1. Materials Characterization Lab
www.mri.psu.edu/mcl
Transmission Electron Microscopy (TEM)
& Scanning Transmission
Electron Microscopy (STEM)
Joe Kulik
194 MRI Building
juk12@psu.edu/814-865-0344
15 June 2005
2. Materials Characterization Lab
www.mri.psu.edu/mcl
Summer Characterization Open Houses
Technique Time Date Location
Thermal analysis (TGA, DTA, DSC) 9:45 AM June 8 250 MRL Bldg.
Transmission Electron Microscopy (TEM/STEM) 9:45 AM June 15 114 MRI Bldg
Scanning electron microscopy (SEM) 9:45 AM June 22 541 Deike Bldg.
Analytical SEM 11:00 AM June 22 541 Deike Bldg.
X-ray Diffraction (XRD) 9:45 AM June 29 250 MRL Bldg.
Dielectric Characterization (25 min lecture only) 9:45 AM July 6 250 MRL bldg.
High temperature sintering lab (20 min lecture only) 10:15 AM July 6 250 MRL Bldg.
Focused Ion Beam (FIB) 9:45 AM July 13 114 MRI Bldg
TEM sample preparation 11:00 AM July 13 114 MRI Bldg
Orientation imaging microscopy (OIM/EBSD) 9:45 AM July 20 250 MRL Bldg.
Chemical analysis (ICP, ICP-MS) 9:45 AM July 27 541 Deike Bldg.
Atomic Force Microscopy (AFM) 9:45 AM August 3 114 MRI Bldg
Small angle x-ray scattering (SAXS) 9:45 AM August 10 541 Deike Bldg.
Particle Characterization 9:45 AM August 17 250 MRL
X-ray photoelectron spectroscopy (XPS/ESCA) 9:45 AM August 24 114 MRI Bldg
Auger Electron Spectroscopy (AES) 11:00 AM August 24 114 MRI Bldg
NOTE LOCATIONS: The MRI Bldg is in the Innovation Park near the Penn Stater Hotel; MRL Bldg. is on Hastings Road.
More information: www.mri.psu.edu/mcl
3. Materials Characterization Lab
www.mri.psu.edu/mcl
Materials Characterization Lab Locations
Bldg Telephone
MRL 863-7844
MRI 865-0337 MRI Bldg:
Hosler 865-1981 XPS/ESCA, SIMS,
E&ES 863-4225
TEM, HR-TEM, FE-
Auger, AFM, XRD
MRL Bldg:
Hosler Bldg:
SEM, XRD, OIM, DTA,
SEM, ESEM, FE-
DSC, TGA, FTIR, Penn Stater
SEM, EPMA, ICP,
Hotel
Raman, AFM, Powder,
E&ES Bldg: ICP-MS,BET, SAXS
dielectric, prep, shop,
SEM
IC, UV-Vis
Route 322
Steidle Bldg:
Atherton Street
Nanoindenter
(322 Business)
I-99
Park Ave.
0
0 0
0 0 0 0
Ave. 0
0 0 0 0
Park 0
Beaver
0
0
Stadium
0
0
0
Centre
0
0
Porter Road
Community
Univ
Shortlidg
Hospital
0
0
Burrowes Road
ersi
ty D
e
Pollock Road
Road
rive
North
Hastin
Deike Bldg: gs Ro
ad
College Ave.
