tin and bulk lead-free solder alloys’,

J. Electron. Mater., 2004, 33, 1412–1423.

513. A. U. Telang, T. R. Bieler: ‘Characterization of microstructure

and crystal orientation of the tin phase in single shear lap Sn–3.5

Ag solder joint specimens’, Scr. Mater., 2005a, 52, 1027–1031.

514. A.U. Telang, T.R. Bieler: ‘Orientation imaging microscopy of

lead-free Sn–Ag solder joints’, JOM, Jun. 2005b, 44–49.

515. A. U. Telang, T. R. Bieler: ‘The role of special boundaries during

solidification and microstructure evolution in lead free solder

joints’, Mater. Sci. Forum, 2005c, 495–497, 1419–1424.

516. M. J. Thomas, B. P. Wynne, W. M. Rainforth: ‘An alternative

method to separate and analyse the microtextures and micro-

structures of primary alpha grains and transformed beta grains in

near-a titanium alloy Timetal 834’, Mater. Charact., 2005, 55,

388–394.

517. S. C. Tjong: ‘SEM, EDX and XRD studies of the scales formed

on the Fe–Mn–Al–C system in oxidizing–sulphidizing environ-

ments’, X-Ray Spectrom., 1991, 20, 225–238.

518. T. Tomida: ‘Decarburization of 3% Si–1.1%Mn–0.05%C steel

sheets by silicon dioxide and development of {100},012.

texture’, Mater. Trans., 2003, 44, 1096–1105.

519. T. Tomida, S. Uenoya, N. Sano: ‘Fine-grained doubly oriented

silicon steel sheets and mechanism of cube texture development’,

Mater. Trans., 2003, 44, 1106–1115.

520. S. Torizuka, O. Umezawa, K. Tsuzaki, K. Nagai: ‘Relationship

between size, shape and crystallographic orientation of ferrite

grains formed at grain boundaries of deformed austenite in a low

carbon steel’, Proc. HSLA Steels’2000, (ed. G. Liu et al.), 255–

259; 2000, Beijing, The Metallurgical Industry Press.

521. P. C. Tortorici, M. A. Dayananda: ‘Interdiffusion and diffusion

structure development in selected refractory metal silicides’,

Mater. Sci. Eng. A, 1999, A261, 64–77.

522. C. Trager-Cowan, S. K. Manson-Smith, D. A. Cowan,

F. Sweeney, D. McColl, A. Mohammed, R. Timm, P. G.

Middleton, K. P. O’Donnell, D. Zubia, S. D. Hersee:

‘Characterisation of nitride thin films by electron backscattered

diffraction’, Mater. Sci. Eng. B, 2001, B82, 19–21.

523. V. Traskine, P. Volovitch, L. Barrallier, Y. Kucherinenko,

P. Protsenko, Z. Skvortova: ‘Finite size scaling in grain boundary

wetting’, J. Mater. Sci., 2005, 40, 2349–2353.

524. P. W. Trimby, D. J. Prior: ‘Microstructural imaging techniques: a

comparison between light and scanning electron microscopy’,

Tectonophysics, 1999, 303, 71–81.

525. A. Tronche, A. L. Greer: ‘Electron back-scatter diffraction study

of inoculation of Al’, Philos. Mag. Lett., 2001, 81, 321–328.

526. A. P. Tschiptschin, C. M. Garzon, N. B. De Lima: ‘Texture

evolution during high temperature gas nitriding of duplex stainless

steels’, Mater. Sci. Forum, 2002, 408–412, 1347–1352.

527. N. Tsunekage, H. Tsubakino: ‘Influence of sulphur additions on

impact properties of bainitic or martensitic steels’, Mater. Sci.

Technol., 2002, 18, 964–972.

528. M. Ueda, H. Y. Yasuda, Y. Umakoshi: ‘Effect of grain boundary

character on the martensitic transformation in Fe–32at.%Ni

bicrystals’, Acta Mater., 2001a, 49, 3421–3432.

529. M. Ueda, H. Y. Yasuda, Y. Umakoshi: ‘Stress-induced martensi-

tic transformation in Fe–Ni bicrystals’, Acta Mater., 2001b, 49,

4251–4258.

