05 Han Wei FIB Tech ThermoFisher
Fabrication of High Quality S/TEM sample with
Focused Ion Beam
Proprietary & Confidential
The world leader in serving science
Rich Technology Heritage – A History Of FIRSTS
1949 Philips introduces it first production TEM system
1966 Solid-State 5 Angstrom TEM delivered
1971 FEI Company founded
1977 High-Resolution SEM introduced
1986 Computerized CM TEM Series introduced
1989 World’s First Variable Pressure SEM introduced
1993 World’s First DualBeam™ (FIB/SEM) by FEI
1998 All-in-One Integrated Tecnai™ TEM
2000 World’s first small stage DualBeam
2003 World’s first Semiconductor FAB DualBeam
2004 FEI TEM breaks the 1 Angstrom barrier
2005 FEI’s all-new Titan™ S/TEM introduced with sub-Angstrom resolution
2006 First DOE TEAM project instruments shipped for 0.5 Angstrom resolution
2008 World’s First Extreme High Resolution SEM
2009 World’s Fastest Analytical S/TEM - Tecnai Osiris
2011 World’s First Integrated Light-Electron Microscope
2
Proprietary & Confidential
Helios NanoLab
450HP & F1
20 years of DualBeam
Helios NanoLab
600
Strata DB-STEM 237
DualBeam 620
DualBeam 830
Helios NanoLab
450, 650 & 600i
Strata DB 235
Strata
400/400 STEM
Versa3D
1993
1994
1995
1996
1997
1998
1999
2000
2001
2002
2003
2004
2005
2006
2007
2008
2009
2010
2011
2012
2013
Helios NanoLab
660
DualBeam 820
Altura 835
Nova NanoLab
Q3DFEG
Helios NanoLab
1200
Expida 1265
Q3D200i
Scios
What is a DualBeam?
4
Principle of a DualBeam – Helios NanoLab
FIB
Tomahawk
52º
Ga LMIS
Proprietary
4mm
Beams
Coincidence
Point
SEM
FIB
Electrons
Ions
Ions
SPI
Live imaging while milling
5
Proprietary & Confidential
SEM – Elstar
Column and
integration
identical to
the Magellan,
even the final
objective lens
DualBeam
Dualbeam has an ion column to image, mill and deposit
IMAGING
Ion channeling shows stronger contrast
on a platinum aperture than is seen
with electron beam imaging
6
Proprietary & Confidential
MILLING
Milling removed the surface to expose
the interior of lead-tin solder with
integrated flux cores
DEPOSITION
Platinum protective layer deposited
easily on both conductive and nonconductive materials
Important DualBeam Applications
• SEM imaging & analysis
• FIB imaging
• Site-specific cross section preparation
• Serial sectioning imaging/analysis=“3D” applications
• TEM sample preparation
• NanoPrototyping
• Device Edit (DE)=Circuit Edit (CE)=Microsurgery
=Chip Repair
Confi
dentia
l–
7
Proprietary & Confidential
Nano
Port
Benefits of a DualBeam FIB/SEM for TEM
Sample preparation
➢ Fast - prepare most samples in under 1 hour
➢ Site-specific – end-point accurately on sub 30nm features
➢ Orientation independent – choose the milling angle to
match the required orientation of the lamella
➢ Possible to prepare multiple lamella from 1 bulk sample at
multiple locations
➢ Sample independent – soft and hard materials are easily
handled, as well as powders, large bulk samples etc.
➢ Easily study interfaces of materials with different milling
rates.
