Principal of EBSD

General View of EBSD EBSD Pattern Generation Crystal systems and their symmetry

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Variety of materials are used around us .

What is the criteria to select materials?

Strength stiffness Density/weight Hardness Workability Conductivity Cost Reliability Safety

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What decide the property of material?

Elements
Composition/ Distribution Crystal structure/ Phase

Texture
Grain size/shape Orientation Boundary Deformation / Heat treatments
Element analysis? Texture measurement? Property measurement?
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Property of materials are decided by combination of these factors.

How we can analyze them????

Different Property due to orientation

Weak Orientation

Because materials properties are anisotropic. We all know that the strength of wood varies with the direction of the grain.
Strong Orientation

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Example of fire accident

Fire at the tall building in Spain 2005/02/12

Before the fire

After the fire

Can we use this iron frame for reconstruction of this building?

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Different property due to texture

If microstructure is different, the materials show different properties.

Rolled texture

Re-crystallized texture

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Isnt the anisotropy averaged out in a polycrystal?

Not necessarily. A material will be isotropic if all of the grains have random orientations. But if the grains have similar orientations then the bulk material will exhibit anisotropy similar to the constituent crystals. The distribution of crystal orientations is called texture. Most forming processes produce materials with texture.

Electron Beam Diffraction Generation of EBSD Patterns

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EBSD Pattern
Electron backscatter diffraction patterns (or EBSPs) are obtained in the SEM by focusing a stationary electron beam on a crystalline sample. The sample is tilted to approximately 70 degrees with respect to the horizontal. The diffraction pattern is imaged on a phosphor screen. The image is captured using a low-light CCD camera. The bands in the pattern represent reflecting planes in the diffracting crystal volume. Thus, the geometrical arrangement of the bands is a function of the orientation of the diffracting crystal lattice.

Electron Diffraction
There are 4 ways to get Electron Diffraction patterns.

SEM

TEM

ECP

EBSP
Bulk Sample

Spot Diffraction

Kikuchi Pattern

Thin film Sample

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Braggs Law

n = 2d sin B

h eV 2mo eV 1 + 2m c 2 o

Generation of EBSD Patterns

Intensity distribution of inelastic scattered electrons Electrons come out from the sample surface
Sample surface

Band formation with Kikuchi patterns

Weaker beam Crystal Plane Bright line Stronger beam

Lattice plane

Dark line

Incident beam Red arrows show the electrons come out from sample surface. Crystal planes Sample surface

As shown in right figure, bands in EBSD pattern corresponds crystal planes.

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Generation of EBSD Patterns

Diffracted electrons propagate as corn shape. Then the bands in EBSD pattern become hyperbola lines. EBSD patterns show the real lattice.

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EBSD Patterns at different Acc. Voltage

Only band width in EBSD patterns change depending on Acc. Voltage.

10kV

40kV

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Generation of EBSD Patterns

High spatial resolution
Spatial resolution depends on SEM probe size Shottky FE-SEM 10~15nm LaB6 filament SEM 100~200nm filament S EM 200~300nm

Kikuchi Pattern from sample surface

Volume to generate EBSD pattern

Depth of Information is very shallow

depends on Acc. Voltage and samples

Inelastically scattered electrons (Noise) 1m

About 30-50 nm ~ nearly one extinction distance

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Crystal system and symmnetry

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Unit Cell Lattice Parameters

a, b & c Vectors defining the unit cell (crystallographic axes)

a, b & c are the lengths of these vectors

and , & are the angles between them. Together these form the set of lattice constants or parameters.

c
Crystal plane: A set of lattice points that lie in one plane. Crystal direction: A set of lattice points that lie along a line. Crystal axes: The reference vectors that define the unit cell.

a
a

Directions in the Crystal

c OA 1, 1 & 1/2 uvw = [221] O a A 2 a [uvw] direction <uvw> set of crystallographically equivalent directions

b
[001] [101] c [112] [111] [1213]

[021] a3 [ 010] [110] a1

[1100] a2 [1120]

[100]

Indices in hexagonal and trigonal crystals

a3

a2

<-1 2 -1 0>

<0, 1, -1, 0> a1 <0, 1, -1, 0, 0>

Rule u v t w = indices = integers t = -(u+v) (All of a1, a2, a3 and c must be used.)

