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http://www.youtube.com/watch?

v=yqLlgIaz1L0 see atoms by TEM


http://emalwww.engin.umich.edu/education_materials/microscopy.html
A Question from Last Year Final Exam
Recommend an instrumental method that will provide
information about the chemical composition and crystal
symmetry of precipitates (small black dots of ~0.1m wide) in a
polycrystalline sample with micrometer-sized grains as shown
below. State your reasons. [10 marks]

Precipitates
Limits of OM, SEM, SPM and XRD
BT
NN
BT
NN
EDS
G.B.
G.B.

BT-BaTiO
3
NN-NaNbO
3

G.B.-Grain boundary
M.G.J.-multiple grain
junction
Lateral resolution: ~m
Details of microstructure:
e.g., domain structure,
chemical inhomogeneity
phase distribution, grain
boundaries, interfaces,
precipitates, dislocations,
etc.
NN/BT
M.G.J.
0.2m
core
shell
Chemical analysis at a nanometer scale
in a Transmission Electron Microscope
(TEM)
Why TEM?
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 such as chemical
composition (at nm scale), bonding
(distance and angle), electronic
structure, coordination number data from
the sample.
TEM is the most efficient and versatile
technique for the characterization of
materials.
http://www.youtube.com/watch?v=yqLlgIaz1L0 see atoms by TEM
Lecture-6
Transmission Electron Microscopy (TEM)
Scanning Transmission Electron Microscopy (STEM)
What is a TEM?
How it works - gun, lenses, specimen holder
Resolution

What can a TEM do?
Imaging and diffraction
Imaging-diffraction and phase contrast
Diffraction-Selected area electron diffraction (SAED)
and Convergent beam electron diffraction (CBED)
Chemical analysis
EDS, Electron Energy Loss Spectroscopy (EELS)
Energy Filtered Imaging
http://emalwww.engin.umich.edu/education_materials/microscopy.html
http://www.youtube.com/watch?v=6fX1m2rImiM to~2:40 History & applications
Lecture-6
Transmission Electron Microscopy (TEM)
Scanning Transmission Electron Microscopy (STEM)
What is a TEM?
How it works - gun, lenses, specimen stage
Resolution

http://www.youtube.com/watch?v=fxEVsnZT8L8 ~2:20-2:40 fluorescence screen
What is TEM?
TEM is an microscopy technique that functions
similar to a light microscope, which uses a beam of
exited electrons as a light source to provide
mophorlogical, compositional and crystallographic
information of an ultra thin specimen.

The image is formed by the interaction of the
electrons transmitted through the specimen, which
is then magnified and focused on a fluorescence
screen containing a layer of photographic film.
http://www.youtube.com/watch?v=C3uU8c376Aw&list=PLIRAzwu_npNcnPGi2sOk2aaNaS3vzU-N1
Milestones of Science: Ernst Ruska and the Electron Microscope at~5:00-7:15 and ~9:03-9:23
Comparison of OM and TEM
Principal features of an optical microscope and a
transmission electron microscope, drawn to emphasize the
similarities of overall design.
Electron Gun
EDS Detector
Condenser
Lens
Specimen Holder Objective Lens
Magnifying
Lenses
CM200 (200kV)
SAD Aperture
TV Monitor
Viewing Chamber
Camera
Chamber
Cost: > $4,000,000
Column
Binocular
http://www.youtube.com/watch?v=6fX1m2rImiM at~2:40-4:40
Structure and Function of TEM
http://www.youtube.com/watch?v=2wEmsDh_l_A at~0:30
http://www.youtube.com/watch?v=fToTFjwUc5M
Vacuum
The electron microscope is built like a series of
vessels connected by pipes and valves separate
all the vessels from each other.

The vacuum around the specimen is around 10
-7

Torr.
The vacuum in the gun depends on the type of
gun, either around 10
-7
Torr (the tungsten or
LaB
6
gun) or 10
-9
Torr (for the Field Emission
Gun).
The pressure in the projection chamber is usually
only 10
-5
Torr (and often worse). This pressure is
not very good because the projection chamber
holds the negatives used to record images. Even
though we dry the negatives before putting them
in the microscope, they still will give off so many
gases that the vacuum in the projection chamber
never gets very good.


