Beruflich Dokumente
Kultur Dokumente
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
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