EBSD Explained Web
EBSD Explained Web
EBSD Explained Web
EBSD Explained
Introduction
Basics of EBSD
Cam
era
SEM Column
Forescatter diodes
Phosphor screen
(University of Sydney).
EBSD
Industries
Materials
Metals, Alloys
Grain size
Aerospace
Intermetallics
Automotive
Global texture
Nuclear
Ceramics
Local texture
Microelectronics
Thin Films
Earth Science
Solar Cells
Academia
Geological
Substructure analysis
Semiconductors
Phase identification
Superconductors
Ice
Phase transformation
Fracture analysis
Bone, teeth
Dete
ctor
SEM Stage
Controller
2 EBSD Explained
EBSD Explained 3
Basics of EBSD...
Pattern formation and detection
Band intensity
The following model describes the principle features of pattern formation and detection for EBSD analysis. A beam
of electrons is directed at a point of interest on a tilted crystalline sample. The atoms in the material inelastically
scatter a fraction of the electrons, with a small loss of energy, to form a divergent source of electrons close to
the surface of the sample. Some of these electrons are incident on atomic planes at angles that satisfy the Bragg
equation:
The mechanisms giving rise to the Kikuchi band intensities and profile shapes are complex. As an approximation,
the intensity of a Kikuchi band for the plane (hkl) is given by:
where n is an integer, is the wavelength of the electrons, d is the spacing of the diffracting plane, and the angle
of incidence of the electrons on the diffracting plane.
These electrons are diffracted to form a set of paired large-angle cones that correspond to each diffracting plane.
The image produced on the phosphor screen contains characteristic Kikuchi bands which are formed where the
regions of enhanced electron intensity intersect the screen (Fig. 2). The pattern seen is a gnomonic projection of the
diffracted cone, making the band edges appear hyperbolic.
where fi() is the atomic scattering factor for electrons and ( xi yi zi ) are the fractional coordinates in the unit cell for atom i. A
collected diffraction pattern should be compared with a simulated pattern calculated using the previous equation.
This ensures only planes that produce visible Kikuchi bands are used when solving the diffraction pattern. The
optimum number of reflectors to use depends on the phases that the system needs to distinguish between, and on
the crystal symmetry of the phases.
4 EBSD Explained
Fig. 3. The spherical diffraction patterns generated by different orientations of a cubic structure.
EBSD Explained 5
Basics of EBSD...
Calibrating an EBSD system
In order for an EBSD system to work correctly, it must
first be calibrated. Typically, the EBSD system calibration
involves measuring the sample-to-screen distance and
the pattern-centre position on the phosphor screen.
The pattern centre is the point on the screen closest to
the generation point of the diffraction pattern on the
sample.
AZtecHKL
Once an EBSD system has been calibrated, it
becomes possible to automatically index the
diffraction patterns and calculate the crystal
At a glance...
orientation. This is typically accomplished using
the following steps:
Fig. 5. The Hough transform converts lines into points in Hough space.
6 EBSD Explained
Fig. 6. Finding the position of the Kikuchi bands in the diffraction pattern using
the Hough transform.
A) Diffraction pattern collected from silicon at 20kV accelerating voltage;
= x cos + y sin
D) The indexed diffraction pattern with the blue cross indicating the position of
the pattern centre.
EBSD Explained 7
EBSD Developments
EDS Detector
Pole Piece
FSD
EBSD Detector
Band detection
Band detection is a fundamentally important aspect
of EBSD and is critical in terms of data quality.
Improvements in band detection can increase the
number of correctly indexed points, especially for
materials that exhibit indistinct bands or have low
quality patterns, such as those consisting of highly
strained or partially recovered microstructures.
Sample
50 mm
Na
Al
Fe
Without TruPhase
With TruPhase
Indexing routines
Refined accuracy
A) The relative positioning of the sample, EDS and EBSD detectors inside the SEM chamber.
B) A forescatter diode (FSD) image of the area of the sample being analysed.
C) Na element map, the highest concentration is found in albite.
D) Al element map, the highest concentration is found in muscovite.
E) Fe element map, the highest concentration is found in biotite.
F) A phase map acquired using traditional EBSD. Due to their similar crystal structures, biotite and muscovite are poorly differentiated, resulting
in a speckled appearance.
