Focused Ion Beam &

Electron Backscattered
Diffraction
ENMT 604009

Wahyuaji NP – Myrna Ariati

Departemen Teknik Metalurgi dan Material FTUI

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Class info
• Credits : 2
• Semester : 4
• Prerequisite : Physical Metallurgy I
• Grading Systems : Homework, In Class Assgn., Finaltest
• Textbook :
• Callister, William D. 2007. Materials Science and Engineering, John Wiley &
Sons.
• Der Voort, Van. 1984. Metallography Principles and Practice, McGraw-Hill
Book Company.
• Goodnew, Peter J; Humphrey, John. 2000. Electron Microscopy and Analysis,
CRC Press
• Petzow, Gunter. 1991. Metallographic Etching, University Microfilms.
• ASM Handbook Vol 9 – Metallography and Microstructures, ASM
International
• Zhang, Sam; Li, Lin; Kumar, Ashok. 2008. Materials Characterization
Techniques, CRC Press.
• Schwartz, A.J.; Kumar, M.; Adams, B.L.; Field, D.P. 2009. Electron Backscatter
Diffraction in Materials Science, Springer US.
Class Schedule
Date Subject Note
03 April 2018 Class Review. Optical Microscope, Scanning Electron Microscope
10 April 2018 Focused Ion Beam, Electron Backscattered Diffraction
17 April 2018 Energy Dispersive Spectroscopy, X-Ray Fluorescence, Optical
Emission Spectroscopy
24 April 2018 X-Ray Diffraction, Transmission Electron Microscopy Homework
01 Mei 2018 Public Holiday
08 Mei 2018 Quiz In Class Assignment
15 Mei 2018 Software Assissted Metallography & Insitu Metallography
22 Mei 2018 Final Test
Class Rules
• Attendance is important but not mandatory
• No sleep in class
• Candies and drinks are allowed
• Late arrival is acceptable
• Don’t be noisy
• Homework submission
• Submit electronically
• Minus 10 points per day for late submission
• No plagiarism, no copy-paste
• Quiz, Mid test & Final test
• No cheating, no cell-phone, no restroom-break
• Late arrival is acceptable, however, no additional time
• Your answer-book will not be returned
• Any complaints or questions, please come to my office directly
FIB Introduction
• Electrons, used in scanning electron microscopes and
transmission electron microscopes, are not the only
charged particles that can be accelerated and focused
using electric and magnetic fields.
• An ion is an atom or molecule in which the total number
of electrons is not equal to the total number of protons,
giving it a net positive or negative electrical charge.
FIB Introduction
• In a scanning electron microscope, the relatively low-
mass electrons interact with a sample non-destructively
to generate secondary electrons which, when collected,
provide high quality image resolution down to the sub-
nanometer range.
• A focused ion beam (FIB) instrument is almost identical
to a SEM, but uses a beam of ions rather than electrons.
FIB Ion Sources
• Most widespread instruments are using liquid-metal ion
sources (LMIS), especially gallium ion sources.
• In a gallium LMIS, gallium metal is placed in contact with
a tungsten needle and heated gallium wets the tungsten
and flows to the tip of the needle where the opposing
forces of surface tension and electric field form the
gallium into a cusp shaped tip called a Taylor cone.
• The tip radius of this cone is extremely small (~2 nm).
The huge electric field at this small tip (greater than 1 x
108 volts per centimeter) causes ionization and field
emission of the gallium atoms.
FIB Ion Sources
• Source ions are then generally accelerated to an energy
of 1–50 keV (kiloelectronvolts), and focused onto the
sample by electrostatic lenses. LMIS produce high
current density ion beams with very small energy spread.
A modern FIB can deliver tens of nanoamperes of current
to a sample, or can image the sample with a spot size on
the order of a few nanometers.
FIB Ion Milling
• The focused ion beam can directly modify or "mill" the
specimen surface, via the sputtering process, and this
milling can be controlled with nanometer precision.
• By carefully controlling the energy and intensity of the
ion beam, it is possible to perform very precise nano-
machining to produce minute components or to remove
unwanted material.
FIB Deposition
• In addition, ion beam assisted chemical vapor deposition
can be used to deposit material with a level of precision
similar to FIB milling.
• A small quantity of a specifically selected precursor gas is
injected into the vicinity of the beam, where it is
decomposed by the beam, depositing the nonvolatile
decomposition products on the specimen surface while
the volatile products are extracted by the vacuum
system.
FIB Milling / Deposition
FIB Ion Milling
FIB Deposition
FIB Milling / Deposition
FIB Imaging
• The FIB's two imaging modes, using secondary
electrons and secondary ions, both produced by the
primary ion beam, offer many advantages over SEM

