The Meeting of National Graduate School of Nanoscience

Focused Ion Beam Technique in

Nanofabrication
Antti Suutala

Microelectronics and Materials Physics Laboratories

University of Oulu

9.6.2009 // 1
 Outline

• The Focused Ion Beam (FIB) Instrument

• Dual-Beam (FIB-SEM) Systems
• Ion – Solid Interactions
• Gases for Deposition and Enhanced Etch
-------------------------------------------------------------
• Device Edits and Modifications
• FIB In-Situ Lift-Out TEM Specimen Technique
• Patterning and Deposition Examples

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 The Focused Ion Beam (FIB) Instrument

• The basic FIB instrument consists of a vacuum system and chamber, a

liquid metal ion source, an ion column, a sample stage, detectors, gas
delivery system

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 The Focused Ion Beam (FIB) Instrument

• The instrument is very similar to a scanning electron microscope (SEM)

• FIB instruments may be stand-alone single beam instruments or

alternatively, FIB columns can be incorporated into other analytical
instruments such as an SEM, TEM, or secondary ion mass spectrometry
(SIMS)

• The most common of which is a FIB/SEM dual platform instrument

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 The Focused Ion Beam (FIB) Instrument

• The capabilities of the FIB for small probe (diameter ~ 5 nm) sputtering
are made possible by the liquid metal ion source (LMIS)

• Gallium is currently the most commonly used LMIS for FIB instruments
for a number of reasons:
– Low melting point
– Low volatility
– Low vapour pressure
– Excellent mechanical, electrical, and vacuum properties
– Emission characteristics enable high angular intensity with a small
energy spread

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 The Focused Ion Beam (FIB) Instrument

• A schematic diagram of a Ga LMIS

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 The Focused Ion Beam (FIB) Instrument

• Typical accelerating voltage in FIB

systems ranges from 1 to 30 keV

• The ion column typically has two

lenses; the condenser lens (1, probe
forming) and the objective lens (2,
focus)

• A set of apertures define the probe

size and provides a range of ion
currents (10 pA – 30 nA)

• Cylindrical octopole lenses perform

multiple functions such as beam
deflection, alignment, and stigmation
correction

• Beam blankers are used to deflect

the beam away from the centre of the
column
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 The Focused Ion Beam (FIB) Instrument

• Large working distance (1.5-2 cm) permits the introduction of samples

with varied topography without concern for field variations

• The sample stage typically has the ability to provide 5-axis movement
(X, Y, Z, rotation and tilt)

• The bombardment of charged species to the surface of an insulator can

cause sample charging

• Charge reduction methods:

– Good grounding of the specimen
– Coating the sample (C, W, Pt, Au, Cr, etc.)
– The use of an electron flood gun
– Imaging or milling with the SEM column turned on in dual platform
system

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 Dual-Beam (FIB-SEM) Systems

• A dual-beam system allows sample preparation, imaging, and analysis

to be accomplished in one tool

• The ion beam and the electron beam complement each other in charge
reduction, protective depositions, and imaging information

• The electron beam can be used to monitor the ion beam milling to
endpoint precisely on the feature of interest

• The dual beam provides unparalleled flexibility in 3D structural analysis

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 Dual-Beam (FIB-SEM) Systems

• The typical dual-beam column configuration is a vertical electron column

with a tilted ion column. In this case, the sample will be tilted to 52
degrees for milling normal to the sample surface.

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 Dual-Beam (FIB-SEM) Systems

• The electron beam can be used for imaging without concern of

sputtering the sample surface

• Electron beam deposition of materials can be used to produce very low

energy deposition that will not affect the underlying surface of interest as
dramatically as ion beam assisted deposition

• Non-destructive imaging of the sample may be accomplished with an

integrated SEM

• Additional peripherals such as EDS and EBSD may be used for

elemental or crystallographic information

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 Ion-Solid Interactions

• The ability to mill, image, and deposit material using a FIB instrument
depends critically on the nature of the ion beam – solid interactions

• When the beam strikes the sample surface, many species are generated
including sputtered atoms and molecules, secondary electrons, and
secondary ions

• Sputtering occurs as the result of a series of elastic collisions where

momentum is transferred from the incident ions to the target atoms
within a collision cascade region

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 Ion-Solid Interactions

• A schematic diagram below illustrate some of the possible ion beam -

material interactions that can result from ion bombardment of a solid.
Milling takes place as a result of physical sputtering of the target.

