DIFFRACTION PHENOMENA IN SEM

by
Muhammad faheem khan
Roll# MM-11
The EBSD technique 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
that can provide microstructuralnformation in the form of grain
size and shape, phase identification and distribution,
crystallographic sample texture, phase and grain boundary
characteristics.

Electron backscatter diffraction (EBSD) is a powerful
technique which allows crystallographic Information to be
obtained from samples in the scanning electron microscope
(SEM).
INTRODUCTION



What is EBSD

Accelerated electrons in the primary beam of a scanning
electron microscope (SEM) can be diffracted by atomic layers in
crystalline materials. These diffracted electrons can be detected
when they impinge on a phosphor screen and generate visible
lines, called Kikuchi bands, or "EBSP's" (electron backscatter
patterns).
Typical SEM EBSD set-up
incident electron beam:
8-40kV, 0.01-50nA
Specimen:
Surface normal
typically
inclined 60-80
to beam
EBSD detector - position
usually constrained by
chamber geometry
EBSD detector distance
set to give ~90
angular range in EBSP
emitted
electrons
low-light sensitive (now
digital; originally analogue)
Diffraction Pattern-Observation Events
OIM computer asks Microscope Control Computer to place a
fixed Diffraction Pattern-Observation Events electron beam on a
spot on the sample
A cone of diffracted electrons is intercepted by a specifically
placed phosphor screen
Incident electrons excite the phosphor, producing photons
A Charge Coupled Device (CCD) Camera detects and amplifies
the photons and sends the signal to the OIM computer for
indexing

Diffraction Patterns-Source
Electron Backscatter Diffraction Patterns
(EBSPs) are observed when a fixed, focused
electron beam is positioned on a tilted
specimen
Tilting is used to reduce the path length of
the backscattered electrons
To obtain sufficient backscattered electrons,
the specimen is tilted between 55-75o,
where 70o is considered ideal
The backscattered electrons escape from
30-40 nm underneath the surface, hence
there is a diffracting volume
Note that and


oy ~2.5 to 3 times spot size


oy ~2.5 to 3 times spot size
e
-
beam
oz
oy
ox
20-35
o

Diffraction Patterns
There are two distinct artifacts
Bands
Poles
Bands are intersections of diffraction
cones that correspond to a family of
crystallographic planes
Band widths are proportional to the
inverse interplanar spacing
Intersection of multiple bands
(planes) correspond to a pole of those
planes (vector)
Note that while the bands are bright,
they are surrounded by thin dark lines
on either side
Diffraction Patterns-Anatomy of a Pattern
There are two distinct artifacts
Bands
Poles
Bands are intersections of diffraction
cones that correspond to a family of
crystallographic planes
Band widths are proportional to the
inverse interplanar spacing
Intersection of multiple bands
(planes) correspond to a pole of those
planes (vector)
Note that while the bands are bright,
they are surrounded by thin dark lines
on either side
Diffraction Patterns-SEM Settings
Higher Accelerating Voltage also
produces narrower diffraction bands (a
vs. b) and is necessary for adequate
diffraction from coated samples (c vs.
d)
Larger spot sizes (beam current)
may be used to increase diffraction
pattern intensity
High resolution datasets and non-
conductive materials require lower
voltage and spot size settings
Increasing the Accelerating Voltage increases the energy of the
electrons Increases the diffraction pattern intensity
a. b.
c. d.
Pattern capture-Background
The background is the fixed variation in the captured frames due to the spatial
variation in intensity of the backscattered electrons
Removal is done by averaging 8 frames (SEM in TV scan mode
Live signal Averaged signal
Note the variation of intensity in the images. The brightest point (marked with X)
should be close to the center of the captured circle.
The location of this bright spot can be used to indicate how appropriate the
Working Distance is. A low bright spot = WD is too large and vice versa
X
Detecting Patterns-Hough Transform
Lines in the captured pattern with points (xi,yi) are transformed into the
length of the orthogonal vector, r and an angle q
A modified Hough Transform is used, and changes the reference frame of
the pattern (transforms it)
The average grayscale of the line (xi,yi) in Cartesian space is then assigned
to the point (r,u) in Hough space
O x
y