Secondary electrons mode Secondary ions mode

FIB Imaging
• FIB secondary electron images show intense grain
orientation contrast. As a result, grain morphology can
be readily imaged without resorting to chemical etching.
Grain boundary contrast can also be enhanced through
careful selection of imaging parameters.
• FIB secondary ion images also reveal chemical
differences, and are especially useful in corrosion
studies, as secondary ion yields of metals can increase by
three orders of magnitude in the presence of oxygen,
clearly revealing the presence of corrosion
EBSD Introduction
• Electron backscatter diffraction (EBSD), also known as
backscatter Kikuchi diffraction (BKD), is an SEM based
microstructural-crystallographic technique to measure
the crystallographic orientation.
• In EBSD a stationary electron beam strikes a tilted
crystalline sample and the diffracted electrons form a
pattern on a fluorescent screen. This pattern is
characteristic of the crystal structure and orientation of
the sample region from which it was generated. It
provides the absolute crystal orientation with sub-micron
resolution. It is a very powerful tool for microstructural
characterisation.
Kikuchi Band

Nickel diffraction pattern

Poly-Si diffraction pattern
EBSD Introduction
• An EBSD detector system will typically consist of following:
• A phosphor screen which is fluoresced by electrons from the sample to
form the diffraction pattern.
• A sensitive charge coupled device (CCD) camera together with optics for
viewing the diffraction pattern on the phosphor screen.
• A lead glass window behind the phosphor screen to block the radiation.
• Vacuum seals which allow the camera to operate at atmospheric
pressure without degrading the chamber pressure.
• Movement control which allows the detector to be positioned at
different positions; retracted position will be so that the detector
doesn’t interfere with normal SEM work.
• An interface in order to mount the detector onto the relevant SEM port.
• A computer to control EBSD experiments; collect and analyse the
diffraction patterns as well as display results and do further processing.
• Optional FSD detectors mounted around the phosphor screen.
• Electronic hardware that controls the SEM scanning.
• Communication control of SEM stage and column.
EBSD Introduction
EBSD Introduction
• For EBSD, a beam of electrons is directed at a point of interest on a
tilted crystalline sample approximately 70° relative to normal
incidence of the electron beam in the SEM
• The mechanism by which the diffraction patterns are formed is
complex, but the following model describes the principal features.
• 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 which satisfy
the Bragg equation

• where n is an integer, λ is the wavelength of the electrons, d is the

spacing of the diffracting plane, and θ is the angle of incidence of
the electrons on the diffracting plane.
Kikuchi Bands Formation
• These electrons are
diffracted to form a set of
paired large angle cones
corresponding to each
diffracting plane.
• When used to form an
image on the fluorescent
screen, the regions of
enhanced electron
intensity between the
cones produce the
characteristic Kikuchi
bands of the electron
backscatter diffraction
pattern
Kikuchi Bands Formation
• The centre lines of the Kikuchi bands correspond to the
projection of the diffracting planes on the phosphor
screen.
• Hence, each Kikuchi band can be indexed by the Miller
indices of the diffracting crystal plane which formed it.
Each point on the phosphor screen corresponds to the
intersection of a crystal direction with the screen. In
particular, the intersections of the Kikuchi bands
correspond to the intersection of zone axes in the crystal
with the phosphor screen. These points can be labelled
by the crystal direction for the zone axis.
Kikuchi Bands Formation