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 Ion-Solid Interactions

• 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

• The quality of the milled cuts or CVD regions depends critically on the
interactions between the impinging ion beam and the target

• The response of a given target material to the ion beam is strongly

dependent on factors such as beam current, incident ion energy,
trench/feature geometry, raster pattern, and milling angle

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 FIB Gases for Deposition and Enhanced
Etch

• Gas delivery systems can be used in conjunction with the ion beam to
produce site specific deposition of metals or insulators or to provide
enhanced etching capabilities

• The gas molecules are adsorbed on the surface in the vicinity of the gas
inlet, but decompose only where the ion beam strikes

• Repeated adsorption and decomposition result in the buildup of material

in the ion scanned region

• The chemical precursors are obtained from a gas, liquid, or solid source
that can be heated if required to produce the desired vapour pressure

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 FIB Gases for Deposition and Enhanced
Etch

• Figure below shows the spatial relationship of the gas source, the
focused ion beam, the sample surface, and the volatilized and sputtered
species

• Schematic drawing shows the deposition/controlled material removal

principle. The enhanced etch process is shown. If adsorbed gas
decomposes to non-volatile products, then deposition will take place.

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 FIB Gases for Deposition and Enhanced
Etch

• Metals, such as W or Pt, are deposited by ion beam assisted chemical

vapour deposition (CVD) of a precursor organometallic gas

• The ion beam assisted CVD process consists of a fine balance between
sputtering and deposition. If the primary beam current density is too high
for the deposition region, milling will occur

• Chemically enhanced sputtering is facilitated by the introduction of select

species into the FIB chamber. For example, halogen-based species may
enhance sputtering rates for specific substrate materials in the presence
of the Ga+ ion beam.

• Water has been shown to provide enhanced etching for carbonaceous

materials

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 Device Edits and Modifications

• One application that stands out is the ability of the FIB system to carry
out device/circuit modifications on prototype chips

• Gallium beam interaction with the substrate is inherently destructive. The

damage inflicted is essentially twofold:
– Impact damage due to heavier mass of the Ga+ ions
– Surface charging effects

• Modifications carried out on prototype chips include:

– Making new connections using metal deposition ( W or Pt)
– Breaking connections
– Making probe points for tapping signals

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 Device Edits and Modifications

• Modifications may be to fix design errors, or carry out design edits

presented by customers

• Prototype chips can be worked on iteratively until the right result is

achieved

• Implementation procedure
– Sample grounding
– Imaging
– On-Chip navigation
– Milling vias
– Filling vias
– Making connections and disconnecting lines
– Cleanup

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 Device Edits and Modifications

• Sample Grounding
– Being grounded is vital to the health of the chip, as the beam striking
the surface has a positive charge which has to be dissipated as it is
being worked on

• Imaging
– The use of low beam current (30-50 pA)
– Apply a local platinum or global carbon coat

• On-Chip Navigation
– Dead reckoning; Visual references to reach the target location
– 3-point alignment; Stage of the FIB system is realigned using the co-
ordinates from the chip obtained from the chip database
– CAD Navigation; Database information for the layout of the chip

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 Device Edits and Modifications

• Milling vias
– Vias are typically milled using the same beam current used to image
the sample (30-50 pA). Vias for top-level metal connections are
usually a couple of microns on the side.
– On lower level metals, via size needs to increase because of the
higher aspect ratio and to avoid metal to bridge on top of the via
– Larger contact areas ensure lower contact resistance
– The enhanced etch gas used to assist the milling of oxides
enhances the milling rate about 7-9 times. Etch gas also essentially
convert the sputtered material into a volatile compound and
minimizes redeposition

• Filling vias
– Vias are filled by depositing a Pt or W plug
– The deposition box should be smaller than the mill box to make sure
that the deposited metal makes a contact to the layer below and
does not bridge across the top of the via and cause “voiding”
– Deposition time should not be too short or too long (~ 2.5 minutes)

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 Device Edits and Modifications

• Making connections and disconnecting lines

– Typical connections run about 5-100 um long, 0.5-2 um wide and
about 0.5-1 um thick
– In order to avoid refilling of cuts with redeposition, lines are cut after
all depositions are complete
– Typical beam currents for exposing the lines to be cut are similar to
ones used for exposing lines (30-50 pA). There is a risk of exposing
the underlying metal levels, when using a higher beam current.
– The use of enhancing etch gases produce cleaner cuts

