Electron Back-Scatter Diffraction in

the Scanning Electron Microscope:

An Overview

www.hkltechnology.com

Talk Outline
What is EBSD?
Historical Perspective
Crystallography & pattern formation
Data Collection
Recent Developments
Conclusions

What is EBSD?
EBSD - electron backscatter diffraction
SEM based technique to measure crystal
orientations
Applicable to any crystalline material (in theory)
Provides the absolute crystal orientation with submicron resolution
A useful tool for discriminating between phases

EBSD or EBSP?
EBSD - electron backscatter diffraction
EBSP electron backscatter diffraction pattern
BKD Backscattered Kikuchi Diffraction
And some commercial names....

(C)OM (Crystal) Orientation Mapping

ACOM Automated Crystal Orientation
Mapping
OIM - Orientation Imaging Microscopy

Talk Outline
What is EBSD?
Historical Perspective
Crystallography & pattern formation
Data Collection
Recent Developments
Conclusions

EBSD History Early Work

EBSP like patterns were
first observed by
Kikuchi (1928) in the
Transmission Electron
Microscope (TEM).
Von Boersch (1937)
extended Kikuchis
work

Mica

EBSD History
Alam et al.
Alam, Blackman and
Pashley (1954) used a
cylindrical specimen
chamber and film
camera to produce highangle Kikuchi patterns
from cleaved LiF, KI,
NaCl, PbS2 crystals.
Lead Sulphide

EBSD History the birth of

modern EBSD

Venables and Harland

(1972) observed EBSPs in
the Scanning Electron
Microscope (SEM) by using
a 30mm diameter fluorescent
imaging screen and a closed
circuit television camera.
Dingley (later 1980s)
developed the combination
of phosphor and television
camera, and combined them
with a graphical overlay.
EBSP from Dingley's
group note
calibration marks

EBSD History continued

experiments in the 1980s
Commercial software
(1989) was developed
to analyse Electron
Channeling Patterns
(ECP) and EBSPs.
EM film for high
quality EBSPs & phase
identification (1980s)
EBSP from a superalloy
collected with EM film

EBSD History commercial

systems in the 1990s
Automatic methods for
indexing EBSPs
(1990s) and control of
SEMs gave rise to
mapping and phase
discrimination.
Digital cameras, EDX
data and phase
databases provide
information for phase
identification (1999 - )

Phase map from

duplex steel

EBSD History the present day

High speed mapping
becomes a reality
Dual/Cross beam
system (Electron + Ion
beam) for 3D
microscopy
Combined chemical and
crystallographic
mapping
Orientation map of Nisuperalloy, collected at
>65 points / sec

EBSD set up:

Resulting diffraction pattern

(EBSP)

 Spatial resolution: down to 10s of nm

Max sample size: SEM dependent (typically
up to 100 x 50mm)

EBSD
Performance

Angular resolution: 0.25-1 at present

Probe current: >0.25 nA
Accelerating voltage: >5 kV
Specimen tilt: 60-75
Working distance: 10-40 mm
Speed: 0.010 - 1 second per measurement
Sample preparation: electropolishing,
collidal silica polishing , ion beam milling or
etching

Talk Outline
What is EBSD?
Crystallography & pattern formation
Data Collection
Recent Developments
Conclusions

EBSP crystallography

EBSP symmetry comes from lattice symmetry

Crystal system, Laue group, space group

To build a crystal
Start with unit cell
Add a basis
Repeat ad infinitum...

[uvw] is a crystal direction,

<uvw> is a family of directions
(hkl) is a crystal plane,
{hkl}is a family of planes.

EBSP formation

Electron beam strikes

specimen
Scattering produces
electrons travelling in all
directions
Electrons that satisfy the
Bragg condition
(n=2d.sin) for a plane
(hkl) are channeled
Kikuchi bands
Electrons strike the
phosphor and produce light
Which is detected by a CCD
camera and digitised
The resulting EBSP is
automatically analysed and
indexed...

Iron unit cell

Phosphor

Spherical
Kikuchi map

EBSD Resolution

Although EBSPs are created by

backscattered electrons, the signal
does not come from the whole BSE
interaction volume
Instead, the diffraction signal
effectively originates from a "point
source" in the top few nm
This means that the EBSD
technique can obtain very high
resolutions (<20nm)

Resolution Example 1
Copper interconnect test
sample
Analysed on the LEO Supra
55VP

Twin domains 10-20 nm

wide are clearly
resolved using a 5nm
step size

Resolution Example 2
Pt thin film
Analysed on the JEOL
6500F

=0.08 m; BC; Step=0.005 m; Grid55x49

Grains with a mean

diameter of 35nm are
clearly resolved using a
5nm step size

=0.08 m; GB+tri-x; Step=0.005 m; Grid55x49

Body centred cubic Iron

{200}
{100}

[001]

(011)

{110}

[011]
[100]

[010]

[001]

Iron EBSP
<111> is central
Note: <111> has 3
fold symmetry, but is
close to 6 fold.

[011]

[101]
[201]
[311]
[100]

[111]

[210] [110]

[010]

Body and Face centred cubic Iron

bcc

fcc

Plane Intensity No.