530. M. Ueda, H. Y. Yasuda, Y. Umakoshi: ‘Controlling factor for

nucleation of martensite at grain boundary in Fe–Ni bicrystals’,

Acta Mater., 2003a, 51, 1007–1017.

531. M. Ueda, H. Y. Yasuda, Y. Umakoshi: ‘Martensitic and reverse

transformation in Fe–Ni bicrystals’, Mater. Sci. Forum, 2003b,

426–432, 1505–1510.

532. M. Ueda, H. Yasuda, Y. Umakoshi: ‘Reverse transformation in

Fe–Ni bicrystals’, ISIJ Int., 2004, 44, 1924–1930.

533. O. Umezawa, K. Hirata, K. Nagai: ‘Influence of phosphorus

micro-segregation on ferrite structure in cast strips of 0.1 mass% C

steel’, Mater. Trans., 2003, 44, 1266–1270.

534. K. Une, K. Nogita, S. Ishimoto, K. Ogata: ‘Crystallography of

zirconium hydrides in recrystallized zircaloy–2 fuel cladding by

electron backscatter diffraction’, J. Nucl. Sci. Technol. (Jpn),

2004, 41, 731–740.

535. K. Une, S. Ishimoto: ‘EBSP measurements of hydrogenated

Zircaloy–2 claddings with stress-relieved and recrystallised

annealing conditions’, J. Nucl. Mater., 2006, 357, 147–155.



536. M. L. Vaillant, T. Gloriant, I. Thibon, A. Guillou, V. Keryvin,

T. Rouxel, D. Ansel: ‘Partial crystallization of as-quenched

Zr55Cu30Al10Ni5 bulk metallic glass induced by oxygen’, Scr.

Mater., 2003, 49, 1139–1143.

537. C. Van der Eijk, Ø. Grong, J. Hjelen: ‘Quantification of inclusion

stimulated ferrite nucleation in wrought steel using the SEM-

EBSD technique’, Proc. Int. Conf. on ‘Solid–solid phase

transformations’99’, (ed. M. Koiwa et al.), 1573–1576; 1999,

Sendai, The Japan Institute of Metals.

538. I. Van Driessche, G. Penneman, J. S. Abell, E. Bruneel, S. Hoste:

‘Chemical approach to the deposition of textured CeO2 buffer

layers based on sol gel dip coating’, Mater. Sci. Forum, 2003, 426–

432, 3517–3522.

539. H. E. Vatne, M. Karlsen, J. Hjelen: ‘Determination of lattice

plane spacings from electron back-scatter patterns’, Proc.

EUREM–11, (ed. P. Hawkes), II480–II481; 1998, Brussels, The

Commitee of European Societies of Microscopy.

540. J. A. Venables, C. J. Harland: ‘Electron back-scattering patterns –

A new technique for obtaining crystallographic information in

the scanning electron microscope’, Philos. Mag., 1973, 27, 1193–

1200.

541. B. Verlinden, P. Bocher, E. Girault, E. Aernoudt: ‘Austenite

texture and bainite/austenite orientation relationships in TRIP

steel’, Scr. Mater., 2001, 45, 909–916.

542. J. M. Vitek, S. S. Babu, S. A. David, J.-W. Park: ‘Microstructure

development in single crystals welds’, Mater. Sci. Forum, 2003,

426–432, 4123–4128.

543. J. M. Vitek, S. S. Babu, J. W. Park, S. A. David: ‘Analysis of stray

grain formation in single crystal nickel-based surperalloy welds’,

Proc. Superalloys 2004, (ed. K. A. Green et al.), 459–465; 2004,

Warrendale, PA, TMS.

544. A. Wagner, B. A. Shollock, M. McLean: ‘Grain structure

development in directional solidification of nickel-base super-

alloys’, Mater. Sci. Eng. A, 2004, A374, 270–279.

545. N. Wang, S. Mokadem, M. Rappaz, W. Kurz: ‘Solidification

cracking of superalloy single- and bi-crystals’, Acta Mater., 2004,

52, 3173–3182.

546. P. Wang, D. Veeraraghavan, M. Kumar, V. K. Vasudevan:

‘Massive-parent interphase boundaries and their implications on

the mechanisms of the aRcM massive transformation in Ti–Al

alloys’, Metall. Mater. Trans. A, 2002, 33A, 2353–2371.