Indices in hexagonal and trigonal crystals

<-1 2 -1 1>

<-1 2 -1 3> <0 0 0 1> <0 0 0 1>

(1 0 -1 0)<-1 2 -1 3>

(1 0 -1 0)<-1 2 -1 1>

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Lattice Planes
(hkl) Miller indices of a plane
c/l

a/h

b/k

{hkl} set of symmetrically equivalent planes

(010)

(110)

(111)

(112)

(1210)

(1011)

(1100)

Interplanar or d-Spacing
2 dimensional examples

b
(11)

a
(10)

d010
dhkl = a( h2

d020
+ + (for cubics)

k2

l2)-1/2

(21)

(15)

= 2dhklsin

Lines of lowest indices have the greatest spacing and density of lattice points

dhkl = V[h2b2c2sin2 + k2a2c2sin2 + l2a2b2sin2 + 2hlab2c(coscos cos) + 2hkabc2(coscos cos) + 2kla2bc(coscos cos)]-1/2 V = abc[1 - cos2 - cos2 - cos2 2coscoscos]1/2

Band width is inversely proportional to d-spacing

Color

(hkl) 111 200 220 311 331 042

d-spacing 2.31 2.00 1.41 1.21 0.92 0.89

111 222 333

Zone Axes
Zone Axis The line of intersection of two planes is the zone axis of the zone in which the two planes are located

Zone Rule

[002]

u = k1l 2 l 1k2 v = l 1 h2 h 1 l 2 w = h 1k2 k1h 2

Weiss Zone Law hu + kv + lw = 0

Use space group information to locate atom positions in the unit cell.

Structure Factor Kinematic Calculation

Structure Factor
In case of Cubic/FCC : Atom positions in Unit cell: (0,0,0),(,,0),( 0, ,), (,0, )

Fhkl = f [1 + cos (h + k ) + cos (k + l ) + cos (l + h)]

When all h, k, l becomes even or odd, Fhkl has a value of 4 and make visible bands. All other cases, the intensity becomes 0 and bands are not visible. For example, FCC structure has (220)or (111) bands, but not (211). In case of Cubic/BCC : Atom positions in Unit cell: (0,0,0),(,,)

F hkl = f [1 + cos ( h + k + l )]
When summation of h, k, l becomes even, Fhkl has a value of 2 and make visible bands. For example, BCC structure has (220)or (211) bands, but not (111) or (311) bands.
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Classification of Crystals

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Crystal Lattice
Lattice :
An array of points in space arranged such that each point has identical surroundings

Bravais Lattice:
The unique lattice which can be build by translation and point symmetry in 3 di mension. They are based on 7 crystal systems and its extension. Total number of Bravais lattice is 14 of 3 dimensional lattices.

Point Group:
Point group is defined by symmetry operation which holds consistency around one point such as Rotation, Mirror and Inversion. Point group is classified into 32 groups.

Space Group:
Adding Screw and Glide operation to Point group makes whole 230 Space grou p. Any crystals except quasi crystal are classified into one of these crystal group s.

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Seven Crystal Systems

Crystal systems Rotation Lattice Parameter Relationships

Triclinic Monoclinic Orthorhombic Tetragonal Rhombohedral Hexagonal Cubic

No rotation symmetry One 2 holds rotation Three 2 holds rotations normal to each other One 4 holds rotations One 3 holds rotations One 6 holds rotations Four 3 holds rotations.

abc abc abc a=bc a=b=c a=bc a=b=c

= = 90 < = = = 90 = = = 90 = = < 12090 = = 90, = 120 = = = 90

Seven Crystal Systems are defined by rotation symmetry.

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Triclinic

c a b

No rotation symmetry

Only translation is available

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Lattices with perpendicular axises

Monoclinic
One 2 holds rotation b c c b a

Orthorhombic
a Three2 holds rotations

Tetragonal
One 4 holds rotation c a

Cubic
Four 3 holds rotations

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Lattices with 3 holds rotation axis

Rhombohedral Hexagonal

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Symmetries in EBSD Patterns

Seven Crystal systems
32 Point Groups
Lattices delivered by rotation, inversion , mirror, improper rotation, etc. Symmetries we can see in the EBSD patterns

14 Bravais Lattice
Lattices delivered from simple lattice by combination of translation and point symmetry This Bravais lattices are reflected in the EBSD pattern as structure factors.

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Symmetry Operation (Rotation)

1 hold rotation(2) 2 holds rotation() 3 holds rotation(2/3) 4 holds rotation(/2) 6 holds rotation(/3)

Symbol for this rotation operation is Number

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Symmetry Operation (Mirror pl ane)

Green plane is a mirror plane

Symbol for this mirror operation : m

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Symmetry Operation (Inversion)

Bring the points to opposite position with respect to the center.

(x, y, z) (x, y, z)

Symbol for this Inversion operation : -

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(n)
_

(n/m)

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Seven Crystal Systems

Rotation Axes Crystal Systems (32) 2 Triclinic (2) Monoclinic (3) Orthorhombic (3) Trigonal* (5) (Rhombohedral) Tetragonal (7) Hexagonal (7) Cubic (5) 1 3 3 4 6 6 3 1 4 4 1 3 6 1 Mirror Planes 1 3 3 5 7 9 Center of Inversion yes yes yes yes yes yes yes Lattice Parameter Relationships abc abc abc a=b=c a=bc a=bc a=b=c = = 90 < = = = 90 = = 90, = 120 = = = 90 = = 90, = 120 = = = 90

The conventional cell of the hexagonal system is frequently used for trigonal crystals The system with the highest symmetry in each class is shown (see webmineral.com)

Symmetry in Material database

OIM-DC / Phase page

Herman Morgan expression This is Hexagonal, then

The 1st index: around <0001> axis The 2nd index: around<10-10>axis The 3rd index: around<1-210>axis More explanations. 6/m : <0001> axis is 6holds rotation symmetry and the plane normal to this axis is mirror plane. m : The plane normal to this <10-10> axis is mirror plane. m : The plane normal to this <1 -2 1-10> axis is mirror plane.