{110} 100% x6
{200} 51%
x6
{112} 32% x12
{220} 23%
x6
{013} 17% x12
{222} 13%
x4
{123} 10% x24
Plane Intensity No.
{111} 100% x4
{200} 77%
x3
{220} 38%
x6
{113} 26% x12
{222} 23%
x4
{400} 16%
x3
{133} 13% x12
{240} 12% x12
bcc h+k+l=2n (i.e. no {111})
fcc h, k, l all odd or all even

Phase discrimination

Differences in interplanar
angles allow similar
looking EBSPs from bcc
and fcc Iron to be
distinguished.

bcc Iron
bcc Iron

fcc Iron

fcc Iron

Talk Outline
What is EBSD?
Crystallography & indexing
Data Collection
Recent Developments
Conclusions

Indexing & Automation

Live EBSP

Automatic analysis
Beam/Stage control

Hough space

Move beam
or stage
Detect Bands

Save data
to file
Phase and
orientation

Index EBSP

A single automated EBSD run provides a

complete characterisation of the microstructure:

Phase distribution
Texture strength
Grain size
Boundary properties
Misorientation data
Slip system activity
Intra-granular deformation
Plus much, much more

all provided while you get on with something else...!

Worked example of automated

EBSD
Analysis of polycrystalline samples of halite
(NaCl cubic)
Some samples have been experimentally
deformed
Variations in grain size and in extent of
subgrain development necessitate analysis at
different scales
Data source: Utrecht University, using a Philips XL30 FEG

Stage scan
orientation map of
polycrystalline
halite
100100 grid, step 100 m.

Analysis time: 4:04 hrs

4 mm

Beam scan orientation

map of polycrystalline
halite
300300 grid, 5 m step

Analysis time: 36 minutes

500 m

EBSD on different scales I

Large area scan

of polycrystalline
halite

3.5 mm

Compression
Stage scan, 350300 grid, 25 m spacing

EBSD on different scales II

Viewing intragrain microstructure and local lattice orientation variations...
A

200 m
Reflected light image

200 m

Beam scan, 250250 grid, 2.5 m spacing

Absolute and relative misorientation changes

across transect A-B.
6

A
5

Misorientations
relative to 1st
data point

A
Misorientation / degrees

Misorientations
between adjacent
data points

B
1

0
0

100

200

300

Distance / microns

400

500

EBSD data Maps

Phase distribution, Texture, Grain size / shape, Boundary properties,
Misorientation, Slip system activity, Intra-granular deformation....

EBSP quality

Orientation fcc

Orientation bcc

Phase map

Misorientation angles for fcc

EBSD data
Boundaries
Misorientation axis / angle
001

10-15 (49pts)

15-20 (59pts)

20-25 (76pts)

25-30 (78pts)

Rot. Axes in
crystal coordinates
[Duplex.cpr]
Fe-FCC (m3m)
Complete data set
6790 data points
Equal Area projection
Upper hemispheres
Forbidden zone limits:
upper angle
lower angle

111
101

CSL map for fcc

30-35 (120pts)

35-40 (253pts)

40-45 (168pts)

50-55 (231pts)

55-60 (5595pts)

60-65 (29pts)

45-50 (132pts)

Rot. Axes in
crystal coordinates
[Duplex.cpr]
Fe-FCC (m3m)
Complete data set
6790 data points
Equal Area projection
Upper hemispheres
Forbidden zone limits:
upper angle
lower angle

EBSD data
texture
ODFs

2=0

2=5

2 =1 0

2 =1 5

2 =2 0

2 =2 5

2 =3 0

2 =3 5

2 =4 0

2 =4 5

2 =5 0

2 =5 5

2 =6 0

2 =6 5

2 =7 0

2 =7 5

1
1.5
2
2.5

Pole Figures
=90
2 =8 0

2 =8 5

1 =9 0

Talk Outline
What is EBSD?
Crystallography & indexing
Data Collection
Recent Developments
Conclusions

Some Recent Developments

1. Improved camera technology increased
sensitivity and faster data acquisition
2. Combined EDX and EBSD for integrated
mapping and phase identification
3. Use of dual/cross beam instruments to obtain 3D
EBSD (combined FIB and electron beam)

EBSD detectors
Low light EBSP camera
Silicon intensified target (SIT)
8 bit, very noisy

CCD TV type video signal

8 bit less noisy

Slow scan CCD

12 bit, low noise, high speed, binning

Binning

Increases signal, reduces noise

Higher speed but at lower resolution

EBSPs - Feldspar

Old Camera

New Camera

Example Orientation Maps

Single Zircon Grain: substructured at one
edge, but a single orientation in centre.
21,545 points,
27 minutes (13 pts / s)

Ni-superalloy
60,000 points
17 minutes (63 pts / sec)
93% indexing

Halite - NaCl
121,204 points
48 minutes (42 pts / sec)
93% indexing

3D-EBSD

Talk Outline
What is EBSD?
Crystallography & indexing
Data Collection
Recent Developments
Conclusions

Conclusions
EBSD is an SEM-based technique that has been
known for 50 years, but only widely applied in the
last 10 years
EBSD is now a fast, automated technique,
applicable to most crystalline materials
EBSD provides phase identification, texture and
boundary characteristics.....