547. Q. G. Wang, D. Apelian, L. Arnberg, S. Gulbrandsen-Dahl,

J. Hjelen: ‘Solidification of eutectic in hypoeutectic Al–Si alloys’,

Trans. Am. Foundrymen’s Soc., 1999, 107, 249–256.

548. R. Wang, J. Gui, X. Chen, S. Tan: ‘EBSD and TEM study of self-

accommodating martensites in Cu75.7Al15.4Mn8.9 shape memory

alloy’, Acta Mater., 2002, 50, 1835–1847.

549. S. C. Wang, M. Aindow, M. J. Starink: ‘Effect of self-

accommodation on a/a boundary populations in pure titanium’,

Acta Mater., 2003, 51, 2485–2503.

550. T. T. Wang, P. R. Morris, B. L. Adams: ‘Characterization of the

morphological and lattice orientational microstructure of as-cast

aluminum ingot’, Metall. Trans. A, 1990, 21A, 2265–2275.

551. R. J. H. Wanhill, ‘Embrittlement of ancient silver’, J. Failure

Anal. Prevent., 2005, 5, 41–54.

552. N. Warnken, D. Ma, M. Mathes, I. Steinbach: ‘Investigation of

eutectic island formation in SX superalloys’, Mater. Sci. Eng. A,

2005, A413–A414, 267–271.

553. A. Wasilkowka, R. Petrov, L. Kestens, E. A. Werner,

C. Krempaszky, S. Traint, A. Pichler: ‘Microstructure and texture

changes in a low-alloyed TRIP-aided steel induced by small

plastic deformation’, ISIJ Int., 2006, 46, 302–309.

554. T. Watanabe: ‘An approach to grain boundary design for strong

and ductile polycrystals’, Res. Mech., 1984, 11, 47–84.

555. T. Watanabe, K. Obara, S. Tsurekawa: ‘In situ observations on

interphase boundary migration and grain growth during a/c phase

transformation in iron alloys’, Mater. Sci. Forum, 2004, 467–470,

819–824.

556. T. Watanabe, S. Tsurekawa, H. Fujii, T. Kanno: ‘The control of

texture and grain boundary microstructure by magnetic anneal-

ing’, Mater. Sci. Forum, 2005a, 495–497, 1151–1158.

557. T. Watanabe, K. Obara, S. Tsurekawa, G. Gottstein: ‘A

mechanism of plane matching boundary-assisted a/c phase

transformation in Fe–Cr alloy based on in situ observations’,

Z. Metallkd., 2005b, 96, 1196–1203.

558. Y. Watanabe, H. Eryu, T. Yamamoto, S. Adiarwanto, H. Miura:

‘Evaluation of casting textures in Al/Al3Ti platelet functionally

graded material fabricated by a centrifugal solid-particle method’

Mater. Sci. Forum, 2002, 408–412, 1771–1776.

559. T. Waterschoot, L. Kestens, B. C. De Cooman: ‘Hot rolling

texture development in CMnCrSi dual-phase steels’, Metall.

Mater. Trans. A, 2002, 33A, 1091–1102.

560. S. Weiß, D. Mattissen, W. Dudzinski: ‘Microstructure of laser-

beam-welded iron-based superalloy A286 after high-temperature

creep’, Adv. Eng. Mater., 2002, 4, 142–146.

561. H. Wendrock, J. Richter, A. Guth: ‘The determination of small

areas of retained austenite in TRIP-steels using high resolution

electron back scattering diffraction’, Prakt. Metallogr., 2001, 38,

314–324.

562. D. A. West, B. L. Adams: ‘Analysis of orientation clustering in a

directionally solidified nickel-based ingot’, Metall. Mater. Trans.

A, 1997, 28A, 229–236.

563. G. D. West, S. Birosca, R. L. Higginson: ‘Phase determination

and microstructure of oxide scales formed on steel at high

temperature’, J. Microsc., 2005, 217, 122–129.

