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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