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Focused Ion Beam & Electron

Backscattered Diffraction
Tech. of Microstructural Analysis
Wahyuaji NP
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
150 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 doesnt 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, is the wavelength of the electrons, d is the


spacing of the diffracting plane, and 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 The Kikuchi band width depends The symmetry of the
superimposed on the on the d-spacing of the crystal is shown in the
diffraction pattern in the corresponding plane. The (200) diffraction pattern. For
orientation which generates plane d-spacing is wider than example, four fold
this pattern. The crystal planes the (2-20) plane so the Kikuchi symmetry is shown
are labelled which correspond bands from (200) planes are around the 001 direction
to the (2-20) in blue and (020) narrower than those from (2-20) by four symmetrically
in yellow Kikuchi bands in the planes equivalent <013> zone
diffraction pattern 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 - ) 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 (, ) 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

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