8
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 1: Surface protection - Deposit a conductive layer (GIS)
Ellapsed
Time:
0:16:00
9
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 2a: Lamella pre-preparation - trenching
Ellapsed
Time:
0:21:00
10
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 2b: Lamella pre-preparation - undercut
Ellapsed
Time:
0:25:00
11
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 3a: In Situ Lift Out – lamella welding
Ellapsed
Time:
0:30:00
12
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 3b: In Situ Lift Out – lamella cut free from bulk
Ellapsed
Time:
0:33:00
13
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 3c: In Situ Lift Out – lamella extraction
Ellapsed
Time:
0:35:00
14
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 3d: In Situ Lift Out – lamella precise orientation (rotation)
Ellapsed
Time:
0:37:00
15
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 3d: In Situ Lift Out – Welding on TEM grid and cut free
Ellapsed
Time:
0:51:00
16
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 4: Final lamella thinning – 30 kV FIB polishing
Ellapsed
Time:
1:06:00
17
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 4: Final lamella thinning – 5 kV FIB polishing
Ellapsed
Time:
1:14:00
18
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 4: Final lamella thinning – 2 kV FIB polishing
Ellapsed
Time:
1:22:00
19
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 4: Final lamella thinning – 1kV FIB polishing
Ellapsed
Time:
1:30:00
20
Proprietary & Confidential
Controllably preparing ultra-thin samples
With FEI’s fully integrated in situ lift-out (INLO) solution
FEI EasyLiftTM
21
• Integrated & intuitive controls
• Precise and repeatable motion
• Stable & reliable operation
• Hitachi’s INLO IP licensing provided
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 5: In Situ STEM inspection: BF, DF, HAADF
22
Proprietary & Confidential
Sample Preparation
Enabling technologies
23
Proprietary & Confidential
Fast, reliable S/TEM Sample Preparation
Make the highest quality sample surfaces with low voltage cleaning
Amorphous layer measurements on samples prepared at 5kV, 2kV, and 500V
30kV CCS + 5kV Box
24
30kV CCS + 5kV + 2kV Box
Titan HRTEM ~ 500V Cleaned Surface
Sample Preparation for HR-STEM: GaN
1
STEM Resolution
Measured with the TEAM
0.5 Column
2
63pm
63pm
Z contrast image (raw data)
3
4
0.49A
5
Z contrast image (filtered)
0.58A
0.53A
0.63A
Preparation method:
• In-situ lift-out in Helios NanoLab
GaN power spectrum
• final polishing performed using 1kV FIB
transfers till 49pm
• Total preparation time: 1 hour including lift out
25
25
FEI Copyright © 2011
26
Consistently preparing high quality samples
With FEI’s EasyLift™ - fully integrated in-situ lift-out (INLO) solution
FEI EasyLiftTM
• Integrated & intuitive controls
• Stable & reliable operation
• Precise and repeatable
motion
38°
Tilt
Tilt52°
0°
STEM
INLO
Polish
Dedicated holders
• UMB to flexibly configure the holder configuration
• Pre-tilted holder to allow for sample prep + FIB
polishing + STEM without breaking the vacuum
26
Proprietary & Confidential
Pre-tilted
Holder
for INLO + FIB
polishing +
STEM
UMB
27
Consistently preparing high quality samples
Precisely monitoring the process & endpointing
Fast Monitoring
27
Real time SEM imaging
during FIB milling (SPI)
Highest resolution, precise
monitoring
Automated, rapid switching between
FIB and SEM (iSPI)
Info: iSE+eSE/BSE, 52° tilt
Info: pure eSE/BSE, 52°tilt
Proprietary & Confidential
Endpointing with strong
materials contrast & surface
sensitivity
live (synchronized) FIB imaging
while FIB milling (iRTM)
Info: iSE, top-down
AutoTEM 4
Guided S/TEM Sample Preparation
28
AutoTEM 4 Software – Intuitive User Interface
Site list
Template selection
Position in bulk
TEM grid position
Run/Stop
29
AutoTEM 4 Software – Automation Modes
• Automatic
• Automatic with manual recovery
• Guided
30
• Automatic
• Guided
• Automatic with manual recovery
• Guided
AutoTEM 4 Software – Expert results from novice users
Robust, predictable results for a wide range of materials
Bi2212
LED
display
Aluminium alloy
Catalytic activated
Filter
SrTiO
3
31
Polystyrene
Continued innovation with 3 new DualBeam launches in 2017
Scios 2
32
32
Proprietary & Confidential
Helios G4
Helios PFIB G4
SCIOS
Scios
• Highest contrast and fast imaging with the
unique Trinity detection scheme.
• Fastest and most reliable integrated S/TEM
sample preparation with Sidewinder™ HT
and Easylift™
• Instant productivity for inexperienced
operators with unique User Guidance for
common DualBeam activities.
• Highest throughput 3D characterization
34
Helios NanoLab G4
Pushing the limits of extreme high resolution, sample preparation
and prototyping
• Highest resolution with most precise
contrast
• Accurately create varied nanoscale
functional prototype devices
• Prepare the highest quality ultra-thin
samples for HR S/TEM or atom probe
• Access high resolution, multiscale and
3D information
35
Helios G4 PFIB DualBeam
• Access high resolution, large volume, multi-scale
and multi-modal subsurface and 3D information
• Fast and easy preparation of high quality Ga+ free
TEM and APT samples
• Unique guided TEM sample preparation workflow
• Extreme high resolution imaging with the most
precise contrast
• Fast precise micromachining of complex structures
for prototyping and in situ mechanical testing
36
WISAT 2009 – TIFR Mumbai
From State-of-the-Art to Advanced TEM Sample Prep. using DualBeams
Dualbeams offer a fast and flexible alternative
for TEM sample preparation:
• Large range of samples can be prepared
• Site specific with high resolution SEM/FIB imaging
• Monitor the preparation process in real time
• Fast
• Automation for increased speed
• Reliable
• Able to produce HR-(S)TEM quality samples
• Easy to use
37
Thank You!
