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Transmission Electron Microscopy (TEM)
In a typical TEM a static beam of electrons at 100-200kV accelerating
voltage illuminate a region of an electron transparent specimen which is
immersed in the objective lens of the microscope.
The transmitted and diffracted electrons are recombined by the objective
lens to form a diffraction pattern in the back focal plane of that lens and a
magnified image of the sample in its image plane. A number of intermediate
lenses are used to project either the image or the diffraction pattern onto a
fluorescent screen for observation.
The uniqueness of TEM is the ability to obtain full morphological (grain
size, grain boundary and interface, secondary phase and distribution,
defects and their nature, etc.), crystallographic, atomic structural and
microanalytical information such as chemical composition (at nmscale),
bonding (distance and angle), electronic structure, coordination number
datafromthesample.
A simple analog
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An alternative comparison
JEOL 2010F
Electron gun
Probe forming lenses - Cond.
Specimen holder
Magnifying lenses - Int. & Proj.
Objective Lens
HAADF Detector
(high angle annular dark-field)
Viewing Chamber
Camera Chamber
STEM Detector &/or EELS
XEDS Detector
Basic features of
an analytical
electron
microscope
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FEI Titan
Vacuum
The electron microscope is essentially a series of connected
vessels separated by valves.
The vacuum near the specimen is around 10
-7
Torr. The
vacuum in the gun depends on the type of gun, either around
10
-7
Torr (tungsten or LaB
6
) or 10
-9
Torr (for a Field Emission
Gun).
The pressure in the projection chamber was usually the worst.
The projection chamber holds the negatives used to record
images. These negatives can outgas, limiting the ultimate
vacuum. [digital recording eliminates this!]
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The Lenses in TEM
Condenser lenses(two)-control how
strongly beam is focused (condensed)
onto specimen. At low Mag. spread
beam to illuminate a large area, at high
Mag. strongly condense beam.
Objective lens-focus image (image
formation) and contribute most to
the magnification and resolution of the image.
Four lenses form magnification
system-determine the magnification
of the microscope. Whenever the
magnification is changed, the currents
through these lenses change.
Image Formation in TEM
Ray Diagram for a TEM
Control contrast
Control brightness,
convergence
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Why Electrons?
Improved Resolution!
In the expression for the resolution
(Rayleighs Criterion)
r = 0.61/nsino
-wavelength,
V-accelerating voltage, n-refractive index
o-aperture of objective lens, very small in TEM
sino o so r=0.61/o o~0.1 radians (5.5
o
)
Green Light 200kV Electrons
~400nm ~0.0025nm
n~1.7 oil immersion n~1 (vacuum)
r~150nm (0.15m) r~0.02nm (0.2)
1/10
th
size of an atom!
unrealistic!
Resolution Limited by
Lens Aberrations
point is imaged
as a disk.
Spherical aberration is caused by the
lens field acting inhomogeneously on
the off-axis rays.
point is imaged
Chromatic aberration is caused by the
variation of the electron energy (PS
voltage) so electrons are not
monochromatic.
r
min
~0.91(C
s

