2010

March 2-5 EBSD Workshop

Electron BackScattered Diffraction
basics and applications

François Brisset (ICMMO)

Thanks to René de Kloe, Stuart Wright, Matt Nowell, John Carpenter
 ICMMO
Institut de Chimie Moléculaire et des Matériaux d'Orsay
(Orsay Molecular Chemistry and Material Institute)
280 persons
9 Research Teams 4 Research axes
• Synthèse organique et méthodologie
• Procédés et substances naturelles
• Catalyse moléculaire • Chemistry and Health
• RMN en milieu orienté • Chemistry for Energy
• Chimie bioorganique et bioorganique • Chemistry for Information
• Chimie inorganique • Chemistry for the Environment
• Glycochimie moléculaire et macromoléculaire
• Etude des matériaux hors équilibre
• Physicochimie de l’état solide

1 support team

UMR 8182 CNRS

[Link]
 Support team

Administration and general services

Personal, Financial&Purchases, Health&Security, Network, Communication, etc.

Instruments
10 Services including EM (SEMs and TEM)

Workshops
Glass and Mechanic

UMR 8182 CNRS

[Link]
 Books

New edition

- Provides a fundamental basis for electron backscatter diffraction

- Includes coverage of the crystallography required for application
and discussion of the state of hardware and software available
today
 diary
• Tuesday
– AM : General EBSD introduction
– PM : SEM/EBSD calibration and training session
• Wednesday
– AM : Sample preparation, Acquisition tutorials
– PM : SEM training session
• Thursday
– AM : Controlled pressure effect, Analysis tutorials, In-situ examples
– PM : SEM training session
• Friday
– Rui's conference on EBSD
– PM : SEM training session
 Some EBSD general

• What about electrons and backscattered

electron coefficient at 70° tilt.
α α α

0° 50° 70°

Electronic trajectories (in red, backscattered electrons)

η = n er
n If α is increasing the
interaction volume goes up
towards the surface and η
increases

If η is increasing its
dependency to Z decreases
 EBSD system
W, FEG hot cathod (cold), (LaB6)

Indexation Mapping

Camera PC
screen controls :
window camera, scanning, stage

Possible associated detectors : BSE, ACE and EDS det.

Electron BackScatter Diffraction
• Electron backscatter diffraction
patterns (or EBSPs) are
obtained in the SEM by
β focusing a stationary electron
e- beam on a crystalline sample.
• The sample needs to be tilted
to approximately 70° with
respect to the horizontal. The
diffraction pattern is imaged on
a phosphor screen.
• The image is captured using a
sensitive CCD camera.
• The bands in the pattern
phosphor screen sample represent reflecting planes in
the diffracting crystal volume.
 Bragg’s law
incident
electrons

sample

Diffraction of electrons from one side of a

lattice plane (Note: in EBSD both side - that
gives a pair of lines : the Kikuchi band)
Essentially an infinite source
of electrons scattering in all
λ = 2dhkl sinθ
nλ directions

λ wavelength, d lattice spacing, θ diffraction angle

 Electron BackScatter Diffraction
Diffraction occurs in all directions at more
or less one Bragg angle

Generated surfaces are conics

pairs of cones – plan families
{hkl & -h-k-l}

Conics interceptions with a screen give

"lines" pairs called Kikuchi band

Width = 2θ & pp d
1 band = 1 family plan
2 band intersections = 1 zone axis

1 pattern will gives angular relations

to calculate an orientation
 Spatially specific techniques
• Synchrotron Radiation
– Low Spatial Resolution (5µm), moderate angular resolution (1-2°), Good statistics, 3-d
information, difficult mathematical reconstruction, poor availability
• Polarized Light
– Not very quantitative, inexpensive, good accessibility, 2-d, limited materials
• TEM Diffraction (Kikuchi patterns, Spot patterns, CBED)
– High spatial resolution, good accuracy, extremely limited area, difficult sample preparation, as
of yet - limited automation, some 3-d information, poor statistics
• Electron Channeling
– Poor spatial resolution (5-10µm), moderate accuracy (0.5°), 2-d, no automation, poor
statistics.
• Kossel X-Ray Diffraction
– Poor spatial resolution (10µm), good accuracy (0.1°), 2-d, limited materials, no automation,
poor statistics.
• Electron Backscatter Diffraction
– Good spatial resolution (~10/20nm), good angular resolution (~0.5°), reasonable statistics
with automation, good availability, 2-d
Values as of 2007
EBSD – "two" main application areas