FEI Copyright © 2009
Focused Ion Beam
Proprietary & Confidential
The world leader in serving science
Rich Technology Heritage – A History Of FIRSTS
1949 Philips introduces it first production TEM system
1966 Solid-State 5 Angstrom TEM delivered
1971 FEI Company founded
1977 High-Resolution SEM introduced
1986 Computerized CM TEM Series introduced
1989 World’s First Variable Pressure SEM introduced
1993 World’s First DualBeam™ (FIB/SEM) by FEI
1998 All-in-One Integrated Tecnai™ TEM
2000 World’s first small stage DualBeam
2003 World’s first Semiconductor FAB DualBeam
2004 FEI TEM breaks the 1 Angstrom barrier
2005 FEI’s all-new Titan™ S/TEM introduced with sub-Angstrom resolution
2006 First DOE TEAM project instruments shipped for 0.5 Angstrom resolution
2008 World’s First Extreme High Resolution SEM
2009 World’s Fastest Analytical S/TEM - Tecnai Osiris
2011 World’s First Integrated Light-Electron Microscope
2
Proprietary & Confidential
Helios NanoLab
450HP & F1
20 years of DualBeam
Helios NanoLab
600
Strata DB-STEM 237
DualBeam 620
DualBeam 830
Helios NanoLab
450, 650 & 600i
Strata DB 235
Strata
400/400 STEM
Versa3D
1993
1994
1995
1996
1997
1998
1999
2000
2001
2002
2003
2004
2005
2006
2007
2008
2009
2010
2011
2012
2013
Helios NanoLab
660
DualBeam 820
Altura 835
Nova NanoLab
Q3DFEG
Helios NanoLab
1200
Expida 1265
Q3D200i
Scios
What is a DualBeam?
4
Principle of a DualBeam – Helios NanoLab
FIB
Tomahawk
52º
Ga LMIS
Proprietary
4mm
Beams
Coincidence
Point
SEM
FIB
Electrons
Ions
Ions
SPI
Live imaging while milling
5
Proprietary & Confidential
SEM – Elstar
Column and
integration
identical to
the Magellan,
even the final
objective lens
DualBeam
Dualbeam has an ion column to image, mill and deposit
IMAGING
Ion channeling shows stronger contrast
on a platinum aperture than is seen
with electron beam imaging
6
Proprietary & Confidential
MILLING
Milling removed the surface to expose
the interior of lead-tin solder with
integrated flux cores
DEPOSITION
Platinum protective layer deposited
easily on both conductive and nonconductive materials
Important DualBeam Applications
• SEM imaging & analysis
• FIB imaging
• Site-specific cross section preparation
• Serial sectioning imaging/analysis=“3D” applications
• TEM sample preparation
• NanoPrototyping
• Device Edit (DE)=Circuit Edit (CE)=Microsurgery
=Chip Repair
Confi
dentia
l–
7
Proprietary & Confidential
Nano
Port
Benefits of a DualBeam FIB/SEM for TEM
Sample preparation
➢ Fast - prepare most samples in under 1 hour
➢ Site-specific – end-point accurately on sub 30nm features
➢ Orientation independent – choose the milling angle to
match the required orientation of the lamella
➢ Possible to prepare multiple lamella from 1 bulk sample at
multiple locations
➢ Sample independent – soft and hard materials are easily
handled, as well as powders, large bulk samples etc.
➢ Easily study interfaces of materials with different milling
rates.