4. Materials Characterization Lab
www.mri.psu.edu/mcl
Outline
― Overview of TEM/STEM
―MCL capabilities
― Examples of applications from PSU investigations
― How to get started
― Campus resources
― a brief lab tour
6. (Conventional) TEM
Materials Characterization Lab
www.mri.psu.edu/mcl
Image Mode
Electron Gun Diffraction contrast
from dislocatios
Condenser 1
Condenser 2
Specimen
Objective
High resolution of
Objective
twins in InP
Aperture
nanowires
Intermediate
Lens
1st Image
Projector
Lens
2nd Image
Final Image
7. Materials Characterization Lab
www.mri.psu.edu/mcl
Diffraction
Mode
Diffraction pattern
from ordered
perovskite structure
Final
Diffraction
Pattern
8. Materials Characterization Lab
www.mri.psu.edu/mcl
Scanning TEM (STEM)
Scan
Coils
Front Focal Plane
Condenser/Objective Specimen
Field Region
Back Focal Plane (BFP)
Imaging of BFP to detector plane
Dark field Bright field
detector detector
9. Materials Characterization Lab
www.mri.psu.edu/mcl
X-ray Energy Dispersive Spectroscopy
Reversed biased p-i-n junction
n
p i
Electron-hole
pairs
Incident high-kV
electron beam
Output
Characteristic
V
X-rays
Thin
Sample
t
11. Materials Characterization Lab
www.mri.psu.edu/mcl
Electron Energy Loss Spectroscopy (EELS)
Final microscope
lens
Loss
spectrum
Electron prism
Detector
spectrometer Quadrupole
magnifiers
Expanded
spectrum
13. Materials Characterization Lab
www.mri.psu.edu/mcl
JEOL JEM-2010
LaB6 Cathode
Accelerating voltage: 200 keV
Ultra high resolution pole piece
(0.5 mm Cs)
Point-to-point resolution: 0.20 nm
Gatan TV rate camera
Specimen Holders
JEOL single tilt
Gatan double tilt
Stage tilt: +/-10°
Energy dispersive x-ray
spectroscopy (EDS)
30 mm2 detector area
140 eV resolution
Spatial resolution: <2 nm
14. Materials Characterization Lab
www.mri.psu.edu/mcl
JEOL JEM-2010F
Field emission gun
Ultra high res pole piece (0.5 mm Cs)
1.9 Å point-to-point resolution
Bright-field/dark-field STEM
CCD camera
Energy-Dispersive X-ray Spectroscopy
EDAX Detector 138 eV resolution at Mn
Ka
30 mm2 detector area
Electron Energy Loss Spectroscopy
(EELS) with 0.7 eV resolution
Specimen Holders
JEOL Single tilt low background holder
Gatan Analytical holder with Be specimen
cup
Gatan Tilt-rotation holder with Be
specimen cup
Gatan Double tilt liquid nitrogen holder
15. Materials Characterization Lab
www.mri.psu.edu/mcl
Examples from PSU Research
• BaTiO3 Dielectrics for capacitors, G.Y. Yang et al.
• Shallow Ohmic Contacts to p-InAs for Heterojunction Bipolar
Transistors, E. Lysczek, S. Wang J. Robinson, & S. Mohney
• Au-Catalyzed Growth of Ge nanowires, T. Trammell, J. Kulik, & E.
Dickey
• Niobium Oxide Characterization with EELS, M. Olszta & E.
Dickey
• GaN Film on Composition-Graded AlGaN Buffer on Si, X. Weng &
E. Dickey
• Spectral Imaging of Si Nanowires, J. Wang et al.
• Twinning Superlattice in InP Nanowires, J. Wang et al.
16. Materials Characterization Lab
www.mri.psu.edu/mcl
Microstructure of BaTiO3 Dielectric
G.Y. Yang et al.
100 nm
Conventional Perovskite
101 111
Structure:
• as-produced BME capacitors
010
• Partial BaTiO3 grains in
the degraded BME capacitors
[101]
Perovskite framework
+ modulation:
• Most BaTiO3 grains in
the degraded BME capacitors
100 nm
Co-existence of the modulated
and ordered structures
• Some BaTiO3 grains in
the degraded BME capacitors
17. Materials Characterization Lab
www.mri.psu.edu/mcl
Microstructure of BaTiO3 Dielectric
G.Y. Yang et al.
101 111 111
010
(11
1)
2 nm
2 nm
Modulated structure Long range ordered structure
High-resolution TEM images of BaTiO3
in the degraded Ni-BaTiO3 MLCCs
18. Materials Characterization Lab
www.mri.psu.edu/mcl
Microstructure of BaTiO3 Dielectric
G.Y. Yang et al.
Relative chemical shift between the dielectric grains
on different structural states indicating Ti reduction
Ti L2,3
OK
A BCD
a. PME-as-produced MLC*
BaTiO3.00
b. BME-as-produced MLC
BaTiO2.93
c. BME-degraded regular
BaTiO2.86
d. BME-degraded modulated
BaTiO2.60
e. BME-degraded ordered
BaTiO2.60
460 480 500 520 540 560
Energy-Loss (eV)
19. Materials Characterization Lab
www.mri.psu.edu/mcl
Microstructure of BaTiO3 Dielectric
G.Y. Yang et al.