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.
B
http://www.youtube.com/watch?v=C3uU8c376Aw&list=PLIRAzwu_npNcnPGi2sOk2aaNaS3vzU-N1
at~5:50-7:00
How it works? The Lenses in TEM
Running water
Cu coils
Magnetic material
http://www.youtube.com/watch?v=j2A6KeWrqeM&feature=related
at~0:20-0:44
Schematic of the Optics of a TEM
Control
brightness,
convergence
Control contrast
How it works? Image Formation in TEM
A disc of metal
under in over
focus focus focus
http://www.youtube.com/watch?v=6fX1m2rImiM at~3:00-4:45
Why Electrons? Resolution
-wavelength, =[1.5/(V+10
-6
V
2
)]
1/2
nm

V-accelerating voltage, n-refractive index
o-aperture of objective lens, very small in TEM
sino o and so r=0.61/o o~0.1 radians
200kV Electrons
~0.0025nm
n~1 (vacuum)
r~0.02nm (0.2) 1/10
th
size of an atom!
UNREALISTIC! WHY?
In expression for the resolution
(Rayleighs Criterion)
r = 0.61/nsino
Green Light
~400nm
n~1.7 oil immersion
r~150nm (0.15m)
Electrons
0.1 radians ~ 5.5
o
o-beam convergence

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 and
thus 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.
Beam and Specimen Interaction
(EDS)
(EELS)
SAED & CBED
diffraction
BF
DF
HREM
Imaging
Scanning Transmission Electron Microscopy


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 (ADF)
detector.



JEOL 2000FX
Analytical Electron Microscope

STEM detector
or EELS
HAADF
Detector
HAADF-high angle
annular dark-field
Scanning
beam
specimen
BF ADF

ADF

BF
DF
(STEM)
http://en.wikipedia.org/wiki/Scanning_transmission_electron_microscopy
http://www.youtube.com/watch?v=WJUL22UoCLI Scanning transmission electron holography microscope
Specimen Holder
a split polepiece
objective lens
holder
beam


Heating and straining
Twin specimen holder
Double tilt heating
Rotation, tilting, heating, cooling and straining
http://www.youtube.com/watch?v=j2A6KeWrqeM&feature=related at~0:56-1:42
Specimen Holder with Electrical
Feedthroughs
http://www.youtube.com/watch?v=fxEVsnZT8L8 at~3:00-3:34
Specimen Preparation-Destructive
Dispersing crystals or powders on a carbon film on a grid



3mm
Making a semiconductor specimen with a Focused Ion Beam (FIB)


1. a failure is located and a strip of Pt is placed as a protective cover.
2. On one side of the strip a trench is milled out with the FIM.
3. The same is done on the other side of the strip (visible structure).
4. The strip is milled on both sides and then the sides connecting the
strip to the wafer are cut through.
5. The strip is tilted, cut at the bottom and deposited on a TEM grid.


1
2
3
4 5
http://www.youtube.com/watch?v=F0ZNUykXovk Preparing specimen
Specimen Preparation-2
Ion-milling a ceramic


3mm
Ultrasonic cut
grind
Dimple center part
of disk to ~5-10m
ion-mill until a hole
appears in disk

Ar (4-6keV, 1mm A)
Jet-polishing metal



Drill a 3mm
cylinder
Cut into disks
and grind

A disk is mounted in a
jet-polishing machine
and is electropolished
until a small hole is
made.

a thin stream of acid
+ -
Ultramicrotomy-using a (diamond) knife blade
Mainly for sectioning biological materials.
To avoid ion-milling damage ultramicrotome can also be used
to prepare ceramic TEM specimens.
http://www.ims.uconn.edu/~micro/Dimple%20Grinding2.pdf TEM specimen preparation
What can a TEM do? Imaging
BF and DF imaging
HREM
Objective
Aperture
(OA)
BF - Bright Field
DF - Dark Field
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
http://micro.magnet.fsu.edu/primer/virtual/virtualzoo/index.html
Diffraction, Thickness and Mass Contrast
Disk specimen
thickness
thinner
thicker

1
2
3
4
5
6
7
8
G.B.
.
.
.
.
. . .
.
. . .
.
.
.
.
. . ..
.
.
. .
.
.
High
mass
Low
mass
T T
S S
S
Bright Dark
Strong
diffraction
Weak diffraction
8 grains are in different orientations
or different diffraction conditions
thickness
fringes
BF images
BF and 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.

mass-thickness
contrast
BF
DF
DF
DF imaging
only diffracted
beams are
allowed to pass
the aperture to
form images.


