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ECH 6931
Spring 2019
Cross Section
Focused Ion Beam
Dirk van derWal / Hans Mulders FEI Presentation Looking below the surface
Focused Ion Beam
OUTLINE
FIB / SEM instrumentation
Electron Solid Interaction
Ion Solid Interaction
Focused Ion Beam milling - sputtering
FIB Induced Pt and C Deposition
Electrons Induced Pt and C Deposition
Cross Section
FIB template stripping
Sample preparation for TEM
Additional Capabilities of Dual Beam FIB
FIB slice and view. 3D reconstruction
End Point Monitor
Charge neutralizer
Focused Ion Beam
FIB Quanta 3D
SED
Sample chamber
Quanta 3D DualBeam® is a combination of two systems:
• Secondary electrons
• Backscattered electrons
• X- rays;
• Auger electrons
• Cathodoluminescance
Sample
Focused Ion Beam
FIB SEM
52°
15mm
30mm
Focused Ion Beam
The better choice of liquid metal is Gallium (atomic number 31, melting temperature 29 C
or 84 F). Liquid gallium partially wets heated tungsten filament and drawn into the cone
by applied electric field.
Nearly liquid metal at room temperature for minimal heating (stays superheated for hours)
Low volatility for long life (up to 1500 hr)
Non-reactive to W tip
Low energy spread and high angular intensity for excellent probes
Heavy ion for sputtering
Focused Ion Beam
Ion Column
Sample
Electron Column
Ion Column
Sample
Focused Ion Beam
SEM images
Focused Ion Beam
Ga stimulated SEM
Focused Ion Beam
Interactions between the incident ion and the solid occur at the expense of the
initial kinetic energy of the ion. Consequently, if the ion is not backscattered out of
the target surface, the ion will eventually come to rest, implanted within the target
at some depth below the specimen surface.
SEM images
Focused Ion Beam
When a target atom is knocked from its position, it can contribute to the collision
cascade.
Sputtering occurs if sufficient momentum is transferred from the collision cascade to a
surface or near surface particle.
The main parameters that govern the energy loss rate of the incident ion are its energy
(Eo), the atomic masses (MI and M2), and atomic numbers (Z1 and Z2), of the ion and the
target atoms, respectively. The nature of the cascade is dependent on the ratio of the
target to ion masses (M2/MI) and the incident ion energy.
The classification of collision cascades is divided into three regimes:
Regime I is called the single knock-on regime, and occurs when either MI << M2 or
Eo is low. In this regime, the recoil atoms do not receive enough energy to generate a
cascade and sputtering is minimal.
Regime II is the linear cascade regime where Eo is moderate and MI = M2. In this
regime recoil atoms receive enough energy to generate a cascade. Regime II is where
the FIB generally operates.
Regime III is called the spike regime where MI >> M2 and/or Eo is large. The result
is that the majority of the atoms within the spike volume move during the collision
cascade. Regime III is seldom reached during conventional FIB operation
Focused Ion Beam
TRIM calculations showing the relationship between the total stopping power and the mass density (left) and
melting temperature (right)for target elements Z= 1-92 at a Ga+ energy of 25 keV and 0" incident angle
Focused Ion Beam
Dose - is denoting the quantity particles absorbed by a sample. Dose has units
of ions/cm2.
Beam current - is also a measure of how many ions are delivered per unit
time. The beam current is measured in amperes, which is equivalent to units of
charge per unit time or Coulombs (C)/sec.
Ion-Solid Interactions
SPUTTERING
The sputtering yield, Y, is defined as the number of ejected particles per incident ion.
Sputtering can be considered as a transfer of kinetic energy from the incident ion to target
atoms result in the ejection of surface and near surface atoms, also referred to as knock-on
sputtering. Sputtering yields for typical FIB energies vary between 10 -1<Y<10 2 depending
on target and incident angle.
EJECTION DIRECTION
Ion-Solid Interactions
BACKSPUTTERING
Backsputtering occurs when an incident ion is scattered either directly back, or after
some number of multiple collisions, out of the target. (This phenomenon is analogous to
backscattering in electron-solid interactions). As shown in figure below, the
backsputtering yield of the incident ion increases with angle of incidence. In addition,
comparing the backsputtering yields between Si and Cu in figure 9 shows an increase
in backsputtering with an increase in mass ratio M2/M1. Materials with a higher mass
(Cu), have a correspondingly higher backsputtering yield of incident ions. Thus, more
particles are available for the possibility of redeposition.
Focused Ion Beam
The material dependence of sputtering yield (Y(Z)) for different elements shown below.
Material with a high relative Y(Z) will mill rapidly at any incident angle.
Focused Ion Beam
Ion-Solid Interactions
REDEPOSITION
FIB’s are most often used to create features of high aspect ratio
(i.e., deep narrow trenches). Sputtered material and backsputtered
ions may therefore deposit on surfaces that are in close proximity
to the active milling site (e.g., the sidewalls of a deep narrow
trench). Thus, surface degradation due to redeposition of
sputtered material must also be considered during FIB milling.