564. A. J. Wilkinson: ‘Measuring strains using electron backscatter

diffraction’, in ‘Electron backscatter diffraction in materials

science’, (ed. A. J. Schwartz et al.), 231–245; 2000, New York,


565. G. O. Williams, V. Randle, J. R. Cowan, P. Spellward: ‘The

role of misorientation and phosphorus content on grain growth

and intergranular fracture in iron–carbon–phosphorus alloys’,

J. Microsc., 2004, 213, 321–327.

566. A. W. Wilson, J. D. Madison, G. Spanos: ‘Determining phase

volume fraction in steels by electron backscattered diffraction’,

Scr. Mater., 2001, 45, 1335–1340.

567. A. W. Wilson, G. Spanos: ‘Application of orientation imaging

microscopy to study phase transformations in steels’, Mater.

Charact., 2001, 46, 407–418.

568. T. L. Wolfsdorf-Brenner, P. W. Voorhees, J. Sutliff: ‘Texture

evolution and the role of grain boundaries in skeletal formation

during coarsening in solid–liquid mixtures’, Metall. Mater. Trans.

A, 1999, 30A, 1955–1969.

569. S. Wollmer, S. Zaefferer, M. Goken, T. Mack, U. Glatzel:

‘Characterization of phases of aluminized nickel base superalloys’,

Surf. Coat. Technol., 2003, 167, 83–96.

570. T. G. Woodcock, J. S. Abell, M. G. Hall: ‘Characterization of

textured NiO films for application as buffer layers in high

temperature superconducting tapes’, J. Microsc., 2002a, 205, 231–

237.

571. T. G. Woodcock, J. S. Abell, T. C. Shields, M. G. Hall: ‘The effect

of different oxidation routines on the properties of surface

oxidised epitaxial NiO layers on biaxially textured Ni tapes’,

Physica C, 2002b, 372C–376C, 862–865.

572. T. G. Woodcock, J. S. Abell, J. Eickemeyer, B. Holzapfel: ‘Crystal

orientation mapping of NiO grown on cube textured Ni tapes’,

J. Microsc., 2004, 216, 123–130.

573. S. I. Wright, J. D. Cotton: ‘Microtextural characterization of a

beryllium weldment’, Text. Microstruct., 1995, 23, 7–19.

574. S. I. Wright, D. P. Field, D. J. Dingley: ‘Advanced software

capabilities for automated EBSD’, in ‘Electron backscatter

diffraction in materials science’, (ed. A. J. Schwartz et al.), 141–

152; 2000, New York, Kluwer Academic/Plenum Publishers.

575. S. I. Wright, D. P. Field, M. M. Nowell: ‘Impact of local texture

on recrystallization and grain growth via in situ EBSD’, Mater.

Sci. Forum, 2005, 495–497, 1121–1130.

576. S. I. Wright, M. M. Nowell: ‘EBSD image quality mapping’,

Microsc. Microanal., 2006, 12, 72–84.

577. J. Wu, P. J. Wray, C. I. Garcia, M. Hua, A. J. DeArdo: ‘Image

quality analysis: a new method of characterizing microstructures’,

ISIJ Int., 2005, 45, 254–262.

578. S. H. Wu, J. C. Huang, Y. N. Wang: ‘Evolution of microstructure

and texture in Mg–Al–Zn alloys during electron-beam and gas

tungsten arc welding’, Metall. Mater. Trans. A, 2004, 35A, 2455–

2469.

579. R. Wuhrer, K. Moran, P. Huggett, M. R. Phillips, B. Ben-Nissan:

‘X-ray mapping and electron back scattered diffraction of phases

in welded materials’, Microsc. Microanal., 2004, 10, (Suppl. 2),

916–917.

580. K. Xia, G. Tausig: ‘Liquidus casting of a wrought aluminum alloy

2618 for thixoforming’, Mater. Sci. Eng. A, 1998, A246, 1–10.

581. K. Xu, A. M. Russell: ‘Texture-strength relationships in a

deformation processed Al–Sn metal–metal composite’, Mater.

Sci. Eng. A, 2004, A373, 99–106.

582. X. Xu, R. M. Ward, M. H. Jacobs, P. D. Lee, M. McLean: ‘Tree-

ring formation during vacuum arc remelting of Inconel 718: Part

1. Experimental investigation’, Metall. Mater. Trans. A, 2002a,

33A, 1795–1804.