8
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 1: Surface protection - Deposit a conductive layer (GIS)
Ellapsed
Time:
0:16:00
9
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 2a: Lamella pre-preparation - trenching
Ellapsed
Time:
0:21:00
10
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 2b: Lamella pre-preparation - undercut
Ellapsed
Time:
0:25:00
11
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 3a: In Situ Lift Out – lamella welding
Ellapsed
Time:
0:30:00
12
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 3b: In Situ Lift Out – lamella cut free from bulk
Ellapsed
Time:
0:33:00
13
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 3c: In Situ Lift Out – lamella extraction
Ellapsed
Time:
0:35:00
14
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 3d: In Situ Lift Out – lamella precise orientation (rotation)
Ellapsed
Time:
0:37:00
15
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 3d: In Situ Lift Out – Welding on TEM grid and cut free
Ellapsed
Time:
0:51:00
16
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 4: Final lamella thinning – 30 kV FIB polishing
Ellapsed
Time:
1:06:00
17
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 4: Final lamella thinning – 5 kV FIB polishing
Ellapsed
Time:
1:14:00
18
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 4: Final lamella thinning – 2 kV FIB polishing
Ellapsed
Time:
1:22:00
19
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 4: Final lamella thinning – 1kV FIB polishing
Ellapsed
Time:
1:30:00
20
Proprietary & Confidential
Controllably preparing ultra-thin samples
With FEI’s fully integrated in situ lift-out (INLO) solution
FEI EasyLiftTM
21
• Integrated & intuitive controls
• Precise and repeatable motion
• Stable & reliable operation
• Hitachi’s INLO IP licensing provided
Proprietary & Confidential
Preparing highest quality thin samples
Example: preparation of an ultra-thin GaN sample
Step 5: In Situ STEM inspection: BF, DF, HAADF
22
Proprietary & Confidential
Sample Preparation
Enabling technologies
23
Proprietary & Confidential
Fast, reliable S/TEM Sample Preparation
Make the highest quality sample surfaces with low voltage cleaning
Amorphous layer measurements on samples prepared at 5kV, 2kV, and 500V
30kV CCS + 5kV Box
24
30kV CCS + 5kV + 2kV Box
Titan HRTEM ~ 500V Cleaned Surface
Sample Preparation for HR-STEM: GaN
1
STEM Resolution
Measured with the TEAM
0.5 Column
2
63pm
63pm
Z contrast image (raw data)
3
4
0.49A
5
Z contrast image (filtered)
0.58A
0.53A
0.63A
Preparation method:
• In-situ lift-out in Helios NanoLab
GaN power spectrum
• final polishing performed using 1kV FIB
transfers till 49pm
• Total preparation time: 1 hour including lift out
25
25
FEI Copyright © 2011
26
Consistently preparing high quality samples
With FEI’s EasyLift™ - fully integrated in-situ lift-out (INLO) solution
FEI EasyLiftTM
• Integrated & intuitive controls
• Stable & reliable operation
• Precise and repeatable
motion
38°
Tilt
Tilt52°
0°
STEM
INLO
Polish
Dedicated holders
• UMB to flexibly configure the holder configuration
• Pre-tilted holder to allow for sample prep + FIB
polishing + STEM without breaking the vacuum
26
Proprietary & Confidential
Pre-tilted
Holder
for INLO + FIB
polishing +
STEM
UMB
27
Consistently preparing high quality samples
Precisely monitoring the process & endpointing
Fast Monitoring
27
Real time SEM imaging
during FIB milling (SPI)
Highest resolution, precise
monitoring
Automated, rapid switching between
FIB and SEM (iSPI)
Info: iSE+eSE/BSE, 52° tilt
Info: pure eSE/BSE, 52°tilt
Proprietary & Confidential
Endpointing with strong
materials contrast & surface
sensitivity
live (synchronized) FIB imaging
while FIB milling (iRTM)
Info: iSE, top-down
AutoTEM 4
Guided S/TEM Sample Preparation
28
AutoTEM 4 Software – Intuitive User Interface
Site list
Template selection
Position in bulk
TEM grid position
Run/Stop
29
AutoTEM 4 Software – Automation Modes
• Automatic
• Automatic with manual recovery
• Guided
30
• Automatic
• Guided
• Automatic with manual recovery
• Guided
AutoTEM 4 Software – Expert results from novice users
Robust, predictable results for a wide range of materials
Bi2212
LED
display
Aluminium alloy
Catalytic activated
Filter
SrTiO
3
31
Polystyrene
Continued innovation with 3 new DualBeam launches in 2017
Scios 2
32
32
Proprietary & Confidential
Helios G4
Helios PFIB G4
SCIOS
Scios
• Highest contrast and fast imaging with the
unique Trinity detection scheme.
• Fastest and most reliable integrated S/TEM
sample preparation with Sidewinder™ HT
and Easylift™
• Instant productivity for inexperienced
operators with unique User Guidance for
common DualBeam activities.
• Highest throughput 3D characterization
34
Helios NanoLab G4
Pushing the limits of extreme high resolution, sample preparation
and prototyping
• Highest resolution with most precise
contrast
• Accurately create varied nanoscale
functional prototype devices
• Prepare the highest quality ultra-thin
samples for HR S/TEM or atom probe
• Access high resolution, multiscale and
3D information
35
Helios G4 PFIB DualBeam
• Access high resolution, large volume, multi-scale
and multi-modal subsurface and 3D information
• Fast and easy preparation of high quality Ga+ free
TEM and APT samples
• Unique guided TEM sample preparation workflow
• Extreme high resolution imaging with the most
precise contrast
• Fast precise micromachining of complex structures
for prototyping and in situ mechanical testing
36
WISAT 2009 – TIFR Mumbai
From State-of-the-Art to Advanced TEM Sample Prep. using DualBeams
Dualbeams offer a fast and flexible alternative
for TEM sample preparation:
• Large range of samples can be prepared
• Site specific with high resolution SEM/FIB imaging
• Monitor the preparation process in real time
• Fast
• Automation for increased speed
• Reliable
• Able to produce HR-(S)TEM quality samples
• Easy to use
37
Thank You!
FEI Copyright © 2009