G) A phase map acquired using the TruPhase routine in AZtec where EDS data is collected simultaneously to EBSD data and used to inform the
solution given for the EBSP. This method successfully differentiates the biotite and muscovite mica in the sample.
8 EBSD Explained
* patent pending
Sample courtesy of
Dr Elisabetta Mariani,
University of Liverpool.
EBSD Explained 9
PhaseID
Phase discrimination
The detected Kikuchi pattern is generated by the electron beam interacting with the crystal structure in the surface
layer of the sample. This means that the EBSP carries information about the crystal structure it was generated from.
By analysing the EBSP, we can get information not just about the orientation of the crystal but also information that
makes it possible to distinguish between different crystal structures, and hence phases. An example is shown in Fig. 9.
Fig. 9. The discrimination of the two phases present in a sample of tungsten hardened alloy. A) A phase map showing the two separate phases
(Ni is shown in red and W in blue). B) A typical EBSP obtained for W. C ) A typical EBSP for Ni.
Typically EBSPs are analysed by looking at the angles between the detected bands. If only this information is used,
then it is possible to distinguish between phases that have different unit cell structures as long as one structure is
not just a scaling of another (Fig. 10).
Modern systems can extract information about the width of the bands within the EBSPs, which helps to distinguish
between phases of same structure type but different lattice parameters.
To build a crystal
- Start with unit cell
- Add a basis
- Repeat ad infinitum...
Unit cell
Basis
10 EBSD Explained
EBSD Explained 11
Point analysis
PhaseMap
Based on the saved information, it is possible to generate different map displays. For example, it is easy to generate
a map showing how the phases are distributed within the sample. This can be done by assigning a colour to each
phase, and colouring the map pixel based on which phase was found during the analysis (e.g. Fig. 9).
where hi is the peak height of the Hough transform of the ith most intense Kikuchi band, and sh is the standard
deviation of the Hough transform, however it is normally calculated in a more advanced way. The pattern quality
parameter will associate a number with how sharp or well defined the band positions are in the EBSP. This means
that the pattern quality (e.g. Fig. 12) will be influenced by several factors: phases, orientation, contamination,
sample preparation and the local crystalline perfection.
Fig. 11. Point analysis of grains in steel showing the diffraction pattern generated and the
calculated crystal orientation in Euler Angles.
Mapping
The typical sequence for manual point analysis is:
1. Position beam
2. Acquire EBSP
3. Detect bands
4. Index based on phase list
5. Save the result. At each beam position, the system typically saves:
When all the parameters have been setup, such that no further user intervention is required, this flow can be
automated to cover a large area of the sample. During mapping of the sample, the above sequence is carried out
for each beam position as the beam automatically moves across the sample surface.
12 EBSD Explained
50 mm
Pattern quality maps will often reveal features invisible in the electron image such as grains, grain boundaries,
internal grain structure and surface damage such as scratches. This makes the pattern quality map very useful
during the analysis of the data but also as a simple tool for checking if the sample stayed in focus during the data
collection or if the sample drifted.
EBSD Explained 13
Euler angles
The determined orientations are normally described
by a set of Euler angles. Euler angles are the
most commonly used way to describe the sample
orientation relative to the crystal, where each
crystal structure has been given a certain reference
orientation. This involves rotating one of the
coordinate systems about various axes until it comes
into coincidence with the other. There are several
conventions on how the rotations are to take place.
The most commonly used way is to use the Bunge
notation where the three Euler angles: (phi1, phi,
phi2) represent the following rotations, which are
shown schematically in Fig. 13:
B
D
Orientation maps
The simplest way of generating an
orientation map is by plotting the
3 Euler angles using an RGB colour
scheme; this is often referred to as
an Euler map (Fig. 14).
The Euler coloured maps give
a basic presentation of the
microstructure. However there are
limitations of the Euler maps. One
of the issues is that small orientation
changes dont always correspond to
small changes on the colour scale,
which can cause confusion when
looking at an Euler map.
To accommodate these issues,
a different type of map display
is often used. The Inverse Pole
Figure (IPF) colour scheme uses a
different colour scheme, which is...
50 mm
Fig. 15. Crystal orientation maps obtained for a sample of tungsten
hardened alloy (shown in Figs. 8 and 14) collected at 20 kV
accelerating voltage.
Fig. 14. An all Euler angle colouring orientation map for the sample of tungsten hardened
alloy shown in Fig. 9. Note the colour wrapping that is characteristic of Euler colouring.