3
)
1/4
Practical resolution of microscope. C
s

coefficient of spherical aberration of lens

(~mm)
as a disk.
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Specimen Holder
a split polepiece
objective lens
holder
beam
Heating and straining
Twin specimen holder
Double tilt heating
Rotation, tilting, heating, cooling and straining
Specimen Holder with Electrical Feedthroughs
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Beam and Specimen Interaction
(EDS)
(EELS)
SAED & CBED
diffraction
BF
DF
HREM
Imaging
Scanning Transmission Electron Microscopy (STEM)
In STEM, the electron beam
is rastered (scan coil) across
the surface of a sample in a
similar manner to SEM,
however, the sample is a thin
TEM section and the
diffraction contrast image is
collected on a solid-state
detector.
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Imaging in the TEM
Two principal kinds:
Diffraction contrast imaging.(bright field / dark field)
Use either a non-diffracted or diffracted beam and
remove all other beams from the image by the use of an
objective aperture.
Phase contrast or high resolution imaging.(HREM)
Use all of the diffracted and non-diffracted beams (by
using a large objective aperture or none at all) and add
them back together (phase and intensity) to form a
phase contrast image
Silicon <100> zone axis
pattern.
Selected Area Diffraction
Parallel Electron Beam
Sample
Diffraction Plane
Selected Area Diffraction
Parallel Illumination.
Lens Aberration limits
resolution to ~1 m.
Objective Lens
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BF & DF Imaging Diffraction Contrast
Objective
aperture
C-film
amorphous
crystal
D
T
BF image
C-film
crystal
D
T
C-film
crystal
DF image
Diffraction + mass/thickness= Contrast
Objective
aperture
DDF CDF
Beam
tilt
T-transmitted
D-diffracted
Hole in OA
OA OA
DDF displacive DF; CDF centered DF
Bright Field (BF) and Dark Field (DF) Imaging
Incident beam
specimen
transmitted beam
diffracted beam
objective aperture
hole in objective
aperture(10-100m)
BF imaging-only transmitted beam is allowed
to pass objective aperture to form images.
BF
DF
DF
DF imaging
only diffracted
beams are
allowed to pass
the aperture to
form images.
Particles in Al-Cu
Alloy.
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Phase Contrast Imaging
High Resolution Electron Microscopy
(HREM)
Use a large objective
Aperture (get both beams).
Phases and intensities of
diffracted and transmitted
beams are combined to
form a phase contrast
image.
T
D
Si
Objective
aperture
Electron diffraction pattern recorded
From both BN film on Si substrate.
BN
Electron Diffraction
Specimen
foil
T D
u e
-
L 2u
r
d
hkl
[hkl] SAED pattern
L -camera length
r -distance between T and D spots
1/d -reciprocal of interplanar distance(
-1
)
SAED selected area electron diffraction
Geometry for
e-diffraction
Braggs Law: = 2dsinu
=0.037 (at 100kV)
u=0.26
o
if d=4
= 2du
r/L=sin2u
as u 0
r/L = 2u
r/L = /d or
r = Lx
1
d
hkl
Reciprocal
lattice
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Why are there so many spots?
Reciprocal lattice
k wave vector
lkl = 1/
wavelength of electron
SAED Patterns of Single Crystal,
Polycrystalline and Amorphous Samples
a b c
a. Single crystal Fe (BCC) thin film-[001]
b. Polycrystalline thin film of Pd
2
Si
c. Amorphous thin film of Pd
2
Si. The diffuse
halo is indicative of scattering from an
amorphous material.
r
1
r
2
200
020
110
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Diffraction Spot Intensity
Spot intensity: I
hkl
o lF
hkl
l
2
F
hkl
- Structure Factor
F
hkl
= E f
n
exp[2ti(hu+kv+lw)]
N
n=1
f
n
atomic scattering factor
f
n
o Z, sinu/
h,k,l are Miller indices and u,v,w fractional coordinates
Specimen Preparation-Destructive
Dispersing crystals or powders on a carbon film on a grid
3mm
Mechanical Thinning
Grind, Lap
Machine & Slice
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Cross-Sections
Substrate
Four pieces of a specimen
formed from thin film(s) on a
substrate.
Thin Film
The four pieces are
glued together ( face-to-face ,
and face-to-back ) to form
a cross section.
Glue
Cross-Sections...
A 2.8mm diameter piece
is drilled from the
cross section.
The 2.8mm diameter rod
is placed within a 3mm
external diameter metal tube.
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Cross-Sections...
Thin slices are cut from the rod,
and mechanically thinned to
~100

m.
~100 m
3.0mm
Mechanical Thinning
Planar Thinning Dimple Grinding
Holder Holder
Dimple
Wheel
Holder
Beveled Plate
Specimen
Thin
Region Planar Thinning
Disc
Specimen
V
Pumped
ElectrolyteJ et
Pumped
ElectrolyteJ et
Electro-Chemical Thinning
Ion Gun
Ion Gun
Specimen
Ion Milling
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Focused Ion Beam (FIB) Milling
FIB
beam
Sample
epoxied
togrid
Grid
Samplemilled
byFIBbeam
TEM
beam
Focused Ion Beam (FIB) System
focus a Ga ion beam to a few tens of nanometers to mill the
specimen
interaction of Ga ion beamwith the specimen also generates
secondary electrons that can beused for SEM imaging. So we
can observetheareaunder milling during themilling process.
FIB permitsselected area milling.
high specimen milling rates as well as high positional accuracy
for milling of the area(s) of interest.
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FIB procedure
a. Select an area of interest,
Coat with a layer of metal (Pt)
b. Make trench using
high current ion beam
c. Thinning the wall
d. Cut the wall and remove
http://www.labcompare.com/623-Videos/139165-AURIGA-Laser-FIB-SEM-Microscope-
from-ZEISS/
Applications of TEM
TEM
Conventional TEM
Microstructure, morphology (grain size, orientation),
phase distribution and defect analysis (point defects,
dislocations and grain boundaries)
In situ TEM
Irradiation and deformation experiments
Environmental cells (corrosion)
Phase transformations
(hot- and cold-stage, electric field)
Analytical TEM (Z-contrast imaging)
Chemical composition-EDS, EELS, ELNES,
EXELFS, Z-contrast imaging
CBED-lattice strain, thickness, charge density
HRTEM
Lattice imaging, structure of complex materials
and atomic structure of defects (interfaces)
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Sub-Nanometric EDS Analysis
(JEOL-2010F Field-emission TEM)
MBE-grown InGaAsP/InP
Multi-quantum well structure
EDS spectra taken with a 5
Probe. A.1nm InGaAsP layer
B.~3nm away from interface
Within InP matrix.
-
-
A
B
A
B
InGaAsP
InP
HREM
In-situ nano-indentation
See movie
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Limitations of TEM
Sampling
Interpretation of image
Beam damage
Specimen preparation