Particles in Al-Cu
Alloy.
thin platelets ll e
Vertical, dark
Particles e.
Phase Contrast Imaging
High Resolution Electron
Microscopy (HREM)
Use a large objective
aperture.
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: =2d
hkl
sinu
hkl
=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
http://www.matter.org.uk/diffraction/electron/electron_diffraction.htm
X-ray
crystal
polycrystal
=[1.5/(V+10
-6
V
2
)]
1/2
nm
e-beam is almost
parallel to {hkl}
e-beam
Zone axis
of crystal
sample
http://www.youtube.com/watch?v=fxEVsnZT8L8 at~3:00-3:34
Reciprocal Lattice
A reciprocal lattice is another way of view a crystal
lattice and is used to understand diffraction patterns.
A dimension of 1/d (
-1
) is used in reciprocal lattices.
g reciprocal lattice vector
2-D Reciprocal Lattices
Real space:
Unit cell vectors: a,b
d-spacing direction
a d
10
[10]
b d
01
[01]

Reciprocal space:
Unit cell vectors: a*,b*
magnitude direction
a* 1/d
10

b

b* 1/d
01

a


A reciprocal lattice can
be built using reciprocal
vectors. Both the real
and reciprocal construc-
tions show the same
lattice, using different
but equivalent
descriptions.


[01]
[10] (10)
(01)
Note: each point in the reciprocal
lattice represents a set of planes.
a*
b*
01
02
10
11
12
20
21
22
For every real lattice there is an equivalent reciprocal lattice.
http://www.youtube.com/watch?v=iC15RHX4gpQ
http://www.matter.org.uk/diffraction/geometry/2d_reciprocal_lattices.htm
3-D Reciprocal Lattice
Real space:
Unit cell vectors: a,b,c
magnitude direction
a d
100
[100]
b d
010
[010]
c d
001
[001]


Reciprocal space:
Unit cell vectors: a*,b*
magnitude direction
a* 1/d
100

b and c

b* 1/d
010

a

and c

c* 1/d
001

a

and b



Note: as volume of unit cell in real space increases the
volume of unit cell in reciprocal space decreases, and
vice versa. a*,b* and c* are parallel to corresponding a,b and
c, and this is only true for the unit cells of cubic, tetragonal
and orthorhmbic crystal systems.
Orthorhombic
http://www.matter.org.uk/diffraction/geometry/3d_reciprocal_lattices.htm
http://www.matter.org.uk/diffraction/geometry/reciprocal_lattice_exercises.htm
Lattice Vectors
Real space lattice vector
corresponds to directions
in crystal and it can be
defined as:


r=ua+vb+wc
a,b and c are unit cell vectors,
u,v and w are components of
the direction index [uvw].
A reciprocal lattice vector
can be written as:

g*=ha*+kb*+lc*
a*,b* and c* are reciprocal
unit vectors, and h,k and l
are the Miller indices of the
plane (hkl).
Effect of Spacing of planes in Real Space on
Length of Reciprocal Vector, g
In a crystal of any structure, g
hkl
is normal to the (hkl)
plane and has a length inversely proportional to the
interplanar spacing of the planes.
(111)
-
d
111
-
[111]

-
http://www.matter.org.uk/diffraction/geometry/reciprocal_vector_g.htm
Why are there so many spots?
Ewald Sphere and Diffraction Pattern


SAED pattern XRD pattern
Reciprocal Lattice
k wave vector
lkl = 1/
wavelength of electron
k wave vector
lkl = 1/
wavelength of electron
The Ewald Sphere and Diffraction Pattern
Ewald Sphere Construction
Braggs Law
http://www.matter.org.uk/diffraction/geometry/ewald_sphere_diffraction_patterns.htm
1/
T
D
Reciprocal Lattice
A set of real
lattice planes
XRD
R
R=1/
R
R=1/
SAED
Why there are so
many diffraction
spots in ED?
SAED
A TEM technique to
reduce both the area
and intensity of the
beam contributing to a
diffraction pattern by
the insertion of an
aperture into the
image plane of the
objective lens. This
produces a virtual
diaphragm in the plane
of the specimen.

SAD
aperture
Virtual
aperture
specimen
Objective
lens
Diffraction
pattern
Back focal
plane
Selected Area Electron Diffraction
parallel beam
Focusing SAED Pattern at Fixed Screen
by changing magnetic lens strength
specimen lens
screen
Transmitted beam
Diffracted beam
Spot pattern SAED gives 2-D information
http://www.matter.org.uk/diffraction/electron/electron_diffraction.htm
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
Diffraction Spot Intensity
Spot intensity: I
hkl
o lF
hkl
l
2
F
hkl
- Structure Factor
F
hkl
= E f
j
exp[2ti(hu+kv+lw)]
N
j=1
f
j
atomic scattering factor
f
j
o Z, sinu/
h,k,l are Miller indices and u,v,w fractional coordinates
200
131 (311)?
_
[013]
_
SAED
the table
SAED
d
hkl
= L/r
hkl

50nm
SAED Patterns
TEM
Convergent beam electron diffraction (CBED)
Chemical analysis
EDS, Electron Energy Loss Spectroscopy (EELS)
Energy Filtered Imaging

Secondary Ion Mass Spectroscopy (SIMS)
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