583. X. Xu, W. Zhang, P. D. Lee: ‘Tree-ring formation during vacuum

arc remelting of Inconel 718: Part II. Mathematical modelling’,

Metall. Mater. Trans. A, 2002b, 33A, 1805–1815.

584. S. Yamaura, Y. Igarashi, S. Tsurekawa, T. Watanabe: ‘Structure-

dependent intergranular oxidation in Ni–Fe polycrystalline alloy’,

Acta Mater., 1999, 47, 1163–1174.

585. S. Yamaura, Y. Igarashi, S. Tsurekawa, T. Watanabe: ‘Grain

boundary engineering for the control of oxidation embrittlement’,

in ‘Properties of complex inorganic solids 2’, (ed. A. Meike et al.),

27–37; 2000, New York, Kluwer Academic/Plenum Publishers.

586. S. Yamaura, S. Tsurekawa, T. Watanabe: ‘The control of

oxidation-induced intergranular embrittlement by grain boundary

engineering in rapidly solidified Ni–Fe alloy ribbons’, Mater.

Trans., 2003, 44, 1494–1502.

587. K. L. Yang, J. C. Huang, Y. N. Wang: ‘Phase transformation in

the b phase of super a2 Ti3Al base alloys during static annealing

and superplastic deformation at 700–1000uC’, Acta Mater., 2003,

51, 2577–2594.

588. L. C. Yang, I. Dumler, C. M. Wayman: ‘Studies of herringbone

domain structures in lead titanate by electron back-scattering

patterns’, Mater. Chem. Phys., 1994, 36, 282–288.

589. S. Yang, U. Krupp, H.-J. Christ, V. B. Trindade: ‘The relation-

ship between grain boundary character and the intergranular

oxide distribution in IN718 superalloy’, Adv. Eng. Mater., 2005, 7,

723–726.

590. Y. Yang, Y. A. Chang, L. Tan, W. Cao: ‘Multiphase equilibria in

the metal-rich region of the Mo–Ti–Si–B system: thermodynamic

prediction and experimental validation’, Acta Mater., 2005, 53,

1711–1720.

591. Z. Yang, H. F. Zhang, A. M. Wang, B. Z. Ding, Z. Q. Hu:

‘Rheocast structure in a hypoeutectic high chromium white iron’,

Mater. Sci. Eng. A, 2003, A343, 251–256.

592. H. Y. Yasuda, T. Sakata, Y. Umakoshi: ‘Variant selection in

transformation texture from the b to a phase in Cu–40 mass% Zn

alloy’, Acta Mater., 1999, 47, 1923–1933.

593. H. Yasuda, I. Ohnaka, R. Ishii, S. Fujita, Y. Tamura:

‘Investigation of the melt flow on solidified structure by a

levitation technique using alternative and static magnetic fields’,

ISIJ Int., 2005, 45, 991–996.

594. T. Yokomizo, M. Enomoto, O. Umezawa, G. Spanos, R. O.

Rosenberg: ‘Three-dimensional distribution, morphology and

nucleation site of intragranular ferrite formed in association with

inclusions’, Mater. Sci. Eng. A, 2003, A344, 261–267.

595. T. Yokota, M. Fujioka, M. Niikura: ‘Grain structure of Fe–

0.3mass%C–9mass% Ni steel processed through aRcRa’ trans-

formation caused by spontaneous reverse transformation’, ISIJ

Int., 2005, 45, 736–742.

596. N. Zaafarani, D. Raabe, R. N. Singh, F. Roters, S. Zaefferer:

‘Three-dimensional investigation of the texture and microstruc-

ture below a nanoindent in a Cu single crystal using 3D EBSD

and crystal plasticity finite element simulations’, Acta Mater.,

2006, 54, 1863–1876.

597. S. Zaefferer, U. Glatzel: ‘Orientation relationship of phases in an

oxidation protection coating on a Ni-based superalloy single

crystal’, Mater. Sci. Forum, 2002, 408–412, 1531–1536.

598. S. Zaefferer, J. Ohlert, W. Bleck: ‘A study of microstructure,

transformation mechanisms and correlation between microstruc-

ture and mechanical properties of a low alloyed TRIP steel’, Acta

Mater., 2004, 52, 2765–2778.