Orientation Imaging
Microscopy
Phase Identification (OIM)
 1 - Phase identification
EBSD

EDS Spectrum

Fe2TiO4

Candidate Phases

Database
EBSD – "two" main application areas

Orientation Imaging
Microscopy
Phase Identification (OIM)
2 - Orientation Imaging Microscopy - OIM

ϕ1, Φ, ϕ2
In an OIM scan the beam is stepped across the sample surface in a regular grid. At each point the EBSP
is captured and automatically indexed and the orientation and other information recorded (such as
the quality of the EBSP, an indexing reliability factor, the secondary detector intensity and EDS data.)
 SEM settings

0.6nA Beam Current 2.4nA Beam Current 9.45nA Beam Current

4.62 Seconds 1.56 Seconds 0.6 Seconds

SEM conditions play a role. As beam current goes up, exposure time goes down. By
keeping the camera gain constant, pattern quality doesn’t change much.
 Camera settings

Minimum Gain Mid-Range Gain Maximum Gain

2.76 Seconds 0.55 Seconds 0.15 Seconds

While judging pattern quality, it is also important to recognize the effects of camera settings.
Here three different camera gain settings are used. As gain goes up, exposure time goes down and
noise goes up.
 Camera resolution

1024 x 1024 512 x 512 128 x 128

2x2 8x8

The resolution of the camera will also affect pattern quality assessment.
Often for orientation mapping, camera gain is increased along with decreasing resolution to
increase camera frame rate.
 As-collected EBSD pattern
This is the pattern as-collected from
the camera system on a Ni alloy
sample.
Only a fraction of all electrons that
hit the detector carry diffraction
information.
Notice the intensity gradient and
the low contrast within the image.
 Background correction
1. Position beam within a grain and collect EBSD pattern
2. Background
3. Subtract background from pattern for improved EBSD pattern
 Camera resolution or binning

1x1 4x4 10 x 10

Clearly there are many ways of processing and presenting EBSD patterns.

Overall which way is better?

That's a compromise between rate of acquisition and pattern quality, at the end the important is to
index correctly
 Camera binning

4x4 6x6 10 x 10 4x4 10 x 10

Not cleaned cleaned

Sometime at the end the difference is not so obvious

 EBSD pattern indexing

How do we get from here ……………

… to ………………………… here
Calibration
 Calibration
- A correct indexation
- A good orientation

- PC coordinates : x* , y*, z* and WD

- monocristal Si (100) tilted at 70,45° zone

axis <114> is the PC

-Calibration file saved (*)

- Auto-tune, iterative procedure for each

new sample scanned (fit adjustment)
How do we find the bands?
– A. Hough transform
 Hough transform
Consider 4 pixels along a line. For each pixel in the line, all possible ρ values are calculated for θ’s
ranging in values from 0 to 180 degrees using the equation:
ρ = xcosθθ + ysinθθ. This produces 4 sinusoidal curves. This curves intersect at a point at a ρ, θ
coordinate corresponding to the angle of the line (θ θ) and its position relative to the origin (ρ
ρ).
Thus, a line in image space transforms to a point in Hough Space.
Hough transform

When the Hough transform is calculated, the Kikuchi

bands can be identified as bright peaks
 Pattern indexing: triplet solutions
• Determine a crystal orientation for each possible combination of three bands.
• The limited accuracy of the band detection requires the use of a tolerance so that
each triplet could represent multiple orientations.

Angle (hkl)1 (hkl)2

25.2 200 311
29.5 111 311
31.5 220 311
35.1 311 311
35.3 111 220
45.0 200 220
50.5 311 311
54.7 111 200
58.5 111 311
60.0 220 202
63.0 311 131
64.8 220 311
70.5 111 111
72.5 200 131
80.0 111 311
84.8 311 131
90.0 111 220
90.0 200 020
90.0 200 022
90.0 220 113
90.0 220 220
 Pattern indexing: triplet solutions

n # triplets

3 1
n!
# triplets =
(n − 3)!⋅3! 4 4

5 10

For a given number of bands, n, used for

6 20
pattern indexing, the number of band triplets is
determined by this formula.
7 35
Typically 7 to 9 detected bands are used for
automatic indexing.
8 56

9 84
 Pattern indexing: triplet voting
Detected
bands

Orientation solutions are calculated

for all combinations of three bands
( triplets ).
The orientation with the highest
number of votes is selected.