u
I II
IV III
=0
=n
=-n
2n = Hough bin size
Transformed (Hough) space
I: 0rn ; 0qp/2
III: -n r<0 ; 0qp/2
II: 0rn ; p/2<q p
IV: -n r<0 ; p/2<q p
O
II
III IV
Hough Transform
The Hough transform is also known as the Radon
transform. The literature suggests that the actual
transformation used in OIM is a modification of the
original Radon transform. This modified transform is
designed for use with digital images.
The objective of the Hough transform is to
convert the parallel lines found in EBSD patterns
into points. These points can more easily be
identified and used in automatic computation.
r =x cos+y sin where r is the perpendicular
distance from the origin and the angle with
the normal.
The coordinate transformation is such that points in the Cartesian plane
transform to lines in the Hough plane. Or, more than one value of p and q
can satisfy the equation given above.
Thus, the numerical implementation of the transform is called an
accumulator: the intensity at each Cartesian point is added to the set of
cells in the Hough plane along the line that corresponds to that point. Thus
the intensity at points 1,2 & 3 in the example above, contribute equally to
the points along lines 1,2 & 3 in the Hough plane.
Detecting Patterns-The Hough of one band
Since the patterns are composed of bands, and not lines, the
observed peaks in Hough space are a collection of points and not just
one discrete point

Lines that intersect the band in Cartesian space are on average
higher than those that do not intersect the band at all
Transformed (Hough) space
Indexing requirements
SEM geometry:
beam energy, specimen & detector positions & orientations
usually fixed per SEM
Crystallography:
sample lattice parameters & Laue/space group
input per phase (i.e. composition) as required
Diffraction characteristics:
relative diffraction intensities from different (hkl) lattice planes
calculated per phase as required
Indexing Patterns-Identifying Bands
Procedure:
Generate a lookup table from given lattice parameters and
chosen reflectors (planes) that contains the inter-planar angles
Generate a list of all triplets (sets of three bands) from the
detected bands in Hough space
Calculate the inter-planar angles for each triplet set
Since there is often more than one possible solution for each triplet, a
method that uses all the bands needs to be implemented
Indexing Patterns-Voting Scheme
Consider an example where there exist:
Only 10 band triplets (i.e. 5 detected bands)
Many possible solutions to consider, where each
possible solution assigns an hkl to each band. Only
11 solutions are shown for illustration
Triplets are illustrated as 3 colored lines
If a solution yields inter-planar angles
within tolerance, a vote or an x is
marked in the solution column
The solution chosen is that with most
number of votes
Confidence index (CI) is calculated as



Once the solution is chosen, it is compared
to the Hough and the angular deviation is
calculated as the fit
Solution #
# votes
B
a
n
d