The indexing of the diffraction pattern shown in figure on the right. Kikuchi bands
are labelled with the Miller indices of the crystal planes that generated them (red).
The planes project onto the screen at the centre of the bands. Kikuchi band
intersections are labelled with crystal direction that meets the screen at this point
(white). This direction is the zone axis of the planes corresponding to the
intersecting Kikuchi bands
 Kikuchi Bands Formation
The nickel crystal unit cell
superimposed on the
diffraction pattern in the
orientation which generates
this pattern. The crystal planes
are labelled which correspond
to the (2-20) in blue and (020)
in yellow Kikuchi bands in the
diffraction pattern
The Kikuchi band width depends
on the d-spacing of the
corresponding plane. The (200)
plane d-spacing is wider than
the (2-20) plane so the Kikuchi
bands from (200) planes are
narrower than those from (2-20)
planes
The symmetry of the
crystal is shown in the
diffraction pattern. For
example, four fold
symmetry is shown
around the 001 direction
by four symmetrically
equivalent <013> zone
axes
Kikuchi Bands Formation
• The pattern is a gnomonic projection of the diffracted
cones of electrons onto the phosphor screen.
• The semi-angle of the diffracted cones of electrons is (90
- θ) degrees. For EBSD this is a large angle so the edges of
the Kikuchi bands approximate to straight lines.
• For example, the wavelength of 20 kV electrons is
0.00859 nm and the spacing of the (111) plane in
aluminium is 0.233 nm making the cone semi-angle
88.9°. The width w of the Kikuchi bands close to the
pattern centre is given by
Kikuchi Bands Formation
• where l is the distance from the sample to the screen.
Hence, planes with wide d-spacings give thinner Kikuchi
bands than narrow planes.
Pattern Identification
• Once an EBSD system has been calibrated, it becomes possible to
automatically index the diffraction patterns and calculate the crystal
orientation. This is typically accomplished using the following steps:
• The diffraction pattern is transferred from the camera inside the detector to
the EBSD software.
• The Hough transform is used to calculate the positions of the Kikuchi bands.
• Having identified the Kikuchi band positions and from knowing the calibrated
geometry, it is possible to calculate the angles between the detected bands.
• The calculated angles are compared with a list of interplanar angles for the
analysed structure(s).
• The possible solutions are sorted to find the best fit and the orientation
matrix is calculated.
• This whole process is automatic and takes less than a few milliseconds
on modern computers.
• The Kikuchi band positions are found using the Hough transform. The
transform between the coordinates (x,y) of the diffraction pattern and
the coordinates (ρ, θ) of Hough space is given by:
Pattern Identification
• Using the system calibration, the angles between the
planes producing the detected Kikuchi bands can be
calculated.
• These are compared with a list of inter-planar angles for
the analysed crystal structure to allocate Miller indices to
each plane.
• The final step is to calculate the orientation of the crystal
lattice with respect to coordinates fixed in the sample.
This whole process takes less than a few milliseconds
with modern computers.
Pattern Identification

Kikuchi bands Hough transform Peak identified

Lines & peak identification Indexed pattern

Pattern Identification
Pattern Identification
EBSD Summary
• When an electron beam is incident on a tilted crystalline
sample, electron backscatter diffraction patterns are formed
on a suitably placed phosphor screen.
• The diffraction pattern consists of a set of Kikuchi bands which
are characteristic of the sample crystal structure and
orientation.
• The centre line of each Kikuchi band corresponds to the
intersection with the phosphor screen of the diffracting plane
responsible for the band.
• The position of the Kikuchi bands can be found automatically
with the Hough transform and used to calculate the crystal
orientation of the sample region that formed the pattern