Indexed
pattern 2 4 9 2 1 1 1 1 1 1 1

Assuming 5 bands
 Pattern indexing: confidence index
The number of votes for the best
and second best orientation
solutions is used to calculate the
Confidence Index.

The Confidence Index gives an

indication if the indexing solution is
correct.

It is a measure for the

difference between the two
best solutions

V1 – V2
CI =
V Ideal

9 - 4 Assuming 5 bands
CI = = 0.5
10
A correct solution typically has CI > 0.1
 Pattern indexing : orientation
ND
3 Euler angles
ϕ 1, Φ , ϕ 2

Rolling Dir, Transverse Dir, Normal Dir

(Metallurgical representation) tilt axis

Crystal rotation from ϕ1 around [001]axis or z crystal axis

________________________ Φ___________[100] or x __________________
_________________________ ϕ _________ [001] or z __________________
2

3 Euler angles : describe necessary rotations to bring the crystal axes into
coincidence with the principal axes of the sample
 Indexing success vs. # of bands used - IPF
4 bands 5 bands 6 bands
Dual-phase Ti
IPF direction maps
// ND
Note : this is sample
dependant

7 bands 8 bands

9 bands 10 bands
 EBSD spatial resolution

Spot 2, 80 nm gs Spot 3, 90 nm gs

Different analysis areas

EBSD Grain Size Resolution
Step size: 2 nm
Unprocessed data (no cleanup)

6 nm grain

Spatial (position) resolution is better

than grain size resolution
 EBSD analysis

EBSD on polycrystalline Al2O3

 “Grains” in OIM
Grains in EBSD are formed by an algorithm
that groups sets of connected and similarly
oriented points into “grains”.
For each point in the scan, the neighbors
of this point are checked to see if they are
within the grain tolerance Angle of the
given point.
If a neighboring point is found to be within
the tolerance angle then the neighbors of
this point are checked to see if they are
within the tolerance angle of this point.
The procedure is repeated over and over
again until the set of connected grains is
bounded by points which exceed the
tolerance angle.
Grain size parameters – tolerance angle
1 degree tolerance 15 degrees tolerance
Grain size parameters – min grain size
1 “Pixel” 3 “Pixels”
 Grains in OIM

0.5º definition 1º definition 10º grain definition

What materials can be analysed using
Orientation Imaging Microscopy?

[111]

[001] [101] Inverse pole figure map showing crystal

Image Quality map of deformed steel
directions parallel to the sample normal

If the sample is crystalline and the question is related to a feature of the

microstructure, it can be studied using Orientation Imaging Microscopy
 Local misorientation maps
Image Quality Map Local Misorientation Map

Average
misorientation
of a pixel with its
6 neighbours
coloured from
blue to red (0 to
5°)

EBSD pattern from EBSD pattern from

recrystallised material deformed material

sharp
blurred
 Maps: colour & gray scale

Combined IQ and EDS maps showing the distribution of Fe and Cr in an oxidised reaction zone
on steel
 OIM interactive analysis
Misorientation analysis

Misorientation Angle

0.15
Number Fraction

0.10

0.05

0.00
10 20 30 40 50 60 70 80 90 100
Misorientation Angle [degrees]
Interactive analysis:
all maps, charts, and plots are linked,
allowing fast determination of spatial
distributions
OIM interactive analysis
Pole figures

Interactive analysis:
all maps, charts, and plots are linked,
allowing fast determination of spatial
distributions
 OIM interactive analysis
Grain size analysis

Grain Size (diameter)

0.12

0.10
Area Fraction

0.08

0.06

0.04

0.02

0.00
0.1 1 10 100
Grain Size (Diameter) [microns]

Interactive analysis:
all maps, charts, and plots are linked,
allowing fast determination of spatial
distributions
 Application – multiphase materials,
duplex steel

Duplex austenite (FCC) - ferrite (BCC) stainless

steel – phase differentiation.
Above : phase image
Right top : orientation map, austenite
Right bottom : orientation map ferrite
 Application – multiphase materials,
duplex steel

Duplex austenite (FCC) - ferrite (BCC) stainless

steel – phase differentation.
The orientation relationship between the phases
can be studied for understanding variant
selection.
Application – multiphase materials,
duplex steel

25.0
0% 20%
40% 60%
20.0

15.0

10.0

5.0

0.0
bain K-S N-W G-T

(B) Bain, K-S (Kurdjumov-Sachs), N-W (Nishiyama-Wassermann)

G-T (Greninger-Troiano) orientation relationships
 Think at...
• Help really useful, a lot of
information even from
crystallography, theory, how
maps, charts, figures are defined,
etc.
• Preferences (to setup some
default settings)
Help
Preferences
Various Operations
on data set
 Operation on dataset
Geometric partition

Complete
zone
 Merge

Increase statistic
Assembly of several data sets
 Multicharts

Data comparison tool

 combine graphs from several data sets
 1. dataset
Copy document / Paste
dataset or partition

2. Open another
dataset

3. dataset 1 4. dataset 2 The full set is

copy doc. paste recalculated
and drawn
 Partitions
Highlight / Non-Highlight

IQ
+
part.