When an atom leaves a target material as a sputtered particle, it is ejected with a finite
kinetic energy. A sputtered particle can, therefore, be considered a projectile capable of
producing secondary interactions with local targets that lie in its trajectory. Depending on the
energy of impact and the sticking coefficient of the material, the sputtered atom may be
redeposited on the surface that it strikes. The sticking coefficient is a statistical measure of a
material's affinity to adhere to a surface, with a value of 1 equal to a 100% probability for
sticking. It has been observed that there is very little difference in sticking probabilities for
different materials for the low energy range exhibited by FIB sputtered. However the
geometry of the feature to be milled and the sputtering yield play critical roles in the amount
observed redeposition effects.
Focused Ion Beam
REDEPOSITION
The geometry of the feature to be milled and the sputtering yield play critical roles in the
amount observed redeposition effects. Figures a-c are SEM images of three trenches milled at
normal incidence in (100) Si and different doses.. The images shows that redeposition as the
aspect ratio is increased.
The shallowest trench has a fairly smooth appearance on the sidewalls and bottom. The
second trench is beginning to show some roughening of the sidewalls and corners which is
consistent with the
appearance of
redeposited material.
Also, the sidewalls are
beginning to show a
greater deviation from
the vertical direction. The
third case clearly shows
the effects of
redeposition. The
sidewalls have roughened
considerably and the
shape conforms to a
1.5 x 1012 Ga+ ions 3 x 1012 Ga+ ions 6 x 1012 Ga+ ions definitive "V".
in 4 minutes in 8 minutes in 16 minutes
Focused Ion Beam
REDEPOSITION
Redeposition is a function of a number of physically and chemically controlled variables,
some of which include:
The kinetic energy of the atoms leaving the surface;
The sticking coefficient of the target materials – SBE;
The geometry of the feature being milled;
Sputtering yield of the target materials
1.5 x 1012 Ga+ ions 3 x 1012 Ga+ ions 6 x 1012 Ga+ ions
in 4 minutes in 8 minutes in 16 minutes
Focused Ion Beam
An inherent ion-solid interaction in the FIB process is the result of ion implantation into the
target surface. The degree of ion implantation depends on ion energy, angle of incidence, ion
species, and target material as discussed above. Sample preparation by FIB uses the process
of ion bombardment to selectively remove material. Atoms that are displaced from their
equilibrium positions by the impingement of energetic ions generate a collision cascade
within the target material. Sputtering occurs if sufficient momentum is transferred to a
surface atom. One consequence of ion implantation can be the development of a surface
amorphous phase.
• Semiconductor • Bulk/Monolithic
• Metals • Fibers/Powders
• Ceramics • Geological
• Composites • Pharmaceutical
•Biological
Focused Ion Beam
Azom.com
Iisb.fraunhofer.de
Anff.act.anu.edu.au cmi.epfl.ch
Focused Ion Beam
52°
Focused Ion Beam
Pt protective layer:
Sputtering at the
edge 3x time faster
than surface
Focused Ion Beam
Deposition materials:
Methylcyclopentadienyl
(CH3C5H4)(CH3)3 Pt 30 C
Pt
Phenanthrene
C
Tungsten hexacarbonyl
W
W (CO)6 55 C melting point
O2 and thetramethoxylane
SiO2 (TMOS)Si(OSH3)4
Al Thrimethylamine alane
Focused Ion Beam
Pt deposition
Focused Ion Beam
Pt Deposition 3D Structure
2. Pt Deposition 3D Structure
OUTLINE
FIB / SEM instrumentation
Cross Section
FIB template stripping
Sample preparation for TEM
Additional Capabilities of Dual Beam FIB
FIB slice and view. 3D reconstruction
Pt protective layer:
Sputtering at the
edge 3x time faster
than surface
Focused Ion Beam
CROSS-SECTION VIEWING
AT 0° TILT and ROTATED
180°
Focused Ion Beam
52°
Focused Ion Beam
((CH3)3Pt(CnCH3) GIS
Focused Ion Beam
Dirk van derWal / Hans Mulders. FEI Presentation Looking below the surface
Focused Ion Beam
J.F Walker, R.F.Broom Inst Rhys Conf Ser., 157, 473 (1996)
Focused Ion Beam
52°
Focused Ion Beam
((CH3)3Pt(CnCH3) GIS
Focused Ion Beam
HR TEM
after FIB thinning
at 30 kV
and at 5 kV
• Charge neutralizer
Focused Ion Beam
SEM images of
vanadium oxide
nanotubes obtained at
different energies of
primary electron beam
http://www.microscopy.ethz.ch/
se-von-V.htm
Charge effect elimination in SEM
3. Low Vacuum SEM
Charge neutralizer
Charge accumulation.
When a specimen is nonconductive a negative charge from the electron beam (or positive charge
from Ion beam) tends to accumulate on the sample surface, thus effecting the final image.
Charge neutralization is a special
electron beam mode used for ion beam
imaging or milling of non-conductive
samples. The ions can positively charge
the sample causing an image drift and
spoiling the beam probe quality. In
charge neutralization mode, the electron
beam produced by the electron beam
column is used to compensate for the
positive charging. The electron beam is
unblanked during the imaging or milling.
It does not scan and is usually strongly
defocused.
Focused Ion Beam
Thanks