t
r
i
p
l
e
t
s

0.6
10
4 10
triplets band of number
S2 of votes # - S1 of votes #
CI =

= =
EBSD Pattern Recognition
EBSD pattern recognition
EBSD patterns are unique for a specific crystal orientation
The pattern is controlled by the crystal structure: space
group symmetry, lattice parameters, precise composition
Within each pattern, specific bands (i.e. pairs of cones of
diffraction) represent the spacing of specific lattice planes
(i.e. d
hkl
)
EBSD pattern recognition compares the pattern of bands
with an atlas of all possible patterns in order to index the
crystal orientation depicted
This process WAS manual it is NOW automated !
Example - next slide
pyrite
EBSD Patterns
Unique for crystal orientation &
composition at the point of
beam incidence
Can be >100 of total crystal
projection - easy to index as
symmetry decreases
Spatial resolution (s1m)
Some pattern details:
diffraction from
specific lattice plane
width = 1/d-spacing
1st order diffraction
2nd order diffraction
major crystal
pole
HOLZ ring
Example: pattern indexing
Original pattern
manual/auto-indexed bands
Computer indexed pattern
EBSD Problems
Spatial resolution
Angular resolution
Specimen preparation
Spatial resolution
Depends on the penetration &
deviation of electrons into a sample
(plus beam diameter)
Typically ranges from few m for
W-filament SEM to a few 100nm for
FEG SEM
Penetration depends on:
sample atomic number
accelerating voltage
beam current
(plus, coating depth &
surface damage - see
later)
Several Monte Carlo based
simulation packages are
available via the Web
(e.g.
http://www.gel.usherbrooke.ca/casino/index.html)
Example:
R
R
P
P
note down slope effect of tilting
Angular Resolution
Angular resolution of an individual EBSD pattern is typically
~1
Also important when determining the misorientation between
two (adjacent) crystal lattices (e.g. grains) misorientation
analysis is becoming a popular application of EBSD as it
provides information on sample properties & behaviour
But, calculations of misorientation axes from 2 individual
measurements with misorientation of <15 contain
increasingly large errors
Angular resolution depends typically on basic EBSD set-up
configuration, EBSD pattern quality & hence indexing
software (parameters, composition, pseudo-symmetry,
etc.)
Examples
Angular resolution 1:
sample-detector considerations
Small detector distance Large detector distance
good for indexing but
poor angular resolution
poor for indexing but good angular
resolution
important for constraining
misorientation axes.
Angular resolution 2:
effect of angle imaged
Changes in high resolution EBSD patterns can be used to define better
rotation angles & more accurate misorientations
large angular spread:
low angular resolution
low angular spread:
good angular resolution
Orientation Contrast
Imaging
polycrystalline sample
Control of crystal orientation
on emission signal
note variation in image grey-scale level - depends on penetration &
emission, which depend on crystal orientation
EBSD microstructural images
Electron beam is scanned over an area of a tilted sample, rather than
positioning the beam on a point for EBSD patterns
quartzite
FSE Orientation Contrast image of variation in crystal orientation -
contrast variations only qualitative (next slide)
FSE signal detected
by silicon devices
attached to EBSD
detector
Forescattered
electrons (FSE) with
intensities determined
by penetration (i.e.
crystal orientation) are
emitted towards the
EBSD detector
Automated EBSD Analysis
Automated EBSD analysis
Computer controlled movement
of the electron beam across a
sample
EBSD pattern captured at each
point
Indexing of EBSD patterns is via
pattern recognition software
Software writes the crystal orientation
(3 Euler angles), & phase information
per pattern to a data-base for later
analysis
BUT important to run a manual visual
check of solutions before the
automated analysis!
Automated EBSD
analyses
orientation contrast
crystal orientation variation pattern quality - strain
provides a variety of
information
crystal orientation pole figures
many other parameters:
e.g. misorientation
(becoming very important in
microstructural analysis)
P
T
Specimen Requirements
Specimen Preparation
Polished blocks, thin-sections, natural fractured or grown
surfaces
Surface damage (m-mm) created by mechanical polishing
must be removed:
chemical-mechanical (syton) polish
etching
electro-polishing
ion beam milling
Insulating samples may require very thin carbon coat, but
uncoated samples may perform OK - next
Charging Problems
Reduce charging by coating but only at expense of image
detail &/or resolution
Note: specimen damage can occur in absence of charging
K-feldspar. 20keV ~15nA (after D.J. Prior)
Uncoated 3-5nm
C coat
Effect of coating on OC images
200m
uncoated ~4nm C ~8nm C
(after D.J. Prior)
Summary
Orientation contrast images:
variations in crystallographic orientation & sample microstructure
EBSD patterns:
full crystallographic orientation of any point in OC image
Spatial resolution:
~100nm (FEG, metals) to ~1m (W, rocks)
Angular resolution:
~1 - 2 (misorientation >5 )
Materials:
most metals & ceramics; many minerals - depends on composition
Automated analysis:
100s of EBSD patterns/second (record ~800/sec via stage scanning)
but indexing accuracy may suffer (use of fast or sensitive EBSD
detectors increasing depending on requirements)
EBSD Applications
What can EBSD be used for?
Measuring absolute (mis)orientation of known materials -
most popular/obvious usage
Phase identification of known polymorphs - becoming
popular
Calculating lattice parameters of unknown materials -
difficult, only possible for relatively simple structures?
Measuring elastic strain
Estimating plastic strain on the scale of the electron
beam activation volume
Recommended applications
Tremendous significance for many types of materials
research, including:
- deformation & recrystallisation
- understanding processing histories
- effects of pre-heating & heat treatments
- identifying phases in multi-component systems
- microstructural characterisation & calibration
(including boundary geometry, etc.)
- modelling microstructural processes
- constraining micro-chemical data
- etc.
Example applications
Crystal orientation data from
SEM/EBSD
Individual orientation measurements related to
microstructure:
crystal lattice preferred orientations/texture analysis (i.e. inverse/pole
figures, orientation distribution functions
misorientation data (similar types of plots)
Non destructive
data be collected from representative samples
Automated
statistically large/viable data sets acquired
BUT! Samples must be oriented:
Materials - RD, ND, TD
Rocks X, Y, Z or NSEW
Selected bibliography
Field, D.P. 1997. Recent advances in the
application of orientation imaging.
Ultramicroscopy 67, 1-9.
Humphreys, F.J. 1999. Quantitative
metallography by electron backscattered
diffraction. Journal of Microscopy 195, 170-
185.
Electron backscattered Diffraction in
Material science By Adam j.schwartz
THANKS
Indexing requirements
SEM geometry:
beam energy, specimen & detector positions & orientations
usually fixed per SEM
Crystallography:
sample lattice parameters & Laue/space group
input per phase (i.e. composition) as required
Diffraction characteristics:
relative diffraction intensities from different (hkl) lattice planes
calculated per phase as required