IPF …
Create a project
Export a template Bath Mode
Start
batch mode
 Analyse
Mode Batch

Select
complementary
operation

Select model project

Automatic
creation of
project
 Clean up

grain dilatation
pseudo- symmetry
see others in the help – look for clean-up
 Grain dilation

most of the time it is very useful…

Do not hesitate to change the default
value 2 by a superior one, depending
on your data set.
 Grain dilation

Grain Dilation can actually work too well. Plausible microstructures can be
generated out of nearly random data (take care, always compare with
original data).
 Grain dilation
When using the grain dilation, it is often best to perform this one iteration at a time to
grow the grains out one level.
Pseudo-symetry – grain effect
Clean-up
Pseudo-symetry – why
Clean-up

OIM DC
Hough Page

rotation
 1
6 2

3 et 4

1bis
Clean-up
Pseudo-symetry – result Clean-up

before correction after one correction

Sample Preparation Techniques
for EBSD
Why is proper Sample Preparation so important to EBSD?

Contamination layers

Residual deformation

"good" material
Why is proper Sample Preparation so important to EBSD?
tilt 0° Fe - 20keV tilt 70°
η ~ 30% η ~ 60%

Energy Distribution

Escape depth
This is the important
point, the escape depth is
very small, so sample
should be crystallized on
165 nm < ~ 50 nm
the top surface.
Why is proper Sample Preparation so important to EBSD?

•EBSD patterns are formed from the near-

incident energy backscattered electrons

•Diffraction region forms within the top

10-50 nanometers of specimen

Top surface region must be free from

contamination layers or residual
deformation

•Specimen is tilted
approx. 70 degrees

Usually, as flat as
70°
possible
•Possible obstruction
 A unique Sample Preparation or not?

•General Polishing Techniques

•Overview of equipment/consumables

•Mechanical Polishing

•What constitutes a high quality EBSD pattern? (IQ)

•Advanced Polishing Techniques (difficult materials)

•Ion Etching/broad beam, dual beam FIB

•Electro polishing

•Chemical Etching

•Conductive Coatings
 General Polishing Techniques
•Overview of equipment/consumables

Sectioning equipment

High speed cut-off wheel Low speed diamond saw

Band Saw

High speed saw Low speed diamond saw

•Fast operation •Slower cut rates
•Cut variety of materials •Typically smaller specimens
•More deformation at •Less deformation at surface
surface
 General Polishing Techniques
•Overview of equipment/consumables

Mounting equipment

Hot mount/ Cold Mounting

•Used when samples cannot
compression withstand heat or pressure
•Sample must withstand •Many samples at once
pressure and heat •Acrylics chosen for rapid
•Conductive mounts cure times
•Uniform size mount •Epoxies chosen for flow
•Economical and penetration– used when
•Fast better adhesion, less shrinkage
and clarity are required

Hot mount press

 General Polishing Techniques
•Overview of equipment/consumables
Grinding/polishing wheels

Manual grinder/polisher Semi-automatic grinder/polisher Vibratory polisher

List of commonly used consumables

•SiC discs: 240, 320, 400, 600, 800, 1200 grit

•Polishing cloths
Low-napped synthetic rayon used with
Very good all purpose polishing cloth
- diamond (9-0.25 micron)
- colloidal silica or alumina (0.06-0.02 micron)
•9, 6, 3, 1, 0.10, 0.05 micron polycrystalline diamond suspensions
 General Polishing Techniques
List of "special" commonly used consumables
•0.5 micron cerium oxide (very soft materials : Pb, Sn)
•30, 15, 3, 1, 0.5, 0.1 micron diamond lapping films
(especially useful for : ceramics and very hard materials)
•3, 1, 0.25 micron polycrystalline diamond aerosol spray
(for use on : materials that react to water-Mg)
•0.05 micron nanopolish (non-water based final polish)