599. K. L. Zeisler-Mashl, T. A. Lograsso: ‘The occurrence and

periodicity of oscillating peritectic microstructures developed

during directional solidification’, Metall. Mater. Trans., 1997,

28, 1543–1552.

600. Y. Zhang, G. Vincent, N. Dewobroto, L. Germain, X. Zhao,

L. Zuo, C. Esling: ‘The effects of thermal processing in a magnetic

field on grain boundary characters of ferrite in a medium carbon

steel’, J. Mater. Sci., 2005, 40, 903–908.

601. Y. D. Zhang, C. Esling, M. L. Gong, G. Vincent, X. Zhao, L. Zuo:

‘Microstructural features induced by a high magnetic feld in a

hypereutectoid steel during austenitic decomposition’, Scr.

Mater., 2006, 54, 1897–1900.

602. J. C. Zhao, B. P. Bewlay, M. R. Jackson: ‘Determination of Nb–

Hf–Si phase equilibria’, Intermetallics, 2001, 9, 681–689.

603. J. C. Zhao, M. R. Jackson, L. A. Peluso, L.N. Brewer: ‘A

diffusion-multiple approach for mapping phase diagrams, hard-

ness and elastic modulus’, JOM, 2002, 54, 7, 42–45.

604. J. C. Zhao, M. R. Jackson, L. A. Peluso: ‘Determination of the

Nb–Cr–Si phase diagram using diffusion multiples’, Acta Mater.,

2003, 51, 6395–6405.

605. J. C. Zhao: ‘Reliability of the diffusion-multiple approach for

phase diagram mapping’, J. Mater. Sci., 2004, 39, 3913–3925.

606. J. C. Zhao, M. R. Jackson, L.A. Peluso: ‘Mapping of the Nb–Cr–

Ti phase diagram using diffusion multiples’, Z. Metallkd., 2004a,

95, 142–146.

607. J. C. Zhao, M. R. Jackson, L. A. Peluso: ‘Evaluation of phase

relations in the Nb–Cr–Al system at 1000uC using a diffusion-

multiple approach’, J. Phase Equilib. Diffusion, 2004b, 25, 152–

159.

608. J.-C. Zhao: ‘Combinatorial aproaches as effective tools in the

study of phase diagrams and composition–structure–property

relationships’, Prog. Mater. Sci., 2006, 51, 557–631.

609. Y. Zhong, J. Liu, R. A. Witt, Y.-H. Sohn, Z.-K. Liu: ‘Al2(Mg,Ca)

phases in Mg–Al–Ca ternary system: First-principles prediction

and experimental identification’, Scr. Mater., 2006, 55, 573–576.

610. Y. Zhou, K. T. Aust, U. Erb, G. Palumbo: ‘Effects of grain

boundary structure on carbide precipitation in 304L stainless

steel’, Scr. Mater., 2001, 45, 49–54.

611. Y. H. Zhu, W. B. Lee, C. F. Yeung, T. M. Yue: ‘EBSD of Zn rich

phases in Zn–Al based alloys’, Mater. Charact., 2001, 46, 19–23.

612. Y. H. Zhu, W. B. Lee, S. To: ‘Use of EBSD to study stress

induced microstructural changes in Zn–Al based alloy’, Mater.

Sci. Eng. A, 2003a, A348, 6–14.

613. Y. H. Zhu, W. B. Lee, S. To: ‘Ageing characteristics of cast Zn–Al

based alloy (ZnAl7Cu3)’, J. Mater. Sci., 2003b, 38, 1945–1952.

614. Y. H. Zhu: ‘General rule of phase decomposition in Zn–Al based

alloys (II) – on effects of external stresses on phase transforma-

tion-’, Mater. Trans., 2004, 45, 3083–3097.

615. F. Zimmermann, M. Humbert: ‘Determination of the habit plane

characteristics in the b– a’ phase transformation induced by stress

in Ti–5Al–2Sn–4Zr–4Mo–2Cr–1Fe’, Acta Mater., 2002, 50, 1735–

1740.



Application of Electron Back Scatter Diffraction

Documents

Transcript of Application of Electron Back Scatter Diffraction