(a)
7Å
111
111
2/ 2/ 2/
[0001]h // [111]p
⅔⅔⅔ 3
33
⅓⅓⅓ /3
1/ 1/ 1
O 2-
33 Ba 2+
000 Partially
000 Ti 3+ vacated O2-
Ti 4+ site
Superlattice:
7Å
Ba(Ti4+1/3Ti3+2/3)O2.67
HRTEM images, structural model, and simulated image of
long-range ordering structure of
BaTiO3 in the Degraded Ni-BaTiO3 MLCCs
20. Materials Characterization Lab
www.mri.psu.edu/mcl
Pd/W/Au (3/50/145nm)
Lysczek, Wang, Robinson, Mohney
In
Aged 250°C 9h Au
• Reaction Depth = 6 ± 2 nm
W
• Some small voids present
Pd-As, Voids
• Indium out-diffusion
InAs
• Shallow and uniform reaction
Buffer layer
22. Materials Characterization Lab
www.mri.psu.edu/mcl
Pt/W/Au (3/50/145nm)
Lysczek, Wang, Robinson, Mohney
Au
W
Pt-Au-In-As
InAs
Buffer Layer and Au
Buffer Layer
Aged 250°C 9h
• Reaction Depth = 36 ± 7nm in areas without Au penetration
• Tungsten diffusion barrier failed to keep Au out in one spot
23. Materials Characterization Lab
www.mri.psu.edu/mcl
Growth of Ge nanowires
Trammell, Kulik, Dickey
Identification of Au particles on Ge nanowires.
E-beam probe size is < 1 nm.
24. Materials Characterization Lab
www.mri.psu.edu/mcl
Niobium Oxide Characterization with EELS
M. Olszta, E. Dickey
A
51500
B
C
CCD Photodiode Counts (a.u.)
A B
Counts (arb. units)
D
Nb2O5
C E
36500
D
E
NbO2
A
21500
NbO
6500
530.00 540.54 551.08 561.62
Energy Loss (eV)
25. Materials Characterization Lab
www.mri.psu.edu/mcl
GaN Film on Si via Composition-Graded AlGaN Buffer
X. Weng, E. Dickey, J. Redwing
0002 Two-Beam Bright-Field Image
GaN
The composition-graded
AlGaN buffer layer
significantly reduces the
threading dislocation
density in the GaN film
AlGaN
200 nm
Si
26. Materials Characterization Lab
www.mri.psu.edu/mcl
Electron energy loss spectral image of a Si nanowire
J. Wang et al.
SiOx L3 map
Si L3 map
O K map
50 nm 1 2
Si+SiOx
Si+SiOx
SiOx
SiOx
Si L2,3
O K edge
100 200 300 400 500
Energy Loss (eV)
SiOx L2,3
80 100 120 140 500 550
Energy Loss (eV) Energy Loss (eV)
28. Materials Characterization Lab
www.mri.psu.edu/mcl
How to get started
• Contact me (Joe Kulik) to discuss your needs
• Attend training session
– Sessions are by appointment
– Informal
– Typically 2 trainees per session
• Provide budget and fund number!
• TEM can be time consuming for beginners
– If time is an issue, find a collaborator
– There are many users at PSU
29. Materials Characterization Lab
www.mri.psu.edu/mcl
Sample preparation
Material must be thin (< 100 nm)
High resolution requires thickness ~20 nm
Preparation methods:
– Metals can be electropolished
– Semiconductors and ceramics can be mechanically
thinned followed by ion thinning to achieve
electron transparency
– Very fine grained powders, nanowires,
nanoparticles can be dispersed on a support film
(e.g., lacey carbon)
– Focused Ion Beam thinning is also an option
• MCL has a dual-platform FIB (FIB/SEM)
30. Materials Characterization Lab
www.mri.psu.edu/mcl
TEM Fees
Instrument time:
Philips EM420T: $30/hr
JEOL JEM-2010: $35/hr
JEOL JEM-2010F: $50/hr
Staff time: $30/hr
Training fee: $300 (Includes ~16 hours of instrument time
with ~ 4 to 8 hours of personalized instruction as necessary)
Consultation time to discuss your samples, data, etc is free.
31. Materials Characterization Lab
www.mri.psu.edu/mcl
Campus resources- coursework
1. Materials Science 531, Transmission electron microscopy, 3-credits:
Overview of TEM, STEM and applications (Spring only)
2. Transmission electron microscopy, 1-credit lab course:
Simple alignment of electron optical column, basic experiments in electron
diffraction and imaging (Consult Course Schedule)
32. Materials Characterization Lab
www.mri.psu.edu/mcl
Campus resources- people
1. MCL (Joe Kulik, Jinguo Wang)
2. Elizabeth Dickey, Associate Professor of Materials Science & Engineering
3. Peter Heaney, Associate Professor of Geosciences
4. Arthur Motta, Professor of Nuclear Engineering
5. Theresa Mayer, Associate Professor of Electrical Engineering
6. Clive Randall, Professor of Materials Science & Engineering
7. Mary Beth Williams, Assistant Professor of Chemistry
8. Suzanne Mohney, Professor of Materials Science & Engineering
Other resources:
• www.mri.psu.edu/mcl/techniques/tem.asp (links, applications, etc)
• MRI links to publications and abstract (Web of Science) searching
(www.mri.psu.edu/linkspubs/)
• Microscopy Society of America (MSA) (http://www.microscopy.org/)