•0.05, 0.02 micron colloidal silica (pH 9)

•0.05 micron colloidal alumina (very aggressive-pH 3.5)

by example, use polycrystalline diamond when you need…

•Superior surface finishes in less time
•Less subsurface deformation
•Higher removal rates due to more cutting surfaces per particle
•Uniform removal when polishing samples composed of different materials or hardness
•Improved edge retention
 General Polishing Techniques
1 - Grinding
•Initial grinding to create planar surface
•Subsequent grinding steps to remove previous deformation
•Use new SiC paper each time
•15 seconds maximum grinding time

Abrasive Grade Comparison Chart

US industrial Mesh
240 280 320 360 400 600 800 1200
European FEPA or P-Grading
280 360 400 600 800 1200 2400 4000
Micron Grading
52 40 35 26 22 15 10 5
 General Polishing Techniques

2 - Polishing
•Begin with 9, 6, 3 micron diamond solution with
softer materials (5-10 minutes)

•1 micron alpha alumina (5-10 minutes)

•0.3/0.25 micron alpha alumina (5-10 minutes)

And next

•0.05/0.02 micron colloidal silica (several seconds to

several hours)
 General Polishing Techniques

3 - Final polishing with colloidal silica

•Silicon dioxide particles dispersed in chemically aggressive
carrier.
•PH values range from 8 to 10
•Creates chemical/mechanical polishing action
•Excellent in removing final deformation layer from surface
•Works well on nearly all materials
•Particular effectiveness on ceramic, geological IC, and
softer materials
•0.02 micron colloidal silica better for softer materials,
(lead, Aluminum, etc.)
 General Polishing Techniques
•Overview of equipment/consumables

Cleaning/Etching equipment

Ultrasonic Cleaner
(Ethanol, acetone,
Isopropyl alcohol, etc.)
Ion-etcher/coating machine
 Advanced Polishing Techniques

•Electrolytic polishing
•Chemical polishing
•Etching and double beam polishing

Some other techniques to use

• Conductive coating
• PC SEM
 Electro Polishing
•Electro polishing is removal of surface material by electrolytic action.

• The sample ground to 600 grit or finer and made the anode in an electrolytic cell containing
the appropriate electrolyte.

• Remnant deformation layers and surface irregularities removed, leaving a smoothed and
brightened surface finish when correct combination of temperature, voltage, current density,
and time is employed.

•The literature on electro-polishing is extensive, with many different solutions published for a
wide variety of metals. Many of these are listed in the Appendix H of Metallography
Principles and Practice by George Vander Voort.
 Electro Polishing

Disadvantages:
•Some electrolytes are poisonous, highly corrosive and can be explosive.

•Results can be difficult to reproduce, due to the number of variables that can
affect the polish, including:
-surface area to be polished
-orientation of sample/cathode in bath
-ratio of cathode to anode surface area
-anode to cathode spacing
-bath temperature/age
-degree of bath agitation
-current density and voltage
-time
 Chemical Etching
•Specimen is submersed in or swabbed with chemical solution
that selectively removes surface material.

•This technique is effective for removing any remaining surface

deformation due to the higher surface energy of the deformed
crystal lattice.

•Important to choose proper etchant for best results. Solution

that leaves film or residue not desirable.

•Must not create topographical differences that would affect

EBSD pattern (shadowing). Keep etching times short.

•Good choice for many materials is Nital (5% Nitric Acid

95% Ethanol)
 Ion etching

Using broad beam

•For some samples, mechanical, electro or chemical

polishing are not feasible options (thin films, IC, etc.)
•Ion etching is a alternative preparation technique for
EBSD analysis
•Ionized inert gas is accelerated towards the sample, and
the impact removes sample material
Results of Ion etching experiment on Ni sample

•Best results obtained with 2.5 kV tilted etch

•For higher energies, tilted etching did not improve
results.
•This may be explained by the interaction volume of the
ions with the sample material.
•While Ion Etching does damage the sample surface
compared to mechanical polishing, it does have
applications where traditional polishing is not possible
 Ion etching application

Aluminium alloy

SE image Mechanical polishing Ion beam polishing

- Matrix : no polishing Matrix and precipitates :
- Precipitates : good good polishing
polishing
Using Control Pressure SEM on
EBSD analyses
instead of coating ?
Why use control pressure SEM for EBSD analyses ?