• Clean-up
– Clean up is typically required if there are several modifications in
close proximity to each other and only if the metal deposition over
sprays overlap
– Milling around the deposition paths using individual mill boxes
– Imaging surface while the enhanced etch flow of gas is on
– One needs to be extremely careful so as not to mill too much into
the top surface

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 Device Edits and Modifications

Deposited W lines
Milling and filling a via

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 Device Edits and Modifications
Cleaned overspray

Line cuts Milling andWfilling

Deposited line via

Milling and filling via

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 FIB In-Situ Lift-Out TEM Specimen
Technique

• The objective of the FIB In-Situ Lift-Out (INLO) method is to

produce a high quality electron transparent membrane to be
imaged in the TEM

• A primary advantage is that specimens may be prepared from

the starting bulk sample with little or no initial specimen
preparation

• If an insulating material is to be FIB milled, a conductive

coating may be applied to the sample to prevent charging

• INLO technique requires a vacuum compatible probe assembly

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 FIB In-Situ Lift-Out TEM Specimen
Technique

• TEM Specimen preparation begins by using the ion beam (or

ebeam) CVD process to deposit a 0.5-1 um thick metal line

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 FIB In-Situ Lift-Out TEM Specimen
Technique

• Next, high beam currents are used to mill large amounts of

material away from the front and back of the region of interest.
Then the bottom and the right edge are cut free leaving just a
tab of material on the left side holding the specimen

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 FIB In-Situ Lift-Out TEM Specimen
Technique

• The manipulator probe is positioned to touch a FIB milled piece

of sample. The FIB is then used to attach the probe to the
sample using the FIB CVD capabilities

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 FIB In-Situ Lift-Out TEM Specimen
Technique

• Then the sample is lifted out of the bulk material…

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 FIB In-Situ Lift-Out TEM Specimen
Technique

• …and the probe/sample assembly is then positioned onto a

TEM slotted grid

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 FIB In-Situ Lift-Out TEM Specimen
Technique

• The CVD operation is used to attach the sample to the grid.

Once the sample is secured to the grid, the probe is FIB milled
free from the sample
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 FIB In-Situ Lift-Out TEM Specimen
Technique

• The sample is then FIB milled to electron transparency

thickness (<100 nm) and finely polished using conventional FIB
milling practices.
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 FIB In-Situ Lift-Out TEM Specimen
Technique

• Artefacts

• The high energy ion bombardment in the specimen can accumulate into
several thousand volts of charge which can lead into large craters and
local melting due to electrostatic discharge

• Since the rate of specimen material removal by the FIB is sensitive to

the hardness, atomic number, and topology of the surface, ridges and
grooves are cut into the surface of the specimen causing a so called
“waterfall” effect when the beam encounters soft or low atomic number
specimen surfaces

• The creation of amorphous layers are probably the greatest problem

confronting TEM examination of thin TEM specimens

• Implanted ions in the specimen cause gallium contamination. Likewise

some of material sputtered off the specimen by the ion beam in one
portion of the specimen may land on another part of the specimen
creating sputter-contamination artefacts

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 Patterning and Deposition Examples

Core structure for nano-aperture

device

• FIB-milled circular corrugation pattern

on quartz: Groove depth 100 nm, width
300 nm and, spacing 300 nm

• Focused electron beam deposited

nano-post using tetraethyl orthosilicate
(TEOS) (SiO4C8H20) as precursor gas

• TEOS decomposes into a solid

transparent dielectric material under
electron irradiation

• Diameter ~ 100 nm

• Height several μm

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 Patterning and Deposition Examples

• Focused electron beam deposited corkscrew

• Tetraethyl orthosilicate (TEOS) (SiO4C8H20) as

precursor gas

• TEOS decomposes into a solid transparent

dielectric material under electron irradiation

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 Patterning and Deposition Examples

a) b)

FESEM micrographs of the FIB-milled master moulds on Au-coated SiO2 substrate for nano
imprint lithography (NIL). a) Binary grating: period 1050 nm, depth 400 nm, b) Blazed grating:
period 1063 nm, depth (at the end) 1000 nm.
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 Patterning and Deposition Examples

a) b)

FESEM micrographs of the FIB-milled bitmap patterns on Au-coated SiO2 substrate to

demonstrate the capability of the complex patterning in FIB system.

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 Questions? Anyone?

Nanoscale Patterning and Deposition

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