50 mm
50 mm
14 EBSD Explained
EBSD Explained 15
Misorientations
EBSD has a significant advantage over many other microstructural characterisation techniques in that it can
measure the misorientation between two crystals (i.e. the difference in the orientation). In order to define a
misorientation, it is easiest to consider a triclinic crystal i.e. one that has no symmetry. For any two triclinic
crystals, there is a unique rotation axis and rotation angle which maps one crystal lattice onto the other. These
are referred to as the Misorientation Axis and the Misorientation Angle.
When the crystals in question have some symmetry, then there is no longer a unique axis-angle pair that
describes the misorientation between 2 crystal lattices. Depending on the symmetry, there may be up to 24
symmetrically equivalent axis-angle pairs that match 2 crystal lattices. It is not possible to determine which
of these different solutions is correct, and therefore it is convention to take the solution that has the lowest
misorientation angle (also referred to as the disorientation angle).
In a similar way, generating a map that shows the spatial distribution of the grain boundaries can often provide
additional information about the microstructure. A typical example would be to generate a map showing lowangle
A boundaries (which can give information about substructure of individual grains) together with high-angle
boundaries (which define the grain structure), Fig. 16.
A
CSL boundaries typically have a significant impact on the material properties, which means that from a materials
engineering viewpoint it becomes important to determine the ration of CSL boundaries and their distribution within
the material. An example from twinned nickel is in Fig. 18. As shown on the CSL histogram, the S3 boundary is the
most frequently occurring CSL boundary, which is also shown on the map where all the S3 (60, [111]) boundaries
are coloured red.
Texture
A
100 mm
Fig. 16. Grain boundary data for a sample of tungsten hardened alloy (shown in Fig. 9).
A) Grain boundary positions superimposed on the pattern quality image with grain boundaries higher than 2 degrees
highlighted in purple, higher than 10 degrees in black, and phase boundaries are in red;
B) Histogram of grain sizes from the Tungsten (W) phase. The average grain size is shown to be 17 m.
16 EBSD Explained
Fig. 18. CSL boundary data measured by EBSD for a Nickel sample.
A) Pattern quality map for a sample of Nickel;
B) Coincident site lattice (CSL) boundary positions superimposed on the previous pattern quality image;
C) The boundaries are colour coded by CSL type as shown in the histogram of CSL found.
EBSD Explained 17
In most materials, grains do not have a completely random orientation distribution, and when the distribution is
not random, the sample is said to have a preferred orientation or texture. Based on the orientation information
acquired from several points within each phase, it is possible to statistically check whether a given phase has a
preferred orientation. This can be done in several ways; one way would be to look at maps highlighting the points
with an orientation close to a specified reference orientation, referred to as texture maps. They can be very useful
because they contain information about the spatial distribution of the reference texture (Fig. 19).
Another approach is to generate pole figures for the identified phases, and to use the pole figures to reveal
information about the texture within a given phase. If there are several phases within the sample, pole figures can
easily be used to identify relationships between the orientations near the interface boundaries (Fig. 20).
50 mm
200 mm
Fig. 19. Area fractions for multiple reference textures for a sample of
cold rolled Al Mg alloy.
18 EBSD Explained
EBSD Explained 19
Pole figures are tools for plotting 3D orientation information in 2D (such as on a sheet of paper or a computer
screen). They are useful for showing the orientations of specific crystallographic planes and directions within a
sample (i.e. for plotting the texture) and, as such, are invaluable for EBSD.
A pole figure plots crystallographic directions in the sample coordinate system, whereas an inverse pole figure plots
sample directions in the crystallographic coordinate system. For example, instead of plotting the <111> directions in
terms of the rolling direction (RD) and normal direction (ND), an inverse pole figure could plot the rolling direction
in terms of the major crystal directions (i.e. [100], [110] and [111]). Inverse pole figures have several benefits over
conventional pole figures, such as:
A pole figure shows the projected position of a particular set of crystallographic planes, where the poles (or
normals) have been projected onto a sphere and then onto a circle. There are two main methods for doing this, the
stereographic and equal area projection. This section explains the stereographic projection.
If we start with a single crystal, shown by the unit cell on the left in Fig. 21, it is orientated in a particular manner
relative to the sample, bottom left of Fig. 21.
Each data point appears as a single point in an inverse pole figure. In many pole figures, for higher symmetry
phases, a single data point may be represented by multiple points on the pole figure (e.g. 3 symmetrically
equivalent {100} poles).