BSE detector

Low vacuum: (10 – 200 Pa)

gas: N2 – H2O – air

* e-
*
charge neutralisation
e-

non-conductive specimen
 control pressure SEM
skirt effect

How to minimise the skirt effect:

1: Lower the pressure as much as possible.

0.1 Torr

1 Torr
 control pressure SEM
skirt effect
How to minimise the skirt effect:
2: Decrease the working distance as much as possible

5 mm

20 mm

Note:
Usable WD range is limited because of
camera position
 control pressure SEM
skirt effect
How to minimise the skirt effect:
3: Increase the accelerating voltage.

20 kV

10 kV

Note:
Use the highest possible voltage
 control pressure SEM
skirt effect
How to minimise the skirt effect:
4: Use a gas with lower Z

H20 vapour

Air
 EBSD analysis in low vacuum

Main reasons:

avoid charging (beam drift,...)

• coating
• use gaz

avoid the need for conductive coatings

 Coating effects on SE images

SE Images from ZrO2

No Coating

10 Å Carbon

orientation
contrast
20 Å Carbon

less orientation
contrast anymore
 Coating effects on EBSD patterns

Why Avoid coating ?

ZrO2 ZrO2 ZrO2

Coating : Au-Pd Coating : Au-Pd Coating : carbon
Thickness : 1 nm Thickness : 7 nm Thickness : 10 nm

Coating can suppress pattern

 Coating effects on EBSD patterns
EBSP Image Quality vs. Coating Thickness
Normalized IQ

Coating Thickness (Å)

Carbon coating
 Coating effects on EBSD patterns
EBSP Image Quality vs. Coating Thickness
1
0.9 C on Ni
Au/Pd on Ni
0.8
C on Si
Normalized IQ

0.7
Au/Pd on Si
0.6
0.5
0.4
0.3
0.2
0.1
0
0 20 40 60 80 100
Coating Thickness (Å)

If a coating is used use a low Z element

 Sequence of EBSD patterns

High vaccum 0.1 mbar – 10 Pa 0.4 mbar – 40 Pa

0.6 mbar – 60 Pa 1.0 mbar – 100 Pa 1.3 mbar – 130 Pa

 EBSD scan results at various pressure

Ni sample

High vaccum 0.6 mbar – 60 Pa 1.3 mbar – 130 Pa

99.3% CI>0.2 97.4% CI>0.2 84.8% CI>0.2
 EBSD scan results at 15 Pa, 4x4 binning

Alumina

No coating

N2 - pressure 15 Pa
Cleaned scan
Step 0.2 microns

740 000 points

area (µm x µm) : 95 x 270

Original scan
 Conclusion
• Gas avoids the deposition of a coating
• Gas removes the charging effect
• Gas spreads the beam and the BSE
• Gas decreases the quality of the EBSD patterns

•But

• Charging effect usually are removed as soon as 20-40 Pa

• The pressure is low enough to avoid most of the scattered effect because of HV
• The pressure is low enough to avoid a large decrease of the pattern quality

Then

It is a very good solution to use a pressure control SEM for non conductive sample
In-situ experiments
 3D Data Reconstruction

• Once images are acquired, reconstruction process

• Image
correlation
alignment to
get a better
result and
reduce shift
effect between
images
Serial Sectioning – Grain Extraction
 3D tools

• Transparency
• Objects selection
• Multi-selection of objects
 3D tools – grain representation
• Rotation and zoom functions
Recrystallisation & Grain Growth

0 min 30 min 45 min

60 min 90 min 120 min

Heating Stage Experiments
 Heating Stage Experiments

Cobalt
Transition Temperature = 422°C

Beta: FCC Phase Alpha: HCP Phase

 Heating Stage Experiments
phase transformation - reversibility
510
410
310
210
110
10
96.00 97.00 98.00 99.00 100.00 101.00 102.00 103.00
 Heating Stage Experiments
phase transformation - Misorientation
β-Co (fcc) α-Co (hcp)

α-Co

β-Co

Alignment of [111] and

[0001] axes of α and β
cobalt at phase transition
 Tensile Test: Setup

Displace the sample to a given strain step and then hold during the scan. (Tend to
get some variance in the force measured before and after the scan)
Scan Rates of approximately 60 points per second. ~6 minute scans

As deformation progresses, the surface

roughens making it progressively difficult to
obtain good OIM scan data.
The scanning area is also displacing making
it necessary to “find” it again after each
strain step.
Better to notch the sample in order to
guarantee that necking occurred in the scan
region.
Tensile Test