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Symmetry axis for Herman-Morgan expression

Crystal Systems Triclinic Monoclinic Orthorhombic Tetragonal 1st index None [010] in case of b-axis normal [001] in case of c-saix normal [100] [001] Hexagonal axis [0001] [10-10], [01-1-1] [-1-120] Rhombohedral axis [001] [1-10], [01-1] [-101] [10-10] Hexagonal Cubic [0001] [100] [01-10] [-1-120] [111] [1-100] [12-30] [-2-130] [110] [010] [100] [010] [001] [1-10] [110] 2nd Index 3rd Index

Trigonal* (Rhomboh edral)

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Bravais Lattice
7 m3m

14

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Bravais Lattice
a a a
Simple Cubic (P)

a a

a a a a a

c a a

c a

Body-Centered Cubic (I)

Face-Centered Cubic (F)

Simple Tetragonal (P)

Body-Centered Tetragonal (I)

c a b a

c b a

c b a

c b

a a

Simple Orthorhombic (P)

Body-Centered Orthorhombic (I)

Base-Centered Orthorhombic (C)

Face-Centered Orthorhombic (F)

Rhombohedral (R)

c
120

c c a b
Simple Monoclinic (P)

c b a
Base-Centered Monoclinic (C)

a a

b
Triclinic (P)

Hexagonal (P)

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Symmetry in EBSD Pattern

How OIM uses symmetry info of the crystal to index this pattern?

Mirror plane

4 holds rotation

OIM itself doesnt consider the information of crystal symmetry when it index EBSD patterns. Information of crystal symmetry is considered when it build the material files for indexing the patterns. After indexing the patterns, crystal symmetry information is also considered to calculate equivalent orientations.

2 holds rotation

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Indexing procedure of EBSD patterns

(Symmetry, Lattice parameter and reflectors) OIM-DC

Set-up material file(s)

1. All equivalent crystal planes are listed. 2. Angles between crystal planes are calculated.

Capture EBSD Patterns. Detecting Bands

Unfortunately, crystal symmetry is not considered in this process.

Indexing of detected bands Calculate crystal orientation Consider all equivalent crystal planes
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List up inter planer angles and compare to look-up table which delivered from material file(s). Mirror indices of the band is decided by angular relations.

OIM Analysis software calculate relations of equivalent crystal planes for orientation maps, plots and charts.

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Present situation of EBSD pattern indexing

Crystal symmetry information is used to calculate angular relations of equivalent crystal planes. When OIM indexes detected bands, crystal symmetry information is not considered. It just check the angular relations among bands.
Left example is the pattern from Ni-Sn alloy. Possible phases are listed as below.

Ni3Sn4 : Monocrinic a = 12.2, b = 4.056, c = 5.21 = 90 = 105.05 = 90 NiSn : Hexagonal a = 4.09, b = 4.09, c = 5.18 = 90 = 90 = 120 Ni4Sn : Tetragonal a = 5.11, b = 5.11, c = 4.88 = 90 = 90 = 90

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Present situation of EBSD pattern indexing

Ni3Sn4 NiSn Ni4Sn

Ni3Sn4 Vote Fit CI 112 0.71 0.000

NiSn 120 0.8 0.075

Ni4Sn 112 0.91 0.075

Seeing the results of indexing, all three phase look reasonably OK. If we consider , Vote value, Fit value and CI value, NiSn (Hexagonal) looks most likely phase.

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Present situation of EBSD pattern indexing

Lets check detail of indexing when it is indexed as NiSn hexagonal. If this pattern is a hexagonal pattern, the green lines shown by red and yellow arrows are all equivalent crystal planes. So the intensity should be nearly same.

The band shown by yellow arrow is missing Then it is not appropriate to consider this pattern as hexagonal.

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Present situation of EBSD pattern indexing

Same as Hexagonal, if this pattern is indexed as Tetragonal, the bands shown by red and yellow arrows are equivalent bands. So the intensity of the bands should be nearly same. But it doesnt look like that.

The bands shown by yellow arrow is much weaker . Then it is difficult to consider it as Tetragonal patterns.

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Summary
EBSD Pattern shows real lattice, not reciprocal lattice. So we can see the symmerty of the crystal directly in the patterns. We can distinguish 7 crystal systems and 14 Bravasis lattice from EBSD patterns. It is effective to check intensity of equivalent bands to distinguish similarly indexed patterns.

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