It is often easier to pick out particular fibre textures using an inverse pole figure.
Inverse pole figures are often used as a default colouring scheme for orientation maps (by colouring the three
corners of the inverse pole figure triangle with the primary colours).
The appearance of an inverse pole figure depends on the Laue group of the relevant phase. This determines the
size of the unit triangle i.e. the symmetrically equivalent space in the whole stereographic projection. For
example, a triclinic crystal (Laue group 1) has no symmetry and therefore the whole pole figure is necessary to show
all the possible crystal directions. Therefore for triclinic structures, the inverse pole figure is like a pole figure a full
circle.
Fig. 21. The production of a stereographic projection for a single crystal (in this case a unit cell), which is orientated in a particular manner to
the sample.
The {100} plane normals, of which there are 6 for this cubic crystal, would project onto a sphere as shown in the
second drawing. A plane, parallel to the sample surface and passing through the centre of our sphere would
intersect the sphere as a circle.
We now join the points where the {100} plane normals touch the sphere to the spheres opposite pole. This is
shown in the third image. Note: only the upper hemisphere points are shown. It is possible to repeat the process
for the lower hemisphere points. In general, in materials science, it is conventional to plot in the upper hemisphere,
whereas in the Earth sciences the lower hemispheres are commonly used.
If we now look at just the circle, we will see that the three-dimensional crystallographic directions have been
converted into points. This is the {100} pole figure. This can be repeated with the orientations of other grains
to give a pole figure that shows the distribution of that particular set of planes within the sample. If there is a
tendency for the points to be arranged in a particular manner, then we have a texture.
20 EBSD Explained
As the symmetry of the structure increases, the size of the symmetrically equivalent region decreases until, for Laue
group 11 (cubic high), there are 24
symmetrically equivalent regions in
the full circle. This is shown in Fig.22,
with the standard unit triangle
highlighted in the IPF colouring
scheme.
EBSD Explained 21
3D EBSD
As shown by different examples, EBSD can provide information from the sample surface. However, there is often
a requirement to get the same type of information from a 3D volume to study grain structures, grain size and
interface boundaries. Depending on the dimensions of the volume of interest, this can be achieved in several ways.
For large scale features, it is possible to use mechanical sectioning techniques to expose a new surface at different
depths of the sample. For small scale features, it is not practical to take the sample out of the SEM chamber and
then reposition it to collect more data. One solution is to use an SEM combined with a focused ion beam (FIB-SEM),
where the ion column can be used to mill away the surface between each EBSD map.
sensitive EBSD detector, otherwise the data acquisition time increases significantly, which leads to drift and stability
problems.
Fig. 25. The geometry of a system set up for TKD. Thinned samples
are mounted horizontally in the SEM chamber and positioned towards
the top of the EBSD detectors phosphor screen.
Recently an alternative technique to improve the spatial resolution has been demonstrated, and is becoming
popular. The technique is called Transmission Kikuchi Diffraction (TKD or t-EBSD), and it makes use of a
conventional EBSD system, however with the sample placed in a different geometry (Fig. 25).
For TKD, the sample must be thinned so that it is electron transparent (as for TEM). In this case, the scattering
event takes place on the lower surface of the sample as the electron beam exits from the sample. This means that
the sample can be placed at a shorter WD than for conventional EBSD, which in itself gives an improvement in
the spatial resolution. Secondly, due to the geometry, it is generally not required to tilt the sample more than 10
degrees (dependent on the setup) to be able to collect a good collection geometry while keeping the EBSD detector
in its normal geometry. Again, this leads to an improvement in spatial resolution.
TKD is still a new technique but it has already proven very useful for acquiring orientation data from materials with
a small grain size or high level of deformation, as shown by the maps on the front cover and the back page
(Fig. 26).
22 EBSD Explained
EBSD Explained 23
1 mm
www.oxford-instruments.com/EBSD
The materials presented here are summary in nature, subject to change, and intended for general information only.
Additional details are available. Oxford Instruments NanoAnalysis is certified to ISO9001, ISO14001 and OHSAS
18001. AZtec and Tru-I are Registered Trademarks of Oxford Instruments plc, all other trademarks acknowledged.
Oxford Instruments plc, 2015. All rights reserved. Document reference: OINA/EBSD Explained/0215.